Deicing and antifreeze composition thickened by layered silicates
Abstract
Gegenstand der Erfindung ist ein Enteisungs- oder Vereisungsschutzmittel, enthaltend 35 bis 93 Gew.-% mindestens eines Glykols und 0,01 bis 15 Gew.-% mindestens eines wasserlöslichen Schichtsilicats, sowie Wasser ad 100 Gew.-%, bezogen auf das Gewicht des Enteisungsmittels.
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10 claims: 8 independent, 2 dependent
- 1Deicing or anti-icing agent containing 35 to 93 weight .-% at least one glycol and 0.01 to 15 wt .-% of at least one water-soluble Phyllosilicate, and water ad 100 wt .-%, based on the weight of the Deicing.
- 6Deicing or anti-icing agent according to one or more of Claims 1 to 5, comprising 0.1 to 5 wt .-% of organic thickeners from the Group of the homo- or copolymers of unsaturated carboxylic acids such as Acrylic acid, methacrylic acid and their derivatives such as esters and amides, and also Cellulose ethers (alkyl, hydroxyalkyl and Carboxyalkylcelluloseether), Polyethylene glycols, polyvinyl pyrrolidones, polyvinyl alcohols, polyethylene oxides, Xanthan gum.
- 8Deicing or anti-icing agent according to one or more of Claims 1 to 7, comprising as layer silicates compounds of general formula (Al (2-y) Mg y ) [Si (4-x ) Al x O 20 (OH) 2 ] - (X + y), where x and y are integer values can accept, which cause a charge balance, Al 3+ by Mg 2+ and Fe 3+ And Si 4+ by Al 3+ may be substituted and other cations such as K + , Li + , Ca 2+ and Mg 2+ or other anions such as F - or OH - can be incorporated in the crystal structure.
- 9Deicing or anti-icing agent according to one or more of Claims 1 to 7, comprising as layer silicates compounds of general formula [Si 8th (Mg a Li b H c )O 20 (OH) (4-y) F y ] - z Wherein accept a, b, c, y and z are integer values can cause a charge balancing, Mg 2+ by Al 3+ and Fe 3+ And Si 4+ by Al 3+ may be substituted and other cations such as K + , Li + , Ca 2+ and Mg 2+ or also other anions such as F - or OH - can be incorporated in the crystal structure.
- 10Using 0.01 to 15 wt .-% of at least one water-soluble Layered silicate for thickening a composition comprising 35-93 wt .-% at least one glycol and water to 100 wt .-% contains.
Independent claims8
93 paragraphs, as filed
The present invention relates to layered thickened water / glycol mixtures, which can be used as a deicing and anti-icing agents. These Mixtures serve to remove frozen precipitation such as snow and ice from Surfaces, and to prevent a re-icing of surfaces.
Of particular importance are deicing and anti-icing agent for Treatment of aircraft surfaces. During takeoff, these fluids should by the occurring shear stresses of the aircraft surfaces flow away. For simplicity, all of these fluids is hereinafter referred to as Aircraft de-icing or deicing referred.
During the winter months plane surfaces can by frozen Precipitates are occupied. This frozen precipitation must before starting the aircraft to be removed because they cause a severe decrease of the Start necessary buoyancy lead.
A distinction is made between deicing agents used primarily to remove frozen precipitation are used, and anti-icing agents on already de-iced and hence cleaned aircraft surfaces reicing to counteract.
In general, to remove frozen precipitation on deicing Water / glycol-based uses. The glycol serves as a freezing point Medium. In addition, surfactants are included, which of the surface tension Deicing decrease and thus the wetting of the aircraft surfaces improve. In addition, de-icing fluid corrosion inhibitors, defoamers, Dyes and flame-retardant substances. Such non-thickened Deicing distinguished by Newtonian flow behavior. That means, that their viscosity is independent of shear. According to the SAE (Society of Automotive Engineering) -Convention are non-thickened deicing with Newtonian Flow behavior than Type I fluids referred. Type I fluids are depending diluted outside temperature with a different amount of water and with Spraying vehicles hot applied to the aircraft surfaces. blank With their help to remove frozen deposits effectively. However, type I fluids only very limited protection on before refreezing.
In contrast to pure deicing anti-icing agents in addition thickener substances. The improved caused thereby viscosity of these fluids protection against re-icing, since the fluid flows at rest very slowly from the aircraft surfaces and thus over a long Period absorb freezing precipitation. get icing agent by the thickening agent used therein is a non-Newtonian, pseudoplastic flow behavior. The viscosity of these fluids is shear dependent. in the Moment of takeoff, decreases the viscosity of the fluid by the increasing Drag heavily on it and can thus rapidly from the aircraft surfaces flow away. Depending on the anti-icing time a distinction between Type II and Type IV fluids. Type III fluids are distinguished by a particularly pseudoplastic Flow behavior, so they de-icing aircraft with a low Start speed serve.
Aircraft deicing must satisfy a large number of requirements. According to the SAE specifications AMS (Aerospace Material Standards) 1424 and AMS 1428 not only the runoff and the icing protection time are examined, but also many other physical properties.
This includes for example the storage stability of aircraft deicing. The Viscosity of aircraft de-icing must during storage over a not change long period. A good aircraft deicing may not corrosive be, especially not to aluminum, magnesium, steel and acrylic. It must be environmentally friendly and should support fire. In addition, thickened aircraft deicing must be shear stable. The fluids be applied by spraying vehicles, that of a high mechanical load causing fluid. The deicing compositions must not exceed 20% of their losing original viscosity. Finally allowed residues of Aircraft deicing, the aerodynamically after the start of the aircraft in quiet zones of the wings have accumulated, and thus could not drain, form no gel deposits. is In the latter two properties a need for further development.
