FI89603C

Low smoke modified polypropylene insulation compositions and process for the preparation thereof

Abstract

A flame retardant insulation composition comprising the following components:- (a) in the range of from 5 to 40 per cent by weight of a hydrogenated monoalkylarene (A)-conjugated diene (B) block copolymer containing at least two A blocks and at least one B block;(b) in the range of from 1 to 20 per cent by weight of a plasticizer;(c) in the range of from 1 to 40 per cent by weight of functionalized or not functionalized polypropylene;(d) in the range of from 10 to 85 per cent by weight of a hydrated inorganic filler which optionally has been surface treated with a coupling agent;(e) and optionally in the range of from 0.25 to 10 per cent by weight of a functionalized low molecular weight polypropylene wax, which composition in the absence of component (e) contains a hydrated inorganic filler which has been surface treated with a coupling agent, and process for the preparation thereof by combining components (a) to (d) and optionally (a) to (e).

FI89603C, drawing sheet 1 — Sheet 1 of 23

Term

Term ended

Expired 25 November 2006, 19.8 years ago.

14 claims: 9 independent, 5 dependent

1
Patentt ivaat imukset 1. Palamista hidastava eristysseos, tunnettu siltä, että se sisältää seuraavia aineosia:(a) 5 - 40 paino-% hydrattua monoalkyyliareenin (A) ja konjugoidun dleenin (B) segmenttikopolymeeria, joka sisältää vähintään kaksi A-segmenttiä ja vähintään yhden B-segmentin;(b) 1 - 20 paino-% pehmitintä;(c) 1 - 40 paino-% funktionaaliseksi tehtyä tai funktionaaliseksi tekemätöntä polypropeenia;(d) 10 - 85 paino-% hydratoitua epäorgaanista täyteainetta, joka on valinnaisesti pintakäsitelty liitäntäaineella;(e) valinnaisesti 0,25 - 10 paino-% funktionaaliseksi tehtyä alhaisen molekyylipainon polypropeenivahaa, joka seos komponentin (e) puuttuessa sisältää hydratoitua epäorgaanista täyteainetta, joka on pintakäsitelty liitäntäaineella.
2
Patenttivaatimuksen 1 mukainen seos, tunnettu siitä, että segmenttlkopolymeeri on hydrattu s tyreeni-butadieeni-styreeni segmentt ikopolymeeri.
3
Patenttivaatimuksen 1 tai 2 mukainen seos, tunnettu siitä, että polypropeeni on tehty funktionaaliseksi maleiinihappoanhydridillä.
4
Minkä tahansa edellä olevan patenttivaatimuksen mukainen seos, tunnettu siitä, että pehmitin on mineraaliöljy tai styreeni-butadleenikaksisegmenttikopolymeeri.
5
Minkä tahansa edellä olevan patenttivaatimuksen mukainen seos, tunnettu siitä, että täyteaine on alumiinioksiditrihydraatti.
6
Minkä tahansa patenttivaatimuksen 1-4 mukainen seos, tunnettu siitä, että täyteaine on magnesiumhydroksidi . 8 9 6 0ό
7
Minkä tahansa edellä olevan patenttivaatimuksen mukainen seos, tunnettu siitä, että liltäntäaine on rasvahapon metallisuola, maleaattl, silaani, titanaatti tai sirkoniumaluminaatti.
8
Patenttivaatimuksen 7 mukainen seos, tunnettu siitä, että liltäntäaine on oleaatti tai stearaatti.
9
Minkä tahansa edellä olevan patenttivaatimuksen mukainen seos, tunnettu siitä, että hydratoidun magnesiumhydroksidin keskimääräinen sekundäärihiukkasen koko on välillä 0,6 - 1,2 pm.
10
Minkä tahansa edellä olevan patenttivaatimuksen mukainen seos, tunnettu siitä, että hydratoidun magnesiumhydroksidin kristalliitin sivusuhde on yli 4.
11
Minkä tahansa edellä olevan patenttivaatimuksen mukainen seos, tunnettu siitä, että funktionaaliseksi tehty alhaisen molekyylipainon polypropeenivaha on maleiinihappoanhydridillä funktionaaliseksi tehty, alhaisen molekyylipainon polypropeenlvaha.
12
Minkä tahansa edellä olevan patenttivaatimuksen mukainen seos, tunnettu siitä, että se sisältää 15 - 20 paino-% komponenttia (a), 4 - 8 paino-% komponenttia (b), 4 - 8 paino-% komponenttia (c) ja 63 - 75 paino-% komponenttia (d).
13
Patenttivaatimuksen 12 mukainen seos, tunnettu siitä, että se sisältää 0,5-5 paino-% komponenttia (e).
14
Menetelmä minkä tahansa edellä olevan patenttivaatimuksen mukaisen palamista hidastavan eristysseoksen valmistamiseksi, tunnettu siitä, että liitetään yhteen (a) 5 - 40 paino-% hydrattua monoalkyyliareenin (A) ja konjugoidun dieenin (B) segmenttikopolymeeria, joka sisältää vähintään kaksi A-segmenttiä ja vähintään yhden B-segmentin;(b) 1 - 20 paino-% pehmitintä;(c) 1 - 40 paino-% funktionaaliseksi tehtyä tai funktionaaliseksi 8960ό tekemätöntä polypropeenia;(d) 10 - 85 paino-% hydratoitua epäorgaanista täyteainetta, jota on valinnaisesti pintakäsitelty liitäntäaineella;(e) ja valinnaisesti 0,25 - 10 paino-% funktionaaliseksi tehtyä alhaisen molekyylipainon 5 polypropeenivahaa, joka seos komponentin (e) puuttuessa sisältää hydratoitua epäorgaanista täyteainetta, joka on pintakäsitelty liitäntäaineella.

