CN112048177A - Environment-friendly cable insulation protection material and preparation method thereof - Google Patents
Environment-friendly cable insulation protection material and preparation method thereof Download PDFInfo
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- 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
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Abstract
The invention discloses an environment-friendly cable insulation protective material which is characterized by comprising the following components in parts by weight: 20-30 parts of 4, 4-diaminodiphenyl sulfide/1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate, 30-50 parts of 3,3' -diamino-4, 4' -difluorodiphenyl sulfone/carboxyl-terminated polybutadiene rubber polycondensate, 3-6 parts of 2,2' -dihydroxy-4, 4' -dimethoxybenzophenone-5, 5' -disulfonic acid, 0.5-1.5 parts of phosphorus pentoxide, 2-4 parts of epoxy-terminated hyperbranched polyphosphate, 1-2 parts of coupling agent, 1-2 parts of vulcanizing agent and 1-3 parts of nano boron fiber. The invention also provides a preparation method of the environment-friendly cable insulation protective material. The environment-friendly cable insulation protective material disclosed by the invention is excellent in comprehensive performance, good in flame retardance, weather resistance and performance stability, good in heat resistance, corrosion resistance and insulativity, safe and environment-friendly to use and long in service life.
Description
Technical Field
The invention relates to the technical field of cable materials, in particular to an environment-friendly cable insulation protection material and a preparation method thereof.
Background
With the rapid growth of the economy and the continuous improvement of the level of science and technology in China, the pace of various economic constructions is rapidly accelerated, and the demand of various industries on cables is increased. The cable protection material is located outside the cable core material, and forms a cable together with the conductive core material inside the cable, so that the cable protection material is an important protection layer for a cable core, and plays a role in protecting the cable from being damaged by the outside and ensuring the electricity utilization safety. The quality of the cable protective material is directly related to the quality of the cable. Therefore, the development of the cable protective material with excellent comprehensive performance is very important.
The cable protective material in the prior art mostly adopts rubber or polyvinyl chloride material as main material, and the material can also protect the cable from being exposed, and has the problems of electric leakage and the like. However, the problems of abrasion, electric leakage, corrosion, high-temperature deformation and the like often occur in the using process, and the normal use of the cable is influenced. The products of rubber combustion have great pollution to the environment, polyvinyl chloride contains halogen, and a large amount of smoke and toxic and corrosive gas are released during combustion, so that the dangerous factors in fire hazard can prevent people from safely evacuating and extinguishing fire, and the life and property are seriously lost. In addition, the cable protective materials on the market have the defects of poor flame retardant property and weather resistance, insufficient performance stability, and further improvement of heat resistance, corrosion resistance and insulation property.
The Chinese invention patent with the application number of 201810158704.X discloses a flame-retardant cable protective sleeve, which comprises the following raw materials in parts by weight: 20-30 parts of polyvinyl chloride resin, 15-26 parts of polypropylene resin, 12-19 parts of chloroprene rubber, 8-13 parts of natural rubber, 7-14 parts of activated calcium carbonate, 2-6 parts of antimony trioxide, 3-5 parts of zinc oxide, 3-7 parts of paraffin, 1-3 parts of stearic acid, 2-4 parts of antioxidant, 2-5 parts of plasticizer, 6-12 parts of modified montmorillonite and 4-8 parts of high-wear-resistance carbon black. The flame-retardant cable protective sleeve disclosed by the invention is good in flame retardant property, good in weather resistance and mechanical property and good in stability. The chlorine contained in the smoke can release a large amount of smoke and toxic and corrosive gases during combustion, pollute the environment and are not beneficial to environmental protection.
Therefore, the environment-friendly cable insulation protective material which has excellent comprehensive performance, good flame retardant property, weather resistance and performance stability, good heat resistance, corrosion resistance and insulativity, is safe and environment-friendly to use is developed, meets the market demand, has wide market value and application prospect, and plays an important role in promoting the development of the wire and cable industry.