US 4,954,279 describes the microemulsion of an oil in a water / glycol mixture. In addition, thickening agents and surfactants are present. Since all components in an Microemulsion be present, important fluid properties such as storage stability, improved especially at very low temperatures.
US 5,118,435 discloses a deicing composition based on the synergistic Effect which is achieved by the combination of two polyacrylates as the thickener. The viscosity of the fluid is independent of temperature, so that the film thickness of the deicing composition applied at each possible outdoor temperature is low, and the fluid thus when the aircraft always flows well.
US 5,273,673 discloses deicers, which by a content of comprise alkyl phenol significantly improved retention times. US 5,386,968 discloses that the same surfactant class of an improvement Derivative is diluted unthickened aircraft suitable.
US 5,334,323 discloses that the neutralization of the thickener serving Polyacrylic acid with a mixture of NaOH and KOH can be performed. Thus, the aircraft deicing is particularly tiefviskos and flows well from.
US 5,750,047 discloses that the icing protection time of thickened deicing is to increase by polyacrylates considerably.
US 5,772,912 discloses environmentally friendly deicing for a wide Applications based on xanthan as thickener.
US 5,817,252 discloses the combination of two non-ionic surfactants with different HLB value to the diffusion of the frozen precipitation to control so that the deicing remains active for longer. The same principle can be applied to SAE Type II fluids according to US 5,935,488.
From the prior art it is clear that from when developing Aircraft deicing been almost exclusively on improving Derivative and Liquid Flow has focused.
Until now, the synthesis thickened aircraft deicing exclusively Thickener used on an organic basis. Such are preferably crosslinked Homo- or copolymers of unsaturated carboxylic acids such as acrylic acid, methacrylic acid and their derivatives such as esters and amides, and also cellulose ethers (alkyl, Hydroxyalkyl and carboxyalkyl cellulose ether), polyethylene glycols, polyvinylpyrrolidones, Polyvinyl alcohols, polyethylene oxides, xanthan gum, and the like, or mixtures of such water-soluble polymers. The thickening mechanism of all these organic polymers based on the formation of a polymer network in the Glycol solution.
However, all thickeners mentioned here under mechanical stress are more or less irreversibly damaged. This is demonstrated by a irreversible viscosity loss at high shear stress by fast-running Stirrers, pumps or when flowing through small pipe cross sections. The mechanical stress caused connected a fraction of the polymer chains and thus irreversible damage to the polymer network.
There is therefore the task of designing aircraft de same time as, that they under mechanical stress such as pumping or spraying with sprayers lose as little viscosity.
In addition, all tend here said thickening agent under certain external Conditions to gel formation. to collect aircraft deicing after Start in aerodynamically quiet areas of the aircraft, so dry this Residues of the low air pressure at altitudes from 5,000 m completely. These residues may swell greatly, if you are with moisture such as rain water get in touch. The resulting gels may at low temperatures, as occur at high altitudes, freezing and thereby the elevator block, whereby the aircraft is no longer completely maneuverable.
All aircraft deicing based conventional thickeners form clearly visible amounts of gel residues. Depending on the type of thickener can be these gels during the rehydration more or less with the water well replace. It would be desirable fluid residue accumulating within the first Diving operations could completely rinse through the water.
Therefore, there is also the task of formulating aircraft deicing so that dried fluid residues can not form gel residues with rainwater.
Surprisingly, it has now been found that anti-icing agent which, in addition to generally customary, known ingredients of anti-icing agents such as for example, glycols, surfactants, basic and acidic compounds to regulate the pH and corrosion protection means at the same time as layer silicates contain thickeners, under mechanical stress no viscosity loss show. In addition, these anti-icing agent form after drying only Such residues which dissolve after rehydration completely in water and thus do not form sparingly soluble gels.
It is in these thickeners are water-soluble phyllosilicates which For example, the mineral family of the smectites belong to which both naturally occurring as synthetically produced hectorites and bentonites, or montmorillonites . count These inorganic thickeners are characterized by the fact that they absorb water and organic molecules such as glycols between the silicate layers can, so that they are useful as thickeners for aqueous systems.
Aircraft deicing based on these thickeners not only meet the Requirement for a high static viscosity and yield value in the same time good pronounced pseudoplasticity, but they are under mechanical stress additionally extremely shear stable. Moreover, let parched dissolve residues of these aircraft deicing fully with the aid of water and do not form sparingly soluble gels. These phyllosilicates can be either alone or in combination with the above organic use thickeners. It is notable that the concentrations of let abovementioned organic thickeners much lower, if in Combination be used with layered.
The present invention thus relates to a deicing or Icing agent containing 35 to 93 weight .-% of at least one glycol and 0.01 to 15 wt .-% of at least one water-soluble sheet silicate, and water ad 100 wt .-%, based on the weight of the deicing.
Another object of the invention is the use of 0.01 to 15 wt .-% at least one water-soluble sheet silicate for thickening a Composition 35-93 wt .-% of at least one glycol and water ad 100 percent by .-%.
Another object of the invention is a method for thickening a Deicing or anti-icing agent, that contains 35 to 93 weight .-% of at least a glycol and water to 100 wt .-% contains, giving him 0.01 to 15 wt .-% at least one water-soluble sheet silicate is added.
