CN114426728A - Silane crosslinking type cable insulation material capable of being extruded efficiently - Google Patents
Silane crosslinking type cable insulation material capable of being extruded efficiently Download PDFInfo
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- CN114426728A CN114426728A CN202111274530.1A CN202111274530A CN114426728A CN 114426728 A CN114426728 A CN 114426728A CN 202111274530 A CN202111274530 A CN 202111274530A CN 114426728 A CN114426728 A CN 114426728A
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- coupling agent
- silane
- silane coupling
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- insulation material
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- 238000004132 cross linking Methods 0.000 title claims abstract description 28
- 239000012774 insulation material Substances 0.000 title claims abstract description 28
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910000077 silane Inorganic materials 0.000 title claims abstract description 25
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 75
- 238000012545 processing Methods 0.000 claims abstract description 38
- 239000002994 raw material Substances 0.000 claims abstract description 33
- 239000006057 Non-nutritive feed additive Substances 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 27
- 150000004756 silanes Chemical class 0.000 claims abstract description 27
- 229920000098 polyolefin Polymers 0.000 claims abstract description 24
- 239000011810 insulating material Substances 0.000 claims abstract description 23
- 238000002156 mixing Methods 0.000 claims abstract description 21
- 238000001125 extrusion Methods 0.000 claims abstract description 19
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 15
- 239000003999 initiator Substances 0.000 claims abstract description 14
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000005303 weighing Methods 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 24
- -1 polypropylene Polymers 0.000 claims description 22
- 239000002904 solvent Substances 0.000 claims description 16
- DREPONDJUKIQLX-UHFFFAOYSA-N 1-[ethenyl(ethoxy)phosphoryl]oxyethane Chemical compound CCOP(=O)(C=C)OCC DREPONDJUKIQLX-UHFFFAOYSA-N 0.000 claims description 12
- 239000003054 catalyst Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000000178 monomer Substances 0.000 claims description 12
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 12
- 239000000654 additive Substances 0.000 claims description 11
- 230000000996 additive effect Effects 0.000 claims description 11
- IYPLTVKTLDQUGG-UHFFFAOYSA-N dodeca-1,11-diene Chemical compound C=CCCCCCCCCC=C IYPLTVKTLDQUGG-UHFFFAOYSA-N 0.000 claims description 11
- 239000013067 intermediate product Substances 0.000 claims description 10
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical group C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 6
- 229920000092 linear low density polyethylene Polymers 0.000 claims description 6
- 239000004707 linear low-density polyethylene Substances 0.000 claims description 6
- 229920001684 low density polyethylene Polymers 0.000 claims description 6
- 239000004702 low-density polyethylene Substances 0.000 claims description 6
- 239000004743 Polypropylene Substances 0.000 claims description 5
- 238000005469 granulation Methods 0.000 claims description 5
- 230000003179 granulation Effects 0.000 claims description 5
- 229920001155 polypropylene Polymers 0.000 claims description 5
- XOUQAVYLRNOXDO-UHFFFAOYSA-N 2-tert-butyl-5-methylphenol Chemical compound CC1=CC=C(C(C)(C)C)C(O)=C1 XOUQAVYLRNOXDO-UHFFFAOYSA-N 0.000 claims description 4
- 239000008187 granular material Substances 0.000 claims description 4
- 125000001501 propionyl group Chemical group O=C([*])C([H])([H])C([H])([H])[H] 0.000 claims description 4
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 3
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 3
- 239000012752 auxiliary agent Substances 0.000 claims description 2
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 claims description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims 1
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 claims 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 16
- 238000002360 preparation method Methods 0.000 abstract description 13
- 238000012986 modification Methods 0.000 abstract description 8
- 230000004048 modification Effects 0.000 abstract description 8
- 125000000217 alkyl group Chemical group 0.000 abstract description 5
