CN103435896A - Microwave induced crosslinking polyolefin insulation material and preparation method thereof - Google Patents
Microwave induced crosslinking polyolefin insulation material and preparation method thereof Download PDFInfo
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- CN103435896A CN103435896A CN2013104215737A CN201310421573A CN103435896A CN 103435896 A CN103435896 A CN 103435896A CN 2013104215737 A CN2013104215737 A CN 2013104215737A CN 201310421573 A CN201310421573 A CN 201310421573A CN 103435896 A CN103435896 A CN 103435896A
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Abstract
The invention relates to a microwave induced crosslinking polyolefin insulation material and a preparation method thereof. The invention aims to solve the problems of low strength, low heat-deformation temperature and low solvent resistance in the common polyolefin material, and the problems of complex technique, harsh protecting requirements, low production efficiency, high product cost and poor stability in the existing crosslinking method. The microwave induced crosslinking polyolefin insulation material provided by the invention is prepared from dry polyolefin resin, silane coupling agent, microwave absorber, water bringing agent, polyfunctional group crosslinking agent, crosslinking accelerator and antioxidant. The preparation method comprises the following steps: 1. weighing the components; 2 banburying the components in a Banbury mixer, melting and mixing, and granulating in a single screw extruder to obtain sample granules; and 3. tabletting the obtained sample granules in a vulcanizer, and carrying out microwave induced crosslinking reaction in microwave equipment to obtain the microwave induced crosslinking polyolefin insulation material. The invention is applicable to the fields of wire cable insulation, polyolefin boards and tube products.
Description
Technical field
The present invention relates to a kind of crosslinked polyolefin insulating material and preparation method thereof.
Background technology
Polyolefine material has that tensile strength is high, impelling strength good, wear-resisting, self lubricity and electric property good, and the good advantages such as processibility, it has been widely used in electronics, electrical equipment, automobile, machinofacture, chemical industry, food, daily necessities and medicine and hygiene fields.But in the cable material Application Areas, the intensity of common polyolefine material, heat-drawn wire and solvent resistance are low, can't meet the requirement in practical application.
For the above-mentioned shortcoming of polyolefine material, crosslinked is a kind of effective terms of settlement.Make at present the crosslinked existing preparation method of polyolefine material mainly contain chemical crosslink technique, crosslinking electron beam irradiation method and silane cross-linking method.Existing research shows, polyolefine material has special sorption to microwave, and under the effect of microwave, molecule can heat up rapidly, and after temperature acquires a certain degree, corresponding decomposition reaction occurs the molecule that decomposition reaction or inducing peripheral can occur self.Therefore, introducing microwave absorbing material in the silane crosslinked insulating material system can be at microwave induced lower generation moment high temperature, can decompose if exist in system the molecule that produces water, system can produce after microwave induced and have the crosslinked internal water molecule of catalysis silane molecule.Crosslinkedly can form three-dimensional network structure, can improve on the one hand intensity, resistance toheat and the heat-drawn wire of material, reduced on the other hand the water-intake rate of polyolefine material under wet environment and improved its solvent resistance.
But current cross-linking method has the following disadvantages: chemically crosslinked need to be reacted for a long time in High Temperature High Pressure and specific equipment, and energy expenditure is large, and production efficiency is low; And, because the polyolefinic melt temperature of majority is high, peroxide initiator can decompose in advance, causes precrosslink.High-energy radiation cross-linking apparatus investment is high, Operation and Maintenance is complicated, requirement of shelter is harsh, and product cost is high, and the high-energy radiation energy is higher simultaneously, causes the deterioration of the destructurized and correlated performance of material internal.Crosslinked with silicane is that silane is passed through to fusion-grafting, and it is received on macromolecular chain, and then side group is hydrolyzed, and dehydrating condensation under the catalyzer condition forms Si-O-Si crosslinked, but need poach when crosslinked, expends man-hour long, and product stability is poor.
Summary of the invention
The intensity, heat-drawn wire and the solvent resistance that the objective of the invention is in order to solve common polyolefine material are low, and existing crosslinking complex process, requirement of shelter harshness, production efficiency is low, facility investment is high, product cost is high, the problem that product stability is poor, and a kind of microwave induced crosslinked crosslinked polyolefin insulating material provided and preparation method thereof.
A kind of microwave induced crosslinked crosslinked polyolefin insulating material of the present invention, it is to be produced aqua, 0.1-5 part multi-group crosslink agent, 0.01-5 part crosslinking accelerator and 0.07-0.5 part oxidation inhibitor and made by the polyolefin resin of 100 parts of dryings, 0.1-4 part silane coupling agent, 0.1-5 part microwave absorption, 0.1-5 part.
The preparation method of a kind of microwave induced crosslinked crosslinked polyolefin insulating material of the present invention carries out according to the following steps:
Step 1: polyolefin resin, 0.1-4 part silane coupling agent, 0.1-5 part microwave absorption, 0.1-5 part of taking 100 parts of dryings by mass fraction are produced aqua, 0.1-5 part multi-group crosslink agent, 0.01-5 part crosslinking accelerator and 0.07-0.5 part oxidation inhibitor;
Step 2: banburying in the Banbury mixer that is 160-200 ℃ in temperature by above-mentioned each material, melting mixing 5min; Carry out granulation in the single screw extrusion machine that is 190 ℃-210 ℃ at Temperature Setting, obtain sample particle;
Step 3: the sample particle obtained is placed in to the vulcanizer compressing tablet, making thickness is that 1.0mm length is the sheet material that the 145mm width is 105mm, the frequency adopted in microwave equipment is that 2450MHz, power are the microwave induced crosslinked of 800W, after reaction times is 60s, place 16h in room temperature, obtain microwave induced crosslinked crosslinked polyolefin insulating material.