The deicing and anti-icing agent according to the invention are particularly well suited for the de-icing of aircraft suitable. They are but also for de-icing and icing protection of other transport such as motor vehicles or railways suitable, or for any surfaces on which there are an anti-icing should.
The deicing and anti-icing agent according to the invention (hereinafter "Deicing" called), in addition to glycol, water and water-soluble Phyllosilicates contain other ingredients. Such other ingredients are for example, surfactants, corrosion inhibitors, basic compounds or acidic Compounds for pH adjustment and further, organic thickeners. So can an inventive deicing in a preferred embodiment, contain the following items: <sl><li>a) 35-93 wt .-%, preferably 45 to 90 wt .-% of at least one glycol from the group of alkylene glycols having 2 to 3 carbon atoms and oxalkylene glycols with 4 to 6 C atoms,</li><li>b) 0 to 10 wt .-%, preferably 0.02 to 2 wt .-% of at least one Surfactant from the group of nonionic or anionic surfactants,</li><li>c) 0.01 to 5 wt .-%, preferably 0.02 to 2 wt .-% of at least one Corrosion inhibitor</li><li>d) from 0.02 to 15 wt .-%, preferably 0.05 to 10 wt .-% of a water soluble layered,</li><li>e) optionally, at least one basic compound selected from the group of Alkali metal carbonates, alkali metal hydroxides or amines for setting the pH 6-11,</li><li>f) optionally at least one acidic compound from the group of inorganic or organic acids for adjusting the pH 6-11,</li><li>g) optionally, additional organic thickeners from the group of Homo- or copolymers of unsaturated carboxylic acids such as acrylic acid, Methacrylic acid and its derivatives such as esters and amides, and also cellulose ethers (Alkyl, hydroxyalkyl, and carboxyalkyl cellulose ether), polyethylene glycols, Polyvinylpyrrolidones, polyvinyl alcohols, polyethylene oxides, xanthan gum, and</li><li>h) water as the remainder to 100 wt .-%.</li></sl>
The percentages by weight are always based on the weight of the deicer.
The components b, c, e, f and g are not mandatory in the present invention Deicers contain. Preferred deicing includes not only Ingredients a, d and h one or more further components selected from B, C, e, f and g.
The component a) of the deicing composition is preferably Ethylene glycol, propylene glycol (1,2-propylene glycol or 1,3-propylene glycol), Diethylene glycol, dipropylene glycol or a mixture of two or more of these Glycols, propylene glycols being particularly preferred. The glycols serve in particular for lowering the freezing point and, in addition to water, the main component of the Deicing represents.
Component b) may preferably be a fatty alcohol having 6 to 24 carbon atoms, preferably 8 to 18 carbon atoms in the alkyl radical or an alkoxylate thereof having 1 to 10, preferably 1-8 alkoxy groups, especially of ethylene oxide, propylene oxide or a mixture thereof, wherein ethylene oxide is preferred to be. Said alkyl radical in Fatty alcohol may be straight or branched, aliphatic or aromatic, saturated or unsaturated with preferably 1 to 3 double bonds. Examples include: Octyl, decyl, dodecyl, isotridecyl, para-iso-nonylphenyl, para-iso-octylphenyl and Stearyl, oleyl further, Cocosalkyl- and Talgalkylalkohol. Component b) can also be a mixture of said fatty alcohols and / or be fatty alcohol ethoxylates, such as a fatty alcohol mixture with a C<sub>12</sub>alkyl and C<sub>14</sub>Alkyl (C<sub>12</sub>/ C<sub>14</sub>Fatty alcohol).
Component b) may further preferably a potassium and / or Sodium alkylarylsulfonate having one or more, preferably one or two Sulfonate groups, one or more, preferably one or two alkyl groups 5 to 18 carbon atoms, preferably 12 to 18 carbon atoms, and one or more, preferably one or two, benzene rings.
Component c) comprises corrosion inhibitors, such as for deicing composition Based on glycols and water are used. Suitable corrosion inhibitors are alkali metal phosphates, lower alkyl phosphates such as ethyl phosphate, Dimethyl phosphate, isopropyl phosphate, and the like, imidazoles, such as 1 H-imidazole, Methylimidazole, benzimidazole and the like, and triazoles such as benzotriazole and Tolyltriazole. It is also possible thiourea, sodium nitrate or butyne-1,4-diol used will.
As component d) are naturally occurring or synthetically produced water-soluble phyllosilicates. Such, for example, the mineral family of belong smectites, which include both naturally occurring as synthetically produced hectorites and bentonites, or montmorillonites count.
Natural phyllosilicates have, for example, the general formula (Al<sub>(2-y)</sub>Mg<sub>y</sub>) [Si<sub>(4-x)</sub>Al<sub>x</sub>O<sub>20</sub>(OH)<sub>2</sub>]<sup>-</sup><sub>(X + y)</sub>Wherein x and y assume different values can, Al<sup>3+</sup> by Mg<sup>2+</sup> and Fe<sup>3+</sup>And Si<sup>4+</sup> by Al<sup>3+</sup> may be substituted and cations like K<sup>+</sup>, Li<sup>+</sup>, Ca<sup>2+</sup> and Mg<sup>2+</sup> or other anions such as F<sup>-</sup> or OH<sup>-</sup> can be incorporated in the crystal structure.