Independent claims14

274 paragraphs in 11 sections, as filed

Low smoky modified polypropylene insulation blends and method for their preparation

This invention relates to a flame retardant insulation composition and a process for its preparation.

The most common method of reducing the flammability of cable insulation and sheathing materials is to use an organic bromine or chlorine compound in combination with antimony oxide. This system is very effective as a flame retardant, but such materials produce heavy black smoke when burned and also produce hydrogen chloride or hydrogen bromide, which are both corrosive and toxic. As a result, there has been a lot of interest in flame retardant systems that produce smaller amounts of smoke and toxic and corrosive gases when burned. There are two main approaches that will be followed to meet this goal. The first is the removal of halogens from the system and the use of large amounts of alumina trihydrate instead, which aluminum compound is another common flame retardant, or the use of a similar filler, magnesium hydroxide. The second is the development of additives that reduce the formation of smoke and acid gas in halogenated systems. In addition to low smoke and low toxicity, these alloys must also have attractive physical properties in order to be used in cable applications. These properties include hardness, wear resistance, stability to environmental conditions, compressive strength, low temperature flexibility, oil resistance and good electrical properties. At present, there are no low-smoke, low-toxicity, flame retardant materials that are readily available, although some new materials, including metal hydrate-filled polyethylene, are becoming available.

Metal hydrates such as alumina trihydrate and magnesium hydroxide contain water bound to the crystal structure with a metal atom. When these compounds are heated to a sufficiently high temperature, they decompose and release water, which then evaporates. This decomposition and evaporation process binds heat, thus slowing down the initial heating of the insulating material and consequently slowing down the subsequent combustion of the material. However, once this cooling effect has passed, the presence of metal10 dihydrates has only a minor effect on the subsequent combustion process. Unlike the halogenated flame retardant mixture, metal hydrate mixtures with halogen-free polyolefins are rapidly broken down into monomer units and burn relatively cleanly without producing a large amount of smoke. In addition, because metal hydrates only add water to the system, they should not increase the release of toxic or corrosive gases beyond what the system would already produce.

