CN109776888A - A kind of ultralow temperature shrinks thermal contraction casing tube and preparation method thereof - Google Patents
A kind of ultralow temperature shrinks thermal contraction casing tube and preparation method thereof Download PDFInfo
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- CN109776888A CN109776888A CN201910065805.7A CN201910065805A CN109776888A CN 109776888 A CN109776888 A CN 109776888A CN 201910065805 A CN201910065805 A CN 201910065805A CN 109776888 A CN109776888 A CN 109776888A
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- 230000008602 contraction Effects 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 53
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 53
- 238000004381 surface treatment Methods 0.000 claims abstract description 42
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims abstract description 34
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 33
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims abstract description 33
- 239000000347 magnesium hydroxide Substances 0.000 claims abstract description 33
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims abstract description 33
- 239000003063 flame retardant Substances 0.000 claims abstract description 27
- 239000002994 raw material Substances 0.000 claims abstract description 23
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 22
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 19
- 239000000314 lubricant Substances 0.000 claims abstract description 19
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims abstract description 19
- 239000005038 ethylene vinyl acetate Substances 0.000 claims abstract description 18
- 239000000899 Gutta-Percha Substances 0.000 claims abstract description 17
- 240000000342 Palaquium gutta Species 0.000 claims abstract description 17
- 206010070834 Sensitisation Diseases 0.000 claims abstract description 17
- 229920000588 gutta-percha Polymers 0.000 claims abstract description 17
- 230000008313 sensitization Effects 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 239000006229 carbon black Substances 0.000 claims abstract description 14
- 238000005453 pelletization Methods 0.000 claims abstract description 14
- 238000001125 extrusion Methods 0.000 claims abstract description 11
- 238000004132 cross linking Methods 0.000 claims abstract description 9
- 230000005855 radiation Effects 0.000 claims abstract description 8
- 238000004513 sizing Methods 0.000 claims abstract description 4
- 239000002253 acid Substances 0.000 claims description 14
- -1 β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid octadecanol ester Chemical class 0.000 claims description 13
- 150000004982 aromatic amines Chemical class 0.000 claims description 12
- 150000002989 phenols Chemical class 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- 150000002148 esters Chemical class 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- 239000001301 oxygen Substances 0.000 claims description 11
- 230000000694 effects Effects 0.000 claims description 9
- 229920001195 polyisoprene Polymers 0.000 claims description 8
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 7
- 230000001133 acceleration Effects 0.000 claims description 6
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 5
- 229920000642 polymer Polymers 0.000 claims description 5
- OKKRPWIIYQTPQF-UHFFFAOYSA-N Trimethylolpropane trimethacrylate Chemical group CC(=C)C(=O)OCC(CC)(COC(=O)C(C)=C)COC(=O)C(C)=C OKKRPWIIYQTPQF-UHFFFAOYSA-N 0.000 claims description 4
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical group [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 4
- KOMNUTZXSVSERR-UHFFFAOYSA-N 1,3,5-tris(prop-2-enyl)-1,3,5-triazinane-2,4,6-trione Chemical compound C=CCN1C(=O)N(CC=C)C(=O)N(CC=C)C1=O KOMNUTZXSVSERR-UHFFFAOYSA-N 0.000 claims description 3
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- KWUZCAVKPCRJPO-UHFFFAOYSA-N n-ethyl-4-(6-methyl-1,3-benzothiazol-2-yl)aniline Chemical compound C1=CC(NCC)=CC=C1C1=NC2=CC=C(C)C=C2S1 KWUZCAVKPCRJPO-UHFFFAOYSA-N 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 claims description 3
- LQZZUXJYWNFBMV-UHFFFAOYSA-N 1-dodecanol group Chemical class C(CCCCCCCCCCC)O LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims description 2
- 239000003292 glue Substances 0.000 claims description 2
- 229910052736 halogen Inorganic materials 0.000 claims description 2
- 150000002367 halogens Chemical class 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 2
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical class CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 claims description 2
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 claims 1
- 229910052782 aluminium Inorganic materials 0.000 claims 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims 1
- 239000004411 aluminium Substances 0.000 claims 1
- QICVZJNIJUZAGZ-UHFFFAOYSA-N benzene;phosphorous acid Chemical compound OP(O)O.C1=CC=CC=C1 QICVZJNIJUZAGZ-UHFFFAOYSA-N 0.000 claims 1
- DQXBYHZEEUGOBF-UHFFFAOYSA-N but-3-enoic acid;ethene Chemical compound C=C.OC(=O)CC=C DQXBYHZEEUGOBF-UHFFFAOYSA-N 0.000 claims 1
- 235000010354 butylated hydroxytoluene Nutrition 0.000 claims 1
- 229920001577 copolymer Polymers 0.000 claims 1
- 150000003568 thioethers Chemical class 0.000 claims 1
- 239000000052 vinegar Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 6
- 230000032683 aging Effects 0.000 abstract description 5
- 230000018109 developmental process Effects 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000013329 compounding Methods 0.000 abstract description 3
- 235000012254 magnesium hydroxide Nutrition 0.000 description 27
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000008188 pellet Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 230000004913 activation Effects 0.000 description 3