Layered synthetic produced for example, have the general formula (Si<sub>8th</sub>(Mg<sub>a</sub>Li<sub>b</sub>H<sub>c</sub>)O<sub>20</sub>(OH)<sub>(4-y)</sub>F<sub>y</sub>]<sup>-</sup><sub>z</sub>Wherein accept a, b, c, y and z values different can, Mg<sup>2+</sup> by Al<sup>3+</sup> and Fe<sup>3+</sup>And Si<sup>4+</sup> by Al<sup>3+</sup> may be substituted and cations like K<sup>+</sup>, Li<sup>+</sup>, Ca<sup>2+</sup> and Mg<sup>2+</sup> or other anions such as F<sup>-</sup> or OH<sup>-</sup> can be incorporated in the crystal structure.
The component e) is preferably a basic pH adjusting agent from the group of Alkali metal hydroxides such as NaOH and KOH, alkylamines, such as butylamine, hexylamine, Octylamine and isononylamine, and alkanolamines such as mono-, di- and triethanolamine. The alkali metal hydroxides are particularly preferred. Comprises the inventive Deicing such a basic compound, their content is at preferably 0.1 to 5 wt .-%, based on the weight of the deicing.
The component f) is preferably an acidic pH regulator from the group of inorganic or organic acids, such as phosphoric acid, phosphorous acid, Mono- and dicarboxylic acids with alkyl groups having 2 to 12 carbon atoms, preferably 4 to 8 carbon atoms, and one or more, preferably one or two Benzene rings. Does deicer according to the invention such an acid pH regulator, its content is preferably 0.1 to 5 wt .-%, based on the weight of the deicing.
The component g) is a water soluble thickening agent. There are preferred cross-linked homo- or copolymers of unsaturated carboxylic acids such as acrylic acid, Methacrylic acid and its derivatives such as esters and amides, and also cellulose ethers (alkyl, Hydroxyalkyl and Carboxyalkylcelluloseether), polyethylene glycols, Polyvinylpyrrolidones, polyvinyl alcohols, polyethylene oxides, xanthan gum, and like or mixtures of such water-soluble polymers. Does deicer according to the invention, such a thickening agent, as is whose content is preferably 0.1 to 5 wt .-%, based on the weight of the Deicing.
The deicing composition according to the invention generally contain at least 5, preferably at least 10 wt .-% water.
Further, in the de-icing agents, defoamers, dyes, Complexing agents and antioxidants may be contained.
The novel deicing composition is carried out by Mixing together the individual components in any order, resulting in the Example can be carried out in a stirrer-equipped container.
The invention will now be illustrated by examples:
The deicing is after mechanical stress no appreciable have irreversible viscosity loss. To study the viscosity loss in Laboratory used a Brookfield counter-rotating mixers, consisting of two shear blades, which rotate in opposite directions. The shear blades move at a Rotational speed of 3,500 revolutions per minute. Upon immersion of the Counter Rotating mixer in an aircraft deicing, the thickener molecules by the narrow gap between the two shearing blades pressed through, in which they each can be irreversibly damaged thickener type. The occurring here Viscosity loss leads to a reduction of the derivative action.
The completely dried deicing should not form any residues swell by rehydration to give sparingly soluble gels. To investigate the Gelation are aluminum sheets from 2024-T3 material with an area of 100 mm x 50 mm x 1 mm. The surface of the plates is carried aged alternate brief immersion in each sodium hydroxide and nitric acid, can adhere that fluid and gel residues better. The aluminum sheet is four Seconds completely immersed in the fluid to be examined and subsequently dried at a temperature between 30 ° C and 35 ° C. This step is to 24 hours six times repeatedly with the same plate. Within this first test phase forms gradually a dry residue on the Aluminum surface.
In the second test section, the sheet with the fluid residue of 30 is immersed seconds in demineralized water and carefully out of the Water drawn. After 60 seconds, the weight of the plate with the swollen fluid residue is weighed. This rehydration is a total times repeated ten. Subsequently, one can over the course of the change in weight assess the gelation of the fluid.
example 1
There is first a conventional SAE type IV deicing by mixing the following components:<tables><table><tgroup cols="2"><tbody><row><entry align="right">50.00 wt .-%</entry><entry align="left">1,2-propylene glycol</entry></row><row><entry align="right">0.05 wt .-%</entry><entry align="left">tolyltriazole</entry></row><row><entry align="right">0.33 wt .-%</entry><entry align="left">linked polyacrylic acid</entry></row><row><entry align="right">0.12 wt .-%</entry><entry align="left">C<sub>12/16</sub>Fatty alcohol ethoxylated with 6 mol of ethylene oxide</entry></row><row><entry align="right">0.18 wt .-%</entry><entry align="left">sodium hydroxide</entry></row><row><entry align="right">48.87 wt .-%</entry><entry align="left">Water.</entry></row></tbody></tgroup></table></tables>
The components were by vigorous stirring and heating to 60 ° C within dissolved 3 h. The deicing composition obtained was tested for viscosity and Shear stability investigated: <tables><table><tgroup cols="3"><tbody><row><entry align="left">Viscosity (0.3 rpm, 20 ° C) (viscosity at rest)</entry><entry align="left">Viscosity (60 rpm, 20 ° C) (flow viscosity)</entry><entry align="left">Viscosity (0.3 rpm, 20 ° C), (viscosity at rest) (after mechanical stress by Counter Rotating Mixer)</entry></row><row><entry align="left">25,000 mPas</entry><entry align="left">820 mPas</entry><entry align="left">20,100 mPas</entry></row></tbody></tgroup></table></tables>
In a spindle rotation speed of 0.3 rpm, the deicing a Viscosity of 25,000 mPas. This value is in the for SAE Type IV deicing usual range. Increasing the spindle revolutions to 60 rpm, the viscosity is lowered to 820 mPas. This rheological behavior as is called pseudoplastic, ensures that the deicing composition at the start of Aircraft completely flows off from the surfaces. Burdened you this Deicing using a Brookfield counter-rotating mixer (5 min / 3500 rpm) and measures the viscosity of this sample after a lapse of 5 minutes again, there is the viscosity at rest only at 20,100 mPas. The deicing met just the prerequisite of a SAE type IV deicing composition with respect to the derivative action. at a further mechanical stress could be the viscosity of the deicer fall below the permitted range for this and it could therefore no longer to Protection are employed by aircraft from reicing.
