The preparation of synthetic fibres suitable for use in paper production

The invention relates to a process for producing synthetic fibers for use in papermaking of such size that they are directly suitable for making paper without prior cutting or comminution, wherein a solution of a polyolefin in a suitable solvent, optionally including surface active agents, is pigments and fillers, is ejected at a temperature higher than the boiling point of the solvent under normal conditions and under autogenous or more than autogenous pressure through a nozzle in a zone of lower pressure, and the resulting fiber-like elements are collected.

The generic term synthetic paper usually includes all fibrous or non-fibrous carriers that replace the traditional paper in terms of the ability to withstand writing and printing on printing, although they often exhibit very different properties from traditional paper.

As non-fibrous natural paper replacements, for practical use, films of polymeric material have spread, which are usually mono- or biorientated, and their surfaces are obtained by application of a coating material, by chemical-physical treatments or by the use of opacifiers, extenders, etc. were modified.

As a substitute for traditional paper, such carriers have disadvantages in use in both printing and engineering papermaking operations; this also applies to the price, and therefore such a carrier remains limited to very specific uses and excluded from mass consumption.

Included in the field of fibrous synthetic papers are all such carriers formed as a whole from synthetic fibers or mixtures of synthetic fibers with natural fiber material, in particular cellulose pulp (cellulose pulp). The interest in using synthetic fibers in this field may therefore be compounded, first, by the need to modify the properties of traditional paper, and second, by the need to find new sources of the fibrous one

Materials are explained due to the growing demand for standard pulps.

The essential fibrous carriers made entirely of synthetic material are so-called spunbond materials; they are obtained directly from thermoplastic polymeric starting materials which, after melting, are converted into continuous or discontinuous filaments by a conventional spinning process. These are then used in a conventional manner to form a type of nonwoven and preferably bonded together by means of glues and adhesives and in some cases by the action of heat and pressure. The spread of the spin-bonding process finds its limits both through the complicated technology used to form the felts or Fleeces and in the subsequent conversion treatments is required, as well as in the properties of the resulting paper, which can be used almost exclusively only for packaging, but not for printing.

In the field of fibrous material carriers, interest has recently been directed to the development of processes for the production of such synthetic fibers or fibrils which at least partially replace the cellulosic fibers in paper pulps, preferably using paper making techniques and equipment can. Due to the different nature of the synthetic fibers, as opposed to cellulosis fibers, the use of fiber pulp blends may require significant changes in the papermaking cycle. Ideal would be the availability of fibers which, when added to standard paper pulps, could be treated in the same way as normal fibers. Attempts to produce fibers of synthetic materials having these properties have already been made; for example, in U.S. Pat. Nos. 2,999,788 and no. No. 2,988,782 Process for the production of fibrous particles of very small thickness and 10 to 100 μ lengths, commonly called fibrils (or fibrids), characterized in that a synthetic polymer solution is gradually added with vigorous stirring to a precipitating agent for the polymer Adds polymer. However, this method is limited to the use of condensation polymers; In addition, due to their high cost, the microfibers thus produced, despite their interesting properties, have no practical application.

In the French Pat. No. 2,037,342 paper types are described, which are made of polypropylene fibers in admixture with cellulosisehen fibers. However, the polypropylene fibers are made by spinning and then cutting the granulated polymer; this is a costly process that makes the production of paper from such fibers uneconomical.

Recently, the production of fibrils from olefin polymers has been proposed directly during the polymerization of the monomers (reactor fiber), wherein the polymerization in the presence of suitable

Solvent and is carried out under high shear with constant stirring. Such a process is described in Italian Patent No. 876479. The fibrils thus obtained, which are between a few tenths of an inch and a few millimeters in length, are particularly suitable for incorporation into different percentages of paper pulp, and their properties permit their treatment in the usual Pa3

No.337526 pier processing devices. However, the latter process has the disadvantage of requiring special reactors specially designed for this process (since the usual reactors for the polymerization of

Olefins are unsuitable for this purpose), which are useful only for this particular production.

Swiss Patent No. 409381 relates to a process for producing a material suitable for papermaking; this method consists in extruding a polymer solution through a nozzle into a zone of lower pressure at a temperature higher than the boiling temperature of the solvent and under autogenous pressure or at a pressure higher than autogenous pressure, whereupon the plexifade thus formed is cut to staple length and then in a liquid suspended stack is ground. In this way, short fibrous particles (fibrils) are obtained which can be used to prepare paper-like products using the same methods and apparatus as used for natural paper.

The object of the invention differs from this patent in that, according to the invention, a steam or gas jet of high speed is allowed to act at an angle on the extruded solution, whereby at the same time the following results are obtained:

1. Single fibers are obtained in a single operation. whereby one need not concern oneself with the continuous structure of interconnected fibers or fibrids, such as cutting and disintegrating).

Second Each fiber is stretched further in the longitudinal direction, which is advantageous for the mechanical properties thereof and accordingly also for the paper produced therefrom. According to the mentioned

According to the Swiss patent specification, any additional longitudinal orientation of each fibrid can only be achieved by stretching the continuous plexifilament before cutting, which requires unprofitable additional work.

German Offenlegungsschrift 2121512 relates to a process for the production of synthetic paper, wherein

1. a dispersion

A) a mixture of a polyolefin and a solvent for this polyolefin and

B) a dispersion medium having a boiling point lower than the melting point of the polyolefin which is insoluble in the solvent (preferably water),

Second this dispersion is injected through a nozzle at least under the spontaneous pressure obtained by heating the dispersion to form a fibrous material, and

Third the fibrous material is collected and compressed.

This German patent application thus relates to the treatment of (aqueous) emulsions. The polyolefin solution in this case is present in the form of droplets, ie it has already been divided into microscopic particles, each of which may give rise to a fiber. However, working with emulsions involves stabilization problems which are particularly troublesome when the process is carried out on an industrial scale. In any case, the product according to this German disclosure of a fiber bundle, which is not intended according to the invention. In fact, the direct use of bundles or other aggregates of fibers in the manufacture of paper makes it difficult to obtain homogeneous products, and causes problems of homogenization when blending fillers and fibers of different materials in admixture therewith. Such difficulties can only be overcome by first cutting or disintegrating the aggregates into individual fibers, which leads to a deterioration in the mechanical properties of the paper, u. due to the lack of longitudinal orientation of each individual fiber (which, in contrast, is present according to the invention by the use of a steam or gas jet).

German Offenlegungsschrift 1951609 relates

a) to a process for the preparation of microfine olefin polymer aggregates, wherein a 5 to 40 wt .-% polyolefin solution at a temperature of at least 100 ° C in a solvent having a boiling temperature not higher than the temperature of the solution, in the presence of at least 0th , 01% of a surfactant, based on the polyolefin, is ejected through a nozzle into the atmosphere, and

b) a process for the production of paper-like layers from the above-mentioned aggregates, wherein

1. these are micronised in an organic solvent capable of swelling or partially dissolving the polyolefin at a temperature of not higher than 60 ° C,

Second the micro-pieces are homogeneously suspended in this solvent,

Third the suspension is shaped into a layer and

4th the solvent is evaporated from the layer.

By using a certain amount of surface-active agents, only an increase in the degree of fiber formation of the polymer is achieved according to this German Offenlegungsschrift. The

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However, the extrusion product is still in the form of a mass of aggregated micro pieces, so that the use of swelling solvents for adequate disintegration into micro pieces by whipping is necessary.

According to German Offenlegungsschrift 227,021, a hot solution of a thermoplastic polymer is passed from a high pressure zone into a low pressure zone, u. tw. under such conditions of solution concentration, solution temperature and pressure in the low pressure zone that only a portion of the solvent is evaporated to form a gel of precipitated polymer and residual solvent, which gel is then passed through a Dutchman to disentangle the fibers therein.

This German Offenlegungsschrift does not mention the effect of a jet of liquid or vapor or gas on the polymer solution.

The franz. U.S. Patent No. 2,141,139 relates to a process for making fibrous material which can be used for papermaking wherein water disperses into a molten olefin polymer under high pressure conditions and then the molten polymer, together with a countercurrent of further water, through a nozzle into a lower pressure zone is extruded.