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical class C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- UDFARPRXWMDFQU-UHFFFAOYSA-N 2,6-ditert-butyl-4-[(3,5-ditert-butyl-4-hydroxyphenyl)methylsulfanylmethyl]phenol Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CSCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 UDFARPRXWMDFQU-UHFFFAOYSA-N 0.000 description 2
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 230000003679 aging effect Effects 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 230000006870 function Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- VCAFTIGPOYBOIC-UHFFFAOYSA-N phenyl dihydrogen phosphite Chemical class OP(O)OC1=CC=CC=C1 VCAFTIGPOYBOIC-UHFFFAOYSA-N 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 230000006399 behavior Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- 150000005690 diesters Chemical class 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000006353 environmental stress Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000004079 fireproofing Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 125000001972 isopentyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])C([H])([H])* 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 230000006386 memory function Effects 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 238000007348 radical reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention relates to a kind of ultralow temperature to shrink thermal contraction casing tube and preparation method thereof, belongs to sleeve technology field.The raw material that the ultralow temperature shrinks thermal contraction casing tube includes synthetic guttapercha, ethylene-vinyl acetate copolymer, the active magnesium hydroxide of ultra-fine surface treatment, ultra-fine surface treatment active aluminium hydroxide, expanding halide-free fire-retardant, lubricant, antioxidant, sensitization crosslinking agent and carbon black.Above-mentioned ultralow temperature shrinks thermal contraction casing tube halogen-free flameproof, has preferable mechanics and heat aging performance, while realizing 85 DEG C of low temperature and shrinking completely, has expanded heat-shrink tube product in the application and development of civil field.Preparation method is including compounding raw materials according to the ratio and is granulated, and water cooling conveying, pelletizing obtain masterbatch；Then masterbatch is extruded into tubing；By the tubing crosslinking with radiation after extrusion；Then expansion, cooling, sizing.This method is easy to operate, is suitable for industrialized production.
Description
Technical field
The present invention relates to sleeve technology fields, and in particular to a kind of ultralow temperature shrinks thermal contraction casing tube and its preparation side
Method.
Background technique
Heat-shrinkable T bush is typically the irradiated crosslinked polyalkene material of shape memory function, has good insulated enclosure
Function is widely used in the fields such as automobile, high-speed rail, military affairs, aviation, electronics, electric power, with the promotion of awareness of safety, heat-shrink tube
It may be equally applicable for the protection of domestic electric appliances etc., but the general complete shrinkage temperature of heat-shrink tube needs at least at 110 DEG C or more
Special pucker tool, such as air gun, spray gun, baking oven could be shunk completely, to limit heat-shrink tube in certain domestic environments
Application.
Summary of the invention
The purpose of the present invention is to provide a kind of ultralow temperature shrink thermal contraction casing tube, the ultralow temperature shrink thermal contraction casing tube without
Halogen is fire-retardant, has preferable mechanics and heat aging performance, while realizing 85 DEG C of low temperature and shrinking completely, has expanded heat-shrink tube product
In the application and development of civil field.
The second object of the present invention is to provide a kind of preparation method of above-mentioned ultralow temperature contraction thermal contraction casing tube, this method
It is easy to operate, it is suitable for industrialized production.
The present invention solves its technical problem and adopts the following technical solutions to realize:
The present invention proposes that a kind of ultralow temperature shrinks thermal contraction casing tube, and according to parts by weight, ultralow temperature shrinks thermal contraction casing tube
Raw material include the synthetic guttapercha of 20-50 parts by weight, the ethylene-vinyl acetate copolymer of 10-30 parts by weight, 0-20 weight
Ultra-fine surface treatment activity magnesium hydroxide, the ultra-fine surface treatment active aluminium hydroxide of 5-20 parts by weight, 10-20 parts by weight of part
Expanding halide-free fire-retardant, the lubricant of 0.1-2 parts by weight, the antioxidant of 0.1-2 parts by weight, 0.5-2 parts by weight sensitization
The carbon black of crosslinking agent and 0.5-5 parts by weight.
The present invention also proposes that a kind of above-mentioned ultralow temperature shrinks the preparation method of thermal contraction casing tube, comprising the following steps:
It prepares masterbatch: compounding raw materials and being granulated according to the ratio, water cooling conveying, pelletizing obtain masterbatch；
It squeezes out: masterbatch being extruded into tubing under conditions of 80-100 DEG C；
Irradiation: by the tubing after extrusion be 2.0MeV in electronics acceleration energy and irradiation dose is 5.0Mrad-
Crosslinking with radiation under conditions of 10.0Mrad；
Expansion: the tubing after irradiation is expanded 1.5-3 times under conditions of 150-200 DEG C, cooling, sizing.