Subsequently, the gel performance of this aircraft deicing is examined. Given an aged aluminum sheet is four seconds in the deicing dipped and then dried at a temperature of 30 ° C. This Step is repeated with the same sheet after 24 hours six times.
Then, the sheet with the dried Enteisungsmittelrückstand is for immersed for 30 seconds into demineralized water and carefully out of the Water drawn. After 60 seconds, the weight of the plate with the swollen Enteisungsmittelrückstand weighed. This rehydration is ten times repeated. Subsequently, one can over the course of Weight change assess the gelation of the deicer.
In the aircraft deicing is described under Example 1 reveals that the Dry residue greatly swells with water and then poorly of the aluminum plate detaches again. Would be such an aircraft deicing accumulate after takeoff in aerodynamically quiet areas of aircraft wings and then dry up, so could swell strongly these residues, if you come with moisture such as rain water in contact. The resulting therefrom gel-like residues could at low temperatures, such as in high altitudes occur freeze and thus block the elevators, which the aircraft would no longer be fully maneuverable.
example 2
There is now an inventive SAE type II deicing by mixing the following components:<tables><table><tgroup cols="2"><tbody><row><entry align="right">50.00 wt .-%</entry><entry align="left">1,2-propylene glycol</entry></row><row><entry align="right">0.05 wt .-%</entry><entry align="left">tolyltriazole</entry></row><row><entry align="right">0.15 wt .-%</entry><entry align="left">C<sub>12</sub>/ C<sub>14</sub>Fatty alcohol ethoxylated with 5 mol of ethylene oxide</entry></row><row><entry align="right">1.5 wt .-%</entry><entry align="left">of synthetic. Hectorite (Mg<sub>2.67</sub>Li<sub>0.33</sub>) Si<sub>4</sub>O<sub>10</sub>(OH, F)<sub>2</sub>)N / A<sub>0.33</sub> × H<sub>2</sub>O</entry></row><row><entry align="right">48.3 wt .-%</entry><entry align="left">Water.</entry></row></tbody></tgroup></table></tables>
The components were by vigorous stirring and heating to 60 ° C within dissolved 3 h. The deicing composition obtained was tested for viscosity and Shear stability investigated:<tables><table><tgroup cols="3"><tbody><row><entry align="left">Viscosity (0.3 rpm, 20 ° C) (viscosity at rest)</entry><entry align="left">Viscosity (60 rpm, 20 ° C) (flow viscosity)</entry><entry align="left">Viscosity (0.3 rpm, 20 ° C), (viscosity at rest) (after mechanical stress by Counter Rotating Mixer)</entry></row><row><entry align="left">7,600 mPas</entry><entry align="left">190 mPas</entry><entry align="left">7,400 mPas</entry></row></tbody></tgroup></table></tables>
In a spindle rotation speed of 0.3 rpm, the deicing a Viscosity of 7,600 mPas. This value is in the for SAE type II deicing usual range. Increasing the spindle revolutions to 60 rpm, the viscosity is lowered to 190 mPas. This rheological behavior as is called pseudoplastic, ensures that the deicing composition at the start of Aircraft completely flows off from the surfaces. you now burdened the Deicing using a Brookfield counter-rotating mixer (5 min / 3500 rpm) and measures the viscosity of this sample after a lapse of 5 minutes again, there is the viscosity at rest again at 7,400 mPas. This proves that the Deicing under mechanical stress, such as at high shear stress by high-speed stirrers, pumps or when flowing through small Cable cross-sections occur, can not be irreversibly damaged.
Subsequently, the gel performance of this aircraft deicing is examined. Given an aged aluminum sheet is four seconds in the deicing dipped and then dried at a temperature of 30 ° C. This Step is repeated with the same sheet after 24 hours six times.
Then, the sheet with the dried Enteisungsmittelrückstand is for immersed for 30 seconds into demineralized water and carefully out of the Water drawn. After 60 seconds, the weight of the plate with the swollen Enteisungsmittelrückstand weighed. This rehydration is times repeated a total of ten. Subsequently, one can over the course of Weight change assess the gelation of the deicer.
In the deicing mentioned under Example 2 falls significantly on that ground of the dry residue is much lower than in the Example 1 -described deicing. In addition, this residue can already after fourth dipping operation are completely replaced with water. Dried residues this aircraft deicing composition in aerodynamically quiet zones would with Rainwater do not form sparingly releasable gels, but are rinsed quickly.