According to one embodiment, the additional water is introduced along the inner wall of the extrusion die.

The product consists of a mass of interconnected thin fibers which are transferred by milling into individual short fibers suitable for papermaking.

According to this franz. Patent, the additional water is introduced within the extrusion die, ie it hits the molten polymer in front of the discharge opening. Accordingly, although the water is first supplied at an angle with respect to the direction of polymer extrusion, it actually flows therewith along the length of the nozzle (ie, from the water inlet point to the discharge port), with no

Angle, with the Polymerriehtung itself is formed.

The aim of the invention is thus the creation of fibers substantially from olefin polymers obtained by conventional polymerization processes, the fibers having a similar shape and dimensions as the cellulosic fibers used for papermaking.

The inventive method is characterized in that the ejected, at least partially expanded solution in this zone of lower pressure, a steam or gas jet at high speed at a temperature below the temperature of the solution and at an angle between 30 and

90 ° to the ejection direction of the solution is allowed to act.

The steam or gas jet is hereinafter referred to as flowable mass in the description.

The method is applicable to (kristaUine) polyolefins prepared from monomers of the formula r-ch = ch₂ in which

R is an alkyl or aryl group or a hydrogen atom, such as polyethylene, polypropylene, polypentene-1, poly-4-methylpentene-l, polystyrene, and the copolymers of mixtures of such monomers or mixtures of such polymers.

Linear polyethylene of the type which has been obtained by means of Ziegler catalysts deposited on a support have proven to be particularly suitable (cf., for example, Italian patents 40 No. 853 733, No. 853 734 and No. 860130), and polypropylene having a high content isotactic index, obtained by means of Ziegler-Natta catalysts (cf., for example, Italian Pat. 526101) and mixtures of these polyolefins with minor amounts of other polymers such as polyvinyl chloride, polyvinyl acetate, polymethyl methacrylate, polyamides, polyoxymethylene, cellulose acetate, etc.

For the production of high cohesive fibers, it is possible to use polyolefins of the general formula given above, which have been modified by introduction of polar groups.

It is convenient, but not essential, for the solvent used in the solution to have a boiling temperature below the melting temperature of the polymer. Usually, all liquid or under normal conditions gaseous solvents are useful, which provide homogeneous solutions of the polymer under the working conditions.

Suitable solvents are, for example, aliphatic hydrocarbons, such as n- or isobutane, pentane, hexane, heptane, octane; cycloaliphatic hydrocarbons, such as cyclohexane; aromatic hydrocarbons such as benzene, toluene, xylene; chlorinated hydrocarbons, such as chlorobenzene, trichlorethylene, tetrachlorethylene, trichlorofluoromethane, etc.

In the process one can use a wide range of concentrations of the polymer solutions, which depend on the molecular weight and the type of polymer used. Usually one uses solutions with 1 to 700 g / 1 polymer; for best results solutions with 50 to 400 g / l Polymeri5

No.337526 sat preferred.

The best working conditions for the production of fibers of homogeneous dimensions and without special

Treatment in paper pulps of usable fibers consists in the use of polymeric solutions which, under the working conditions, have absolute viscosities similar to those of one at 130 ° C

Solution of 100 g of polyethylene in 11 hexane with a [η] in tetralin at 135 ° C of 0.9.

To the polyolefin solution may be added pigments, fillers, stabilizers, antistatic agents and / or other substances for modifying the surface properties of the fibers. It has proved to be particularly expedient to add surface-active agents to the solution which make it possible to obtain fibers readily dispersible in water. The dispersibility of the fibers in water is a very important factor in their use for the production of paper by conventional methods. The lack of hydrophilic properties of the polyolefin fibers renders such dispersion difficult to handle in the aqueous substance preparation step. In contrast, the addition of surface-active compounds to the water before or during the dispersion of the fibers has certain disadvantages, such as foaming; the latter causes a layer formation of the synthetic material, if for example with mixtures of

Polyolefin fibers and cellulose fibers work. By adding a wetting agent directly to the polyolefin solution before extruding these difficulties are overcome.

The surfactants used must be uniformly soluble in the solvent and polyolefin. One can use anionic, cationic, nonionic or amphoteric agents. Suitable anionic surfactants for this purpose are, for example, the soaps of fatty acids, the soaps of naphthenic acids, the salts of sulfuric acid esters, the alkali metal sulfonates, the alkyl esters of phosphorous acid or Phosphoric acid, the salts of alkylphosphoric acid esters, the sodium salts of sulfuric acid esters of alkylphenol-polyethylene glycols. Useful cationic surfactants include e.g. the quaternary ammonium alkyl compounds, the aliphatic amines, the basic salts of alkylpyridinium or alkylpicolinium and the alkylbenzimidazole derivatives. Suitable amphoteric surfactants are compounds of the betaine and solvobetaine type as well as the amphoteric compounds from the group of sulfuric acid and phosphoric acid esters. Nonionic surfactants include: the polyoxyethylene alkyl esters and ethers, the polyoxyethylene alkylaryl esters, the higher alcohol fatty acid esters, the polyoxyethylene alkylamines, the alkanolamides of fatty acids, the polyoxyethylene polyoxypropylene block copolymers, and the polyoxyethylene alkyl thioethers.

It is necessary that the surfactant used remain incorporated in the fiber or at least largely adhered to the fiber surface. For this purpose, the surfactant should have a higher boiling temperature than that of the solution at the time of extrusion. Thus, by proper choice of the surfactant, it is possible to substantially improve the fiber property to form a suspension in the aqueous medium. At the same time, the antistatic properties of the fibers and the surface properties of the films produced therefrom are improved.

Conveniently, an amount of surfactant greater than 0.05 weight percent, based on the olefin polymer, is added to the polyolefin solution. For optimum results, amounts of surfactant above 0.1% by weight of the polyolefin are preferred.

For economic reasons, the maximum amount of surface active agent added to the polymer solution for optimum results can be kept below 5% by weight of the polymer, since larger amounts do not provide appreciable benefits in terms of dispersibility of the fibers in water.

The surfactant used in the present invention may be dissolved or dispersed in an organic solvent before, after, or during the dissolution of the polyolefin in this solvent.

The rate at which the solution of polyolefin material is expelled through the nozzle may vary from 1000 to 200,000 m / h, preferably between 1,500 to 50,000 m / h. The solution to be ejected should have a temperature which is at least 40, but preferably 60 ° C above the boiling temperature of the solvent under normal conditions. To obtain fibers of highly convenient morphology, the flowable mass should suitably impact the polyolefin solution at high speed after it has at least partially expanded in the environment of lower pressure in which it is ejected. This is usually accomplished by mounting the nozzle for the high velocity flowable mass in such a manner that the flowable mass meets the solution when the latter is within a certain distance from its exit nozzle. This distance depends essentially on the exit velocity of the solution and, under the preferred working conditions of the invention, is between 1.5 to 15 mm.

Any liquid, gaseous or vaporized substance which is inert and which under working conditions has no dissolving effect on the polyolefin used and is preferably immiscible with the solvent of the polymeric solution can be used as the impinging flowable mass. As a medium for the

Steam at high speed has been found to be particularly suitable for steam because it offers the added benefit of humidifying the fibers compared to other useful flowable substances; DA6

No.337526, they are easier to collect and eliminate sticking due to static electricity, which allows the fibers to charge easily. Optionally, however, one may also use a gas such as nitrogen, oxygen, carbon dioxide, combustion gas or finely divided water drops and mixtures thereof.

The velocity of the impinging flowable mass has been found to be important in terms of the viscosity of the solution used or in relation to the rate at which this solution is expelled through the nozzle. Optimal working conditions are achieved, as was found, at an impact velocity of the flowable mass between 200 and 600 m / sec. Within this range of working conditions, some flowable masses are found to be optimal for obtaining fibers of such a length and ratio between length and diameter that they are useful as a substitute for cellulose fibers in papermaking.