Disclosure of Invention
In view of the above, the invention aims to provide an environment-friendly cable insulation protective material which has excellent comprehensive performance, good flame retardant property, weather resistance and performance stability, good heat resistance, corrosion resistance and insulation property, safe and environment-friendly use and long service life. Meanwhile, the invention also provides a preparation method of the environment-friendly cable insulation protective material, and the preparation method is simple and easy to operate, low in preparation cost, low in requirements on reaction conditions and equipment, high in preparation efficiency and suitable for continuous large-scale production.
In order to achieve the purpose, the invention adopts the technical scheme that:
the environment-friendly cable insulation protective material is characterized by comprising the following components in parts by weight: 20-30 parts of 4, 4-diaminodiphenyl sulfide/1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate, 30-50 parts of 3,3' -diamino-4, 4' -difluorodiphenyl sulfone/carboxyl-terminated polybutadiene rubber polycondensate, 3-6 parts of 2,2' -dihydroxy-4, 4' -dimethoxybenzophenone-5, 5' -disulfonic acid, 0.5-1.5 parts of phosphorus pentoxide, 2-4 parts of epoxy-terminated hyperbranched polyphosphate, 1-2 parts of coupling agent, 1-2 parts of vulcanizing agent and 1-3 parts of nano boron fiber.
Preferably, the coupling agent is at least one of a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH 570.
Preferably, the vulcanizing agent is one or more of dibenzoyl peroxide, tetramethylthiuram disulfide and zinc dibutyl dithiocarbamate.
Preferably, the preparation method of the epoxy-terminated hyperbranched polyphosphate is described in the Chinese patent application No. 201810153507.9, example 8.
Preferably, the carboxyl-terminated polybutadiene rubber has a number average molecular weight of 5000, and is available from Zibozilon chemical Co.
Preferably, the preparation method of the 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone/carboxyl-terminated polybutadiene rubber polycondensate comprises the following steps: adding 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone and carboxyl-terminated polybutadiene rubber into a high boiling point solvent, stirring for 15-25 minutes at 35-55 ℃, then adding (1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride) and N-hydroxysuccinimide, continuing to perform heat preservation reaction for 6-8 hours, then precipitating in water, and then placing the precipitated polymer in a vacuum drying oven for drying at 85-95 ℃ to constant weight to obtain the 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone/carboxyl-terminated polybutadiene rubber polycondensate.
Preferably, the molar ratio of the 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone, the carboxyl-terminated polybutadiene rubber, the high-boiling-point solvent, (1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride) and the N-hydroxysuccinimide is 1:1 (6-10) to 0.8-1.2: 0.5.
Preferably, the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide and N, N-dimethylacetamide.
Preferably, the method for preparing the 4, 4-diaminodiphenyl sulfide/1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate comprises the following steps: dissolving 4, 4-diaminodiphenyl sulfide and 1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate in N-methylpyrrolidone to form a solution, adding the solution into a reaction kettle, replacing the air in the kettle with nitrogen or inert gas, then reacting for 3-5 hours at the temperature of 140-160 ℃ under normal pressure, adding a catalyst into the reaction system, heating to the temperature of 230-260 ℃, carrying out polycondensation reaction for 13-18 hours under the pressure of 100-300Pa, cooling to room temperature, adjusting to normal pressure, precipitating in water, washing the precipitated polymer with ethanol for 3-6 times, and drying in a vacuum drying oven at 80-90 deg.C to constant weight to obtain 4, 4-diaminodiphenyl sulfide/1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate.
Preferably, the catalyst is at least one of thiophosphonate, thiophosphoramide and phosphorous acid; the inert gas is any one of helium, neon and argon.
Preferably, the molar ratio of the 4, 4-diaminodiphenyl sulfide, the 1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate, the N-methylpyrrolidone and the catalyst is 1:1 (6-10) to (0.6-1).