The beneficial effect that ultralow temperature provided by the present application shrinks thermal contraction casing tube and preparation method thereof includes:
Ultralow temperature provided by the present application shrinks thermal contraction casing tube halogen-free flameproof, has preferable mechanics and heat aging performance,
It realizes 85 DEG C of low temperature simultaneously to shrink completely, has expanded heat-shrink tube product in the application and development of civil field.Preparation method behaviour
Make simply, to be suitable for industrialized production.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Thermal contraction casing tube and preparation method thereof is shunk to the ultralow temperature of the application below to be specifically described.
Ultralow temperature involved in the application shrinks thermal contraction casing tube, and according to parts by weight, raw material includes 20-50 parts by weight
Synthetic guttapercha, the ethylene-vinyl acetate copolymers of 10-30 parts by weight, 0-20 parts by weight ultra-fine surface treatment activity
Magnesium hydroxide, the ultra-fine surface treatment active aluminium hydroxide of 5-20 parts by weight, 10-20 parts by weight expanding halide-free fire-retardant,
The lubricant of 0.1-2 parts by weight, the antioxidant of 0.1-2 parts by weight, the sensitization crosslinking agent of 0.5-2 parts by weight and 0.5-5 weight
The carbon black of part.
Optionally, the parts by weight of synthetic guttapercha for example can be 20,30,40 or 50 etc., or 25,35
Or 45 etc., it can also be other any parts by weight numerical value within the scope of 20-50.
The parts by weight of ethylene-vinyl acetate copolymer for example can be 10,20 or 30 etc., or 15 or 25
Deng can also be other any parts by weight numerical value within the scope of 10-30.
The ultra-fine parts by weight for being surface-treated active magnesium hydroxide can be 0,5,10,15 or 20 etc., or 0-20
Other any parts by weight numerical value in range.It is worth noting that representing ultralow temperature when parts by weight are 0 and shrinking thermal contraction
Without the active magnesium hydroxide of ultra-fine surface treatment in the raw material of casing.
The parts by weight of ultra-fine surface treatment active aluminium hydroxide can be 5,10,15 or 20, or 5-20 range
Interior other any parts by weight numerical value.
The parts by weight of expanding halide-free fire-retardant can be 10,15 or 20 etc., can also be other within the scope of 10-20
Any parts by weight numerical value.
The parts by weight of lubricant and antioxidant can be respectively 0.1,0.5,1,1.5 or 2 etc., can also be 0.1-2
Other any parts by weight numerical value in range.
The parts by weight for being sensitized crosslinking agent can be 0.5,1,1.5 or 2 etc., can also be other within the scope of 0.5-2
One parts by weight numerical value.
The parts by weight of carbon black can be 1,2,3,4 or 5 etc., or 0.5,1.5,2.5,3.5 or 4.5 etc., may be used also
Think other any parts by weight numerical value within the scope of 0.5-5.
It is worth noting that above-mentioned each substance can carry out freely in above-mentioned respective range in practical blending process
Combination.
In some embodiments, ultralow temperature shrinks the synthesis that the raw material of thermal contraction casing tube may include 30-40 parts by weight
Gutta-percha, the ethylene-vinyl acetate copolymer of 15-25 parts by weight, 5-15 parts by weight ultra-fine surface treatment activity hydroxide
Ultra-fine surface treatment active aluminium hydroxide, the expanding halide-free fire-retardant of 12-18 parts by weight, 0.5- of magnesium, 10-15 parts by weight
The lubricant of 1.5 parts by weight, the antioxidant of 0.5-1.5 parts by weight, the sensitization crosslinking agent of 1-1.5 parts by weight and 2-4 parts by weight
Carbon black.
In other embodiments, ultralow temperature shrinks synthesis Du that the raw material of thermal contraction casing tube may include 35 parts by weight
Secondary glue, the ethylene-vinyl acetate copolymer of 20 parts by weight, the ultra-fine surface treatment activity magnesium hydroxide of 10 parts by weight, 12.5
The ultra-fine surface treatment active aluminium hydroxide of parts by weight, the expanding halide-free fire-retardant of 15 parts by weight, the lubricant of 1 parts by weight, 1
The antioxidant of parts by weight, the sensitization crosslinking agent of 1.2 parts by weight and the carbon black of 3 parts by weight.
Wherein, synthetic guttapercha is anti-form-1,4- polyisoprene.In some embodiments, anti-form-1, the poly- isoamyl of 4-
The trans content of diene is not less than 95wt%, and 100 DEG C of mooney viscosity ML (3+4) are 40-60, and gel content is no more than 3wt%.On
Preferably processing performance and cryogenic property can be had by stating the trans-1,4-iroprene polymer under parameter.
Vinyl acetate content in ethylene-vinyl acetate copolymer for example can be 15-30wt%, as 15wt%,
20wt%, 25wt% or 30wt% etc., melt index 4-10g/10min, such as 4g/10min, 5g/10min, 8g/10min or
10g/10min etc..By the preparation for shrinking thermal contraction casing tube using ethylene-vinyl acetate copolymer as ultralow temperature in the application
One of raw material is conducive to improve processability and environmental stress crack resistance of ultralow temperature contraction thermal contraction casing tube etc..