Magnesium hydroxide fillers in combination with aluminum20 oxide trihydrate fillers have been used in flame retardant polypropylene blends. Alumina trihydrate is generally more effective as a flame retardant than magnesium hydroxide due to the greater amount of water bound to this filler; however, magnesium hydroxide has certain advantages, such as better processability when incorporated into a polyolefin blend and a higher decomposition temperature than alumina trihydrate (330 ° C / 230 ° C). This increase in the decomposition temperature makes it possible to process the flame retardant polymer mixture containing magnesium hydroxide at a higher temperature than the compound containing alumina trihydrate. Higher processing temperatures allow for much faster processing due to lower viscosities.

For polypropylene, which is readily available at

9 6 0 3 at a windy price, many industrial uses have been found due to its desirable physical properties, such as ease of machining by all conventional methods; the high melting point and compatibility of stereoregular, e.g., isotactic, polypropylene with many other commercial resins, allowing a large number of blends with special properties. The brittleness of these blends can be reduced either by copolymerizing propylene with ethylene to form block copolymers or by blending homopolypropylene rubbers.

A flame retardant insulation composition has now been found which forms a self-extinguishing, low smoke and halogen free insulation composition which has a high elongation at break and is relatively easy to process.

It has been found that making polypropylene functional in an insulating composition improves physical properties, e.g., tensile strength and elongation. It has been found that the problem of brittleness can be substantially eliminated by the use of functionalized polypropylene. Reactive groups have been grafted onto the functionalized polypropylene which adhere to the filler, providing a bond between the polypropylene and the filler, which provides better physical properties.

It has also been found that conventional magnesium hydroxide fillers cannot be successfully blended with rubber-modified polypropylene blends without component (e), a functionalized low molecular weight polypropylene wax. When these mixtures are filled with a significant amount of magnesium hydroxide, they cannot be processed due to agglomeration of the filler particles. When agglomeration occurs, the effective particle size of the filler increases dramatically and therefore the processability and properties of the final product deteriorate.

Therefore, it would be desirable to provide a magnesium hydroxide filler that has good physical properties and does not adversely affect processability by agglomeration.

The fillers can therefore be surface treated with a binder prior to mixing to improve adhesion between the functionalized polypropylene and the filler.

In addition, it has been found that the addition of a small amount of functionalized, low molecular weight polypropylene wax to a blend dramatically improves the tensile strength of these blends.

Accordingly, the present invention is directed to a flame retardant insulating composition comprising the following components:

(a) 5-40% by weight of a hydrogenated block copolymer of monoalkylarene (A) and conjugated diene (B) containing at least two A-segments and at least one B-segment;

(b) 1-20% by weight of a plasticizer;

(d) 10-85% by weight of a hydrogenated inorganic filler, optionally surface treated with a binder;

(e) and optionally 0.25-10% by weight of a functionalized low molecular weight polypropylene wax;

which mixture in the absence of component (e) contains a hydrated inorganic filler surface-treated with a binder.

The compositions of this invention are prepared by combining the required components in the correct proportions in conventional mixing equipment, such as a rubber roller or mixer, for example a Banbury mixer. This is usually done above the melting temperature of the polymeric materials.

The non-functionalized polypropylene or homopolymer should preferably be isotactic and may be, for example, of the type corresponding to Shell PP-5944 S, PP-5520 and PP DX-5088 available from Shell Chemical Company, Houston Texas. Most commercial isotactic polypropylenes are suitable for the compositions of this invention. Syndiotactic homopolymers can also be used.

Functionalized polypropylenes are well known in the art and can be prepared, for example, according to the procedure described in U.S. Patent Nos. 3,480,580 and 3,481,910. -5944 S, PP-5520 and PP DX-5088. Syndiotactic homopolymers can also be used. The preferred functionalized polypropylene is maleic acid hydride functionalized polypropylene of the Plexar 2110 type available from Northern Petrochemical Company, Rolling Meadows, Illinois, USA.