Further investigation of the described in Example 2 Aircraft deicing show that all further requirements of the SAE specification AMS 1428 are fulfilled. Thus, the icing protection time (WSET test) this type II deicing composition is greater than 30 minutes. The 1: 1 dilution with water shows a holdover time of more than 5 minutes. The runoff to be tested all Concentrations in the wind tunnel corresponds to all required temperatures of Minimum requirement. In addition, all material tests are met.
example 3
An inventive SAE type II deicing by mixing the following components:<tables><table><tgroup cols="2"><tbody><row><entry align="right">60.00 wt .-%</entry><entry align="left">diethylene glycol</entry></row><row><entry align="right">0.05 wt .-%</entry><entry align="left">benzotriazole</entry></row><row><entry align="right">0.1 .-%</entry><entry align="left">C<sub>12</sub>/ C<sub>14</sub>Fatty alcohol ethoxylated with 4 moles of ethylene oxide</entry></row><row><entry align="right">1.7 wt .-%</entry><entry align="left">of synthetic. Hectorite (Mg<sub>2.67</sub>Li<sub>0.33</sub>) Si<sub>4</sub>O<sub>10</sub>(OH, F)<sub>2</sub>)N / A<sub>0.33</sub> × H<sub>2</sub>O</entry></row><row><entry align="right">38.15 wt .-%</entry><entry align="left">Water.</entry></row></tbody></tgroup></table></tables>
The components were by vigorous stirring and heating to 60 ° C within dissolved 3 h. The deicing composition obtained was tested for viscosity and Shear stability investigated:<tables><table><tgroup cols="3"><tbody><row><entry align="left">Viscosity (0.3 rpm, 20 ° C) (viscosity at rest)</entry><entry align="left">Viscosity (60 rpm, 20 ° C) (flow viscosity)</entry><entry align="left">Viscosity (0.3 rpm, 20 ° C), (viscosity at rest) (after mechanical stress by Counter Rotating Mixer)</entry></row><row><entry align="left">6,800 mPas</entry><entry align="left">160 mPas</entry><entry align="left">6,400 mPas</entry></row></tbody></tgroup></table></tables>
Loaded to the deicing with a Brookfield Counter Rotating Mixer (5 min / 3.500 rpm) and measures the viscosity of this sample after a lapse of 5 minutes again, the viscosity at rest is 6400 mPas. Thus it is proved that the deicing at high shear stress no irreversible damage suffers.
Examination of the gel behavior of this aircraft deicing composition has shown that the Enteisungsmittelrückstand can quickly rinse with water.
Further investigation of the described in Example 3 Aircraft deicing show that all further requirements of the SAE specification AMS 1428 are fulfilled. Thus, the icing protection time (WSET test) this type II deicing composition is greater than 30 minutes. The 1: 1 dilution with water has a lead time of more than 5 minutes. The runoff to be tested all Concentrations in the wind tunnel corresponds to all required temperatures of Minimum requirement. In addition, all material tests are met.
example 4
An inventive SAE type II deicing by mixing the following components:<tables><table><tgroup cols="2"><tbody><row><entry align="right">50.00 wt .-%</entry><entry align="left">1,2-propylene glycol</entry></row><row><entry align="right">0.05 wt .-%</entry><entry align="left">tolyltriazole</entry></row><row><entry align="right">0.75 wt .-%</entry><entry align="left">Sodium alkylbenzenesulfonate (sodium dodecylbenzenesulfonate)</entry></row><row><entry align="right">1.35 wt .-%</entry><entry align="left">of synthetic. Hectorite (Mg<sub>2.67</sub>Li<sub>0.33</sub>) Si<sub>4</sub>O<sub>10</sub>(OH, F)<sub>2</sub>)N / A<sub>0.33</sub> × H<sub>2</sub>O</entry></row><row><entry align="right">47.85 wt .-%</entry><entry align="left">Water.</entry></row></tbody></tgroup></table></tables>
The components were by vigorous stirring and heating to 60 ° C within dissolved 3 h. The deicing composition obtained was tested for viscosity and Shear stability investigated:<tables><table><tgroup cols="3"><tbody><row><entry align="left">Viscosity (0.3 rpm, 20 ° C) (viscosity at rest)</entry><entry align="left">Viscosity (60 rpm, 20 ° C) (flow viscosity)</entry><entry align="left">Viscosity (0.3 rpm, 20 ° C), (viscosity at rest) (after mechanical stress by Counter Rotating Mixer)</entry></row><row><entry align="left">6,000 mPas</entry><entry align="left">230 mPas</entry><entry align="left">5,900 mPas</entry></row></tbody></tgroup></table></tables>
Loaded to the deicing with a Brookfield Counter Rotating Mixer (5 min / 3.500 rpm) and measures the viscosity of this sample after a lapse of 5 minutes again, so the rest viscosity is 5,900 mPas. Thus it is proved that the deicing at high shear stress no irreversible damage suffers.
Examination of the gel behavior of this aircraft deicing composition has shown that the Enteisungsmitteldrückstand can quickly rinse with water.