- UCQFCFPECQILOL-UHFFFAOYSA-N diethyl hydrogen phosphate Chemical compound CCOP(O)(=O)OCC UCQFCFPECQILOL-UHFFFAOYSA-N 0.000 abstract description 4
- 230000001050 lubricating effect Effects 0.000 abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 24
- 230000000052 comparative effect Effects 0.000 description 17
- 239000003063 flame retardant Substances 0.000 description 10
- 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 7
- 239000004698 Polyethylene Substances 0.000 description 7
- 229920000573 polyethylene Polymers 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 239000004594 Masterbatch (MB) Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000001965 increasing effect Effects 0.000 description 4
- 239000000314 lubricant Substances 0.000 description 4
- WPMYUUITDBHVQZ-UHFFFAOYSA-N 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoic acid Chemical compound CC(C)(C)C1=CC(CCC(O)=O)=CC(C(C)(C)C)=C1O WPMYUUITDBHVQZ-UHFFFAOYSA-N 0.000 description 3
- WOXXJEVNDJOOLV-UHFFFAOYSA-N ethenyl-tris(2-methoxyethoxy)silane Chemical compound COCCO[Si](OCCOC)(OCCOC)C=C WOXXJEVNDJOOLV-UHFFFAOYSA-N 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 239000004718 silane crosslinked polyethylene Substances 0.000 description 3
- HXIQYSLFEXIOAV-UHFFFAOYSA-N 2-tert-butyl-4-(5-tert-butyl-4-hydroxy-2-methylphenyl)sulfanyl-5-methylphenol Chemical compound CC1=CC(O)=C(C(C)(C)C)C=C1SC1=CC(C(C)(C)C)=C(O)C=C1C HXIQYSLFEXIOAV-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000005461 lubrication Methods 0.000 description 2
- 238000005453 pelletization Methods 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 2
- FGHOOJSIEHYJFQ-UHFFFAOYSA-N (2,4-ditert-butylphenyl) dihydrogen phosphite Chemical compound CC(C)(C)C1=CC=C(OP(O)O)C(C(C)(C)C)=C1 FGHOOJSIEHYJFQ-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- HIVGXUNKSAJJDN-UHFFFAOYSA-N [Si].[P] Chemical compound [Si].[P] HIVGXUNKSAJJDN-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000010382 chemical cross-linking Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000002430 hydrocarbons Chemical group 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 150000001282 organosilanes Chemical class 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 125000005373 siloxane group Chemical group [SiH2](O*)* 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
- C08L23/0807—Copolymers of ethene with unsaturated hydrocarbons only containing four or more carbon atoms
- C08L23/0815—Copolymers of ethene with unsaturated hydrocarbons only containing four or more carbon atoms with aliphatic 1-olefins containing one carbon-to-carbon double bond
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/44—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins
- H01B3/441—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins from alkenes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/202—Applications use in electrical or conductive gadgets use in electrical wires or wirecoating
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
- C08L2312/08—Crosslinking by silane
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Organic Insulating Materials (AREA)
Abstract
The invention discloses a silane crosslinking cable insulating material capable of being extruded efficiently, which comprises the following processing raw materials in parts by weight: 80-99 parts of polyolefin, 1-5 parts of modified silane coupling agent, 0.01-1 part of antioxidant assistant, 0.01-1 part of silane initiator and processing assistant: and 0.1-0.75 part of silane coupling agent is added per 100 parts of processing raw materials. The preparation method comprises the following steps: weighing the raw materials except the processing aid in parts by weight, uniformly mixing, putting into a double-screw extruder, extruding and granulating, drawing out strips, cooling by a water tank, and granulating; and adding a processing aid, and uniformly mixing to obtain the cable insulation material. Diethyl phosphate is introduced through modification, so that the high-temperature resistance of the material is greatly improved; long-chain alkyl is introduced through modification, and meanwhile, a silane coupling agent is added into the prepared insulating material to serve as a processing aid, so that the insulating material can play a role in lubricating in the subsequent extrusion molding process, and is easy to process subsequently.
Description
Technical Field
The invention relates to the field of production processes of cable materials, in particular to a silane crosslinking type cable insulating material capable of being extruded efficiently.