The working conditions also include the values ​​of the angle formed by the direction of the flowable jet and the direction of the solution; these values ​​are between 50 and 55 ° for nitrogen, between 80 and 85 ° for carbon dioxide and water vapor and between 40 and 60 ° for oxygen. According to a preferred embodiment of the invention, the high velocity vapor or gas jet is guided in the nozzle so as to move geometrically coaxially with the nozzle ejecting the polyolefin solution. Using these preferred methods results in very uniformly shaped fibers, which is among other things extremely favorable for the production of paper with good surface properties.

The drawings illustrate the method according to the invention and the nature of the Fa20 fibers thus obtained. Fig.l is a diagram of the plant for carrying out the process according to the invention in a continuous manner. Fig. 2 shows in detail a system of the nozzles arranged at right angles and used for the impinging flowable mass or solution in the apparatus of Fig. 1, respectively. Fig. 3 is a longitudinal section of an apparatus with nozzles for carrying out a preferred embodiment of the method according to the invention; In this case, the impinging flowable mass is used in the form of a mass geometrically coaxial with the ejection nozzle of the polyolefin solution. Fig. 4 is a 54X magnification of fiber types obtained in accordance with the present invention.

In Fig. 1, the polymer suspension is introduced in the organic solvent through line -1- in the provided with a stirrer -3- autoclave -2-. The impinging flowable mass introduced through line -4- is expelled through nozzle -5- and impinges upon the polymer solution which is expelled through nozzle-6 from autoclave-2. The nozzle -5-can be in different position to the nozzle -6-, so that the flowable mass hits the solution at different angles and at different distances from nozzle -6-. Then the fibers thus formed are collected in a collecting vessel.

The device shown in Fig. 3 has two coextensive coaxial conduits -1 and 2- which are intended to introduce the polymer solution and the impinging flowable mass and terminate in the nozzles -3 and 4-. A chamber -5- in the form of a truncated cone forms a zone of lower pressure with respect to the pressure in the nozzle -3- during working; in this chamber ~ 5 the expansion of the solution takes place. The end zones -6 and 7- of the walls of the two conduits are such that the axis of the gap 8 defined by these walls, with the axis of the nozzle -3- in the direction of ejection, forms an angle a preferably between about 30 and 90 ° , When working with such a device, the solution is surrounded and struck at any point at an angle from the flowable mass ejected through nozzle -4-.

By suitably changing the zones -6 and 7- and, if possible, the nozzle -4-, it is of course also possible to adjust the temperature conditions according to the invention by feeding the line 45 with the high-speed flowable mass and the line -2- with the polymer solution fed. In this case, the flowable mass remains surrounded by the solution and impinges on it from the inside at an angle.

Of the possible devices for achieving the preferred process conditions, the one with the coaxial nozzle has proved to be particularly useful because it is very compact and these conditions can be realized in two ways.

The following examples illustrate the invention without limiting it.

Example 1 Into a 50-liter stainless steel autoclave provided with a jacket and paddle stirrer at a maximum revolution speed of 300 rpm, there were placed 30 liters of technical hexane and 2 kg of polyethylene obtained by means of depositing on a support Ziegler catalyst and 55 modified with propylene introduced; the polyethylene had the following properties; Melt index = 0.021; [η] in tetralin hot 135 ° C = 3.0; Density = 0.950; Number of methyl groups per 100 carbon atoms = 0.83;

Melting temperature (by DSC) = 132 ° C.

Then, the autoclave was heated by circulating water vapor in the jacket until a solution was obtained under the following conditions: pressure = 2.2 kg / cm²; Temperature of the solution = 108 ° C.

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Then the solution was passed through an annular nozzle of 2 mm diameter below the above

Temperature and pressure conditions at a flow rate of 501 / h from the autoclave into the atmosphere and ejected at a distance of 2.5 mm from the nozzle by a water vapor jet with an impact velocity of 470 m / sec hit from a nozzle of 4 mm Diameter was ejected at right angles to the nozzle of the solution.

This gave a mixture of water vapor, fibers and organic solvent, which was passed via a line to a filter on which the wet fibers were separated from the mixture. The fiber content in the organic solvent was below 0.3% by weight.

In a visual analysis under a microscope, the product consisted of about 50% of individual fibers 10, 1 to 10mm in length and 5 to 50μ in diameter, and about 50% of single, flat, self-rolled fibers of 1 to 10mm in length , a width of 100 to 500 μ and a thickness of 5 to 50μ. By specific surface measurement by means of a PERKIN ELMER Sorptometer by absorption of N₂ showed that the product as a whole a surface area below 1 m²/ g had.

150 g of the fibers thus obtained were mixed with 350 g of sulfite-conifer cellulose in 25 l of water, and this mixture was refined in a Lorentzen-Wettres-Holländer and at intervals repeated samples of the pulp were withdrawn, with which, after appropriate dilution after conventional methods and using laboratory sheet form devices made films. The properties of the films thus obtained are shown in Table 1.

Example 2: The autoclave described in Example 1 was charged with 30 l technical hexane and 3 kg Po20 lyäthylen the manner indicated in Example 1. By introducing steam into the heating mantle, a solution was obtained in the autoclave under the following working conditions:

Pressure 2.4 kg / cm²

Temperature 104 ° C.

By means of the nozzle device described in Example 1, the solution was then discharged from the autoclave at a flow rate of 45 l / h into the surrounding atmosphere and at a distance of

2.5 mm from the exit nozzle hit by a steam jet of an impact velocity of 470 m / sec.

The product collected on the filter consisted of about 50% individual fibers of 1 to 20 mm in length and 5 to 50μ in diameter and about 50% of single, flat self-rolled fibers of 1 length to 20 mm, a width of 100 to 500 μ and a thickness of 5 to μ with a surface area of ​​about 1 m²/G.

150 g of this fibrous product were then mixed with 350 g sulfite-conifer cellulose in 25 l of water and this mixture was used according to the process described in Example 1 for the production of films. The properties of these films are listed in Table 1.

Example 3: The autoclave described in Example 1 was charged with a solution of 30 l of technical hexane and 2.5 kg of polyethylene of the type described in Example 1. After heating the solution in the autoclave, the following conditions were set:

Pressure 2.2 kg / cm²

Temperature 103 ° C.

Then, the solution was ejected from the autoclave at a flow rate of 60 l / h by means of the nozzle device described in Example 1 and struck at a distance of 2 mm from the discharge nozzle by a water vapor jet having an impact velocity of 470 m / sec.

The collected product consisted of about 80% individual fibers of 1 to 5 mm in length and 5 to 20 μ in diameter and about 20% of individual flat self-rolled fibers of 1 to 5 mm in length, 50 in width to 100 μ and a thickness of 5 to 20 μ, the surface area being about 1 m²/ g was.

Then, a series of blends consisting of 120 g of the above product and 280 g of sulphite conifer, birch, hardwood sulphate and kraft cellulose in 201 water were prepared. These blends were used to make films according to the methods described in Example 1. The

Properties of the films thus obtained are shown in Table 2.

Example 4 In the autoclave described in Example 1, which was maintained at the following conditions:

Pressure 14.5 kg / cm²

Temperature 134 ° C,

No. 337526, a solution of 30 liters of trifluoromethane and 3 kg of polyethylene obtained by supported zeolite catalysts was prepared; the polyethylene had the following properties: melt index = 18.5; [η] in tetralin at 135 ° C = 0.9; Density = 0.952; Number of methyl groups per 100 carbon atoms = 0.65; Melting temperature (by DSC) = 130 ° C.

This solution was ejected from the autoclave into the surrounding atmosphere by means of the nozzle device described in Example 1 at a flow rate of 90 l / h and struck at a distance of 3 mm from the outlet nozzle by a steam jet at an impact velocity of 470 m / sec.

Thus, a fibrous product was obtained which consisted of about 80% single fibers of 1 10 to 3 mm in length and 5 to 15μ in diameter and about 20% of individual flat self-rolled fibers of intermediate length 1 to 5 mm, a width between 50 to 100 μ and a thickness between 5 to 15 μ, the surface area of ​​the product being 2 m²/ g was.

From a mixture of 150 g of the product thus obtained with 350 g of sulphite-conifer cellulose in 25 l of water, as in Example 1, films were prepared whose properties are listed in Table 1.