The fillers used in this invention are hydrated inorganic fillers, e.g., hydrated aluminas (A12O33H2O or Al (OH) ^), hydrated magnesium oxide, hydrated calcium silicate and zinc borate. Of these compounds, the most preferred are hydrated alumina and. magnesium hydroxide.

The coupling agents may contain metal salts of a fatty acid, for example oleates or stearates; silanes, maleates, titanates and zirconium aluminates.

The particle size of the filler is relatively insignificant and may be in accordance with the sizes previously used in the art. Preferred particle sizes are less than 5. It has also been found that magnesium hydroxide fillers with a high aspect ratio crystal form and a larger size are also less prone to agglomeration than those with a lower aspect ratio. The aspect ratios of the crystallites should be greater than 4 and the average of the secondary particle (agglomerate)

Functionalized low molecular weight polypropylene waxes are well known in the art and can be prepared, for example, from polymers prepared according to the procedures described in U.S. Patents Nos. 2,269,345 and 3,919,176. The compositions of this invention containing such waxes preferably contain non-functionalized polypropylene and may contain non-functionalized polypropylene as well as functionalized polypropylene.

A particularly preferred functionalized low molecular weight polypropylene wax is normally a solid thermoplastic ethylene-based polymer modified with monomers having reactive carboxyl groups, especially a copolymer having predominantly ethylene and a lower portion, typically 1-30 and preferably 2-20% by weight of ethylene. unsaturated carboxylic acid. Typical examples of such suitable ethylenically unsaturated carboxylic acids (which term includes mono- and polybasic acids, acid anhydrides, and partial esters of polybasic acids) are acrylic acid, methacrylic acid, crotonic acid, fumaric acid, maleic acid, itaconic acid, maleic anhydride, monomethyl maleate, monoethyl maleate, monomethyl fumarate, monoetyylif amaraatti, tripropyleeniglykolimonometyylieetteri, acid maleate or acid maleate of ethylene glycol monophenyl ether. The carboxylic acid monomer is preferably selected from β-ethylenically unsaturated mono- and polycarboxylic acids and acid anhydrides having 3 to 8 carbon atoms per molecule, and partial esters of these polycarboxylic acids having at least one carboxylic acid group in the acid and an alcohol in solution. The copolymer may also contain other copolymerizable monomers, such as an acrylic acid ester. The comonomers can be combined in the copolymer in any way, e.g., as random copolymers, block copolymers, or graft polymers. Such materials and methods for their preparation are well known in the art. Typical examples of such copolymers include ethylene-acrylic acid copolymer, ethylene-methacrylic acid copolymer, ethylene-malic acid copolymer and the like.

Functionalized low molecular weight polypropylene wax is available, for example, from Eastam Chemical Products Inc. under the tradename Epolene E 43.

Hydrogenated monoalkylarene and conjugated diene block copolymers useful in this invention are well known in the art. This block copolymer has, as defined, for example, in U.S. Pat. The block copolymers used in this invention may have a number of different geometric structures, as the invention does not depend on any particular geometric structure, but rather on the chemical composition of each polymer segment. Thus, the structures may be linear, radial, or branched as long as each copolymer has at least two polymer end segments A and at least one middle polymer segment B, as defined above. Methods for making such polymers are known in the art. Reference is made in particular to the use of lithium-based catalysts and in particular lithium alkyls for the preparation of precursor polymers (polymers before hydrogenation). U.S. Patent No. 3,595,942 not only describes some of the polymers of this invention, but also describes suitable methods for their hydrogenation. The structure of the polymers is determined by their polymerization method. For example, linear polymers are obtained by sequentially feeding the desired monomers into a reaction vessel using initiators such as lithium alkyls or dilithiostilbene and the like, or by joining two block copolymers together with a difunctional coupling agent. Branched structures, on the other hand, can be obtained by using suitable coupling agents having functionality of three or more values with respect to the precursor polymers. The coupling can be performed with multifunctional coupling agents such as dihaloalkanes or alkenes and divinylbenzene as well as certain polar compounds such as silicides, siloxanes or esters of monohydric alcohols and carboxylic acids. The presence of any adjuvant residues in the polymer may be disregarded to adequately characterize the polymers that form part of the compositions of this invention. Likewise, in a general sense, precise structures can also be ignored. This invention is particularly applicable to the use of selectively hydrogenated polymers, the configuration of which prior to hydrogenation is typically as follows: polystyrene-polybutadiene-polystyrene (SBS), polystyrene-polyisoprene-polystyrene (SIS), poly (alpha-methylstyrene) -polybutadiene-polybutadiene and poly (alpha-methylstyrene) -polyisoprene-poly (alpha-methylstyrene).