Background
With the rapid development of communication technology, people have higher and higher requirements on the performance of communication cables; meanwhile, the demand of products is also increasing. Polyethylene is one of the commonly used raw materials in the field of current materials, and due to the limitations of high temperature resistance, mechanical properties and processability, the polyethylene material is usually subjected to cross-linking treatment in the application of the wire and cable insulation material, and the commonly used cross-linking methods mainly include three methods: peroxide crosslinking, irradiation crosslinking, and silane crosslinking. Peroxide crosslinking requires precise control of processing conditions, so that the production difficulty is high, and a qualified product cannot be produced due to carelessness, so that huge loss is caused; the radiation crosslinking process is simple, but has the risk of radiation contamination, and the equipment is very expensive, which also results in limited application. The silane crosslinked polyethylene is a chemical crosslinking method, crosslinking is generated by grafting organosilane and polyethylene under certain conditions, the process is simple, and a common extruder is usually adopted for processing.
The traditional silane crosslinked polyethylene is carried out by adopting a two-step method: firstly, grafting silane to polyethylene, mixing catalyst and polyethylene to form catalytic master batch, secondly, extruding and molding the silane-grafted polyethylene and the catalytic master batch, and carrying out crosslinking under hot water or low steam pressure. For example, chinese patent CN201811273920.5 discloses a silane crosslinked polyethylene insulating material for heating cables, and a preparation method and application thereof, the insulating material is prepared by mixing a silane grafted material and a crosslinking catalyst masterbatch, the silane grafted material comprises polyolefin resin, a silane crosslinking agent, a grafting initiator, a first lubricant and a first antioxidant, and the crosslinking catalyst masterbatch comprises: the crosslinking catalyst, the second lubricant and the second antioxidant are prepared by respectively preparing the silane grafting material and the crosslinking catalyst master batch, and then are packaged in proportion for use. However, the method has the main problems that the fluidity of the grafting material is poor, the processing is difficult, the high-speed extrusion cannot be carried out in the second step of extrusion molding, the production efficiency is influenced, and the high-temperature resistance of the insulating material obtained by processing is still not improved. If the conventional lubricant or flame retardant is directly added to polyolefin, the improvement effect on the fluidity and high temperature resistance of polyolefin is desired to be improved because the compatibility of the lubricant or flame retardant with polyolefin is limited.
Disclosure of Invention
The invention aims to solve the problems of low extrusion speed and poor high temperature resistance of polyethylene insulating materials in the existing processing method, and provides a silane crosslinking type cable insulating material capable of being efficiently extruded.
In order to achieve the purpose, the invention adopts the following technical scheme:
a silane cross-linked cable insulating material capable of being efficiently extruded comprises a processing raw material and a processing aid, wherein the processing raw material comprises the following components in parts by weight: 80-99 parts of polyolefin, 1-5 parts of modified silane coupling agent, 0.01-1 part of antioxidant assistant and 0.01-1 part of initiator; the addition amount of the processing aid is as follows: 0.1 to 0.75 portion of the additive is added to 100 portions of processing raw materials by weight portion.
Preferably, the preparation method of the modified silane coupling agent comprises the following steps:
(1) mixing a silane coupling agent and a catalyst in a solvent, dropwise adding diethyl vinylphosphonate in a nitrogen atmosphere at 35-45 ℃, wherein the mass ratio of the silane coupling agent to the diethyl vinylphosphonate is 8: 1-10: 1, and stirring the mixture at 40-60 ℃ for 3-6 hours. Removing the solvent and unreacted monomers under reduced pressure to obtain an intermediate product;
(2) mixing a solvent and an intermediate product with equal mass, heating to 70-90 ℃ in a nitrogen atmosphere, and dropwise adding 1, 11-dodecadiene with the amount ratio of the 1, 11-dodecadiene to the silane coupling agent being 3: 1-6: 1; and after all the components are added, stirring the mixture for 3-6 hours at 70-90 ℃, and removing the solvent and unreacted monomers under reduced pressure to obtain the modified silane coupling agent.
