前苏联专利SU991953A3 Composition based on poly-4-methylpentane-1

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专利摘要:
PURPOSE:A specific hydrocarbon and an ether are incorporated to poly-4-methylpentene-1 to produce said composition with good mechanical properties, flexibility at low temperatures, and dielectric property.
公开号:SU991953A3
申请号:SU782634499
申请日:1978-07-04
公开日:1983-01-23
发明作者:Такемори Хаяси
申请人:Дайнити-Ниппон Кейблз,Лтд (Фирма)；
IPC主号:

专利说明:

This invention relates to a composition based on poly-1-methylpentene-1 for producing an electrically insulating material. Poly-1-methylpentene-1, which has excellent mechanical properties not only at ordinary temperature, but also at high temperatures, and also has excellent dielectric properties over a wide range of temperatures and frequencies, is used as a non-polar, high-temperature crystalline polymer. Therefore, i-1-methylpentene-1 is considered to be a promising material for a variety of applications, especially as an electrically insulating material. However, the disadvantage of this polymer is its poor flexibility, especially at low temperatures. A poly-poly-4-methylpentene-1 polymer composition containing polydiorganosiloxane resin is known. C1. . However, the physical properties, especially. elongation at break, this composition does not improve to the extent necessary. Secondly, using polydiorganosilbk-4 sans are expensive substances. The aim of the invention is to improve the physicomechanical compositions of properties such as flexibility and elongation at break, as well as the development of flame retardants for the poly-4-methylpentene-1-o composition. This goal is achieved by the fact that a composition based on poly-4-methylpentene-1 containing a polymer. as an additive, it contains the olefinic oligomer of the general formula. where R. - alkyl with Cg or C, with this ri and Cg mol. weight 570-2200; at Cj ol. or "4 and, while saying weight 510-1350 in the amount of 5-25 weight. h on 00 weight. h ply-4-methylpentene-1. Poly-4-methylpentene 1 is a 4-methylpentene hpmopolymer or a 4-methylpentene-1 copolymer and at least one or the other monomer copolymerizable with it, as will be described below. . An example of such a polymer is a stereoregular, crystalline polymer having an index. melt lying in the range of 1-100, especially 5-80 measured according to ASTMO 1238-70 / / 260 ° C, loading 5 kg and density in the order of 0.32-0.85 g / cm at. Poly-4-methylpentane-1 is prepared by homopolymerizing 4-methyl-1-1 or by copolymerizing 4-methylpentane with at least one monomer copolymerizable with it in the presence of a Ziegler catalyst. Examples of suitable monomers capable of copolymerizing with 4-methylpentene-1. can serve as a pure or branched aliphatic vinyl hydrocarbons having 215 atoms, for example, such. Ethyl propylene, butene, peuten, hexene ,. octene, 3-methylbutene-1, 3-methylenepentene-1, 4-dimethylpentene-1 and 3-methylhexene-1, as well as aromatic vinyl hydrocarbons containing 815 carbon atoms, such as styrene, o-divinylbenzene, p-divinylbenzene , p-ashylbenzene, p-vinylt toluene and c6-methylstyrene. Poly-4-methylpentene-lj used in the invention contains at least 60 weight. % 4-methylpentene-1 or contains 0.1 to 20 weight. % of one or more of the vinyl-type polymerized aromatic hydrocarbons described above. . Suitable oligomers of formula (1) are compounds obtained by olichmerizations of one or more olefins having 2-20 carbon atoms, such as, for example, butene, c-octene, c-nonon, o6-decene, o-undecene c - dodeden and t. P. in the presence of a Ziegler catalyst or Friedel Crafts catalyst. If the amount of olefinic oligomer used is too low, its ability to modify the physical properties of poly-4-methylpentene-1 is lowered, and if the olefinic oligomer is used in excessive amounts, it degrades the high spatial stability of poly-4-methylpentene-1. Therefore, the olefinic oligomer should be used in a quantity lying in the range of 5-25 wt. h per 100 weight. h poly-4-methylpentene-1. As a result, high spatial stability, flexibility and good processing ability of the composite of the invention are maintained and retarder flame can be introduced into it. The invention can use those inorganic or organic flame retardants that are commonly used as flame retardants for rubber or plastics, for example, substances that melt during combustion to form a film that prevents oxygen from entering and causes flame retardation. burning time, water vapors, carbon dioxide, ammonia and other non-combustible gases are released, which prevent oxygen from entering and provide flame retardation, as well as substances that x combustion decompose or melt and combustion heat is withdrawn in order to both. bake flame slowdown. Examples of suitable flame retardants are inorganic flame retarders such as antimony trioxide and dioxide. antimony trioxide, molybdenum Dinka borate, aluminum hydroxide, silicate dirkoni, ammonium bromide, ammonium phosphate, ammonium sulfate, ammonium chloride and sodium bicarbonate, organic flame retardants, for example, such as tricresyl phosphate, krezilfosfat, triphenyl