It is to be understood that both segments A and B may be either homopolymer or random copolymer segments as long as there is at least one class of segment-characterizing monomers in each segment and as long as segment A separately has

I

8960ό is dominated by monoalkenylarenes and segments B separately are dominated by dienes. The term monoalkenylarene is considered to include, in particular, styrene and its analogs and homologues, which are alpha-methylstyrene and ring-substituted styrenes, in particular ring-methylated styrenes. Preferred monoalkenylarenes are styrene and alpha-methylstyrene and styrene is particularly preferred. Segments B may consist of homopolymers of butadiene or isoprene and copolymers of one of these two dienes with monoalkenylarene insofar as conjugated diene units predominate in segment B. When the monomer used is butadiene, it is preferred that about 35-55 mole percent of the butadiene units condensed in the butadiene polymer segment have the 1,2-configuration. Thus, when such a segment is hydrogenated, the resulting product is a regular copolymer segment of ethylene and 1-butene (EB) or resembles it. If the conjugated diene used is isoprene, the resulting hydrogenated product is or resembles a regular copolymer segment of ethylene and propylene (EP). Ethylene-butene or ethylene-propylene segments prepared by direct polymerization of conjugated diene polymer segments rather than hydrogenation are also contemplated in this invention.

If hydrogenation of the precursor copolymers is required, it is preferred to perform it using a catalyst consisting of the reaction products of an aluminum alkyl compound and nickel or cobalt carboxylates or alkoxides, under conditions such as substantially complete hydrogenation of at least 80% of the aliphatic double aliphatic double aliphatic. Preferred block copolymers are those in which at least 99% of the aliphatic double bonds are hydrogenated while less than 5% of the aromatic double bonds are hydrogenated.

The average molecular weights of the individual segments may vary within certain limits. In most cases, the number average molecular weights of the monoalkenylarene segments are between 5,000 and 125,000, preferably between 7,000 and 60,000, while the average molecular weights of the conjugated diene segments are between 10,000 and 300,000 and preferably between 30,000 and 150,000 either before or after hydrogenation. The total molecular weight of the block copolymer is between 25,000 and 250,000 and preferably between 35,000 and 200,000. These molecular weights are determined in more detail by a tritium calculation method or by measuring the osmotic pressure.

The proportion of monoalkenylarene segments should be about 8-55% by weight of the block copolymer, and preferably about 10-35% by weight.

In addition, the composition in question may contain other components such as plasticizers, for example saturated hydrocarbon or mineral oils, hydrogenated or saturated hydrocarbon resins, together with additives such as stabilizers and oxidation inhibitors. Aliphatic oils and resins take precedence over aromatic oils and resins, as aromatics tend to cyclize, resulting in colored compounds. Preferred oils are mainly aliphatic, saturated mineral oils. Preferred resins are saturated or hydrogenated hydrocarbon resins, such as hydrogenated polymers of dienes and olefins, preferably a styrene-butadiene two-segment copolymer. These additional components must be compatible with the block copolymer component. The choice of other components depends on a number of factors, such as the method of coating the yarn.