For improving the high temperature resistance of polyolefin materials, the existing process usually adds some flame retardants directly into polyolefin, but the directly added flame retardants have the problems of poor compatibility, poor dispersion condition of the flame retardants and the like, and the improvement of the high temperature resistance is not ideal. According to the invention, a silicon-hydrogen addition reaction is adopted, a diethyl phosphate structure is introduced into a silane coupling agent, so that the good dispersibility of organic silicon is utilized, a flame retardant is combined with a high molecular chain through a chemical bond, the compatibility among materials is increased, a silicon-phosphorus synergistic effect can be exerted in the flame retardant process, a carbon layer generated in the organic phosphorus flame retardant process is stabilized by silicon dioxide formed by heating siloxane, organic matters are prevented from contacting with oxygen, and a better flame retardant effect is achieved.
The polysiloxane chain segment has the characteristic of obvious low surface energy, and the siloxane group in the structure promotes the polysiloxane chain to be enriched on the surface of the polyolefin to form a lubricating layer, so that the surface modification of the polyolefin can be realized. In addition, the long-chain alkyl introduced into the modified silane coupling agent can reduce the friction coefficient of polymer chains and promote the slippage effect among molecular chains, thereby promoting the flow of the polymer and enhancing the extrusion performance of the polymer. In the process of introducing the long-chain alkyl, a two-step synthesis method is adopted, and the long-chain alkyl is introduced in the second step, so that the reaction activation energy can be reduced by utilizing the diethyl phosphate structure introduced in the first step, and the reaction yield is increased.
Preferably, the processing aid is a silane coupling agent. The silane coupling agent is added on the surface of the obtained particles in the process of preparing the silane crosslinking type cable insulating material, so that the lubricating effect can be achieved in the next extrusion molding process, the processing performance and the mechanical performance of polyolefin cannot be damaged, the insulating material can obtain better surface performance due to the surface modification effect, and the subsequent processing is easy.
Preferably, the polyolefin is one or a combination of linear low density polyethylene, low density polyethylene and polypropylene.
Preferably, the silane coupling agent is one or a combination of more of 3- (2, 3-glycidoxy) propyl trimethoxy silane, gamma- (methacryloyloxy) propyl trimethoxy silane, vinyl tri (b-methoxyethoxy) silane and N-beta- (aminoethyl) -gamma-aminopropyl methyl dimethoxy silane.
Preferably, the antioxidant auxiliary agent is one or a combination of more of tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, 4' -thiobis (6-tert-butyl-3-methylphenol), 1, 2-bis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl ] hydrazine and tris [2, 4-di-tert-butylphenyl ] phosphite.
Preferably, the initiator is dicumyl peroxide.
Preferably, the preparation method of the silane crosslinking type cable insulation material capable of being extruded efficiently comprises the following steps: (1) weighing the raw materials except the processing aid in parts by weight, and uniformly mixing; (2) extruding and granulating the uniformly mixed raw materials in the step 1, drawing out material strips, cooling and granulating; (3) and (3) adding a processing aid into the granules obtained in the step (2), and uniformly mixing to obtain the cable insulating material.
After extrusion and granulation are finished, a certain amount of silane coupling agent is added, one end of the silane coupling agent can be combined with an organic material, and the other end of the silane coupling agent can be combined with an inorganic material, so that the silane coupling agent can play a role in lubricating a cable insulating material in the subsequent processing process of the cable insulating material into a cylindrical cable insulating layer, and the extrusion efficiency of the cable insulating material is improved.
Preferably, the extrusion granulation adopts a double-screw extruder, and the heating temperature of the double-screw extruder is as follows: the temperature of the first zone is 140-160 ℃, the temperature of the second zone-the fifth zone is 160-205 ℃, and the temperature of the machine head is 205-225 ℃.