phosphate, difeniloktilfosfat three. butyl phosphate, halogen-containing phosphates, such as tris (p-chloroethyl) phosphate, tris (dichloropropyl) phosphate, tris (2, 3-dibromopropyl) phosphate, tris (bromochloropropyl) phosphate, and halogen-containing compounds, for example perchloropentadeclodecan, octopropane, octopropane, octopropylphosphate, tris (bromochloropropyl) phosphate and halogen-containing phosphates; bis (4-hydroxyethoxy-3, 5-dibromophenyl) propane, decabromobiphenyl, pentabromotoluene, tetrabromobisphenol (A). Flame retardants are compounds having a non-flammability parameter (NFP) equal to at least 22, which is measured according to the following test of flush deceleration. The test is on flame retardation. Oxygen index composidium containing 50 weight. h flame retarder to be tested, uniformly mixed with 100 weight. h polyethylene having a melt index of 1-10 and a density of 0.92-0.94 g / cm is measured according to ASTM D 2863-70. The oxygen index of such a composite thus measured will be referred to hereinafter as the non-ignition parameter of the test retarder flame. If the composite of the invention is treated with. using a molding method that requires a short period of time to complete it, such as pressure molding, or injection molding. A flame retarder may be used, the decomposition temperature is not lower than the processing temperature (about), but if the composition is subjected to more complex treatments, for example extrusion molding, that require a relatively long time, it is preferable that the flame retarder has a heel temperature or decomposition temperature higher processing temperatures, above 2. . Particularly preferred flame retardants are organic flame retarders containing at least 5 wt. % phosphorus or 50 weight; halogen, for example, decabromoxyphenyl oxide, tetrabromobisphenol (A), tvtrabrombi sphenol ($), and so on. P. In the invention, one or more flame retardant flame can be used, and a combination of inorganic retarder flame and organic flame retardant flame is particularly preferred. Plam slow down is used in the amount of 5-200 weight. h preferably 10-100 wt. h per 100 weight. h poly-4-methylpentec-1. The proposed co-containment, flame retardant or flame retardant may also include traditional amounts of conventional rubber and plastic additives such as antioxidants, metal deactivators, coloring agents, UV and radiation absorbers, a voltage stabilizer, carbon black, inorganic fillers, and t . P. The composition of the present invention includes a poly-4-methylpentene-1 and an olefin oligomer and can be obtained by melting in a melt, for example, at 240-260 ° C of two components in a roller mill or in a Banbury mixer, KOTOfftje is usually used in rubber or plastic industry . Since Tei epaTypa melts poly-4-metsh1pentena-1 above,. mixing is carried out without air flow in order to prevent deterioration of the properties of these two components during mixing. According to the method of preparing the proposed composition, poly-4-methylpentene-1 granules are mixed, for example, at 4liOO-200 C, preferably at 150-200 seconds, with an olefin oligomer in a high-speed mixer — for example, in a Henshel mixer. at high speed t, for example, at the peripheral speed of rotating blades, equal to 40-100 m / s. 1 is easily impregnated with an olefin oligomer and, therefore, a composition in the form of granules can be obtained below the melting point. poly-4-methylpentene-1 and in the confluence of a short time, for example at 20-70. C for 30-60 min. The composition thus obtained in the form of granules can be directly fed into an extruder with the formation of an extruder. The composition of the invention, which contains flame retarder, antioxidant, metal deactivator, filler and other compounding additives (hereinafter, all these compounding additives will be. referred to as compounding pr (isadki) can be obtained by mixing additives with granules of poly-4-methylpentene-1, impregnation (sown with olefin oligomer described above, or mixing additives, poly-4-methylpentene-1 and olefin oligomer in such an oI mixer, like a roller mill, a Banbury mixer, or an extruder mixer, at the melting point of poly-4-methylpentane 1. Since the mixing temperature is high, the mixing is preferably carried out without air in order to oxidize the mixed components to a minimum. Pryg Mayor Mixer for impl. This mixing can be done by a mixer-extruder. If the compounding additives added to the mixture have a lower TeNmepaTypy melting than the poly-4-methylpentene-1 is preferred. The high-speed mixer of the Heshael type of mixer is used in order to ensure the penetration and mixing of the additive with poly-4-metsh1pentena-1 granules. The mixing ratio of the compounding additive to the polymer material is 1500 wt. h or less compounding additive per 100 weight. h polymeric material, and the amount of polymeric material embedded S composition is 30 weight. h or less, preferably 15 wt. h or less, per 100 weight. h poly-4-methylpentene-1, Beli uses more than 30 weight. h The amount of polymer material has a detrimental effect on