As mentioned above, the compositions can be modified with additional materials such as stabilizers and oxidation inhibitors. Stabilizers and oxidation inhibitors are typically added to the blends to protect the polymers from degradation during the preparation and use of the blend. Combinations of stabilizers are often more effective due to the different degradation mechanisms to which different polymers are exposed. Certain sterically hindered phenols, organometallic compounds, aromatic amines and sulfur compounds are useful for this purpose. Particularly effective types of these materials are:

1. Benzothiazoles such as 2- (dialkyl-hydroxybenzylthio) benzothiazoles.

2. Esters of hydroxybenzyl alcohols, such as benzoates, phthalates, stearates, adipates or acrylates of 3,5-dialkyl-1-hydroxybenzyl alcohols.

3. Stannofenyylikatekolaatit.

4. Sinkkidialkyyliditiokarbamaatit.

5. Alkylphenols, e.g. 2,6-di-tert-butyl-4-methylphenol.

6. Dilauryl thiodipropionate (DLTDP).

Examples of commercially available antioxidants are Ionox 220 for 4,4-methylene-bis (2,6-di-t-butylphenol) and Ionox 330 for 3,4,6-tris- (3,5-di-t-butyl). -p-hydroxybenzyl) -1,3,5-trimethylbenzene, Dalpac 4 C, trade name for 2,6-di (t-butyl) -p-cresol, Naugawhite, trade name for alkylated bisphenol, Butyl Zimate trade name for zinc dibutyldithiocarbamate and Agerite Geltrol, trade name alkylated and arylated bisphenol phosphite. About 0.01-5.0% by weight of one or more antioxidants are generally added to the mixture. Table I below shows typical, preferred and most preferred concentrations of components (a), (b), (c) and (d) in the compositions of this invention, expressed as weight percentages.

Table I

Component Typical Preferred Most preferred

<td>(A)</td><td>Block copolymer</td><td> 5-40</td><td> 10-30</td><td> 15-20</td>

<td>(B)</td><td>Plasticizer (oil)</td><td> 1-20</td><td> 2-15</td><td> 4-8</td>

<td>(C)</td><td>Modified polypropylene</td><td> 1-40</td><td> 2-20</td><td> 4-8</td>

<td>(D)</td><td>filler</td><td> 10-85</td><td> 40-75</td><td> 63-75</td>

<td>(E)</td><td>Functionalized low molecular weight polypropylene wax</td><td> 0,25-10</td><td> 0,5-5</td><td> 1-2</td>

The respective amounts of each component may vary somewhat in the resulting mixture depending on the components used and their relative amounts.

The following examples further illustrate this invention.

Examples 1-11

The components used were as follows:

Segment copolymer 1 is S-EB-S with molecular weights of segments measured by the GPC method of about 29,000 to 125,000 to 29,000.

The block copolymer 2 is S-EB-S with molecular weights of segments measured by the GPC method of about 10,000 to 50,000 to 10,000.

Segment copolymer 3 is S-EB-S with molecular weights of segments measured by the GPC method of about 7,000 to 35,000 to 7,000.

The oil was Penreco 4434 oil manufactured by Penreco Company. Polypropylene was a homopolymer PP 5520, manufactured by Shell Chemical Company. The modified polypropylene was maleic anhydride functionalized polypropylene Plexar 2110, manufactured by Northern Petrochemical Company, Rolling Meadows, Illinois. ATH was alumina13

8960ό Ditrihydrate, 1, Hit Precipitated Hydral 710 B, manufactured by Alcoa. Mg (OH) 2 was obtained from the Ventron Division of Norton Thiocol Inc. and had a secondary (agglomeration) particle size of about 4 μm. The surface-treated Mg (OH) 2 was Kisuma 5 B, manufactured by Kyowa Chemical Industry Ltd., treated with an oleate and having a secondary particle (agglomeration) size of about 0.8 μm.