The invention also aims to provide a preparation method of the environment-friendly cable insulation protective material, which is characterized by comprising the following steps: the components are uniformly mixed according to the parts by weight to form a mixture, and then the mixture is added into a double-screw extruder to be extruded and molded to obtain the environment-friendly cable insulation protective material.
Preferably, the extrusion molding specifically includes the following temperature control parameters: the material supply section 165-.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
(1) the preparation method of the environment-friendly cable insulation protection material provided by the invention is simple and easy to operate, low in preparation cost, low in requirements on reaction conditions and equipment, high in preparation efficiency and suitable for continuous large-scale production.
(2) The environment-friendly cable insulation protective material provided by the invention overcomes the problems of abrasion, electric leakage, corrosion, high-temperature deformation and the like of the traditional cable protective material in the using process, overcomes the defects of poor flame retardant property, environmental protection property and weather resistance, insufficient performance stability and further improved heat resistance, corrosion resistance and insulativity of the cable protective material on the market, and has the advantages of excellent comprehensive performance, good flame retardant property, weather resistance and performance stability, good heat resistance, corrosion resistance and insulativity, safety and environmental protection in use and long service life.
(3) According to the environment-friendly cable insulation protective material provided by the invention, the added 4, 4-diaminodiphenyl sulfide/1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate and the added 3,3' -diamino-4, 4' -difluorodiphenyl sulfone/carboxyl-terminated polybutadiene rubber polycondensate are of polyamide structures, so that the polyamide structures have good compatibility, the molecular chains of the two substances both contain benzene rings, and the sulfonic group on the added 2,2' -dihydroxy-4, 4' -dimethoxybenzophenone-5, 5' -disulfonic acid can react with the benzene rings under the catalysis of phosphorus pentoxide to form a three-dimensional network structure, so that the comprehensive performance is effectively improved. The existence of the silicon-oxygen bond and the polybutadiene structure on the molecular chain of the two substances can effectively ensure the elasticity of the material, and the synergistic effect of the structures such as thioether bond, silicon-oxygen bond, fluorine, phenylsulfone and the like on the molecular chain can effectively improve the insulating property, weather resistance and performance stability of the material.
(4) According to the environment-friendly cable insulation protective material provided by the invention, phosphorus pentoxide and epoxy-terminated hyperbranched polyphosphate are added to realize a synergistic effect, so that the material is better in flame-retardant and fireproof performance, does not contain halogen, and is more environment-friendly; the end epoxy groups on the structure of the end epoxy group hyperbranched polyphosphate ester are easy to chemically react with the end groups of a 4, 4-diaminodiphenyl sulfide/1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate and a 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone/end carboxyl polybutadiene rubber polycondensate, so that all main base materials are connected in a chemical bond form, and the comprehensive performance of the material is effectively improved; the introduction of hyperbranched structures also improves the elasticity. The added nano boron fiber can improve mechanical property and flame retardance. The 2,2' -dihydroxy-4, 4' -dimethoxy benzophenone-5, 5' -disulfonic acid is used as a cross-linking agent, and the introduction of a benzophenone structure can improve the ultraviolet aging resistance of the material.
Detailed Description
In order to make the technical solutions of the present invention better understood and make the above features, objects, and advantages of the present invention more comprehensible, the present invention is further described with reference to the following examples. The examples are intended to illustrate the invention only and are not intended to limit the scope of the invention.
In the embodiment of the invention, the raw materials are all purchased commercially; the preparation method of the epoxy-terminated hyperbranched polyphosphate refers to the following steps: chinese invention patent example 8 with application number 201810153507.9; the carboxyl-terminated polybutadiene rubber has the number average molecular weight of 5000 and is purchased from Zibozilon chemical Co.