The present invention comprises following beneficial effect:
The present invention is by adding microwave absorbing material and producing aqua, and the insulating material inside of electric wire can decomposition reaction be occurred and produce water under microwave induced, further causes the crosslinking reaction between silane molecule.By microwave induced mode, removed the poach process from, water molecules results from the inside of insulating material molecule, little on the mechanical and physical performance impact of system.
Microwave induced crosslinked crosslinked polyolefin insulating material prepared by the present invention, mechanical property strengthens, tensile strength has improved 20%, heat-drawn wire improves 20-30%, and performance index meet the JB/T10437-2004 electric wire with in the crosslinkable polyethylene Insulation Material to crosslinked with silicane electric wire and cable material tensile strength and the desired performance index of gel content, fusing point has improved 13-49 ℃, the stability of material strengthens, water absorption decreased 35.7%-61.3%, the water tolerance of material strengthens.
Preparation method's technique of a kind of microwave induced crosslinked crosslinked polyolefin insulating material of the present invention is simple, easy to operate, energy-conserving and environment-protective, realistic production requirement.Original crosslinking method at least needs poach more than 4 hours, and microwave inducedly crosslinked only needs 60 seconds, has reduced and has prepared the material time used, has improved production efficiency; For the equipment of electron beam to irradiate crosslinked needs more than 1,000,000, microwave equipment is relatively cheap, has reduced facility investment and production cost.The microwave induced silanes crosslinked cable of the present invention can be used for wire cable insulating, polyolefin panels, tubing goods with crosslinked polyolefin insulating material.
Embodiment
Embodiment one: a kind of microwave induced crosslinked crosslinked polyolefin insulating material of present embodiment is characterized in that it is to be produced aqua, 0.1-5 part multi-group crosslink agent, 0.01-5 part crosslinking accelerator and 0.07-0.5 part oxidation inhibitor and made by polyolefin resin, 0.1-4 part silane coupling agent, 0.1-5 part microwave absorption, 0.1-5 part of 100 parts of dryings; Wherein, dry polyolefin resin is, at 80-120 ℃ of temperature, polyolefin resin is carried out to dry gained.
Embodiment two: present embodiment is different from embodiment one: described polyolefin resin is that one or more in HDPE, MDPE, LDPE, LLDPE and EVA polyolefin elastomer are mixed by any ratio and form.Other is identical with embodiment one.
Embodiment three: present embodiment is different from embodiment one or two: described silane coupling agent is vinyltrimethoxy silane (A171), vinyltriethoxysilane (A151), being mixed by any ratio of one or more in γ aminopropyltriethoxy silane, benzene n-formyl sarcolysine ethyl triethoxy silicane alkane, γ-second phenodiazine base propyl trimethoxy silicane, β-(3,4-epoxycyclohexyl) ethyl trimethoxy silane and γ-propyl methacrylate base Trimethoxy silane forms.Other is identical with embodiment one or two.
Embodiment four: present embodiment is different from one of embodiment one to three: described microwave absorption is SiC, SiN, SiB
6and Si
3b
4in one or more be mixed by any ratio and form.Other is identical with one of embodiment one to three.
Embodiment five: present embodiment is different from one of embodiment one to four: described product aqua is Mg (OH)
2, Al (OH)
3, 2ZnOB
2o
33.5H
2o and CdSO
48H
2one or more in O are mixed by any ratio and form.Other is identical with one of embodiment one to four.
Embodiment six: present embodiment is different from one of embodiment one to five: described multi-group crosslink agent is TAC, TAIC, TMPTA, TMPAE, ETAE, tetramethylolmethane tetraene propyl ether or/and one or more in three TEGMA are mixed by any ratio forms.Other is identical with one of embodiment one to five.
Embodiment seven: present embodiment is different from one of embodiment one to six: described crosslinking accelerator is by ethylene-tetrafluoroethylene copolymer, ethene-1, and one or more in chlorotrifluoroethylcopolymer copolymer, ethene-fluoride copolymers, hexachloroethane, tetrachloromethane are mixed by any ratio and form.Other is identical with one of embodiment one to six.
Embodiment eight: present embodiment is different from one of embodiment one to seven: described oxidation inhibitor is to be by phenols, phosphorous acid esters, phosphoric acid ester, containing two or more in the thioesters kind antioxidant, to be mixed by any ratio and to form by oxidation inhibitor; Phenolic antioxidant is 2,6-di-tert-butylphenol, 2,4,6-tri-tert-butylphenol (oxidation inhibitor 246), 4,4 '-thiobis (6-tertiary butyl-3-methylphenol) (antioxidant 300) or four [methylene radical-3-(3 ', 5 '-di-tert-butyl-4 '-hydroxy phenyl) propionic acid] pentaerythritol ester (antioxidant 1010); Phosphorous acid esters or phosphoric acid ester oxidation inhibitor are TPP, tricresyl phosphite (2,4-di-tert-butyl phenyl) ester (irgasfos 168), TIOP or tricresyl phosphate benzene methyl; Containing the thioesters kind antioxidant, be DLTP, LSTP or DTDTP; Composite antioxidant take phenolic antioxidant and phosphorous acid esters, preferably be mixed by any ratio combination containing the thioesters class as it.Other is identical with one of embodiment one to seven.
Embodiment nine: present embodiment is different from one of embodiment one to eight: described a kind of microwave induced crosslinked crosslinked polyolefin insulating material is that, 0.18 part microwave absorption silane coupled by the polyolefin resin of 100 parts of dryings, 0.15 part, 0.16 part produce aqua, 0.35 part of multi-group crosslink agent, 0.026 part of crosslinking accelerator and 0.15 part of oxidation inhibitor and make.Other is identical with one of embodiment one to eight.