Example 5: In the autoclave described in Example 1 under the following conditions:

Pressure 5.1 kg / cm²

Temperature 137 ° C, a solution of 30 1 technical hexane and 3 kg of polyethylene, obtained by means of coated on a support Ziegler catalysts; the polyethylene had the following properties: melt index = 18;

[η] in tetralin at 135 ° C = 0.9; Density = 0.962; Number of methyl groups per 100 carbon atoms = 0.21 and melting temperature (with DSC) = 131.5 ° C. However, with the nozzle device described in Example 1, the nozzles of which were arranged to form an angle of 85 °, the solution was discharged from the autoclave at a flow rate of 95 l / h into the surrounding atmosphere and at a distance of 3 mm from the outlet nozzle at room temperature of one CO₂ Electricity hit with an impact speed of 220 m / sec.

The product thus obtained consisted of about 90% of individual fibers of length between 2 to 4 mm and a diameter of about 5 μ and about 10% of flat fibers with a length of 2 to 4 mm, a width of 50 μ and a Thickness of about 5 μ, the surface area 3.5 m²/ g was.

Example 6: In the autoclave described in Example 1 under the following conditions:

Pressure 4.8 kg / cm²

Temperature of 136 ° C, a solution of synthetic hexane and 3.5 kg of polyethylene, obtained by means of carrier-deposited Ziegler catalysts; the polyethylene had the following intrinsic, melting index = 49; [η] in tetralin at 136 ° C = 0.9; Density = 0.952; Number of methyl groups per 100 carbon atoms = 0.28 and melting temperature (by DSC) - 131 ° C.

The nozzle device described in Example 1 was used, but the angle of the two nozzles was 85 °. The solution was ejected into the surrounding atmosphere and struck at a distance of 2.5 mm from the exit nozzle by a steam jet. The fibers were formed under the following conditions:

Flow rate of the ejected solution 55 1 / h

Impact velocity of water vapor 320 m / sec.

The thus obtained feces-like product consisted of about 70% of individual fibers with a length of 2 to 5 mm and a diameter of 1 to 5 μ and about 30% of individual flat fibers with a length of 2 to 5 mm, a width of 50 to 100μ and a thickness of 1 to 5μ, the surface area being about 3m²/ g was.

From a mixture of 150 g of the product thus obtained and 350 g of cellulose (60% birch, 20% hardwood sulfate and 20% strength) films were prepared according to Example 1, the properties of which are listed in Table 3.

Example 7: In the autoclave described in Example 1, maintaining the following conditions:

Pressure 5.9 kg / om²

Temperature 160 ° C,

No.337526 a solution of 30 1 technical hexane and 4.8 kg of polyethylene produced from Example 6. The process was carried out in the nozzle device described in Example 1, but the nozzles were mounted so that they formed an angle of 80 °. The solution was ejected into the surrounding atmosphere and hit by a steam jet at a distance of 3.5 mm from the nozzle.

The working conditions for producing the fibers were:

Flow rate of the ejected solution 125 1 / h

Impact velocity of the water vapor jet 320 m / sec

The product thus obtained consisted of about 80% fibers of 2 to 5 mm in length and 1 to 5μ in diameter and about 20% of flat fibers of 2 to 5 mm in length, 50 to 50 in length 100 μ and a thickness of 1 to 5 μ, the surface area being 5 m²/ g was.

After the procedure described in Example 1 were prepared from a mixture of 150 g of the thus obtained

Product and 350 g of cellulose (60% birch, 20% hardwood sulphate and 20% kraft) films whose properties are listed in Table 3.

Example 8: In the autoclave described in Example 1, maintaining the following conditions:

Pressure 5.9 kg / cm²

Temperature 155 ° C, a solution of 30 1 technical hexane and 1.8 kg of polyethylene produced by Example 6. The nozzle device described in Example 1 was used, but the nozzles were arranged to form an angle of 50 °. The solution was ejected into the surrounding atmosphere and at a distance of

3.5 mm from the outlet nozzle at room temperature under the following conditions hit by an oxygen jet:

Flow rate of the solution 120 1 / h

Impact velocity of the oxygen jet 470 m / sec.

The product consisted almost entirely of individual fibers about 4 to 5 mm in length and about 5 μ in diameter, the surface area being 11 μm²/ g was. The content of the organic solvent fibers was less than 0.3% by weight.

Example 9: In the autoclave described in Example 1, maintaining the following conditions:

Pressure 5.5 kg / cm²

Temperature 145 ° C, a solution of 351 technical hexane and 3 kg of polyethylene, obtained by means of supported Ziegler catalysts prepared; the polyethylene had the following properties: melt index = 13, ö, [tj] in tetralin at 135 ° C = 1; Density = 0.9543; Number of methyl groups per 100 carbon atoms = 0.6;

Melting temperature (by DSC) = 130 ° C.

In the nozzle apparatus used in Example 1, the nozzles were arranged at right angles. The solution was discharged into the surrounding atmosphere and struck at a distance of 3 mm from the exhaust nozzle by an oxygen jet at room temperature under the following conditions:

Flow rate of the ejected solution 100 1 / h 40 Impact speed of the oxygen jet 470 m / sec.

The product consisted of about 80% fibers of 1 to 3 mm in length with a diameter of 5 to 20 μ and about 20% of flat fibers of 1 to 3 mm in length, 50 to 100 μ in width and a thickness of 5 to 20 μ, where the surface area of ​​the product is 4 m²/ g was.

According to Example 1, films were prepared from a mixture of 150 g of the product thus obtained and 350 g of sulfitic acid niferen cellulose whose properties are listed in Table 4.

Example 10: In the autoclave described in Example 1, maintaining the following conditions:

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Pressure 5.4 kg / cm²

Temperature 142 ° C, a solution of 30 1 technical grade hexane, 2.4 kg polyethylene of Example 9, and 0.6 kg of an ethylene / ethyl acrylate copolymer. The nozzle device described in Example 1 was used, with the nozzles arranged at right angles. The solution was discharged into the surrounding atmosphere and struck at a distance of 3 mm from the discharge nozzle by a steam jet under the following conditions:

Flow rate of the ejected solution 100 1 / h

Impact velocity of the water vapor jet 470 m / sec.

The product consists of about 80% fibers of 1 to 3 mm in length and 5 to 20 μ in diameter and about 20% flat fibers of 1 to 3 mm in length, 50 to 100 μ in width and 5 to 20 μ in thickness, the surface area of ​​the product being 4 m²/ g and the density of the fibers were 0.9450.

According to Example 1, films were prepared from a mixture of 150 g of the product thus obtained and 350 g of sulfite-conifer cellulose, the properties of which are listed in Table 4,

Example 11: The autoclave described in Example 1 was maintained while maintaining the following conditions:

Pressure 5.3 kg / cm²

Temperature 139 ° C, a solution of 35 1 technical hexane, 2.55 kg of polyethylene of Example 9 and 0.45 kg of polyvinyl chloride (K value = 45) produced. The device of Example 1 with right-angled nozzles was used. The solution was ejected into the surrounding atmosphere and struck at a distance of 4 mm from the exit nozzle by a steam jet. The conditions of fiber formation were as follows:

Flow rate of the ejected solution 110 1 / h

Impact velocity of the water vapor jet 470 m / sec.

The product consisted of about 85% fibers of 1 to 3 mm in length and 5 to 15 μ in diameter and about 15% of flat fibers 1 to 3 mm in length, 50 to 100 μ in width and 5 to 15 μ in thickness, which was surface area 5.5 m²/ g, the density of the fibers 0.9905, and the content of organic solvent in the fibers was less than 0.3% by weight.

According to Example 1, films were prepared from a mixture of 150 g of the product thus obtained and 350 g of sulfite-conifer cellulose, whose properties are listed in Table 4. Foil production was facilitated by the greater density of fibrils.

Example 12: The autoclave described in Example 1 was maintained while maintaining the following conditions:

Pressure 3.4 kg / cm²

Temperature 124 ° C, a solution of 351 technical hexane and 3 kg polyethylene of Example 9, to which 3% by weight of TiO₂, based on the polyethylene, were added. However, in the nozzle device used in Example 1, the nozzles were arranged to form an angle of 50 °. The solution was blown into the surrounding atmosphere at a distance of 5 mm from the exit nozzle through a stream of nitrogen under the following conditions at room temperature:

Flow rate of the ejected solution 95 1 / h Impact velocity of the nitrogen jet 470 m / sec.