Ultra-fine surface treatment active aluminium hydroxide and the active magnesium hydroxide of ultra-fine surface treatment divide equally other surface treated agent
Gained after activation processing, surface treating agent for example can be distearyl oxygen isopropoxy Aluminate.
In some embodiments, the dosage of surface treating agent can be aluminium hydroxide or the 0.5- of magnesium hydroxide weight
3wt%, such as 0.5wt%, 1wt%, 1.5wt%, 2wt%, 2.5wt% or 3wt%.
Preferably, ultra-fine surface treatment active aluminium hydroxide and the ultra-fine partial size for being surface-treated active magnesium hydroxide can be with
For 4500-5500 mesh, preferably 5000 mesh.Aluminium hydroxide and magnesium hydroxide are subjected to micronization processes, fineness height, grain can be obtained
The material of diameter narrowly distributing makes it have fire-retardant and filling dual property.
Above-mentioned ultra-fine surface treatment active aluminium hydroxide and the active magnesium hydroxide of ultra-fine surface treatment are in this application
As filler, aluminium hydroxide and magnesium hydroxide are passed through into the clad ratio that the two can be improved in surface treating agent processing respectively, significantly mentioned
The filling capacity of high aluminium hydroxide and magnesium hydroxide promotes the wetting and dispersing of aluminium hydroxide and magnesium hydroxide in organic polymer
Property, the compatibility and binding force of enhancing and high polymer base-material improve the mechanical property of composite material.
It is worth noting that aluminium hydroxide can be improved using distearyl acyl-oxygen aluminum isopropoxide acid esters as surface treating agent
Or cohesive force and interface affinity between magnesium hydroxide and polymer, the fire-retardant of thermal contraction casing tube is shunk conducive to ultralow temperature is improved
Property, heat resistance, moisture resistance and mechanical strength etc..
Optionally, the expanding halide-free fire-retardant in the application is using phosphorus and nitrogen as the halogen-free environmental protection of ignition-proof element
Type fire retardant, contained by ignition-proof element there is synergistic function at fire-retardant aspect, the addition of nitrogen can be improved phosphorus system
The thermal stability of fire retardant overcomes facile hydrolysis and the raw smoke of reduction etc., has good thermal stability, water-soluble small, resistance
Consistency of performance is fired, while the shortcomings that small molecule phosphorus flame retardant is with by fire proofing poor compatibility can be overcome.
In some embodiments, the partial size of expanding halide-free fire-retardant is preferably more than 8 μm, and pH value for example can be
6.0-6.8。
Lubricant for example can be zinc stearate or stearic acid, to improve the processability that ultralow temperature shrinks thermal contraction casing tube
Energy.
Antioxidant for example may include Hinered phenols antioxidant, aromatic amine antioxidant and auxiliary antioxidant.In some realities
It applies in mode, the mass ratio of Hinered phenols antioxidant, aromatic amine antioxidant and auxiliary antioxidant can be such as 1-2:1-2:
1-3。
Optionally, above-mentioned Hinered phenols antioxidant for example may include 2,6- di-tert-butyl-4-methy phenol, it is double
In (3,5- di-tert-butyl-4-hydroxyl benzyl) thioether and β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid octadecanol ester
It is at least one；Aromatic amine antioxidant for example can be 4,4 '-bis- (bis (alpha, alpha-dimethylbenzyl) base) diphenylamines；Auxiliary antioxidant is for example
It may include three (2,4- di-t-butyl) at least one of phenyl-phosphites and thio-2 acid dibasic acid esters.Wherein, thio dipropyl
Acid diester may include double Lauryl Alcohol esters, bi-myristoleyl or double octadecanol esters.
Being sensitized crosslinking agent for example can be trimethylolpropane trimethacrylate or Triallyl isocyanurate.Sensitization is handed over
Join the unsaturated structure that agent has polyfunctional monomer, is radical reaction in irradiation processing, then carries out monomer radical
With the graft crosslinking of base resin.
It holds, the application is by preparing raw material, energy collectively as ultralow temperature contraction thermal contraction casing tube for above-mentioned each substance
It enough realizes halogen-free flameproof, ultralow temperature is made to shrink thermal contraction casing tube with preferable mechanical property and while heat aging performance,
The complete contraction being also able to achieve under 85 DEG C of cryogenic conditions.
In addition, present invention also provides a kind of above-mentioned ultralow temperature to shrink the preparation method of thermal contraction casing tube, such as can wrap
Include following steps:
It prepares masterbatch: compounding raw materials and being granulated according to the ratio, water cooling conveying, pelletizing obtain masterbatch.
It squeezes out: masterbatch being extruded into tubing under conditions of 80-100 DEG C.
Irradiation: by the tubing after extrusion be 2.0MeV in electronics acceleration energy and irradiation dose is 5.0Mrad-
Crosslinking with radiation under conditions of 10.0Mrad.
Expansion: the tubing after irradiation is expanded 1.5-3 times under conditions of 150-200 DEG C, cooling, sizing.