excellent spatial. poly-4methylpentene-1 stability. In order to facilitate the agglomeration of the polymeric material with the compounding additive, and in order to obtain the oyster dispersion of the compounding compound in the polymeric material, it is preferred to use 200-800 weight. h compounding additive for 100. weight. h polymeric material. In order to obtain the proposed composition using a polymeric material, the whole olefinic scigomer to be used can be mixed, for example, at 80-180 ° C, preferably, at 100-140 ° C, with a compounding additive and a polymeric material, and the mixture thus obtained these three components can then be mixed with poly-1-methylpentane-1. On the other hand, the oligomer. can be divided into two parts, one of which is mixed with poly-4-methylpentane-1, and the other is mixed with a mixture of compounding-additive and polymeric material. To achieve such results, any method similar to that described above can be used, according to which the entire amount of olefin oligomer is initially mixed with poly-4-methylpentane-1. A composition comprising poly-4-methylpentene-1 and an olefin oligomer has various advantages. The composition of the invention can be easily manufactured using conventional mixing devices such as an extruder mixer. Using a high-speed blender such as an X-nshel mixer that does not melt poly-4-methylpentene-1 simplifies processing. A high-speed mixer also provides a high-quality product, since low-temperature mixing can be carried out and, as a result, no oxidative deterioration occurs. The proposed composition maintains excellent spatial stability. poly 4-methylpentene-1. In addition, such a composition has sufficient flexibility not only at ordinary temperature, but also at a lower temperature, which allows the composition to be used as an electronic-insulating material. A low molecular weight material mixed with a high molecular weight material is often colored to the surface, but the degree of fading of the olefin oligomer used in the proposed composition is extremely low. This phenomenon is unexpected and has industrial advantages. Poly-4-methylpentene-1 is a hot substance and has relatively low sensitivity to aging and the effects of heavy metals. Such disadvantages of poly-4-methylpentene-1 can be eliminated from the composition in which the appropriate compounding agent can be administered, preferably flame retardant. A composition containing a compounding additive is free from the disadvantages of poly-4-methylpentene-1 and still retains the excellent spatial stability inherent in this substance. If the compound; the additive is a flame retardant, then the stability and flexibility of the composition at low temperatures (e.g., 10-30 ° C) is surprisingly improved compared to the case where the flame retarder is not used. The composition of the invention maintains the excellent spatial stability of poly-4-methylpentene-1 and makes it highly flexible at low temperatures. Thus, the composition can be used as a variety of forming materials. Due to the excellent. the dielectric properties of the composition can be successfully used as an insulating material for electrically conducting wire. The flame retardant composition of the present invention is a Sch1c1m retarding composition with good mechanical properties at temperatures, lying in the range from normal to high temperatures and also has excellent flexibility at low temperatures. Therefore, such a composition can be used as an insulating material, dp electric wires, cut materials used for. interior and exterior surfaces of buildings, or for flame retardant tubes, sheets or tapes. In tab. 1 shows examples of the compositions according to the present invention (1-17) and comparative examples (1-4). Each of the compositions was transferred in a 5-liter Henshel mixer at a stirrer rotation speed of 2,000 rpm for 30 minutes at a temperature in the mixing bath lying in the inter-. shaft 150-200 C. The mixture thus obtained in the form of granules is loaded into a Brabender extruder having a clear diameter of 20 mm at 250-10 ° C to obtain thin sheets with a thickness of 0.5 mm. In each of the examples, the layered material formed by the plurality of sheets thus obtained is subjected to pressure molding at a pressure of 100 kg / cm for 10 minutes. Temperature impact brittleness, elongation at break, and oxygen index of the formed laminate are measured according to I / S K 6760 5. 4, 1 / S 6301 and ASTMO 2863-70, respectively. In comparative example 1, as well as in examples 12, 14 and 16, the laminated material formed under pressure is cut into strips with a size of 15 mm Y x XO mm. Copper plate 0.5 mm thick, 13 mm wide and 90 mm long (cleaned according to ASTM D 1934-68,5. 