The product consisted of about 80% of fibers of 2 to 4 mm in length and 1 to 5 μ in diameter and to

20% flat fibers 2 to 4 mm long, 50 to 100 μ wide and 1 to 5 μ thick. The surface area of ​​the product was 3.5 m²/ g and the density of the fibers 0.98.

According to Example 1, films were prepared from a mixture of 150 g of the product thus obtained and 350 g of sulfite-conifer cellulose, the properties of which are listed in Table 4.

Nr.337526

Example 13: In the autoclave described in Example 1, maintaining the following conditions:

Pressure 5.5 kg / cm²

Temperature 163 ° C, a solution of 30 1 technical hexane, 2.1 kg polypropylene with high isotactic index (obtained by Ziegler catalysts) produced. The polypropylene had the following properties: melt index = 6.7; Density = 0.9085; Melting temperature (by DSC) = 165 ° C.

In the nozzle device used in Example 1, the nozzles were arranged to form an angle of 70 °. The solution was discharged into the surrounding atmosphere and struck at a distance of 7 mm from the discharge nozzle by a steam jet under the following conditions:

Splitting speed of the ejected solution 401 / h

Impact velocity of the water vapor jet 470 m / sec.

The product consisted almost entirely of fibers of 1 to 5 mm in length and 5 to 20 μ in diameter. The surface area of ​​the product was 7 m^z/G.

According to Example 1, films were prepared from a mixture of 150 g of the product thus obtained and 350 g of cellulose (60% birch, 20% hardwood sulphate and 20% strength) whose properties are listed in Table 5.

Example 14: In the autoclave described in Example 1, maintaining the following conditions:

Pressure 4.5 kg / cm²

Temperature 155 ° C, a solution of 30 1 technical hexane and 3 kg low density polyethylene produced with the following properties: melt index = 4.6; Density = 0.9235; Melting temperature (by DSC) = 118 ° C.

In the nozzle device used in Example 1, the nozzles were arranged to form an angle of 60 °. The solution was discharged into the surrounding atmosphere and struck at a distance of 7 mm from the exit nozzle through a nitrogen jet at room temperature under the following conditions:

Flow rate of the ejected solution 30 1 / h Impact velocity of the nitrogen jet 470 m / sec.

The product thus obtained consisted essentially of fibers of 1 to 3 mm in length and 5 to 15 μ Durchm diameter, the surface area 13 m²/ g and the content of organic fiber fibers was less than 0.3% by weight.

According to Example 1, films were prepared from a mixture of 150 g of the product thus obtained and 350 g of cellulose (60% birch, 20% hardwood sulfate and 20% strength) whose properties are listed in Table 5.

Example 15: The autoclave described in Example 1 was maintained while maintaining the following conditions:

Pressure 3.0 kg / cm²

Temperature l40 ° C, a solution of 30 1 technical hexane and 2.1 kg of polyethylene (obtained by Ziegler catalysts without 40 carriers) prepared with the following properties: melt index = 0.47; Density = 0.9603; Number of methyl groups per 100 carbon atoms <0.1; Melting temperature = 134 ° C.

In the nozzle apparatus described in Example 1, the nozzles formed an angle of 70 °. The solution was discharged into the surrounding atmosphere and at a distance of 5 mm from the exit nozzle by CO₂Beam at room temperature under the following conditions:

Flow rate of ejected solution .951 / h

Impact velocity of the carbon dioxide jet 320 m / sec.

The product thus obtained consisted of about 70% of fibers of 1 to 10 mm in length and 5 to 20 μ Durch 12

No. 337526 and about 30% of flat fibers of 1 to 10 mm in length, 50 to 100 μ in width and 5 to 20 μ in thickness.

The surface area was about 2 m²/G.

According to Example 1, films were prepared from a mixture of 150 g of the product thus obtained and 350 g of cellulose (60% birch, 20% hardwood sulfate and 20% strength) whose properties are listed in Table 5.

Example 16: In the autoclave described in Example 1, a solution of 30 1 technical hexane and 3 kg polyethylene of Example 5 was prepared. After heating the solution in the autoclave, the following conditions were encountered:

Pressure 5.6 kg / cm²

Temperature 132 ° C.

In the apparatus used in Example 1, the nozzles were arranged at right angles. The solution was discharged into the atmosphere and struck at a distance of 5 mm from the outlet nozzle under the following conditions by a steam jet:

Flow rate of the solution 90 1 / h

Impact velocity of the water vapor jet 470 m / sec

The product obtained consisted of about 90% of individual fibers of 1 to 3 mm in length and 5 to 15 μ in diameter and about 10% of flat, self-wound fibers of a length of 1 to 3 mm, a width of about 50 μ and a thickness of 5 to 15 μ. The surface area was 2.5 m²/G.

The preparation was repeated 6 times, yielding 15 kg of product.

12 kg of the product were mixed with 27.6 kg of cellulose (60% birch, 20% hardwood sulphate and 20% strength) and

9.5 kg of kaolin mixed in about 1200 1 of water. Then, the mixture was continuously refined in a conical refining apparatus to reach 36 ° SR, whereupon 0.08 kg of an optical bleaching agent, 0.8 kg of glue and 1.2 kg of ketene dimer as a co-agent were added. To this mixture was then added water up to twice the volume of the suspension. The suspension was transferred to the feed vat of a continuous drum machine having a usable width of about 55 cm. In this way, 40 kg of paper were produced, whose properties in Table 6 (Test B) together with the properties of a reference paper only. from 40 kg of cellulose (60% birch, 20% hardwood sulphate and 20% strength) (Test A).

Part of the paper made from the pulp containing the polyethylene fibers was calendered between two rolls maintained at about 140 ° C; the results of this procedure are also listed in Table 6 (Test C).

The following examples show the use of surfactants in the polyolefin solution. Example 17: In a 150-1 autoclave provided with heating mantle and paddle stirrer were 6 kg

Polyethylene introduced with the following properties: melt index = 4.1; Density = 0.9622; CH_G Groups prol00carbon atoms = 0.1; Melting temperature (by DSC) = 133 ° C. Furthermore, 30 g of an ethoxylated stearylamine surfactant and 70 l of technical hexane were added to the autoclave. By heating with oil, the following conditions were set in the autoclave:

Temperature 150 ° C

Total pressure 7 kg / cm

Nitrogen excess 1.6 kg / cm²,

The solution was passed through a tube provided with a steam-heated jacket to a nozzle having a thickness of 2 mm, ejected into the surrounding atmosphere, and struck 2.5 mm from the exit nozzle through a nitrogen jet at room temperature coming from a second nozzle of 4 mm diameter 1mm, which formed with the first nozzle an angle of 50 °.

The working conditions were as follows:

Temperature of the solution at the nozzle Pressure of the solution at the nozzle Nitrogen pressure at the nozzle Flow rate of the solution Impact velocity of the nitrogen

158 ° C

7.2 kg / cm² kg / cm²100 kg / h 320 m / sec.

The resulting product was examined under a microscope. It consisted of 80% fibers from 2 to

No.337526 mm in length and 1 to 5μ in diameter and 30% in flat fibers of 2 to 5 mm in length, 20 to 50μ

Width and 1 to 5 μ thickness. The content of solvent was less than 0.3% by weight. According to measurement with a

Perkin-Elmer Sorptometer, the surface area of ​​the product was 2.9 m²/G.

150 The fibers thus obtained were mixed with 3S0 g of cellulose (60% birch, 20% Kraft and 20% resin wood sulphate in 251 water.) The mixture immediately dispersed.Then the aqueous mixture was refined in a Lorentzen Wettres Dutchman and, after appropriate dilution into commonly used by means of a laboratory sheet-making machine for the production of films whose properties are listed in Table 7.

Example 18: In the autoclave of Example 17, 6 kg of polyethylene having the properties described in Example 17, 30g of nonylphenol ethoxylate surfactant (nonylphenol / ethylene oxide molar ratio = 1: 6) and 70 l of technical hexane were added. After heating with oil, the following conditions were set in the autoclave:

Temperature 155 ° C

Total pressure 8.2 kg / cm²

Nitrogen pressure 1.6 kg / cm?