In some embodiments, above-mentioned mixing includes being kneaded to be kneaded with second for the first time, and being kneaded for the first time is in 90-
20min is carried out under conditions of 110 DEG C in mixer, it is under conditions of 100-120 DEG C in twin-screw extrusion that second, which is kneaded,
It is carried out in pelletizer.
In some embodiments, water cooling conveying is to be mounted on double spiral shells by the way that the material after being kneaded in pelletizer to be input to
It is carried out in underwater pellet cutting system after bar extruding granulator, water tank water temperature for example can be 30-60 DEG C.
Optionally, masterbatch is extruded into tubing and can be after masterbatch removal moisture drying, in single spiral shell equipped with mouth mold, plug
It is carried out on bar extruder.Crosslinking with radiation can carry out in electron accelerator, expansion can in Cylinder vacuum expansion device into
Row.
It holds, the ultralow temperature as made from above-mentioned preparation method, which shrinks thermal contraction casing tube, has preferable mechanics and heat aging
Can, while realizing 85 DEG C of low temperature and shrinking completely, heat-shrink tube product has been expanded in the application and development of civil field.
Feature and performance of the invention are described in further detail with reference to embodiments.
Embodiment 1
The present embodiment provides a kind of ultralow temperature to shrink thermal contraction casing tube, and according to parts by weight, which, which shrinks, is heat-shrinked
The raw material of casing includes the synthetic guttapercha of 20 parts by weight, the ethylene-vinyl acetate copolymer of 10 parts by weight, 5 parts by weight
Ultra-fine surface treatment active aluminium hydroxide, the expanding halide-free fire-retardant of 10 parts by weight, the lubricant of 0.1 parts by weight, 0.1 weight
The antioxidant, the sensitization crosslinking agent of 0.5 parts by weight and the carbon black of 0.5 parts by weight of part.
Wherein, synthetic guttapercha is anti-form-1,4- polyisoprene, the anti-form-1, the trans content of 4- polyisoprene
For 95wt%, 100 DEG C of mooney viscosity ML (3+4) are 40, gel content 3wt%.
Vinyl acetate content in ethylene-vinyl acetate copolymer is 15wt%, melt index 4g/10min.
The active magnesium hydroxide of ultra-fine surface treatment gained after distearyl acyl-oxygen aluminum isopropoxide acid esters activation processing, two is hard
The dosage of acyl oxygen isopropoxy Aluminate is the 0.5wt% of magnesium hydroxide weight.The ultra-fine active magnesium hydroxide of surface treatment
Partial size is 4500 mesh.
The partial size of expanding halide-free fire-retardant is 8 μm, pH value 6.0.Lubricant is zinc stearate.Antioxidant contains quality
Than Hinered phenols antioxidant, aromatic amine antioxidant and the auxiliary antioxidant for 1:1:1.Hinered phenols antioxidant is bis- uncle of 2,6-
Butyl -4- methylphenol；Aromatic amine antioxidant is 4,4 '-bis- (bis (alpha, alpha-dimethylbenzyl) base) diphenylamines；Auxiliary antioxidant is three
(2,4- di-t-butyl) phenyl-phosphite.Sensitization crosslinking agent is trimethylolpropane trimethacrylate.
Embodiment 2
Ultralow temperature provided in this embodiment shrink thermal contraction casing tube the difference from embodiment 1 is that:
According to parts by weight, the raw material which shrinks thermal contraction casing tube includes the synthetic guttapercha of 50 parts by weight, 30
The ethylene-vinyl acetate copolymer of parts by weight, the ultra-fine surface treatment activity magnesium hydroxide of 20 parts by weight, 20 parts by weight it is super
Thin surface treatment active aluminium hydroxide, the expanding halide-free fire-retardant of 20 parts by weight, the lubricant of 2 parts by weight, 2 parts by weight it is anti-
Oxygen agent, the sensitization crosslinking agent of 2 parts by weight and the carbon black of 5 parts by weight.
Wherein, ultra-fine surface treatment active aluminium hydroxide is also after distearyl acyl-oxygen aluminum isopropoxide acid esters activation processing
Gained, the dosage of distearyl acyl-oxygen aluminum isopropoxide acid esters are the 0.5wt% of aluminium hydroxide weight.Ultra-fine surface treatment reactive hydrogen
The partial size of magnesia is 4500 mesh.
Embodiment 3
Ultralow temperature provided in this embodiment shrink thermal contraction casing tube the difference from example 2 is that:
According to parts by weight, the raw material which shrinks thermal contraction casing tube includes the synthetic guttapercha of 30 parts by weight, 25
The ethylene-vinyl acetate copolymer of parts by weight, the ultra-fine surface treatment activity magnesium hydroxide of 5 parts by weight, 15 parts by weight it is super
Thin surface treatment active aluminium hydroxide, the expanding halide-free fire-retardant of 12 parts by weight, the lubricant of 1.5 parts by weight, 0.5 parts by weight
Antioxidant, 1.5 parts by weight sensitization crosslinking agent and 2 parts by weight carbon black.