The following antioxidants were used.

Irganox 1010; tetra-bismethylene-3- (3,5-di-tert-butyl-4-hydroxyphenyl) propionate methane, manufactured by Ciba-Geigy.

Irganox MD-1024, Ciba-Geigy stabilizer, DLTDP, Plastanox DLTDP, American Cyanamid.

The compositions are by weight.

Examples were extruded by coating 0.762 mm samples on an 1.024 mm solid conductor as insulation. All insulating coatings were performed at a melt temperature of 190 ° C.

In Example 1, conventional non-functionalized homopolypropylene was used. Examples 2-11 involved polypropylene functionalized with maleic anhydride. The results are shown in Table II.

λ:

dP Ο Ο ·> κο dP dP O ooo * - v oo m

CM ·

OX o

·.

f-4 m

(01 Hl

Examples 2-11 showed at least twice and even three times the tensile strength compared to Example 1. Modified polypropylene is much more effective in reinforcing these blends. Each example si5 contained treated Mg (OH)2and showed good, comparable physical properties as well as good processability.

Comparative experiments A and B

Comparative Experiments A and B were performed as described in Examples 1-11 and Table III. Table III also shows the properties observed with control mixtures using standard Mg (OH)2and ATH. These either could not be used for coating or were difficult to process, as evidenced by the low screw speed and high power supply.

Table III

Segmenttikopolymeerikumi

Comparative Test

A

<td>Polypropylene</td><td> —</td>

<td>Modified polypropylene</td><td> 7,35%</td>

<td>Surface treated mg (OH) 2</td><td> —</td>

<td>Irganox 1010</td><td> 0,10%</td>

<td>Irganox 1024</td><td> 0,10%</td>

<td>DLTDP</td><td> 0,40%</td>

<td>Tensile strength (MPa)</td><td> *</td>

<td>Elongation at break (%)</td><td> ★</td>

<td>Line speed (ar / s)</td><td>B</td>

<td>Screw speed (RPM)</td><td> *</td>

<td>Power supply (A)</td><td> *</td>

<td>Back pressure (MPa)</td><td> *</td>

<td>Oxygen index%</td><td> *</td>

Could not be used for coating

RPM

8960ό

B

15,70%

7,85%

7,85% 68,00%

0,10%

0,40%

7,79

300

54,5

30,0

8960ό

Examples 12-17

Examples 12-17 were performed as described in Examples 1-11 and Table IV, except that a functionalized low molecular weight polypropylene wax was used. This wax was functionalized with maleic anhydride and was available from Eastman Chemical Products Inc. under the tradename Epolene E 43. The results of Examples 12-17 and Example 1 are shown in Table IV.

Example 1 shows the properties of a blend without a functionalized low molecular weight polypropylene wax component. Examples 12-17 showed significantly improved tensile strength expressed as breaking strength. Larger amounts of functionalized low molecular weight polypropylene wax tended to produce brittle blends.

II

«H Γ * f • H l> s> - <

H Ή ω M

f— <r · »

rt Γ—

rH r ~

Table IV

II

I

f • mi — IO

P

RPM

9 6 C ό

Examples 18-20

Examples 18-20 were performed as described in Examples 1-11 and Table V, except that a functionalized low molecular weight polypropylene wax was used; this wax was the same as used in Examples 12-17. The results are shown in Table V. A comparison between Example 5 and Examples 18-20 shows that the presence of said wax allows for an increase in tensile breaking strength and easier processability, as evidenced by the reduced back pressure and lower power supply in the extruder.