Further investigation of the described in Example 4 Aircraft deicing show that all further requirements of the SAE specification AMS 1428 are fulfilled. Thus, the icing protection time (WSET test) this type II deicing composition is greater than 30 minutes. The 1: 1 dilution with water has a lead time of more than 5 minutes. The runoff to be tested all Concentrations in the wind tunnel corresponds to all required temperatures of Minimum requirement. In addition, all material tests are met.
example 5
An inventive SAE type IV deicing by mixing the following components:<tables><table><tgroup cols="2"><tbody><row><entry align="right">50.00 wt .-%</entry><entry align="left">1,2-propylene glycol</entry></row><row><entry align="right">0.05 wt .-%</entry><entry align="left">tolyltriazole</entry></row><row><entry align="right">0.2 wt .-%</entry><entry align="left">C<sub>12/16</sub>Fatty alcohol ethoxylated with 6 mol of ethylene oxide</entry></row><row><entry align="right">2.25 wt .-%</entry><entry align="left">of synthetic. Hectorite (Mg<sub>2.67</sub>Li<sub>0.33</sub>) Si<sub>4</sub>O<sub>10</sub>(OH, F)<sub>2</sub>)N / A<sub>0.33</sub> x H<sub>2</sub>O</entry></row><row><entry align="right">47.5 wt .-%</entry><entry align="left">Water.</entry></row></tbody></tgroup></table></tables>
The components were by vigorous stirring and heating to 60 ° C within dissolved 3 h. The deicing composition obtained was tested for viscosity and Shear stability investigated:<tables><table><tgroup cols="3"><tbody><row><entry align="left">Viscosity (0.3 rpm, 20 ° C) (viscosity at rest)</entry><entry align="left">Viscosity (60 rpm, 20 ° C) (flow viscosity)</entry><entry align="left">Viscosity (0.3 rpm, 20 ° C), (viscosity at rest) (after mechanical stress by Counter Rotating Mixer)</entry></row><row><entry align="left">19,800 mPas</entry><entry align="left">450 mPas</entry><entry align="left">19,500 mPas</entry></row></tbody></tgroup></table></tables>
Loaded to the deicing with a Brookfield Counter Rotating Mixer (5 min / 3.500 rpm) and measures the viscosity of this sample after a lapse of 5 minutes again, so the rest viscosity is 19,500 mPas. Thus it is proved that the deicing at high shear stress no irreversible damage suffers.
Examination of the gel behavior of this Flugzeugenteisungsmittlers has shown that the Enteisungsmittelrückstand can quickly rinse with water.
Further investigation of the described in Example 5 Aircraft deicing show that all further requirements of the SAE specification AMS 1428 are fulfilled. Thus, the icing protection time (WSET test) This type IV deicing composition is greater than 80 minutes. The 1: 1 dilution with Water has a lead time of more than 5 minutes. The runoff of all to test concentrations in a wind tunnel corresponds to all required temperatures the minimum requirement. In addition, all material tests are met.
example 6
An inventive SAE type IV deicing by mixing the following components:<tables><table><tgroup cols="2"><tbody><row><entry align="right">50.00 wt .-%</entry><entry align="left">1,2-propylene glycol</entry></row><row><entry align="right">0.05 wt .-%</entry><entry align="left">benzotriazole</entry></row><row><entry align="right">0.12 wt .-%</entry><entry align="left">C<sub>12/14</sub>Fatty alcohol ethoxylated with 2 moles of ethylene oxide</entry></row><row><entry align="right">2.6 wt .-%</entry><entry align="left">of synthetic. Saponite ((Mg<sub>3</sub>) Si<sub>3</sub>.<sub>7</sub>Al<sub>0.3</sub>)O<sub>10</sub>(OH)<sub>2</sub>)N / A<sub>0.3</sub> × H<sub>2</sub>O</entry></row><row><entry align="right">47.23 wt .-%</entry><entry align="left">Water.</entry></row></tbody></tgroup></table></tables>
The components were by vigorous stirring and heating to 60 ° C within dissolved 3 h. The deicing composition obtained was tested for viscosity and Shear stability investigated: <tables><table><tgroup cols="3"><tbody><row><entry align="left">Viscosity (0.3 rpm, 20 ° C) (viscosity at rest)</entry><entry align="left">Viscosity (60 rpm, 20 ° C) (flow viscosity)</entry><entry align="left">Viscosity (0.3 rpm, 20 ° C), (viscosity at rest) (after mechanical stress by Counter Rotating Mixer)</entry></row><row><entry align="left">12,600 mPas</entry><entry align="left">300 mPas</entry><entry align="left">12,000 mPas</entry></row></tbody></tgroup></table></tables>
Loaded to the deicing with a Brookfield Counter Rotating Mixer (5 min / 3.500 rpm) and measures the viscosity of this sample after a lapse of 5 minutes again, the static viscosity is 12,000 mPas. Thus it is proved that the deicing at high shear stress no irreversible damage suffers. Examination of the gel behavior of this aircraft deicing composition has shown that the Enteisungsmittelrückstand can quickly rinse with water.
Further investigation of the described in Example 6 Aircraft deicing show that all further requirements of the SAE specification AMS 1428 are fulfilled. Thus, the icing protection time (WSET test) This type IV deicing composition is greater than 80 minutes. The 1: 1 dilution with Water has a lead time of more than 5 minutes. The runoff of all to test concentrations in a wind tunnel corresponds to all required temperatures the minimum requirement. In addition, all material tests are met.