Embodiment 4
Ultralow temperature provided in this embodiment shrink thermal contraction casing tube the difference from example 2 is that:
According to parts by weight, the raw material which shrinks thermal contraction casing tube includes the synthetic guttapercha of 40 parts by weight, 15
The ethylene-vinyl acetate copolymer of parts by weight, the ultra-fine surface treatment activity magnesium hydroxide of 15 parts by weight, 10 parts by weight it is super
Thin surface treatment active aluminium hydroxide, the expanding halide-free fire-retardant of 18 parts by weight, the lubricant of 0.5 parts by weight, 1.5 parts by weight
Antioxidant, 1 parts by weight sensitization crosslinking agent and 4 parts by weight carbon black.
Embodiment 5
Ultralow temperature provided in this embodiment shrink thermal contraction casing tube the difference from example 2 is that:
According to parts by weight, the raw material which shrinks thermal contraction casing tube includes the synthetic guttapercha of 35 parts by weight, 20
The ethylene-vinyl acetate copolymer of parts by weight, the ultra-fine surface treatment activity magnesium hydroxides of 10 parts by weight, 12.5 parts by weight
Ultra-fine surface treatment active aluminium hydroxide, the expanding halide-free fire-retardant of 15 parts by weight, the lubricants of 1 parts by weight, 1 parts by weight
Antioxidant, the sensitization crosslinking agent of 1.2 parts by weight and the carbon black of 3 parts by weight.
Embodiment 6
Ultralow temperature provided in this embodiment shrink thermal contraction casing tube the difference from example 2 is that:
Synthetic guttapercha is anti-form-1, and the trans content of 4- polyisoprene, the anti-form-1,4- polyisoprene is
100 DEG C of 98wt%, mooney viscosity ML (3+4) are 50, gel content 2wt%.
Vinyl acetate content in ethylene-vinyl acetate copolymer is 20wt%, melt index 7g/10min.
Ultra-fine surface treatment active aluminium hydroxide and the active magnesium hydroxide of ultra-fine surface treatment are through distearyl acyl-oxygen isopropyl
Gained after oxygroup Aluminate is activated, the dosage of distearyl acyl-oxygen aluminum isopropoxide acid esters are aluminium hydroxide or magnesium hydroxide weight
The 1.5wt% of amount.Ultra-fine surface treatment active aluminium hydroxide and the ultra-fine partial size for being surface-treated active magnesium hydroxide are 5000
Mesh.
The partial size of expanding halide-free fire-retardant is 5 μm, pH value 6.5.Lubricant is stearic acid.Antioxidant contains mass ratio
For the Hinered phenols antioxidant, aromatic amine antioxidant and auxiliary antioxidant of 1:2:3.Hinered phenols antioxidant is bis- (3,5- bis-
Tertiary butyl-4-hydroxy benzyl) thioether and β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid octadecanol ester be 1 in mass ratio:
Mixture after 1 cooperation；Aromatic amine antioxidant is 4,4 '-bis- (bis (alpha, alpha-dimethylbenzyl) base) diphenylamines；Auxiliary antioxidant is double
Lauryl Alcohol ester.Sensitization crosslinking agent is Triallyl isocyanurate.
Embodiment 7
Ultralow temperature provided in this embodiment shrink thermal contraction casing tube the difference from example 2 is that:
Synthetic guttapercha is anti-form-1, and the trans content of 4- polyisoprene, the anti-form-1,4- polyisoprene is
100 DEG C of 96wt%, mooney viscosity ML (3+4) are 60, gel content 1.5wt%.
Vinyl acetate content in ethylene-vinyl acetate copolymer is 30wt%, melt index 10g/10min.
Ultra-fine surface treatment active aluminium hydroxide and the active magnesium hydroxide of ultra-fine surface treatment are through distearyl acyl-oxygen isopropyl
Gained after oxygroup Aluminate is activated, the dosage of distearyl acyl-oxygen aluminum isopropoxide acid esters are aluminium hydroxide or magnesium hydroxide weight
The 3wt% of amount.Ultra-fine surface treatment active aluminium hydroxide and the ultra-fine partial size for being surface-treated active magnesium hydroxide are 5500 mesh.
The partial size of expanding halide-free fire-retardant is 3 μm, pH value 6.8.Lubricant is zinc stearate.Antioxidant contains quality
Than Hinered phenols antioxidant, aromatic amine antioxidant and the auxiliary antioxidant for 2:1:2.Hinered phenols antioxidant is β-(3,5-
Di-tert-butyl-hydroxy phenyl) propionic acid octadecanol ester；Aromatic amine antioxidant is 4,4 '-bis- (bis (alpha, alpha-dimethylbenzyl) bases) two
Aniline；Auxiliary antioxidant is bi-myristoleyl and three (2,4- di-t-butyl) phenyl-phosphites are after 1:1 cooperates in mass ratio
Mixture.Sensitization crosslinking agent is trimethylolpropane trimethacrylate.