Embodiment ten: the preparation method of a kind of microwave induced crosslinked crosslinked polyolefin insulating material of present embodiment is characterized in that it is to carry out according to the following steps:
Step 1: polyolefin resin, 0.1-4 part silane coupling agent, 0.1-5 part microwave absorption, 0.1-5 part of taking 100 parts of dryings by mass fraction are produced aqua, 0.1-5 part multi-group crosslink agent, 0.01-5 part crosslinking accelerator and 0.07-0.5 part oxidation inhibitor; Wherein, dry polyolefin resin is, at 80-120 ℃ of temperature, polyolefin resin is carried out to dry gained.
Step 2: banburying in the Banbury mixer that is 160-200 ℃ in temperature by above-mentioned each material, melting mixing 5min; Carry out granulation in the single screw extrusion machine that is 190 ℃-210 ℃ at Temperature Setting, obtain sample particle;
Step 3: the sample particle obtained is placed in to the vulcanizer compressing tablet, making thickness is that 1.0mm length is the sheet material that the 145mm width is 105mm, the frequency adopted in microwave equipment is that 2450MHz, power are the microwave induced crosslinked of 800W, after reaction times is 60s, place 16h in room temperature, obtain microwave induced crosslinked crosslinked polyolefin insulating material.
Embodiment 11: present embodiment is different from embodiment nine: the polyolefin resin described in step 1 is that one or more in HDPE, MDPE, LDPE, LLDPE and EVA polyolefin elastomer are mixed by any ratio and form.Other is identical with embodiment ten.
Embodiment 12: present embodiment is different from embodiment nine or ten: the silane coupling agent described in step 1 is vinyltrimethoxy silane (A171), vinyltriethoxysilane (A151), being mixed by any ratio of one or more in γ aminopropyltriethoxy silane, benzene n-formyl sarcolysine ethyl triethoxy silicane alkane, γ-second phenodiazine base propyl trimethoxy silicane, β-(3,4-epoxycyclohexyl) ethyl trimethoxy silane and γ-propyl methacrylate base Trimethoxy silane forms.Other is identical with embodiment ten or 11.
Embodiment 13: present embodiment is different from one of embodiment ten to 12: the microwave absorption described in step 1 is SiC, SiN, SiB
6and Si
3b
4in one or more be mixed by any ratio and form.Other is identical with one of embodiment ten to 12.
Embodiment 14: present embodiment is different from one of embodiment ten to 13: the product aqua described in step 1 is Mg (OH)
2, Al (OH)
3, 2ZnOB
2o
33.5H
2o and CdSO
48H
2one or more in O are mixed by any ratio and form.Other is identical with one of embodiment ten to 13.
Embodiment 15: present embodiment is different from one of embodiment ten to 14: the multi-group crosslink agent described in step 1 is TAC, TAIC, TMPTA, TMPAE, ETAE, tetramethylolmethane tetraene propyl ether or/and one or more in three TEGMA are mixed by any ratio forms.Other is identical with one of embodiment ten to 14.
Embodiment 16: present embodiment is different from one of embodiment ten to 15: the crosslinking accelerator described in step 1 is ethylene-tetrafluoroethylene copolymer, ethene-1, and one or more in chlorotrifluoroethylcopolymer copolymer, ethene-fluoride copolymers, hexachloroethane, tetrachloromethane are mixed by any ratio and form.Other is identical with one of embodiment ten to 15.
Embodiment 17: present embodiment is different from one of embodiment ten to 16: the oxidation inhibitor described in step 1 is by phenols, phosphorous acid esters, phosphoric acid ester, containing two or more in the thioesters kind antioxidant, is mixed by any ratio and forms; Phenolic antioxidant is 2,6-di-tert-butylphenol, 2,4,6-tri-tert-butylphenol (oxidation inhibitor 246), 4,4 '-thiobis (6-tertiary butyl-3-methylphenol) (antioxidant 300) or four [methylene radical-3-(3 ', 5 '-di-tert-butyl-4 '-hydroxy phenyl) propionic acid] pentaerythritol ester (antioxidant 1010); Phosphorous acid esters or phosphoric acid ester oxidation inhibitor are TPP, tricresyl phosphite (2,4-di-tert-butyl phenyl) ester (irgasfos 168), TIOP or tricresyl phosphate benzene methyl; Containing the thioesters kind antioxidant, be DLTP, LSTP or DTDTP; Composite antioxidant take phenolic antioxidant and phosphorous acid esters, preferably be mixed by any ratio combination containing the thioesters class as it.Other is identical with one of embodiment ten to 16.
Embodiment 18: present embodiment is different from one of embodiment ten to 17: described in step 1 by mass fraction take that the polyolefin resin, 0.15 part of 100 parts of dryings is silane coupled, 0.18 part of microwave absorption, 0.16 part produce aqua, 0.35 part of multi-group crosslink agent, 0.026 part of crosslinking accelerator and 0.15 part of oxidation inhibitor.Other is identical with one of embodiment ten to 17.
Embodiment 1
The preparation method of a kind of microwave induced crosslinked crosslinked polyolefin insulating material of the present embodiment, carry out according to the following steps:
One, take respectively LLDPE7042,0.15g silane coupling A 171,0.18g SiC, the 0.16g Mg (OH) of 100g drying
2, 0.35g TAIC, 0.026g crosslinking accelerator ethene fluoride copolymers and 0.15g composite antioxidant; Wherein, composite antioxidant is by the 0.05g antioxidant 1010, and 0.03g tricresyl phosphate benzene methyl and 0.07g DLTP form;
Two, above-mentioned each component taken is put into to design temperature the Banbury mixer banburying of 160-200 ℃, melting mixing 5min, the single screw extrusion machine granulation by 190 ℃ of Temperature Settings～210 ℃ of scopes, obtain sample particle.
Three, the sample particle obtained is placed in to the vulcanizer compressing tablet, making thickness is that 1.0mm length is the sheet material that the 145mm width is 105mm, the frequency adopted in microwave equipment is that 2450MHz, power are the microwave induced crosslinked of 800W, after reaction times 60s, room temperature is placed 16h, obtains a kind of microwave induced crosslinked crosslinked polyolefin insulating material.