Example 1
The environment-friendly cable insulation protective material is characterized by comprising the following components in parts by weight: 20 parts of 4, 4-diaminodiphenyl sulfide/1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate, 30 parts of 3,3' -diamino-4, 4' -difluorodiphenyl sulfone/carboxyl-terminated polybutadiene rubber polycondensate, 3 parts of 2,2' -dihydroxy-4, 4' -dimethoxybenzophenone-5, 5' -disulfonic acid, 0.5 part of phosphorus pentoxide, 2 parts of epoxy-terminated hyperbranched polyphosphate, 1 part of silane coupling agent KH5501 part, 1 part of dibenzoyl peroxide and 1 part of nano boron fiber.
The preparation method of the 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone/carboxyl-terminated polybutadiene rubber polycondensate comprises the following steps: adding 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone and carboxyl-terminated polybutadiene rubber into dimethyl sulfoxide, stirring for 15 minutes at 35 ℃, then adding (1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride) and N-hydroxysuccinimide into the dimethyl sulfoxide, continuing to perform heat preservation reaction for 6 hours, then precipitating the mixture in water, and then placing the precipitated polymer in a vacuum drying oven at 85 ℃ to dry to constant weight to obtain a 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone/carboxyl-terminated polybutadiene rubber polycondensate; the molar ratio of the 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone to the carboxyl-terminated polybutadiene rubber to the dimethyl sulfoxide to the (1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride) N-hydroxysuccinimide is 1:1:6:0.8: 0.5.
The preparation method of the 4, 4-diaminodiphenyl sulfide/1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate comprises the following steps: dissolving 4, 4-diaminodiphenyl sulfide and 1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate in N-methylpyrrolidone to form a solution, adding the solution into a reaction kettle, replacing air in the reaction kettle with nitrogen, then reacting for 3 hours at 140 ℃ under normal pressure, adding thiophosphonate into a reaction system, heating to 230 ℃, carrying out polycondensation reaction for 13 hours under 100Pa, cooling to room temperature, adjusting to normal pressure, precipitating in water, washing the precipitated polymer for 3 times with ethanol, and finally drying in a vacuum drying oven at 80 ℃ to constant weight to obtain the 4, 4-diaminodiphenyl sulfide/1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate; the molar ratio of the 4, 4-diaminodiphenyl sulfide, the 1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate, the N-methylpyrrolidone and the thiophosphonate is 1:1:6: 0.6.
The preparation method of the environment-friendly cable insulation protective material is characterized by comprising the following steps: uniformly mixing the components in parts by weight to form a mixture, and then adding the mixture into a double-screw extruder for extrusion molding to obtain the environment-friendly cable insulation protective material; the extrusion molding specifically comprises the following temperature control parameters: the feeding section is 165 ℃, the compression section is 180 ℃, the head temperature is 190 ℃, the neck mold temperature is 195 ℃, the production speed is controlled to be 250m/min, and the screw rotating speed is controlled to be 40 r/min.
Example 2
The environment-friendly cable insulation protective material is characterized by comprising the following components in parts by weight: 22 parts of 4, 4-diaminodiphenyl sulfide/1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate, 35 parts of 3,3' -diamino-4, 4' -difluorodiphenyl sulfone/carboxyl-terminated polybutadiene rubber polycondensate, 4 parts of 2,2' -dihydroxy-4, 4' -dimethoxybenzophenone-5, 5' -disulfonic acid, 0.7 part of phosphorus pentoxide, 2.5 parts of epoxy-terminated hyperbranched polyphosphate, KH5601.2 parts of a silane coupling agent, 1.2 parts of tetramethylthiuram disulfide and 1.5 parts of nano boron fiber.