Embodiment 8
The present embodiment provides the preparation method that a kind of ultralow temperature that any of the above-described embodiment provides shrinks thermal contraction casing tube, packets
It includes:
It prepares masterbatch: adding raw materials into mixer according to the ratio, be kneaded 20min for the first time under conditions of 90 DEG C, then
Using in double-cone feeding machine investment double-screw extruding pelletizing machine, it is kneaded for second under conditions of 100 DEG C, squeezes out, then input
To being mounted in the underwater pellet cutting system after double-screw extruding pelletizing machine, keeping water tank water temperature is 30 DEG C, water cooling conveying, pelletizing,
Obtain masterbatch.
It squeezes out: by above-mentioned masterbatch removal moisture drying, then on the single screw extrusion machine equipped with mouth mold, plug, in 80 DEG C
Under the conditions of be extruded into tubing.
Irradiation: by the tubing after extrusion in the condition that electronics acceleration energy is 2.0MeV and irradiation dose is 5.0Mrad
Lower crosslinking with radiation.
Expansion: the tubing after irradiation is expanded 1.5 times with Cylinder vacuum expansion device under conditions of 150 DEG C, cooling is determined
Type.
Embodiment 9
The present embodiment and the difference of embodiment 8 are:
It prepares masterbatch: adding raw materials into mixer according to the ratio, be kneaded 20min for the first time under conditions of 100 DEG C, then
Using in double-cone feeding machine investment double-screw extruding pelletizing machine, it is kneaded for second under conditions of 110 DEG C, squeezes out, then input
To being mounted in the underwater pellet cutting system after double-screw extruding pelletizing machine, keeping water tank water temperature is 45 DEG C, water cooling conveying, pelletizing,
Obtain masterbatch.
It squeezes out: by above-mentioned masterbatch removal moisture drying, then on the single screw extrusion machine equipped with mouth mold, plug, in 90 DEG C
Under the conditions of be extruded into tubing.
Irradiation: by the tubing after extrusion in the condition that electronics acceleration energy is 2.0MeV and irradiation dose is 7.5Mrad
Lower crosslinking with radiation.
Expansion: the tubing after irradiation is expanded 2 times with Cylinder vacuum expansion device under conditions of 175 DEG C, cooling is determined
Type.
Embodiment 10
The present embodiment and the difference of embodiment 8 are:
It prepares masterbatch: adding raw materials into mixer according to the ratio, be kneaded 20min for the first time under conditions of 110 DEG C, then
Using in double-cone feeding machine investment double-screw extruding pelletizing machine, it is kneaded for second under conditions of 120 DEG C, squeezes out, then input
To being mounted in the underwater pellet cutting system after double-screw extruding pelletizing machine, keeping water tank water temperature is 60 DEG C, water cooling conveying, pelletizing,
Obtain masterbatch.
It squeezes out: by above-mentioned masterbatch removal moisture drying, then on the single screw extrusion machine equipped with mouth mold, plug, in 100 DEG C
Under the conditions of be extruded into tubing.
Irradiation: by the tubing after extrusion under conditions of electronics acceleration energy is 2.0MeV and irradiation dose is 10Mrad
Crosslinking with radiation.
Expansion: the tubing after irradiation is expanded 3 times with Cylinder vacuum expansion device under conditions of 200 DEG C, cooling is determined
Type.
Test example
By taking embodiment 5 as an example, by the resulting ultralow temperature of the embodiment shrink thermal contraction casing tube by the testing standard in table 1 into
Row test, the results are shown in Table 1.
1 testing standard of table and result
As can be seen from Table 1, ultralow temperature provided herein, which shrinks thermal contraction casing tube, has preferably mechanical property, heat
Ageing properties, low temperature flexibility and resistance to copper corrosion performance energy etc..
In conclusion ultralow temperature provided by the present application shrinks thermal contraction casing tube halogen-free flameproof, there is preferable mechanics and heat
Ageing properties, while realizing 85 DEG C of low temperature and shrinking completely, heat-shrink tube product has been expanded in the application and development of civil field.It is made
Preparation Method is easy to operate, is suitable for industrialized production.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.Reality of the invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of selected implementation of the invention
Example.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of ultralow temperature shrinks thermal contraction casing tube, which is characterized in that according to parts by weight, the ultralow temperature shrinks heat shrinking sleeve
The raw material of pipe includes the synthetic guttapercha of 20-50 parts by weight, the ethylene-vinyl acetate copolymer of 10-30 parts by weight, 0-20 weight
Measure ultra-fine surface treatment activity magnesium hydroxide, the ultra-fine surface treatment active aluminium hydroxide of 5-20 parts by weight, 10-20 weight of part
Part expanding halide-free fire-retardant, the lubricant of 0.1-2 parts by weight, the antioxidant of 0.1-2 parts by weight, 0.5-2 parts by weight it is quick
Change the carbon black of crosslinking agent and 0.5-5 parts by weight.