The microwave induced crosslinked crosslinked polyolefin insulating material obtained and the crosslinking electron beam irradiation, peroxide crosslinking, the common poach silane crosslinked polyethylene (thickness is 1.0mm) that with LLDPE7042, prepare are carried out to performance comparison, and result is as shown in table 1:
The microwave induced crosslinked crosslinked polyolefin insulating material of table 1 and the crosslinking electron beam irradiation, the peroxide that with LLDPE7042, prepare
Crosslinked, the common poach silane crosslinked polyethylene of compound performance comparison result
As shown in Table 1, microwave induced crosslinked with silicane with crosslinking electron beam irradiation, peroxide crosslinking, common poach organosilane crosslinked polyethylene LLDPE7042(thickness, be 1.0mm) compare, the gel content of microwave induced crosslinked crosslinked polyolefin insulating material is crosslinked apparently higher than alternate manner, and tensile strength and heat are extended crosslinked with silicane material, high-temperature stability and the good mechanical performance apparently higher than common poach.
A kind of microwave induced crosslinked crosslinked polyolefin insulating material prepared by the present embodiment, mechanical property strengthens, tensile strength has improved 20%, heat-drawn wire improves 20-30%, and performance index meet the JB/T10437-2004 electric wire and use in the crosslinkable polyethylene Insulation Material crosslinked with silicane electric wire and cable material tensile strength and the desired performance index of gel content, by microwave induced mode, removed the poach process from, water molecules results from the inside of insulating material molecule, mechanical and physical performance impact on system is little, fusing point has improved 13-49 ℃, the stability of material strengthens, water absorption decreased 35.7%-61.3%, the water tolerance of material strengthens.Preparation method's technique of the present embodiment is simple, easy to operate, energy-conserving and environment-protective, production efficiency is high, facility investment is low, the cost of product is low, realistic production requirement.
Embodiment 2
The preparation method of a kind of microwave induced crosslinked crosslinked polyolefin insulating material of the present embodiment, carry out according to the following steps:
One, the LLDPE7066,0.5g silane coupling A 171,0.25g silicon carbide SiC, the 0.27g that accurately take the 100g drying produce aqua AL (OH)
3, 3.75g multi-group crosslink agent TMPTA, the chloro-trifluoro-ethylene copolymer of 0.08g crosslinking accelerator and 0.18g composite antioxidant; Wherein, composite antioxidant is by the 0.06g antioxidant 300, and 0.05g irgasfos 168 and 0.07g DTDTP form;
Two, each component taken in step 1 is put into to design temperature the Banbury mixer banburying of 160-200 ℃, melting mixing 5min, the single screw extrusion machine granulation by 190 ℃ of Temperature Settings～210 ℃ of scopes, obtain sample particle.
Three, the sample particle obtained is placed in to the vulcanizer compressing tablet, making thickness is that 1.0mm length is the sheet material that the 145mm width is 105mm, the frequency adopted in microwave equipment is that 2450MHz, power are the microwave induced crosslinked of 800W, after reaction times 60s, room temperature is placed 16h, obtains a kind of microwave induced crosslinked crosslinked polyolefin insulating material.
A kind of microwave induced crosslinked crosslinked polyolefin insulating material prepared by the present embodiment, mechanical property strengthens, tensile strength has improved 20%, heat-drawn wire improves 20-30%, and performance index meet the JB/T10437-2004 electric wire and use in the crosslinkable polyethylene Insulation Material crosslinked with silicane electric wire and cable material tensile strength and the desired performance index of gel content, by microwave induced mode, removed the poach process from, water molecules results from the inside of insulating material molecule, mechanical and physical performance impact on system is little, fusing point has improved 13-49 ℃, the stability of material strengthens, water absorption decreased 35.7%-61.3%, the water tolerance of material strengthens.Preparation method's technique of the present embodiment is simple, easy to operate, energy-conserving and environment-protective, production efficiency is high, facility investment is low, the cost of product is low, realistic production requirement.
Embodiment 3
The preparation method of a kind of microwave induced crosslinked crosslinked polyolefin insulating material of the present embodiment, carry out according to the following steps:
One, the MDPE FB2310,2.5g silane coupling A 151,1.25g silicon hexaboride SiB, the 1.5g that accurately take the 100g drying produce aqua zinc borate, 4.2g multi-group crosslink agent tetramethylolmethane tetraene propyl ether, 1.2g crosslinking accelerator ethylene tetrafluoroethylene copolymer and 0.25g composite antioxidant; Wherein, composite antioxidant is by 0.1g oxidation inhibitor 2, the 6-di-tert-butylphenol, and 0.05g oxidation inhibitor tricresyl phosphate benzene methyl and 0.1g DLTP form;
Two, each component taken in step 1 is put into to design temperature the Banbury mixer banburying of 160-200 ℃, melting mixing 5min, the single screw extrusion machine granulation by 190 ℃ of Temperature Settings～210 ℃ of scopes, obtain sample particle.
Three, the sample particle obtained is placed in to the vulcanizer compressing tablet, making thickness is that 1.0mm length is the sheet material that the 145mm width is 105mm, the frequency adopted in microwave equipment is that 2450MHz, power are the microwave induced crosslinked of 800W, after reaction times 60s, room temperature is placed 16h, obtains a kind of microwave induced crosslinked crosslinked polyolefin insulating material.