The preparation method of the 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone/carboxyl-terminated polybutadiene rubber polycondensate comprises the following steps: adding 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone and carboxyl-terminated polybutadiene rubber into N, N-dimethylformamide, stirring for 17 minutes at 40 ℃, then adding (1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride) and N-hydroxysuccinimide into the mixture, continuing to perform heat preservation reaction for 6.5 hours, then precipitating the mixture in water, and then placing the precipitated polymer in a vacuum drying oven to be dried to constant weight at 87 ℃ to obtain a 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone/carboxyl-terminated polybutadiene rubber polycondensate; the molar ratio of the 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone to the carboxyl-terminated polybutadiene rubber to the N, N-dimethylformamide to the (1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride) N-hydroxysuccinimide is 1:1:7:0.9: 0.5.
The preparation method of the 4, 4-diaminodiphenyl sulfide/1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate comprises the following steps: dissolving 4, 4-diaminodiphenyl sulfide and 1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate in N-methylpyrrolidone to form a solution, adding the solution into a reaction kettle, replacing air in the reaction kettle with helium, then reacting for 3.5 hours at 145 ℃ under normal pressure, adding thiophosphoramide into a reaction system, heating to 240 ℃, carrying out polycondensation reaction for 14 hours under 150Pa, cooling to room temperature, adjusting to normal pressure, precipitating in water, washing the precipitated polymer for 3-6 times with ethanol, and finally drying to constant weight in a vacuum drying oven at 82 ℃ to obtain the 4, 4-diaminodiphenyl sulfide/1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate; the molar ratio of the 4, 4-diaminodiphenyl sulfide, the 1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate, the N-methylpyrrolidone and the catalyst is 1:1:7: 0.7.
The preparation method of the environment-friendly cable insulation protective material is characterized by comprising the following steps: uniformly mixing the components in parts by weight to form a mixture, and then adding the mixture into a double-screw extruder for extrusion molding to obtain the environment-friendly cable insulation protective material; the extrusion molding specifically comprises the following temperature control parameters: the feeding section is 168 ℃, the compression section is 183 ℃, the head temperature is 193 ℃, the mouth mold temperature is 198 ℃, the production speed is controlled to be 260m/min, and the screw rotating speed is controlled to be 45 r/min.
Example 3
The environment-friendly cable insulation protective material is characterized by comprising the following components in parts by weight: 25 parts of 4, 4-diaminodiphenyl sulfide/1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate, 40 parts of 3,3' -diamino-4, 4' -difluorodiphenyl sulfone/carboxyl-terminated polybutadiene rubber polycondensate, 4.5 parts of 2,2' -dihydroxy-4, 4' -dimethoxybenzophenone-5, 5' -disulfonic acid, 1 part of phosphorus pentoxide, 3 parts of epoxy-terminated hyperbranched polyphosphate, KH5701.5 parts of a silane coupling agent, 1.5 parts of zinc dibutyl dithiocarbamate and 2 parts of nano boron fiber.
The preparation method of the 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone/carboxyl-terminated polybutadiene rubber polycondensate comprises the following steps: adding 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone and carboxyl-terminated polybutadiene rubber into N, N-dimethylacetamide, stirring for 20 minutes at 45 ℃, then adding (1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride) and N-hydroxysuccinimide into the mixture, continuing to perform heat preservation reaction for 7 hours, then precipitating the mixture in water, and then placing the precipitated polymer in a vacuum drying oven to be dried to constant weight at 90 ℃ to obtain a 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone/carboxyl-terminated polybutadiene rubber polycondensate; the molar ratio of the 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone to the carboxyl-terminated polybutadiene rubber to the N, N-dimethylacetamide to the (1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride) and the N-hydroxysuccinimide is 1:1:8:1: 0.5.
The preparation method of the 4, 4-diaminodiphenyl sulfide/1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate comprises the following steps: dissolving 4, 4-diaminodiphenyl sulfide and 1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate in N-methylpyrrolidone to form a solution, adding the solution into a reaction kettle, replacing air in the reaction kettle with neon, then reacting for 4 hours at 150 ℃ under normal pressure, adding phosphorous acid into a reaction system, heating to 245 ℃, carrying out polycondensation reaction for 15 hours under 200Pa, cooling to room temperature, adjusting to normal pressure, precipitating in water, washing the precipitated polymer for 5 times by using ethanol, and finally drying in a vacuum drying oven at 85 ℃ to constant weight to obtain the 4, 4-diaminodiphenyl sulfide/1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate; the molar ratio of the 4, 4-diaminodiphenyl sulfide, the 1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate, the N-methylpyrrolidone and the phosphorous acid is 1:1:8: 0.8.