However, in the apparatus described in Example 17, the nozzles were arranged to form an angle of 60 °. The solution was discharged into the atmosphere as in Example 17 and struck at a distance of 5 mm from the exhaust nozzle by nitrogen flow at room temperature. The working conditions were as follows:

Temperature of the solution at the nozzle 175 ° C

Diameter of the solution ejecting nozzle 2 mm

Flow rate of the solution 108 kg / h

Pressure of the solution at the nozzle 9 kg / cm²

Diameter of nitrogen ejecting nozzle 4 mm

Nitrogen pressure at the nozzle 20 kg / cm²

Impact velocity of nitrogen 370 m / sec.

The product obtained 80% of fibers of 1 to 3 mm in length and 1 to 10 microns in diameter and 20% of flat fibers of 1 to 3 mm in length, 20 to 50 μ width and 1 to 10 μ thickness. The surface area of ​​the product was 2.5 m²/G.

150 The fibers thus obtained were mixed with 350 g of cellulose (60% birch, 20% kraft and 20% hardwood sulphate) in 25 l of water to give immediate, complete dispersion of the fibers in the water. According to Example 1, films were prepared from this aqueous mixture whose properties are listed in Table 7.

Example 19: The autoclave of Example 17 was charged with 6 kg of polyethylene of Example 17, 30 g of a nonylphenol ethoxylate surfactant (1 mole of nonylphenol per 7.5 moles of ethylene oxide) and 70 liters of heptane. After heating with oil, the following conditions were set in the autoclave:

Temperature 165 ° C

Total pressure 7.0 kg / cm²

Nitrogen pressure 2 kg / cm?

In the apparatus used in Example 17, the nozzles formed an angle of 85 °. The polymeric solution was discharged into the atmosphere and struck by a carbon dioxide jet at a distance of 5 mm from the exit nozzle at room temperature. The working conditions were as follows:

Temperature of the solution from the nozzle 172 ° C

Diameter of the solution ejecting nozzle 2 mm

Flow rate of the solution 100 kg / h

Pressure of the solution at the nozzle 9.0 kg / cm²

Diameter of CO₂ ejecting nozzle 4 mm

CO₂ Pressure at the nozzle 19 kg / cm²

Impact velocity of the CO₂ 300 m / sec.

The product consisted almost completely of fibers of 2 to 5 mm in length and 1 to 5 μ in diameter; the

Surface area of ​​the product was 2.5 m²/G.

No. 337526

150 g of the fibers thus obtained were mixed with 350 g of cellulose (60% birch, 20% hardwood sulphate and 20% strength) in 25 l of water and gave an immediate dispersion of the fibers.

According to Example 1, films were produced from this paste whose properties are listed in Table 7.

Example 2 0: The autoclave of Example 17 was charged with 6 kg of polyethylene of Example 17, 30 g of a surfactant of a mixture of ethylene oxide ethoxylated C -C alcohols (molar ratio of atoxylation = 1: 2) and 70 l of technical hexane fed.

By heating with oil, the following conditions were set in the autoclave:

Temperature 172 ° C

Total pressure 12 kg / cm²

Nitrogen pressure 3.5 kg / cm²,

In the apparatus of Example 17, the nozzles were arranged to form an angle of 65 °. The polyethylene solution thus obtained was ejected through the nozzle and struck at a distance of about 3 mm from the exhaust nozzle by nitrogen flow at room temperature. The working conditions were as follows:

Temperature of the solution at the nozzle 190 ° C

Diameter of the solution ejecting nozzle 2 mm

Flow rate of the solution 105 kg / h

Pressure of the solution at the nozzle 12 kg / cm²

Diameter of nitrogen ejecting nozzle 4 mm

Pressure of the nitrogen at the nozzle 21 kg / cm²

Impact velocity of nitrogen 320 m / sec.

The product thus obtained consisted entirely of fibers of 1 to 3 mm in length and 1 to 20 μ in diameter. The surface area of ​​the product was 4.5 m²/G.

150 The fibers thus obtained were mixed with 350 g of cellulose (60% birch, 20% kraft and 20% hardwood sulfate) in 25 l of water to give immediate, complete dispersion. According to Example 1, films were prepared from this composition whose properties are listed in Table 7.

Example 21: The autoclave of Example 17 was charged with 7 kg of polyethylene of Example 17, 3k of a calcined clay containing 95% of its particles of size less than 10μ, 35g of a surfactant 30 of the condensation product of 1 mole of stearic acid with 5.5 moles of ethylene oxide and 80 1 technical hexane charged. By heating, the following conditions were set in the autoclave:

Temperature 148 ° C

Total pressure 7.7 kg / cm²

Nitrogen pressure 2.2 kg / cm²,

In the apparatus used in Example 17, the nozzles were arranged to form an angle of 55 °; the mixture containing the polyethylene in solution was expelled through the nozzle into the atmosphere and struck at a distance of about 4 mm from the exit nozzle by a stream of oxygen at room temperature. The working conditions were as follows:

Temperature of the solution at the nozzle 151 ° C

Diameter of the solution ejecting nozzle 2 mm

Flow rate of the solution 70 kg / h

Pressure of the solution at the nozzle 6 kg / cm²

Diameter of the oxygen ejecting nozzle 4 mm

Oxygen pressure at the nozzle 21 kg / cm²

Impact velocity of oxygen 320 m / sec.

The product thus obtained consisted of 80% fibers of 3 to 5 mm in length and 1 to 5 μ in diameter and 20% of flat fibers of 3 to 5 mm in length, 20 to 50 μ wide and 1 to 5 μ thick. The surface area of ​​the product was 2.5 m²/ g and the density (at 23 ° C) 1.163 g / cm³,

150 g of the fibers thus obtained were mixed with 350 g of cellulose (60% birch, 20% kraft and 20%

Hardwood sulfate) in 25 1 of water and gave an immediate complete dispersion. According to example! were produced with this mass foils whose properties are listed in Table 7.

Nr.337526

Example 22: The autoclave of Example 17 was charged with 7 kg of polyethylene of Example 17, 3 kg of the in

Example 21 described clay, 35 g of a surfactant from the monolaurin ester of sorbitol and 801 technical hexane charged. By heating, the following operating conditions were set in the autoclave:

Temperature 147 ° C

Total pressure 8.7 kg / cm²

Nitrogen pressure 3.5 kg / cm²,

In the apparatus described in Example 17, the nozzles were arranged to form an angle of 70 °. The mixture containing the polyethylene in solution was fed to the nozzle, ejected into the surrounding atmosphere, and struck at a distance of about 4 mm from the exit nozzle by an oxygen stream at room temperature. The working conditions were as follows:

Temperature of the solution at the nozzle Diameter of the nozzle ejecting the solution Flow rate of the solution

Pressure of the solution at the nozzle

Diameter of the oxygen ejecting nozzle Oxygen pressure at the nozzle Impact velocity of the oxygen

165 ° C 2 mm kg / h 8.3 kg / cm^z4 mm kg / cm²320 m / sec.

The product thus obtained consisted of 70% fibers of 1 to 5 mm in length and 1 to 20 μ in diameter and 30% of flat fibers of 1 to 5 mm in length, 20 to 50 μ wide and 1 to 20 μ thick. The surface area of ​​the product was 2.5 m²/ g and the density (at 23OC) 1.166 g / cm³,

A mixture of 150 g of the fibers thus obtained and 350 g of cellulose (60% birch, 20% kraft and 20% hardwood sulfate) was kneaded into 25 l of water to give an immediate complete dispersion. According to Example 1, foils were prepared with this composition characteristics are listed in Table 7.