Therefore, the invention has the following beneficial effects: (1) on the basis of preparing silane cross-linked polyolefin by a traditional two-step method, a silane coupling agent is modified, and an organic phosphorus flame retardant and long-chain alkyl are introduced, so that the high-temperature resistance of the material is greatly improved, and the processing performance of the polyolefin is improved; (2) the silane coupling agent is added into the prepared insulating material as a processing aid, so that the insulating material can play a role in lubrication in the subsequent extrusion molding process, can obtain better surface performance, and is easy to process subsequently.
Detailed Description
The invention is further described with reference to specific embodiments. It is to be understood that these examples are suitable for illustrating the basic features and advantages of the invention, and the invention is not to be limited in scope by the following examples; the implementation conditions used in the examples can be further adjusted according to specific requirements, and the implementation conditions not indicated are generally the conditions used in routine experiments.
Not specifically illustrated in the following examples, all starting materials are commercially available or prepared by methods conventional in the art.
Example 1
The embodiment provides a silane crosslinking cable insulation material capable of being extruded efficiently, which comprises a processing raw material and a processing aid, wherein the processing raw material comprises the following components in parts by weight: 98 parts of polyolefin, 1.5 parts of modified silane coupling agent, 0.2 part of antioxidant assistant and 0.14 part of initiator; the addition amount of the processing aid is as follows: 0.4 part by weight of the additive is added for each 100 parts of processing raw materials. The polyolefin is a mixture of linear low-density polyethylene, low-density polyethylene and polypropylene in a ratio of 1:1:1, the antioxidant additive is a mixture of 1, 2-bis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl ] hydrazine and tris [2, 4-di-tert-butylphenyl ] phosphite, the initiator is dicumyl peroxide, the processing additive is a silane coupling agent, and the silane coupling agent is a mixture of 3- (2, 3-epoxypropoxy) propyl trimethoxy silane and gamma- (methacryloyloxy) propyl trimethoxy silane in a ratio of 1: 1.
The preparation method of the modified silane coupling agent comprises the following steps:
(1) mixing a silane coupling agent and a catalyst in toluene, dropwise adding diethyl vinylphosphonate in a nitrogen atmosphere at 40 ℃, wherein the mass ratio of the silane coupling agent to the diethyl vinylphosphonate is 10:1, and stirring the mixture at 50 ℃ for 5 hours. Removing the solvent and unreacted monomers under reduced pressure to obtain an intermediate product;
(2) taking toluene and an intermediate product with equal mass, heating to 80 ℃ in a nitrogen atmosphere, and dropwise adding 1, 11-dodecadiene with the mass ratio of the 1, 11-dodecadiene to a silane coupling agent; after the addition of all, the mixture was stirred at 80 ℃ for 5 hours, and the solvent and unreacted monomers were removed under reduced pressure to obtain a modified silane coupling agent.
The preparation method of the silane crosslinking type cable insulation material capable of being extruded efficiently comprises the following steps: (1) weighing the raw materials except the processing aid in parts by weight, and uniformly mixing; (2) putting the uniformly mixed raw materials in the step 1 into a double-screw extruder for extrusion granulation, drawing out strips, cooling by a water tank, and pelletizing; (3) and (3) adding a specified amount of processing aid into the granules obtained in the step (2), and uniformly mixing to obtain the cable insulating material. The heating temperature of the double-screw extruder is as follows: the first zone is 150 ℃, the second zone to the fifth zone are 180 ℃, and the temperature of the machine head is 215 ℃.
Example 2
The embodiment provides a silane crosslinking cable insulation material capable of being extruded efficiently, which comprises a processing raw material and a processing aid, wherein the processing raw material comprises the following components in parts by weight: 98 parts of polyolefin, 1.5 parts of modified silane coupling agent, 0.2 part of antioxidant assistant and 0.14 part of initiator; the addition amount of the processing aid is as follows: 0.1 part by weight of the additive is added for each 100 parts of processing raw materials. The polyolefin is a mixture of linear low-density polyethylene, low-density polyethylene and polypropylene in a ratio of 1:1:1, the antioxidant additive is a mixture of tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester and 4,4' -thiobis (6-tert-butyl-3-methylphenol), the initiator is dicumyl peroxide, the processing additive is a silane coupling agent, and the silane coupling agent is a mixture of vinyl trimethoxy silane and vinyl tri (b-methoxyethoxy) silane in a ratio of 1: 1.