example 7
An inventive SAE type IV deicing by mixing the following components:<tables><table><tgroup cols="2"><tbody><row><entry align="right">55.00 wt .-%</entry><entry align="left">1,2-propylene glycol</entry></row><row><entry align="right">0.05 wt .-%</entry><entry align="left">tolyltriazole</entry></row><row><entry align="right">0.12 wt .-%</entry><entry align="left">C<sub>14/16</sub>Fatty alcohol ethoxylated with 6 mol of ethylene oxide</entry></row><row><entry align="right">0.8 wt .-%</entry><entry align="left">nat. Saponite ((Mg<sub>3</sub>) Si<sub>3.7</sub>Al<sub>0.3</sub>)O<sub>10</sub>(OH)<sub>2</sub>)N / A<sub>0.3</sub> × H<sub>2</sub>O</entry></row><row><entry align="right">0.1 .-%</entry><entry align="left">linked sodium</entry></row><row><entry align="right">43.93 wt .-%</entry><entry align="left">Water.</entry></row></tbody></tgroup></table></tables>
The components were by vigorous stirring and heating to 60 ° C within dissolved 3 h. The deicing composition obtained was tested for viscosity and Shear stability investigated:<tables><table><tgroup cols="3"><tbody><row><entry align="left">Viscosity (0.3 rpm, 20 ° C) (viscosity at rest)</entry><entry align="left">Viscosity (60 rpm, 20 ° C) (flow viscosity)</entry><entry align="left">Viscosity (0.3 rpm, 20 ° C), (viscosity at rest) (after mechanical stress agent Counter Rotating Mixer)</entry></row><row><entry align="left">20,600 mPas</entry><entry align="left">120 mPas</entry><entry align="left">20,000 mPas</entry></row></tbody></tgroup></table></tables>
Loaded to the deicing with a Brookfield Counter Rotating Mixer (5 min / 3.500 rpm) and measures the viscosity of this sample after a lapse of 5 minutes again, the static viscosity is 20,000 mPas. Thus it is proved that the deicing at high shear stress no irreversible damage suffers.
Examination of the gel behavior of this aircraft deicing composition has shown that the Enteisungsmittelrückstand can quickly rinse with water.
Further investigation of the described in Example 7 Aircraft deicing show that all further requirements of the SAE specification AMS 1428 are fulfilled. Thus, the icing protection time (WSET test) This type IV deicing composition is greater than 80 minutes. The 1: 1 dilution with Water has a lead time of more than 5 minutes. The runoff of all to test concentrations in a wind tunnel corresponds to all required temperatures the minimum requirement. In addition, all material tests are met.
Every citation, both ways
| Document | Relation | Office | Cited during |
|---|---|---|---|
| AT16825U1 | Cited by | Austria | Search report |
| WO0129146A1 | Cites | World Intellectual Property Organization (WIPO) | Search report |
| WO02062310A1 | Cites | World Intellectual Property Organization (WIPO) | Search report |
| EP0445653A1 | Cites | European Patent Office (EPO) | Search report |
| US5334323A | Cites | United States of America | Search report |
| US5418271A | Cites | United States of America | Search report |
| US5772912A | Cites | United States of America | Search report |
| US5817252A | Cites | United States of America | Search report |
| WO9308230A1 | Cites | World Intellectual Property Organization (WIPO) | Search report |
| WO9810032A1 | Cites | World Intellectual Property Organization (WIPO) | Search report |
14 members in 8 offices
Priority claims5
| Document | Office | Kind | Date |
|---|---|---|---|
| 102004001409 | Germany | A | |
| 102004001409 | Germany | A | |
| 102004001409 | Germany | – | |
| 102004001409 | – | – | – |
| DE20041001409 | – | – | – |
Members14
| Document | Office | Kind | |
|---|---|---|---|
| NO20050038D0 | Norway | D0 | |
| CA2491986A1 | Canada | A1 | |
| NO20050038L | Norway | L | |
| CN1637111A | China | A | |
| EP1553152A2This record | European Patent Office (EPO) | A2 | |
| JP2005194533A | Japan | A | |
| DE102004001409A1 | Germany | A1 | |
| US2006054857A1 | United States of America | A1 | |
| US7037442B2 | United States of America | B2 | |
| RU2004138757A | Russian Federation | A | |
| DE102004001409B4 | Germany | B4 | |
| EP1553152A3 | European Patent Office (EPO) | A3 | |
| RU2385340C2 | Russian Federation | C2 | |
| CN1637111B | China | B |
13 legal events, as the office reported them to INPADOC
Over the term
Point at a mark for the eventEvents
| Event | Code | |
|---|---|---|
| Application withdrawnWithdrawn18W | 18W | |
| Information on the status of an ep patent application or granted ep patentGrantedSTATUS: THE APPLICATION HAS BEEN WITHDRAWNSTAA | STAA | |
| Despatch of communication of intention to grant a patentORIGINAL CODE: EPIDOSNIGR1GRAP | GRAP | |
| First examination report despatched17Q | 17Q | |
| Designation fees paidAKX | AKX | |
| Request for examination filed17P | 17P | |
| Designated contracting statesAK | AK | |
| Request for extension of the european patentAX | AX | |
| Search report despatchedORIGINAL CODE: 0009013PUAL | PUAL | |
| Party data changed (applicant data changed or rights of an application transferred)RAP1 | RAP1 | |
| Designated contracting statesAK | AK | |
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Numbers
- Publication
- 1553152
- Publication, DOCDB
- 1553152
- Publication, EPODOC
- EP1553152
- Application
- 4030574
- Application, DOCDB
- 04030574
- Application, EPODOC
- EP20040030574
Titles3
- German
- Enteisungsmittel und Vereisungsschutzmittel, verdickt mit Schichtsilikaten
- English
- Deicing and antifreeze composition thickened by layered silicates
- French
- Composition pour la protection contre le gel et pour l'élimination de la glace épaissis par des silicates en couches
Classification
- CPC, 2
- C09K3/185
- C09K3/18
- IPC, 1
- C09K3 18
Designated states2
- Contracting states, 1
- Türkiye
- Extension states, 1
- Yugoslavia, later Serbia and Montenegro (until 2006)