A kind of microwave induced crosslinked crosslinked polyolefin insulating material prepared by the present embodiment, mechanical property strengthens, tensile strength has improved 20%, heat-drawn wire improves 20-30%, and performance index meet the JB/T10437-2004 electric wire and use in the crosslinkable polyethylene Insulation Material crosslinked with silicane electric wire and cable material tensile strength and the desired performance index of gel content, by microwave induced mode, removed the poach process from, water molecules results from the inside of insulating material molecule, mechanical and physical performance impact on system is little, fusing point has improved 13-49 ℃, the stability of material strengthens, water absorption decreased 35.7%-61.3%, the water tolerance of material strengthens.Preparation method's technique of the present embodiment is simple, easy to operate, energy-conserving and environment-protective, production efficiency is high, facility investment is low, the cost of product is low, realistic production requirement.
Embodiment 4
The preparation method of a kind of microwave induced crosslinked crosslinked polyolefin insulating material of the present embodiment, carry out according to the following steps:
One, the MDPE3721C, 1.5g silane coupling agent γ aminopropyltriethoxy silane, 1.8g silicon hexaboride SiN, the 0.48g that accurately take the 100g drying produce aqua Mg (OH)
2, 2.5g multi-group crosslink agent PETAE, 3.0g crosslinking accelerator hexachloroethane and 0.4g composite antioxidant; Wherein, composite antioxidant is by the 0.2g antioxidant 1010, and 0.14g oxidation inhibitor TIOP and 0.06g DLTP form;
Two, each component taken in step 1 is put into to design temperature the Banbury mixer banburying of 160-200 ℃, melting mixing 5min, the single screw extrusion machine granulation by 190 ℃ of Temperature Settings～210 ℃ of scopes, obtain sample particle.
Three, the sample particle obtained is placed in to the vulcanizer compressing tablet, making thickness is that 1.0mm length is the sheet material that the 145mm width is 105mm, the frequency adopted in microwave equipment is that 2450MHz, power are the microwave induced crosslinked of 800W, after reaction times 60s, room temperature is placed 16h, obtains a kind of microwave induced crosslinked crosslinked polyolefin insulating material.
A kind of microwave induced crosslinked crosslinked polyolefin insulating material prepared by the present embodiment, mechanical property strengthens, tensile strength has improved 20%, heat-drawn wire improves 20-30%, and performance index meet the JB/T10437-2004 electric wire and use in the crosslinkable polyethylene Insulation Material crosslinked with silicane electric wire and cable material tensile strength and the desired performance index of gel content, by microwave induced mode, removed the poach process from, water molecules results from the inside of insulating material molecule, mechanical and physical performance impact on system is little, fusing point has improved 13-49 ℃, the stability of material strengthens, water absorption decreased 35.7%-61.3%, the water tolerance of material strengthens.Preparation method's technique of the present embodiment is simple, easy to operate, energy-conserving and environment-protective, production efficiency is high, facility investment is low, the cost of product is low, realistic production requirement.
Embodiment 5
The preparation method of a kind of microwave induced crosslinked crosslinked polyolefin insulating material of the present embodiment, carry out according to the following steps:
One, accurately take HDPE5000s, 3.5g silane coupling A 151, the 1.6g tetra-boronation three silicon Si of 100g drying
3b
4, 1.8g produces aqua Cadmium sulfate hydrate, 3.2g multi-group crosslink agent triglycol methacrylic ester, 3.5g crosslinking accelerator ethene-1 and 0.36g composite antioxidant; Wherein, composite antioxidant is by 0.17g oxidation inhibitor 246, and 0.12g oxidation inhibitor TPP and 0.07g LSTP form;
Two, each component taken in step 1 is put into to design temperature the Banbury mixer banburying of 160-200 ℃, melting mixing 5min, the single screw extrusion machine granulation by 190 ℃ of Temperature Settings～210 ℃ of scopes, obtain sample particle.
Three, the sample particle obtained is placed in to the vulcanizer compressing tablet, making thickness is that 1.0mm length is the sheet material that the 145mm width is 105mm, the frequency adopted in microwave equipment is that 2450MHz, power are the microwave induced crosslinked of 800W, after reaction times 60s, room temperature is placed 16h, obtains a kind of microwave induced crosslinked crosslinked polyolefin insulating material.
A kind of microwave induced crosslinked crosslinked polyolefin insulating material prepared by the present embodiment, mechanical property strengthens, tensile strength has improved 20%, heat-drawn wire improves 20-30%, and performance index meet the JB/T10437-2004 electric wire and use in the crosslinkable polyethylene Insulation Material crosslinked with silicane electric wire and cable material tensile strength and the desired performance index of gel content, by microwave induced mode, removed the poach process from, water molecules results from the inside of insulating material molecule, mechanical and physical performance impact on system is little, fusing point has improved 13-49 ℃, the stability of material strengthens, water absorption decreased 35.7%-61.3%, the water tolerance of material strengthens.Preparation method's technique of the present embodiment is simple, easy to operate, energy-conserving and environment-protective, production efficiency is high, facility investment is low, the cost of product is low, realistic production requirement.
Embodiment 6
The preparation method of a kind of microwave induced crosslinked crosslinked polyolefin insulating material of the present embodiment, carry out according to the following steps:
One, accurately take HDPE5300B, the 3.0g silane coupling agent β of 100g drying-(3,4-epoxycyclohexyl) ethyl trimethoxy silane, 1.4g silicon carbide SiC, 1.5g produce aqua Mg (OH)
2, 3.5g multi-group crosslink agent TMPTA, 4.2g crosslinking accelerator tetrachloromethane and 0.32g composite antioxidant; Wherein, composite antioxidant is by the 0.15g antioxidant 1010, and 0.07g irgasfos 168 and 0.1g DTDTP form;
Two, each component taken in step 1 is put into to design temperature the Banbury mixer banburying of 160-200 ℃, melting mixing 5min, the single screw extrusion machine granulation by 190 ℃ of Temperature Settings～210 ℃ of scopes, obtain sample particle.