Example 23: The autoclave described in Example 17 was charged with 7 kg of polyethylene of Example 17, 3 kg of calcined clay of Example 21, 35 g of ethylene oxide ethoxylated C 1 -C 4 -alcohol surfactant (molar ratio of ethoxylation = 1: 5) and 80 1 technical hexane. By heating, the following operating conditions were set in the autoclave:

temperature

total pressure

Stickstoffüberdruek

169 ° C

10.9 kg / cm²2.8 kg / cm²,

The mixture was discharged through a nozzle surrounded by a steam-heated jacket through a nozzle into the surrounding atmosphere and struck at a distance of about 2.5 cm from the outlet nozzle by a saturated steam stream consisting of a second, in the Angle of

85 ° disordered nozzle originated. The working conditions were as follows:

Temperature of the solution at the nozzle 180OC

Diameter of the solution ejecting nozzle 2 mm

Flow rate of the solution 105 kg / h

Pressure of the solution at the nozzle 11.5 kg / cm²

Diameter of steam ejecting nozzle 4 mm

Impact velocity of water vapor 450 m / sec.

The product thus obtained consisted of 90% fibers of 2 to 5 mm in length and 1 to 5 μ in diameter and 10% of flat fibers of 2 to 5 mm in length, 20 to 50 μ wide and 1 to 5 μ thick. The density of the product (at 23 ° C) was 1.168 g / cm^8th,

A mixture of 150 g of the fibers thus obtained and 350 g of cellulose (60% birch, 20% kraft and 20% hardwood sulfate) was kneaded with 25 l of water to give an immediate, complete, homogeneous dispersion. According to Example 1, films were prepared with this composition whose properties are listed in Table 7.

Example 24: Into a 50 liter autoclave equipped with a heating mantle and stirrer were added 1.4 kg of poly (produced with Ziegler catalysts without carrier) having the following properties: melt index = 18; Density = 0.9630; Number of CH 1 groups per 100 carbon atoms = 0.26; melting temperature

- IS

No. 337526 (DSC) = 133 ° C together with 0.6 kg of calcium carbonate with 90% of its particles smaller than 10 μ, 40 g of a surfactant with 4 moles of ethylene oxide ethoxylated alkylphenol and technical hexane. The mixture was then autoclaved by circulating water vapor in the jacket to the following conditions:

Temperature 150 ° C

Pressure 5.4 kg / cm²,

The mixture containing the polyethylene in solution was discharged into the atmosphere through a nozzle of 2 mm diameter and struck at a distance of about 5 mm from the outlet nozzle by a saturated steam jet consisting of a second nozzle of about 90 °

4 mm diameter. The working conditions were as follows:

Flow rate of the solution 15 kg / h

Impact velocity of water vapor 420 m / sec.

The product thus obtained consisted of 70% fibers of 1 to 3 mm in length and 1 to 15 μ in diameter and 30% of flat fibers of 1 to 3 mm in length, 50 to 100 μ in width and 1 to 15 μ in thickness. The content of solvent was less than 0.3% by weight; the density of the product (at 23 ° C) was 1.162 g / cm³,

A mixture of 150 g of the fibers thus obtained and 350 g of cellulose (60% birch, 20% kraft and 20% hardwood sulfate) was kneaded with 25 l of water and resulted in immediate dispersion of the fibrous mixture in the water. According to Example 1, films were produced with the composition thus obtained, the properties of which are listed in Table 7.

Example 25: This example shows the preparation of fibers from a polyethylene solution without surfactants, wherein the dispersibility of the fibers thus obtained in water is compared with that of the fibers prepared in the presence of a surfactant (see previous examples).

The autoclave of Example 24 was charged with 2 kg of polyethylene of Example 24, 0.260 kg of talc and 20 l of technical grade hexane. By heating, the following conditions were set:

Temperature 152 ° C

Pressure 5.2 kg / cm²,

The mixture containing the polyethylene in solution was discharged into the atmosphere through a nozzle of 2 mm diameter and struck at a distance of 1.5 mm from the outlet nozzle by a carbon dioxide jet from a second nozzle of 4 mm diameter at an angle of 90 ° , The working conditions were as follows:

Flow rate of the solution 15 kg / h.

Impact velocity of the CO₂ 450 m / sec.

The product thus obtained consisted of 70% fibers of 1 to 2 mm in length and 1 to 20 μ in diameter 35 and 30% of flat fibers of 1 to 2 mm in length, 50 to 100 μ in width and 1 to 20 μ in thickness. The density of the product (at 23 ° C) was 1.050 g / cm³,

150 g of the fibers thus obtained and 350 g of cellulose (60% birch, 20% kraft and 20% hardwood sulfate) were mixed in 25 l of water. Achieving good dispersion required about 5 minutes. Then the mass was processed as in Example 1 into films whose properties are listed in Table 7,

Example 26: The autoclave of Example 17 was charged with 7 kg of polyethylene of Example 17, 20 g of an ethoxylated stearylamine surfactant, 80 l of technical hexane, and 3 kg of the calcined clay of Example 21. By heating, the following conditions were set in the autoclave:

Temperature 169 ° C

Total pressure 10.9 kg / cm²

Nitrogen pressure 2.8 kg / cm²,

The mixture containing the dissolved polyethylene was passed to a nozzle through a tube surrounded by a steam-heated jacket and ejected into the atmosphere where it was in a

Distance of 2 mm from the outlet nozzle at right angles to a saturated steam jet 17

No.337526 fen was. The working conditions were as follows:

Temperature of the solution at the nozzle 180 ° C

Diameter of the solution ejecting nozzle 2 mm

Flow rate of the solution 150 kg / h

Pressure of the solution at the nozzle 11.5 kg / cm²

Diameter of steam ejecting nozzle 4 mm

Impact velocity of water vapor 450 m / sec.

The product thus obtained consisted of 70% fibers of 1 to 3 mm in length and 1 to 15 μ in diameter and 30% of flat fibers of 1 to 3 mm in length, 20 to 50 μ in width and 1 to 15 μ in thickness. The density of the product (at 23 ° C) was 1.166 g / cm³,

A mixture of 150 g of the fibers thus obtained and 350 g of cellulose (60% birch, 20% strength and 20% hardwood sulfate) was kneaded with 251 water and immediately gave a homogeneous dispersion. According to Example 1, films were produced from this composition whose properties in Table 7.

The following examples illustrate a preferred embodiment of the invention wherein the impinging mass flowable is used geometrically coaxially with the solution ejecting nozzle.

Example 27: In a 2 0-1 stainless steel autoclave provided with a heating mantle and paddle stirrer, 800 g of polyethylene obtained with Ziegler unmodified mono-stage catalysts having the following properties: melt index = 1.6; Density = 0.9525; Number of CH₃Groups per 100 carbon atoms <0.1; Melting temperature (DSC) = 133 ° C; introduced along with 6 g of 20 ethoxylated stearylamine surfactant and 10 l technical hexane. By heating with oil, the following conditions were set in the autoclave:

Temperature 185 ° C

Total pressure 13.0 kg / cm²

Nitrogen pressure 3.5 kg / cm²,

Thus, a solution of polyethylene in hexane was obtained. For the preparation of fibers from this solution, a system of annular coaxial nozzles of the type described in Fig. 3 having the following properties was used:

<td>Diameter of the solution ejecting nozzle -3- diameter of the impinging, flowable</td><td>2</td><td>mm</td>

<td>Mass ejecting nozzle --4--</td><td>4</td><td>mm</td>

<td>Length of the chamber --5--</td><td>10.4</td><td>mm</td>

<td>maximum diameter of chamber -5-</td><td>7.5</td><td>mm</td>

<td>Angle a</td><td>80 °</td><td></td>

As in Fig. 3, the polyethylene solution was passed through a thermally insulated line in line - 1 - while the saturated water vapor was passed in line - 2 -. The working conditions were as follows:

Flow rate of the solution 105 kg / h

Impact velocity of water vapor 210 m / sec.

The product thus obtained consisted of 90% fibers of 4 to 5 mm in length and 1 to 5 μ in diameter 40 and 10% flat fibers of 4 to 5 mm in length, 15 to 20 μ wide and 1 to 5 μ thick. The surface area of ​​the product was about 4 m²/G.

Example 28: In the autoclave of Example 27, 900 g of polyethylene of Example 27 and 10 l of technical hexane were introduced. By heating with oil, the following conditions were set in the autoclave:

Temperature 170 ° C

Total pressure 11.9 kg / cm²

Nitrogen pressure 3.5 kg / cm²,

Fiber production was in the die apparatus of Example 27, but at an angle of 50 °.