3) placed between two such strips. The copper plate and strips are placed between two clean glass plates with a thickness of 2 mm, a width of 16 mm and a length of 100 mm, clamped at both ends, left to stand for 4 days in a bath, through which air is circulated at a constant temperature equal to and after aging, the elongation at break is measured. In addition, some of the pressure molded laminates of Comparative Examples 1-4, Examples 1, 2, 3, 4, 5, 7, 8, 12, 13, and 16 are left to stand at room temperature (about 15-30 ° C) at 6 months and after standing at co HaTJioA temperature, the temperature of impact embrittlement is measured. The results are shown in Table. one. In tab. Figure 2 shows the characteristics of the composition obtained in Comparative Examples 1-44. The composition obtained according to comparative example 4 was so brittle that it was. properties could not be estimated. Poly-4-methylpentene-1 (A) has an average particle size of 3-5 mm, melt index (, load 5 kg) 26 g / 10 min, density (23 ° С) 0.840 g / cm, characteristic absorption bands in IR - areas of 720 cm 790, 849, 870, 917, 993, 1127, 1195, 1230, 1269, 1363, 1437 and 1740. Poly-4-methylpentene-1 (B) has an average particle size of 3-5 mm, melt index (, load 5 kg) 26 g / 10 min, density () 0.830 g / cm. Characteristic absorption bands in the IR region 790 849, 870, 917 993, 1127, 1195, 1230, 1269, 1363 and 1437. Poly-4-methylpentene-1 (C) has an average particle size of 3-5 mm, melt index (, loading 5 kg) 12 g / 10 min, density () 0.840 g / cm, characteristic absorption bands in the IR region 720 cm 790, 849, 870, 917, 993, 1127, 1195, 1230, 1269, 1437 and 1740. Alpha-olefin oligomer. A to E are olefinic oligomers of the formula -1-SnClN At 1 "in which R represents an alkyl group having 8 carbon atoms, average molecular weight and bromine number (. Br is a number) each of the oligomers is presented below (A) mol. , Br is a number equal to 0.5 (B) mol. , Br is a number equal to 0.4 (C) mol. , Br is a number equal to 0.4 (0) mol. , Br number equal to 2.5 (E) mol. , Br is a number equal to 1.5. G-1 is polybutene or consists of a mixture of butene isomers, the main component of which is isobutene of the following formula: Trade name, average molecular weight and bromine number V g (10 O g) of each of the products are given below (D) mol . , Br is a number equal to 0.5 (C) mol. , Br is a number equal to 1.0 (n) mol. , Br is a number equal to 30 ()), they say, Br is a number equal to 8.0. Antioxidants. Tetrakis (methylene -3) 3,5-di-tert-butyl-1-hydroxyphenyl (propionate methane (A). 4,4-Butylidene-bis (3-methyl-6-tert.-butylphenol) (B). 1 Dilauryl thiodipropionate (C). HMOOF (0). Metal deactivator. 3 (M-Salicyolol) amino-1,2,4-triazole. Polymer material. Ethylenebutene-1-copolymer (A) melt index (190 ° C, loading 2.6 kg) 20 g / 10 min, density () 0.89 g / cm. Low density polyethylene (c) melt index (, load 2.6 kg) 10 g / 10 min, density () 0.923 g / cm. Ethylene-propylene copolymer (C) (ED-07P), Moops viscosity () 70, density (23 ° О 0.865 g / cm) Examples 18-20. Polymeric materials listed in table. 1, are thoroughly mixed with flame retardants, antioxidants, and a metal deactivator for 20 minutes at the ratios indicated in Table. 1 ;, in a roller mill, the temperature of which is maintained at the same level — 12P C. The resulting sheets are formed into granules with a size of 2-p5 mm. Such granules and the granules obtained in Example 2 are mixed in predetermined ratios using a Henschel mixer. in a Brabender extruder of the same type as described above (temperature 250-10 C), from which the mixture is extruded in the form of sheets with a thickness of 0.5 mm. The sheets thus obtained are molded under pressure in the same manner as used in Example 1 and in other examples. Then, their temperature of impact embrittlement, elongation at break and oxygen index are measured. The results of these measurements are given in table. 3 The extrudate obtained in examples 18-20 has a smooth surface.
Examples 22, 24, 25 and 26 illustrate the use of an olefin oligomer in an amount of 25 parts by weight. per 100 weight hours | poly-4-methylpentene-1 (PMP). Examples 23g 24 and 26 show the use of a new olefinic oligo “pa I, having an average mol. weight 980 and bromine number 0.3 and corresponding to the general formula
4-Sn, -sn4t
R b
where R is an alkyl radical HIB.
From the results, it can be seen that each composition shown in the examples
It has the best data on testing 5 temperature {ml, brittleness upon impact, elongation at paatXiBe and so on compared with physical properties ({compositions of the compositions described in comparative examples 1-4. 10B of table 4)
obtained in examples 21-26,
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Claims of Composition Based on poly-4-methylpentene-1 containing polymeric up to-65
Table 3
Table 4
100
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-18
-20
-24 400 430 450 25 24 cans, characterized in order. that, in order to improve the physicomechanical properties, it contains, as a polymer additive, an olefinic oligomer of the general formula KI I with -CHG-41 / where V RJ. - al kil with Cj or C, while with C | weight: 570-2,200; at S. ,, mol.ves.980; 95322 or. P and R - CHV, while mol. Ee, 510-1350 in the amount of 5-25 weight.h. per 100 weight.h, poly-4-methylpentene-1. 5 Sources of information taken into account in the examination of US Patent 3,865,877, cl. 260-827, published. 1974 ..