2. ultralow temperature according to claim 1 shrinks thermal contraction casing tube, which is characterized in that the ultralow temperature, which is shunk, to be heat-shrinked
The raw material of casing includes that the synthetic guttapercha of 30-40 parts by weight, the ethylene-vinyl acetate of 15-25 parts by weight are total
The ultra-fine ultra-fine surface treatment work for being surface-treated active magnesium hydroxide, 10-15 parts by weight of polymers, 5-15 parts by weight
Property aluminium hydroxide, the expanding halide-free fire-retardant of 12-18 parts by weight, 0.5-1.5 parts by weight the lubricant, 0.5-
The antioxidant, the sensitization crosslinking agent of 1-1.5 parts by weight and the carbon black of 2-4 parts by weight of 1.5 parts by weight.
3. ultralow temperature according to claim 1 shrinks thermal contraction casing tube, which is characterized in that the ultralow temperature, which is shunk, to be heat-shrinked
The raw material of casing includes the synthetic guttapercha of 35 parts by weight, the ethylene-vinyl acetate copolymer of 20 parts by weight, 10
The ultra-fine active hydroxide of the ultra-fine surface treatment for being surface-treated active magnesium hydroxide, 12.5 parts by weight of parts by weight
Aluminium, the expanding halide-free fire-retardant of 15 parts by weight, the lubricant of 1 parts by weight, the antioxidant of 1 parts by weight, 1.2
The sensitization crosslinking agent of parts by weight and the carbon black of 3 parts by weight.
4. ultralow temperature according to claim 1-3 shrinks thermal contraction casing tube, which is characterized in that the synthesis Cortex Eucommiae
Glue is trans-1,4-iroprene polymer；
Preferably, the trans content of the anti-form-1,4- polyisoprene is not less than 95wt%, 100 DEG C of mooney viscosity ML (3+4)
For 40-60, gel content is no more than 3wt%.
5. ultralow temperature according to claim 1-3 shrinks thermal contraction casing tube, which is characterized in that the ethylene-vinegar
Vinyl acetate content in vinyl acetate copolymer is 15-30wt%, melt index 4-10g/10min.
6. ultralow temperature according to claim 1-3 shrinks thermal contraction casing tube, which is characterized in that the ultra-fine surface
Processing active aluminium hydroxide and the active magnesium hydroxide of the ultra-fine surface treatment divide equally institute after other surface treated agent is activated
?；
Preferably, the surface treating agent is distearyl acyl-oxygen aluminum isopropoxide acid esters；
Preferably, the dosage of the surface treating agent is the 0.5-3wt% of aluminium hydroxide or magnesium hydroxide weight；
Preferably, the ultra-fine surface treatment active aluminium hydroxide and the ultra-fine partial size for being surface-treated active magnesium hydroxide are
4500-5500 mesh.
7. ultralow temperature according to claim 1-3 shrinks thermal contraction casing tube, which is characterized in that the intumescent without
The partial size of halogen fire retardant is no more than 5 μm, pH value 6.0-6.8.
8. ultralow temperature according to claim 1-3 shrinks thermal contraction casing tube, which is characterized in that the antioxidant packages
Include Hinered phenols antioxidant, aromatic amine antioxidant and auxiliary antioxidant；
The Hinered phenols antioxidant includes 2,6 di tert butyl 4 methyl phenol, bis- (3,5- di-tert-butyl-4-hydroxyl benzyls)
At least one of thioether and β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid octadecanol ester, the aromatic amine antioxygen
Agent is 4,4 '-bis- (alpha, alpha-dimethylbenzyl) diphenylamines, and the auxiliary antioxidant includes three (2,4- di-t-butyl) phosphorous acid benzene
At least one of ester and thio-2 acid dibasic acid esters；
Preferably, the thio-2 acid dibasic acid esters includes double Lauryl Alcohol esters, bi-myristoleyl or double octadecanol esters；
Preferably, the mass ratio of the Hinered phenols antioxidant, the aromatic amine antioxidant and the auxiliary antioxidant is 1-
2:1-2:1-3.
9. ultralow temperature according to claim 1-3 shrinks thermal contraction casing tube, which is characterized in that the lubricant is
Zinc stearate or stearic acid；
And/or the sensitization crosslinking agent is trimethylolpropane trimethacrylate or Triallyl isocyanurate.
10. a kind of preparation method for shrinking thermal contraction casing tube such as the described in any item ultralow temperature of claim 1-9, feature exist
In, comprising the following steps:
It prepares masterbatch: being kneaded the raw material according to the ratio and be granulated, water cooling conveying, pelletizing obtain masterbatch；
It squeezes out: the masterbatch being extruded into tubing under conditions of 80-100 DEG C；
Irradiation: by the tubing after extrusion be 2.0MeV in electronics acceleration energy and irradiation dose is 5.0Mrad-
Crosslinking with radiation under conditions of 10.0Mrad；
Expansion: the tubing after irradiation is expanded 1.5-3 times under conditions of 150-200 DEG C, cooling, sizing；
Preferably, being kneaded includes being kneaded to be kneaded with second for the first time, and being kneaded for the first time is under conditions of 90-110 DEG C close
20min is carried out in mill, second, which is kneaded, is carried out in double-screw extruding pelletizing machine under conditions of 100-120 DEG C.
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