Through a tube surrounded by a steam-heated jacket, the polyethylene solution was passed in line-1 while introducing a stream of nitrogen into line -2-. The working 18

No.337526 conditions at the nozzles were as follows:

Temperature of the solution 190 ° C

Flow rate of the solution 95 kg / h

Impact velocity of nitrogen 320 m / sec.

The product thus obtained consisted almost entirely of fibers of 4 to 5 mm in length and 1 to 3 μ thick. The surface area of ​​the product was 3.5 m²/G.

Example 29: In the autoclave of Example 27, 720 g of high syndiotactic index polyethylene obtained with Ziegler catalysts, having the following properties: melt index = 6.5; Density = 0.9083; Melting temperature (DSC) = 160 ° C together with 6 g of a surfactant from the condensation of 1 mole of stearic acid with 5.5 moles of ethylene oxide and 10 1 technical hexane introduced.

By heating, the following conditions were set in the autoclave:

Temperature 171 &lt;&gt; C

Total pressure 8.8 kg / cm²

Nitrogen pressure 3.0 kg / cm²,

Fiber production was in the annular die system of Example 27, but angle a was 45 °.

Through a tube provided with a steam-heated jacket, line -1- was charged with a polypropylene solution, while line -2- was charged with an oxygen stream. The working conditions at the nozzles were as follows:

Temperature of the solution 190 ° C

Flow rate of the solution 90 kg / h

Impact velocity of the oxygen flow 420 m / sec.

The product thus obtained consisted entirely of fibers of 4 to 5 mm in length and 1 to 3 μ in diameter. The surface area was 4 m²/G.

In the following tables, the properties were determined in accordance with the instructions of the Italian Association of Italian Cellulosa e Carta.

Nr.337526

table

<td>porosity</td><td>1550</td><td>920</td><td>450</td><td>320</td><td>2050</td><td>850</td><td>450</td><td>300</td><td>1650</td><td>650</td><td>250</td><td>100</td><td>1000</td><td>1150</td><td>500</td>

<td>Reißfestigk. G</td><td>©</td><td>55</td><td>53</td><td>© ©</td><td>57</td><td>© ©</td><td>© ©</td><td>50</td><td>© c-</td><td>© t</td><td>© O</td><td>©</td><td>38</td><td>c- co</td><td>33</td>

<td>hD • i &lt;M Sat. φ O s S · * V ß</td><td>© rt</td><td>ir- rt</td><td>2.0</td><td>2.1</td><td>i 0.5</td><td>0.8</td><td>0.9</td><td>0.8</td><td>6 * 0</td><td>© rt</td><td>cq rt</td><td>cq rt</td><td>b- ©</td><td>0.8</td><td>0.9</td>

<td>Length at brach xn</td><td>4800</td><td>4500</td><td>5000</td><td>5900</td><td>2000</td><td>2750</td><td>2600 years</td><td>3000</td><td>2700</td><td>© © b- cq</td><td>2500</td><td>2500</td><td>2300</td><td>2900</td><td>2450</td>

<td>Stretching at Brach %</td><td>2.5</td><td>2.5</td><td>© oi</td><td>2.0</td><td>2.0</td><td>2.0</td><td>2.0</td><td>2.5</td><td>2.0</td><td>© rt</td><td>© rt</td><td>1.5</td><td>© cq</td><td>© cq</td><td>© cq</td>

<td>Bruehbelast. kg</td><td>TH</td><td>43</td><td>t</td><td>© ©</td><td>Ι, θ</td><td>© oi</td><td>co cq</td><td>w ci</td><td>© oi</td><td>© cq</td><td>© CO</td><td>3.5</td><td>rt ci</td><td>2.5</td><td>3.0</td>

<td>thickness μ</td><td>130</td><td>130</td><td>120</td><td>120</td><td>150-200</td><td>140-200</td><td>100-180</td><td>© rt</td><td>120-150</td><td>120-140</td><td>120-150</td><td>120-130</td><td>130</td><td>120</td><td>120</td>

<td>2 S &amp; » &lt;»Ts O</td><td>61</td><td>• ςΗ ©</td><td>62</td><td>62</td><td>i⁶²</td><td>61</td><td>59</td><td>b- ©</td><td></td><td>63</td><td>c- ©</td><td>67</td><td>61</td><td>00 ©</td><td>59</td>

<td>Beat SR</td><td>22</td><td>£&gt;</td><td>35.5</td><td>41</td><td>21.5</td><td>27</td><td>34</td><td>1 42</td><td>© cq cq</td><td>M » co</td><td>42</td><td>eq ©</td><td>25.5</td><td>34</td><td>45</td>

<td></td><td>Sulfitkoniferen-</td><td>cellulose</td><td></td><td></td><td colspan="4">example 1</td><td colspan="4">Example 2</td><td colspan="3">Example 4</td>

No.337526®

Ä rt

<td></td><td>th ©</td><td>© ©</td><td>©</td><td></td><td></td>

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Table 3

<td></td><td colspan="4">Cellulose from 60% birch, 20% hardwood sulphate cellulose and 20% strength</td><td colspan="4">Example 6</td><td colspan="3">Example 7</td>

<td>Beat; SR</td><td>26</td><td>38.5</td><td>47.5</td><td>56</td><td>20.5</td><td>26.5</td><td>38</td><td>53</td><td>25</td><td>39</td><td>47.5</td>

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<td>Breaking load; kg</td><td>6.7</td><td>8th</td><td>8th</td><td>8th</td><td>3.7</td><td>3.5</td><td>3, 8</td><td>4.3</td><td>3.5</td><td>4</td><td>4.2</td>

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<td>Length at break; m</td><td>7320</td><td>8600</td><td>8830</td><td>8750</td><td>2850</td><td>3760</td><td>4220</td><td>4700</td><td>3825</td><td>4370</td><td>4590</td>

<td>Tear resistance; G</td><td>41</td><td>44</td><td>40</td><td>38</td><td>40</td><td>39</td><td>39</td><td>38</td><td>40</td><td>41</td><td>40</td>

Nr.337526

table

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Nr.337526

Table 5

<td></td><td colspan="4">Cellulose 60% birch, 20% hardwood sulphate and 20% strength</td><td>example 13</td><td>example 14</td><td>example 15</td>

<td>Beat SR</td><td>26</td><td>38.5</td><td>47.5</td><td>56</td><td>37.6</td><td>37.7</td><td>37.2</td>

<td>Mass; g / m^z</td><td>61</td><td>62</td><td>60</td><td>61</td><td>60</td><td>52</td><td>60</td>

<td>Breaking load; kg</td><td>6.7</td><td>8th</td><td>8th</td><td>8th</td><td>4.1</td><td>4.1</td><td>4.7</td>

<td>Stretching at Fracture; %</td><td>2.5</td><td>2.5</td><td>2.5</td><td>2.5</td><td>2.9</td><td>2.8</td><td>2.8</td>

<td>Length at Fracture; m</td><td>7320</td><td>8600</td><td>8830</td><td>8750</td><td>4670</td><td>5400</td><td>5410</td>

<td>Tear resistance; G</td><td>41</td><td>44</td><td>40</td><td>38</td><td>38</td><td>20</td><td>50</td>

Table 6

<td></td><td>A</td><td>B</td><td>C</td>

<td>Mass; g / m²</td><td>70.4</td><td>68.1</td><td>69.5</td>

<td>Breaking load in longitudinal direction; kg</td><td>6.6</td><td>3.51</td><td>4.8</td>

<td>Breaking load in transverse direction; kg</td><td>2.04</td><td>1.35</td><td>1.8</td>

<td>Length at break in longitudinal direction; m</td><td>6300</td><td>3440</td><td>4250</td>

<td>Length at break in transverse direction; m</td><td>1930</td><td>1350</td><td>1800</td>

<td>average length at break; m</td><td>4110</td><td>2400</td><td>3020</td>

<td>Elongation at break in the longitudinal direction; %</td><td>3.1</td><td>3.0</td><td>3.0</td>

<td>Elongation at break in transverse direction; %</td><td>5.3</td><td>3.8</td><td>3.9</td>

No.337526 tφ v

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No. 337526