权利要求:
Claims (1)
[1]
<claim-text> Formula of the invention </ claim-text> </ td> <td></ td> <td><claim-text> bavku, </ claim-text> </ td> <td><claim-text> ex </ claim-text> </ td> <td><claim-text> h and y n </ claim-text> </ td> <td><claim-text> and I am, </ claim-text> </ td> </ tr><tr> <td colspan = "2"><claim-text> Poly composition - </ claim-text> </ td> <td><claim-text> 4-methyl - </ claim-text> </ td> <td><claim-text> what, with </ claim-text> </ td> <td colspan = "2"><claim-text> goal of improvement </ claim-text> </ td> <td><claim-text> physical furs - </ claim-text> </ td> </ tr></ tbody> </ table><claim-text> pentena-1, containing polymeric dong 65 properties, it contains in ca21 </ claim-text><claim-text> 991953 </ claim-text><claim-text> 22 </ claim-text><claim-text> the quality of the polymer additive is an olefinic oligomer of the general formula </ claim-text><claim-text> sn * </ claim-text><claim-text> " K" / (i where -H;. · </ claim-text><claim-text> - alkyl with C ^ or with C | mol. weight = 570-2200 mol. weight. = 980; </ claim-text><claim-text> 5 </ claim-text><claim-text> C <sub> 411 </ sub>, with C, <sub> r </ sub> </ claim-text><claim-text> or. ^ and - CH-, while mol. les. = 510-1350 </ claim-text><claim-text> in the amount of 5-25 weight.h. per 100 weight parts poly-4-methylpentene-1. </ claim-text><claim-text> Sources of information taken into account in the examination </ claim-text><claim-text> 1. U.S. Patent No. 3865877, </ claim-text><claim-text> cl. 260-827, published. 1974, </ claim-text>

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同族专利:

公开号 | 公开日

US4166057A|1979-08-28|

CA1120637A|1982-03-23|

JPS5414454A|1979-02-02|

BR7804272A|1979-04-17|

GB2002000B|1982-01-27|

GB2002000A|1979-02-14|

FR2396782B1|1983-11-25|

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法律状态:

优先权:

申请号 | 申请日 | 专利标题

JP52080567A|JPS5846142B2|1977-07-05|1977-07-05|

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