The preparation method of the environment-friendly cable insulation protective material is characterized by comprising the following steps: uniformly mixing the components in parts by weight to form a mixture, and then adding the mixture into a double-screw extruder for extrusion molding to obtain the environment-friendly cable insulation protective material; the extrusion molding specifically comprises the following temperature control parameters: the feeding section is 170 ℃, the compression section is 185 ℃, the head temperature is 195 ℃, the neck mold temperature is 200 ℃, the production speed is controlled to be 280m/min, and the screw rotating speed is controlled to be 50 r/min.
Example 4
The environment-friendly cable insulation protective material is characterized by comprising the following components in parts by weight: 29 parts of 4, 4-diaminodiphenyl sulfide/1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate, 48 parts of 3,3' -diamino-4, 4' -difluorodiphenyl sulfone/carboxyl-terminated polybutadiene rubber polycondensate, 5.5 parts of 2,2' -dihydroxy-4, 4' -dimethoxybenzophenone-5, 5' -disulfonic acid, 1.4 parts of phosphorus pentoxide, 3.5 parts of epoxy-terminated hyperbranched polyphosphate, 1.8 parts of coupling agent, 1.8 parts of vulcanizing agent and 2.5 parts of nano boron fiber.
The coupling agent is formed by mixing a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH570 according to the mass ratio of 1:3: 2; the vulcanizing agent is prepared by mixing dibenzoyl peroxide, tetramethyl thiuram disulfide and zinc dibutyl dithiocarbamate according to the mass ratio of 1:3: 2.
The preparation method of the 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone/carboxyl-terminated polybutadiene rubber polycondensate comprises the following steps: adding 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone and carboxyl-terminated polybutadiene rubber into a high boiling point solvent, stirring for 23 minutes at 53 ℃, then adding (1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride) and N-hydroxysuccinimide into the solvent, continuing to perform heat preservation reaction for 7.5 hours, then precipitating the mixture in water, and then placing the precipitated polymer in a vacuum drying oven at 93 ℃ for drying to constant weight to obtain a 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone/carboxyl-terminated polybutadiene rubber polycondensate; the molar ratio of the 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone to the carboxyl-terminated polybutadiene rubber to the high-boiling-point solvent to the (1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride) to the N-hydroxysuccinimide is 1:1:9:1.1: 0.5; the high boiling point solvent is formed by mixing dimethyl sulfoxide, N-dimethylformamide and N, N-dimethylacetamide according to a mass ratio of 1:3: 2.
The preparation method of the 4, 4-diaminodiphenyl sulfide/1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate comprises the following steps: dissolving 4, 4-diaminodiphenyl sulfide and 1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate in N-methylpyrrolidone to form a solution, adding the solution into a reaction kettle, replacing air in the reaction kettle with argon, then reacting for 4.5 hours at 157 ℃ under normal pressure, adding a catalyst into a reaction system, heating to 255 ℃, carrying out polycondensation reaction for 17 hours under 250Pa, cooling to room temperature, adjusting to normal pressure, precipitating in water, washing the precipitated polymer for 6 times with ethanol, and finally drying in a vacuum drying oven at 88 ℃ to constant weight to obtain the 4, 4-diaminodiphenyl sulfide/1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate; the catalyst is formed by mixing thiophosphonate, thiophosphoryl amide and phosphorous acid according to the mass ratio of 1:2: 1; the molar ratio of the 4, 4-diaminodiphenyl sulfide, the 1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate, the N-methylpyrrolidone and the catalyst is 1:1:9.5: 0.9.