Three, the sample particle obtained is placed in to the vulcanizer compressing tablet, making thickness is that 1.0mm length is the sheet material that the 145mm width is 105mm, the frequency adopted in microwave equipment is that 2450MHz, power are the microwave induced crosslinked of 800W, after reaction times 60s, room temperature is placed 16h, obtains a kind of microwave induced crosslinked crosslinked polyolefin insulating material.
A kind of microwave induced crosslinked crosslinked polyolefin insulating material prepared by the present embodiment, mechanical property strengthens, tensile strength has improved 20%, heat-drawn wire improves 20-30%, and performance index meet the JB/T10437-2004 electric wire and use in the crosslinkable polyethylene Insulation Material crosslinked with silicane electric wire and cable material tensile strength and the desired performance index of gel content, by microwave induced mode, removed the poach process from, water molecules results from the inside of insulating material molecule, mechanical and physical performance impact on system is little, fusing point has improved 13-49 ℃, the stability of material strengthens, water absorption decreased 35.7%-61.3%, the water tolerance of material strengthens.Preparation method's technique of the present embodiment is simple, easy to operate, energy-conserving and environment-protective, production efficiency is high, facility investment is low, the cost of product is low, realistic production requirement.
Embodiment 7
The preparation method of a kind of microwave induced crosslinked crosslinked polyolefin insulating material of the present embodiment, carry out according to the following steps:
One, accurately take LDPE LD100, the 3.5g silane coupling agent γ of 100g drying-second phenodiazine base propyl trimethoxy silicane, 1.2g silicon nitride SiN, 1.65g produce aqua zinc borate, 4.9g multi-group crosslink agent TAC, 4.7g crosslinking accelerator tetrachloromethane and 0.27g composite antioxidant; Wherein, composite antioxidant is by the 0.12g antioxidant 300, and 0.04g oxidation inhibitor tricresyl phosphate benzene methyl and 0.11g DLTP form;
Two, each component taken in step 1 is put into to design temperature the Banbury mixer banburying of 160-200 ℃, melting mixing 5min, the single screw extrusion machine granulation by 190 ℃ of Temperature Settings～210 ℃ of scopes, obtain sample particle.
Three, the sample particle obtained is placed in to the vulcanizer compressing tablet, making thickness is that 1.0mm length is the sheet material that the 145mm width is 105mm, the frequency adopted in microwave equipment is that 2450MHz, power are the microwave induced crosslinked of 800W, after reaction times 60s, room temperature is placed 16h, obtains a kind of microwave induced crosslinked crosslinked polyolefin insulating material.
A kind of microwave induced crosslinked crosslinked polyolefin insulating material prepared by the present embodiment, mechanical property strengthens, tensile strength has improved 20%, heat-drawn wire improves 20-30%, and performance index meet the JB/T10437-2004 electric wire and use in the crosslinkable polyethylene Insulation Material crosslinked with silicane electric wire and cable material tensile strength and the desired performance index of gel content, by microwave induced mode, removed the poach process from, water molecules results from the inside of insulating material molecule, mechanical and physical performance impact on system is little, fusing point has improved 13-49 ℃, the stability of material strengthens, water absorption decreased 35.7%-61.3%, the water tolerance of material strengthens.Preparation method's technique of the present embodiment is simple, easy to operate, energy-conserving and environment-protective, production efficiency is high, facility investment is low, the cost of product is low, realistic production requirement.
Embodiment 8
The preparation method of a kind of microwave induced crosslinked crosslinked polyolefin insulating material of the present embodiment, carry out according to the following steps:
One, the LDPE LD615,2.5g silane coupling A 171,0.9g silicon nitride SiC, the 0.45g that accurately take the 100g drying produce aqua AL (OH)
3, 4.6g multi-group crosslink agent TMPAE, 4.1g crosslinking accelerator chlordene methane and 0.19g composite antioxidant; Wherein, composite antioxidant is by 0.08g oxidation inhibitor 246, and 0.05g irgasfos 168 and 0.06g DLTP form;
Two, each component taken in step 1 is put into to design temperature the Banbury mixer banburying of 160-200 ℃, melting mixing 5min, the single screw extrusion machine granulation by 190 ℃ of Temperature Settings～210 ℃ of scopes, obtain sample particle.
Three, the sample particle obtained is placed in to the vulcanizer compressing tablet, making thickness is that 1.0mm length is the sheet material that the 145mm width is 105mm, the frequency adopted in microwave equipment is that 2450MHz, power are the microwave induced crosslinked of 800W, after reaction times 60s, room temperature is placed 16h, obtains a kind of microwave induced crosslinked crosslinked polyolefin insulating material.
A kind of microwave induced crosslinked crosslinked polyolefin insulating material prepared by the present embodiment, mechanical property strengthens, tensile strength has improved 20%, heat-drawn wire improves 20-30%, and performance index meet the JB/T10437-2004 electric wire and use in the crosslinkable polyethylene Insulation Material crosslinked with silicane electric wire and cable material tensile strength and the desired performance index of gel content, by microwave induced mode, removed the poach process from, water molecules results from the inside of insulating material molecule, mechanical and physical performance impact on system is little, fusing point has improved 13-49 ℃, the stability of material strengthens, water absorption decreased 35.7%-61.3%, the water tolerance of material strengthens.Preparation method's technique of the present embodiment is simple, easy to operate, energy-conserving and environment-protective, production efficiency is high, facility investment is low, the cost of product is low, realistic production requirement.
Embodiment 9
The preparation method of a kind of microwave induced crosslinked crosslinked polyolefin insulating material of the present embodiment, carry out according to the following steps:
One, the EVA VA18,4.6g silane coupling agent benzene n-formyl sarcolysine ethyl triethoxy silicane alkane, 2.4g silicon nitride SiC, the 1.7g that accurately take the 100g drying produce aqua Mg (OH)
2, 4.3g multi-group crosslink agent TAIC, 4.6g crosslinking accelerator ethylene-tetrafluoroethylene copolymer and 0.37g composite antioxidant; Wherein, composite antioxidant is by the 0.21g antioxidant 1010, and 0.1g oxidation inhibitor TIOP and 0.06g LSTP form;
Two, each component taken in step 1 is put into to design temperature the Banbury mixer banburying of 160-200 ℃, melting mixing 5min, the single screw extrusion machine granulation by 190 ℃ of Temperature Settings～210 ℃ of scopes, obtain sample particle.