The preparation method of the modified silane coupling agent comprises the following steps:
(1) mixing a silane coupling agent and a catalyst in toluene, dropwise adding diethyl vinylphosphonate in a nitrogen atmosphere at 35 ℃, wherein the mass ratio of the silane coupling agent to the diethyl vinylphosphonate is 10:1, and stirring the mixture at 40 ℃ for 6 hours. Removing the solvent and unreacted monomers under reduced pressure to obtain an intermediate product;
(2) taking toluene and an intermediate product with equal mass, heating to 70 ℃ in a nitrogen atmosphere, and dropwise adding 1, 11-dodecadiene with the mass ratio of the 1, 11-dodecadiene to a silane coupling agent being 6: 1; after the addition of all, the mixture was stirred at 70 ℃ for 6 hours, and the solvent and unreacted monomers were removed under reduced pressure to obtain a modified silane coupling agent.
The silane-crosslinked cable insulation material was prepared as in example 1.
Example 3
The embodiment provides a silane crosslinking cable insulation material capable of being extruded efficiently, which comprises a processing raw material and a processing aid, wherein the processing raw material comprises the following components in parts by weight: 80 parts of polyolefin, 3 parts of modified silane coupling agent, 0.5 part of antioxidant assistant and 0.5 part of initiator; the addition amount of the processing aid is as follows: 0.75 parts by weight of the additive is added to 100 parts of processing raw materials. The polyolefin is a mixture of linear low-density polyethylene, low-density polyethylene and polypropylene in a ratio of 1:1:1, the antioxidant additive is a mixture of 4,4' -thiobis (6-tert-butyl-3-methylphenol) and 1, 2-bis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl ] hydrazine, the initiator is dicumyl peroxide, the processing additive is a silane coupling agent, and the silane coupling agent is a mixture of 3- (2, 3-epoxypropoxy) propyl trimethoxysilane, gamma- (methacryloyloxy) propyl trimethoxysilane and N-beta- (aminoethyl) -gamma-aminopropylmethyl dimethoxysilane in a ratio of 1:1: 1.
The preparation method of the modified silane coupling agent comprises the following steps:
(1) mixing a silane coupling agent and a catalyst in toluene, dropwise adding diethyl vinylphosphonate in a nitrogen atmosphere at 45 ℃, wherein the mass ratio of the silane coupling agent to the diethyl vinylphosphonate is 8:1, and stirring the mixture at 60 ℃ for 3 hours. Removing the solvent and unreacted monomers under reduced pressure to obtain an intermediate product;
(2) taking toluene and an intermediate product with equal mass, heating to 90 ℃ in a nitrogen atmosphere, and dropwise adding 1, 11-dodecadiene with the mass ratio of 3:1 to a silane coupling agent; after the addition of all, the mixture was stirred at 90 ℃ for 3 hours, and the solvent and unreacted monomers were removed under reduced pressure to obtain a modified silane coupling agent.
The silane-crosslinked cable insulation material was prepared as in example 1.
Example 4
The embodiment provides a silane crosslinking cable insulation material capable of being extruded efficiently, which comprises a processing raw material and a processing aid, wherein the processing raw material comprises the following components in parts by weight: 90 parts of polyolefin, 2 parts of modified silane coupling agent, 0.4 part of antioxidant assistant and 0.2 part of initiator; the addition amount of the processing aid is as follows: 0.6 part by weight of the additive is added for each 100 parts of processing raw materials. The polyolefin is a mixture of linear low-density polyethylene and low-density polyethylene 1:1, the antioxidant additive is a mixture of tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester and tri [2, 4-di-tert-butylphenyl ] phosphite, the initiator is dicumyl peroxide, the processing additive is a silane coupling agent, and the silane coupling agent is a mixture of gamma- (methacryloyloxy) propyl trimethoxysilane, vinyl trimethoxysilane and vinyl tri (b-methoxyethoxy) silane 1:1: 1.