Table V

Example

<td>Block polymer 1</td><td> 18,05%</td><td> 17,55%</td><td> 17,05%</td><td> 16,05%</td>

<td>Modified polypropylene</td><td> 7,35%</td><td> 7.35%</td><td> 7,35%</td><td> 7,35%</td>

<td>Functionally made low molecular weight PP</td><td> —</td><td> ( 0f50%</td><td> 1,00%</td><td>i 2,00%</td>

<td>Surface treated Mg (OH) 2</td><td> 70,00%</td><td> 70,00%</td><td> 70,00%</td><td> 70,00%</td>

<td>Irganox 1010</td><td> 0,25%</td><td> 0,25%</td><td> 0,25%</td><td> 0,25%</td>

<td>Irganox 1024</td><td> 0,10%</td><td> 0,10%</td><td> 0,10%</td><td> 0,10%</td>

<td>DLTDP</td><td> 0,25%</td><td> 0,25%</td><td> 0,25%</td><td> 0,25%</td>

<td>Tensile strength (MPa)</td><td> 9,31</td><td> 9,52</td><td> 9,58</td><td> 9,65</td>

<td>Elongation at break (%)</td><td> 330</td><td> 310</td><td> 310</td><td> 220</td>

<td>Line speed (cm / s)</td><td> 25</td><td> 25</td><td> 25</td><td> 25</td>

<td>Screw speed (RPM)1)</td><td> 36</td><td> 30</td><td> 36</td><td> 36</td>

<td>Power supply (A)</td><td> 24</td><td> 23</td><td> 22.5</td><td> 23</td>

<td>Back pressure (MPa)</td><td> 38</td><td> 34</td><td> 33</td><td> 35</td>

RPM

Contents11

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Priority claims
Document	Office	Kind	Date
80279785	United States of America	A	1985-11-27
80280685	United States of America	A	1985-11-27
81470585	United States of America	A	1985-12-30
81470685	United States of America	A	1985-12-30
802797	–	–	–
802806	–	–	–
814705	–	–	–
814706	–	–	–
US19850802797	–	–	–
US19850802806	–	–	–
US19850814705	–	–	–
US19850814706	–	–	–

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Document	Office	Kind
US4622350A	United States of America	A	1986-11-11
US4622352A	United States of America	A	1986-11-11
DK565386D0	Denmark	D0	1986-11-25
FI864793A0	Finland	A0	1986-11-25
NO864720D0	Norway	D0	1986-11-25
DK565386A	Denmark	A	1987-05-28
FI864793A	Finland	A	1987-05-28
AU6566786A	Australia	A	1987-06-04
JPS62131052A	Japan	A	1987-06-13
EP0227139A2	European Patent Office (EPO)	A2	1987-07-01
KR870006095A	Republic of Korea	A	1987-07-09
ZA868914B	South Africa	B	1987-07-29
BR8605782A	Brazil	A	1987-08-25
EP0227139A3	European Patent Office (EPO)	A3	1988-11-09
AU585096B2	Australia	B2	1989-06-08
NZ218397A	New Zealand	A	1989-06-28
US4853154A	United States of America	A	1989-08-01
US4859366A	United States of America	A	1989-08-22
EP0427352A1	European Patent Office (EPO)	A1	1991-05-15
CA1307864C	Canada	C	1992-09-22
NO172055B	Norway	B	1993-02-22
EP0227139B1	European Patent Office (EPO)	B1	1993-05-19
NO172055C	Norway	C	1993-06-02
AT89585T	Austria	T	1993-06-15
ATE89585T1	Austria	T1	1993-06-15
DE3688454D1	Germany	D1	1993-06-24
FI89603B	Finland	B	1993-07-15
DE3688454T2	Germany	T2	1993-09-30
FI89603CThis record	Finland	C	1993-10-25
ES2054615T3	Spain	T3	1994-08-16
JPH0798888B2	Japan	B2	1995-10-25

3 legal events, as the office reported them to INPADOC

Over the term

Point at a mark for the event

Events

Legal events, newest first
	Event	Code
2004-08-31	Patent lapsedLapsedMM	MM
1995-06-12	Patent lapsedLapsedMM	MM
1993-06-16	Publication of examined applicationBB	BB