Three, the sample particle obtained is placed in to the vulcanizer compressing tablet, making thickness is that 1.0mm length is the sheet material that the 145mm width is 105mm, the frequency adopted in microwave equipment is that 2450MHz, power are the microwave induced crosslinked of 800W, after reaction times 60s, room temperature is placed 16h, obtains a kind of microwave induced crosslinked crosslinked polyolefin insulating material.
A kind of microwave induced crosslinked crosslinked polyolefin insulating material prepared by the present embodiment, mechanical property strengthens, tensile strength has improved 20%, heat-drawn wire improves 20-30%, and performance index meet the JB/T10437-2004 electric wire and use in the crosslinkable polyethylene Insulation Material crosslinked with silicane electric wire and cable material tensile strength and the desired performance index of gel content, by microwave induced mode, removed the poach process from, water molecules results from the inside of insulating material molecule, mechanical and physical performance impact on system is little, fusing point has improved 13-49 ℃, the stability of material strengthens, water absorption decreased 35.7%-61.3%, the water tolerance of material strengthens.Preparation method's technique of the present embodiment is simple, easy to operate, energy-conserving and environment-protective, production efficiency is high, facility investment is low, the cost of product is low, realistic production requirement.
Embodiment 10
The preparation method of a kind of microwave induced crosslinked crosslinked polyolefin insulating material of the present embodiment, carry out according to the following steps:
One, accurately take EVA VA28, the 4.2g silane coupling agent γ of 100g drying-propyl methacrylate base Trimethoxy silane, 2.8g silicon hexaboride SiB
6, 2.1g produces aqua Al (OH)
3, 4.6g multi-group crosslink agent TAIC, 4.9g crosslinking accelerator ethene fluoride copolymers and 0.45g composite antioxidant; Wherein, composite antioxidant is by the 0.28g antioxidant 300, and 0.12g oxidation inhibitor Tritolyl Phosphate and 0.05g DLTP form;
Two, each component taken in step 1 is put into to design temperature the Banbury mixer banburying of 160-200 ℃, melting mixing 5min, the single screw extrusion machine granulation by 190 ℃ of Temperature Settings～210 ℃ of scopes, obtain sample particle.
Three, the sample particle obtained is placed in to the vulcanizer compressing tablet, making thickness is that 1.0mm length is the sheet material that the 145mm width is 105mm, the frequency adopted in microwave equipment is that 2450MHz, power are the microwave induced crosslinked of 800W, after reaction times 60s, room temperature is placed 16h, obtains a kind of microwave induced crosslinked crosslinked polyolefin insulating material.
A kind of microwave induced crosslinked crosslinked polyolefin insulating material prepared by the present embodiment, mechanical property strengthens, tensile strength has improved 20%, heat-drawn wire improves 20-30%, and performance index meet the JB/T10437-2004 electric wire and use in the crosslinkable polyethylene Insulation Material crosslinked with silicane electric wire and cable material tensile strength and the desired performance index of gel content, by microwave induced mode, removed the poach process from, water molecules results from the inside of insulating material molecule, mechanical and physical performance impact on system is little, fusing point has improved 13-49 ℃, the stability of material strengthens, water absorption decreased 35.7%-61.3%, the water tolerance of material strengthens.Preparation method's technique of the present embodiment is simple, easy to operate, energy-conserving and environment-protective, production efficiency is high, facility investment is low, the cost of product is low, realistic production requirement.
Embodiment 11
The preparation method of a kind of microwave induced crosslinked crosslinked polyolefin insulating material of the present embodiment, carry out according to the following steps:
One, accurately take the HDPE5000s of 75g drying and LLDPE7042,1.6g silane coupling A 171,0.8g silicon carbide SiC, the 0.75g of 25g drying and produce aqua Mg (OH)
2, 3.9g multi-group crosslink agent TMPTA, 3.5g crosslinking accelerator ethylene tetrafluoroethylene copolymer and 0.25g composite antioxidant; Wherein, composite antioxidant is by the 0.15g antioxidant 1010, and 0.07g irgasfos 168 and 0.03g DTDTP form;
Two, each component taken in step 1 is put into to design temperature the Banbury mixer banburying of 160-200 ℃, melting mixing 5min, the single screw extrusion machine granulation by 190 ℃ of Temperature Settings～210 ℃ of scopes, obtain sample particle.
Three, the sample particle obtained is placed in to the vulcanizer compressing tablet, making thickness is that 1.0mm length is the sheet material that the 145mm width is 105mm, the frequency adopted in microwave equipment is that 2450MHz, power are the microwave induced crosslinked of 800W, after reaction times 60s, room temperature is placed 16h, obtains a kind of microwave induced crosslinked crosslinked polyolefin insulating material.
A kind of microwave induced crosslinked crosslinked polyolefin insulating material prepared by the present embodiment, mechanical property strengthens, tensile strength has improved 20%, heat-drawn wire improves 20-30%, and performance index meet the JB/T10437-2004 electric wire and use in the crosslinkable polyethylene Insulation Material crosslinked with silicane electric wire and cable material tensile strength and the desired performance index of gel content, by microwave induced mode, removed the poach process from, water molecules results from the inside of insulating material molecule, mechanical and physical performance impact on system is little, fusing point has improved 13-49 ℃, the stability of material strengthens, water absorption decreased 35.7%-61.3%, the water tolerance of material strengthens.Preparation method's technique of the present embodiment is simple, easy to operate, energy-conserving and environment-protective, production efficiency is high, facility investment is low, the cost of product is low, realistic production requirement.