The modified silane coupling agent was prepared as in example 1.
The preparation method of the silane crosslinking type cable insulation material capable of being extruded efficiently comprises the following steps: (1) weighing the raw materials except the processing aid in parts by weight, and uniformly mixing; (2) putting the uniformly mixed raw materials in the step 1 into a double-screw extruder for extrusion granulation, drawing out strips, cooling by a water tank, and pelletizing; (3) and (3) adding a specified amount of processing aid into the granules obtained in the step (2), and uniformly mixing to obtain the cable insulating material. The heating temperature of the double-screw extruder is as follows: the first zone is 160 ℃, the second zone to the fifth zone are 190 ℃, and the machine head is 210 ℃.
Comparative example 1
This comparative example differs from example 1 only in that: no processing aid is added in the preparation process.
Comparative example 2
This comparative example differs from example 1 only in that: the addition amount of the processing aid is as follows: 1 part of the additive is added for every 100 parts of processing raw materials in parts by weight.
Comparative example 3
This comparative example differs from example 1 only in that: the preparation method of the modified silane coupling agent comprises the following steps: mixing a silane coupling agent and a catalyst in toluene, dropwise adding diethyl vinylphosphonate in a nitrogen atmosphere at 40 ℃, wherein the mass ratio of the silane coupling agent to the diethyl vinylphosphonate is 10:1, and stirring the mixture at 50 ℃ for 5 hours. And removing the solvent and unreacted monomers under reduced pressure to obtain the modified silane coupling agent.
Comparative example 4
This comparative example differs from example 1 only in that: the preparation method of the modified silane coupling agent comprises the following steps: mixing a silane coupling agent and a catalyst in toluene, heating to 80 ℃ in a nitrogen atmosphere, and dropwise adding 1, 11-dodecadiene with the mass ratio of the silane coupling agent to the silane coupling agent being 5: 1; after the addition of all, the mixture was stirred at 80 ℃ for 5 hours, and the solvent and unreacted monomers were removed under reduced pressure to obtain a modified silane coupling agent.
Comparative example 5
This comparative example differs from example 1 only in that: the raw materials are added with unmodified silane coupling agent.
The insulation materials obtained in the above examples and comparative examples were subjected to extrusion property test and hot elongation property test. The extrusion performance test method comprises the following steps: an SXT1 type extruder is adopted, the extrusion temperature is set to 145-195 ℃ from one area to three areas, the head temperature is 195-215 ℃, the extrusion rotating speed is set to 60rpm at the maximum rotating speed, the extruder is firstly emptied in the testing process, a test material is put into the extruder when the current is the lowest, the current value and the glue yield are recorded every 10s after the current is stabilized for 1 minute, and the test is carried out for 1 minute. The thermal elongation property test conditions are 200 ℃, 0.2MPa and 15min, and the scheme refers to the method of GB/T2951.212008. The results are shown in Table 1.
Table 1 results of performance testing
As can be seen from table 1, the processing aid is added in a suitable proportion in the preparation process in examples 1 to 4, so that the processing performance of the cable insulation material is significantly improved, and the glue yield is significantly higher than that of the cable insulation material without the processing aid in comparative example 1 or the cable insulation material with the processing aid added in excess in comparative example 2. This is probably because the silane coupling agent added later can perform a certain surface modification effect on the cable insulation material in the subsequent processing process, so that the extrusion efficiency of the cable insulation material is increased. In addition, the glue yield of the comparative example 3 is obviously lower than that of the examples 1 to 4, which shows that the introduction of the long-chain hydrocarbon group in the modification process of the silane coupling agent can play a role in lubrication in subsequent processing, and has a certain influence on the processing performance of the cable insulating material. Comparative example 4 although the reaction of 1, 11-dodecadiene and silane coupling agent was performed during the modification, the reaction efficiency of the silane coupling agent with long-chain olefin was decreased and the modification effect of the silane coupling agent was poor because the reaction of the silane coupling agent with vinyl group was not performed in the first step. It can also be found from comparative example 5 and examples 1 to 4 that the cable insulation prepared with the unmodified silane coupling agent has a significantly lower extrusion efficiency than the cable insulation prepared with the modified silane coupling agent. Examples 1-4 the elongation under hot extension load of the cable insulation materials prepared using the modified silane coupling agent as the raw material was significantly lower than that of comparative examples 4 and 5, probably because the introduction of the diethyl phosphate structure enhanced the high temperature resistance of the polyolefin material.
Claims (9)
1. The silane crosslinking cable insulating material capable of being extruded efficiently is characterized by comprising processing raw materials and a processing aid, wherein the processing raw materials comprise the following components in parts by weight: 80-99 parts of polyolefin, 1-5 parts of modified silane coupling agent, 0.01-1 part of antioxidant assistant and 0.01-1 part of initiator; the addition amount of the processing aid is as follows: 0.1-0.75 part by weight of the additive is added to 100 parts of processing raw materials.
2. The silane crosslinking cable insulation material capable of being efficiently extruded according to claim 1, wherein the modified silane coupling agent is prepared by the following steps:
(1) mixing a silane coupling agent and a catalyst in a solvent, dropwise adding diethyl vinylphosphonate in a nitrogen atmosphere at 35-45 ℃, wherein the mass ratio of the silane coupling agent to the diethyl vinylphosphonate is 8: 1-10: 1, stirring the mixture at 40-60 ℃ for 3-6 hours, and removing the solvent and unreacted monomers under reduced pressure to obtain an intermediate product;
(2) mixing a solvent and an intermediate product with equal mass, heating to 70-90 ℃ in a nitrogen atmosphere, and dropwise adding 1, 11-dodecadiene with the amount ratio of the 1, 11-dodecadiene to the silane coupling agent being 3: 1-6: 1; and after all the components are added, stirring the mixture for 3-6 hours at 70-90 ℃, and removing the solvent and unreacted monomers under reduced pressure to obtain the modified silane coupling agent.
3. The silane-crosslinked cable insulation material capable of being efficiently extruded according to claim 2, wherein the processing aid is a silane coupling agent.
4. The silane-crosslinked cable insulation material capable of being efficiently extruded according to claim 1, wherein the polyolefin is one or a combination of linear low density polyethylene, low density polyethylene and polypropylene.
5. The silane-crosslinked cable insulation material capable of being efficiently extruded according to claim 3, wherein the silane coupling agent is one or a combination of 3- (2, 3-glycidoxy) propyltrimethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane, vinyltrimethoxysilane, vinyltris (b-methoxyethoxy) silane and N-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane.
6. The silane-crosslinked cable insulation material capable of being efficiently extruded according to claim 1, wherein the antioxidant auxiliary agent is one or more of pentaerythritol tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], 4' -thiobis (6-tert-butyl-3-methylphenol), 1, 2-bis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl ] hydrazine, and tris [2, 4-di-tert-butylphenyl ] phosphite.
7. The silane-crosslinked cable insulation material of claim 1, wherein the initiator is dicumyl peroxide.
8. A method for preparing the silane-crosslinked cable insulation material of claim 1, which is highly extrudable, comprising: (1) weighing the raw materials except the processing aid in parts by weight, and uniformly mixing; (2) extruding and granulating the uniformly mixed raw materials in the step 1, drawing out material strips, cooling and granulating; (3) and (3) adding a processing aid into the granules obtained in the step (2), and uniformly mixing to obtain the cable insulating material.
9. The method for preparing the silane-crosslinked cable insulation material capable of being extruded efficiently as claimed in claim 8, wherein the extrusion granulation is performed by using a twin-screw extruder, and the heating temperature of the twin-screw extruder is as follows: the temperature of the first zone is 140-160 ℃, the temperature of the second zone-the fifth zone is 160-205 ℃, and the temperature of the machine head is 205-225 ℃.
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