The microwave induced silanes crosslinked cable of embodiment 1-11 gained is carried out to the test of tensile strength, water-intake rate and gel content with the sample of crosslinked polyolefin insulating material, adopt the fusing point of differential scanning calorimetry test material, test result is as shown in table 2:
The test result of sample tensile strength, fusing point, water-intake rate and the gel content of crosslinked polyolefin insulating material for the microwave induced silanes crosslinked cable of table 2
As shown in Table 2, microwave induced silanes crosslinked cable meets in JB/T10437-2004 electric wire use crosslinkable polyethylene Insulation Material crosslinked with silicane electric wire and cable material tensile strength and the desired performance index of gel content by the performance index of crosslinked polyolefin insulating material, and fusing point improves, increase the stability of material; Water absorption decreased, the water tolerance of increase material.
Claims (10)
1. a microwave induced crosslinked crosslinked polyolefin insulating material, is characterized in that it is to be produced aqua, 0.1-5 part multi-group crosslink agent, 0.01-5 part crosslinking accelerator and 0.07-0.5 part oxidation inhibitor and made by polyolefin resin, 0.1-4 part silane coupling agent, 0.1-5 part microwave absorption, 0.1-5 part of 100 parts of dryings.
2. a kind of microwave induced crosslinked crosslinked polyolefin insulating material according to claim 1, is characterized in that described polyolefin resin is that one or more in HDPE, MDPE, LDPE, LLDPE and EVA polyolefin elastomer are mixed by any ratio and form.
3. a kind of microwave induced crosslinked crosslinked polyolefin insulating material according to claim 1, it is characterized in that described silane coupling agent is that one or more in vinyltrimethoxy silane, vinyltriethoxysilane, γ aminopropyltriethoxy silane, benzene n-formyl sarcolysine ethyl triethoxy silicane alkane, γ-second phenodiazine base propyl trimethoxy silicane, β-(3,4-epoxycyclohexyl) ethyl trimethoxy silane and γ-propyl methacrylate base Trimethoxy silane are mixed by any ratio and form.
4. a kind of microwave induced crosslinked crosslinked polyolefin insulating material according to claim 1, is characterized in that described microwave absorption is SiC, SiN, SiB
6and Si
3b
4in one or more be mixed by any ratio and form.
5. a kind of microwave induced crosslinked crosslinked polyolefin insulating material according to claim 1, is characterized in that described product aqua is Mg (OH)
2, Al (OH)
3, 2ZnOB
2o
33.5H
2o and CdSO
48H
2one or more in O are mixed by any ratio and form.
6. a kind of microwave induced crosslinked crosslinked polyolefin insulating material according to claim 1, is characterized in that described multi-group crosslink agent for TAC, TAIC, TMPTA, TMPAE, ETAE, tetramethylolmethane tetraene propyl ether or/and one or more in TEGMA are mixed by any ratio forms.
7. a kind of microwave induced crosslinked crosslinked polyolefin insulating material according to claim 1, it is characterized in that described crosslinking accelerator is ethylene-tetrafluoroethylene copolymer, ethene-1, one or more in chlorotrifluoroethylcopolymer copolymer, ethene-fluoride copolymers, hexachloroethane, tetrachloromethane are mixed by any ratio and form.
8. a kind of microwave induced crosslinked crosslinked polyolefin insulating material according to claim 1, is characterized in that described oxidation inhibitor is by phenols, phosphorous acid esters, phosphoric acid ester, containing two or more in the thioesters kind antioxidant, is mixed by any ratio and forms; Wherein, phenolic antioxidant is 2,6-di-tert-butylphenol, 2,4,6-tri-tert-butylphenol, 4,4 '-thiobis (6-tertiary butyl-3-methylphenol) or four [methylene radical-3-(3 ', 5 '-di-tert-butyl-4 '-hydroxy phenyl) propionic acid] pentaerythritol ester; Phosphorous acid esters or phosphoric acid ester oxidation inhibitor are TPP, tricresyl phosphite (2,4-di-tert-butyl phenyl) ester, TIOP or tricresyl phosphate benzene methyl; Containing the thioesters kind antioxidant, be DLTP, LSTP or DTDTP.
9. a kind of microwave induced crosslinked crosslinked polyolefin insulating material according to claim 1, is characterized in that it is to be made by the polyolefin resin of 100 parts of dryings, 0.15 part of silane coupling agent, 0.18 part of microwave absorption, 0.16 part of product aqua, 0.35 part of multi-group crosslink agent, 0.026 part of crosslinking accelerator and 0.15 part of oxidation inhibitor.
10. a method for preparing microwave induced crosslinked crosslinked polyolefin insulating material claimed in claim 1 is characterized in that it is to carry out according to the following steps:
Step 1: polyolefin resin, 0.1-4 part silane coupling agent, 0.1-5 part microwave absorption, 0.1-5 part of taking 100 parts of dryings by mass fraction are produced aqua, 0.1-5 part multi-group crosslink agent, 0.01-5 part crosslinking accelerator and 0.07-0.5 part oxidation inhibitor;
Step 2: banburying in the Banbury mixer that is 160-200 ℃ in temperature by above-mentioned each material, melting mixing 5min; Carry out granulation in the single screw extrusion machine that is 190 ℃-210 ℃ at Temperature Setting, obtain sample particle;
Step 3: the sample particle obtained is placed in to the vulcanizer compressing tablet, making thickness is that 1.0mm length is the sheet material that the 145mm width is 105mm, the frequency adopted in microwave equipment is that 2450MHz, power are the microwave induced crosslinked of 800W, after reaction times is 60s, place 16h in room temperature, obtain microwave induced crosslinked crosslinked polyolefin insulating material.
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