The preparation method of the environment-friendly cable insulation protective material is characterized by comprising the following steps: uniformly mixing the components in parts by weight to form a mixture, and then adding the mixture into a double-screw extruder for extrusion molding to obtain the environment-friendly cable insulation protective material; the extrusion molding specifically comprises the following temperature control parameters: 173 ℃ of the feeding section, 188 ℃ of the compression section, 198 ℃ of the head, 203 ℃ of the mouth mold, 290m/min of production speed control and 57r/min of screw rotation speed control.
Example 5
The environment-friendly cable insulation protective material is characterized by comprising the following components in parts by weight: 30 parts of 4, 4-diaminodiphenyl sulfide/1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate, 50 parts of 3,3' -diamino-4, 4' -difluorodiphenyl sulfone/carboxyl-terminated polybutadiene rubber polycondensate, 6 parts of 2,2' -dihydroxy-4, 4' -dimethoxybenzophenone-5, 5' -disulfonic acid, 1.5 parts of phosphorus pentoxide, 4 parts of terminal epoxy hyperbranched polyphosphate, 2 parts of silane coupling agent KH5502 parts, 2 parts of tetramethylthiuram disulfide and 3 parts of nano boron fiber.
The preparation method of the 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone/carboxyl-terminated polybutadiene rubber polycondensate comprises the following steps: adding 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone and carboxyl-terminated polybutadiene rubber into N, N-dimethylformamide, stirring for 25 minutes at 55 ℃, then adding (1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride) and N-hydroxysuccinimide into the mixture, continuing to perform heat preservation reaction for 8 hours, then precipitating the mixture in water, and then placing the precipitated polymer in a vacuum drying oven to be dried to constant weight at 95 ℃ to obtain a 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone/carboxyl-terminated polybutadiene rubber polycondensate; the molar ratio of the 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone to the carboxyl-terminated polybutadiene rubber to the N, N-dimethylformamide to the (1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride) to the N-hydroxysuccinimide is 1:1:10:1.2: 0.5.
The preparation method of the 4, 4-diaminodiphenyl sulfide/1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate comprises the following steps: dissolving 4, 4-diaminodiphenyl sulfide and 1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate in N-methylpyrrolidone to form a solution, adding the solution into a reaction kettle, replacing air in the reaction kettle with nitrogen, then reacting for 5 hours at the normal pressure and the temperature of 160 ℃, adding thiophosphonate into a reaction system, heating to 260 ℃, carrying out polycondensation reaction for 18 hours at the pressure of 300Pa, cooling to room temperature, adjusting to the normal pressure, precipitating in water, washing the precipitated polymer for 3-6 times with ethanol, and finally drying in a vacuum drying oven at the temperature of 90 ℃ to constant weight to obtain the 4, 4-diaminodiphenyl sulfide/1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate; the molar ratio of the 4, 4-diaminodiphenyl sulfide, the 1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate, the N-methylpyrrolidone and the thiophosphonate is 1:1:10:1.
The preparation method of the environment-friendly cable insulation protective material is characterized by comprising the following steps: uniformly mixing the components in parts by weight to form a mixture, and then adding the mixture into a double-screw extruder for extrusion molding to obtain the environment-friendly cable insulation protective material; the extrusion molding specifically comprises the following temperature control parameters: the feeding section is 175 ℃, the compression section is 190 ℃, the head temperature is 200 ℃, the neck mold temperature is 205 ℃, the production speed is controlled to be 300m/min, and the screw rotating speed is controlled to be 60 r/min.
Comparative example 1
This example provides an environmentally friendly cable insulation and protection material which is formulated and prepared in the same manner as in example 1, except that no 4, 4-diaminodiphenyl sulfide/1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate is added.
Comparative example 2
This example provides an environmentally friendly cable insulation and protection material, which is prepared in the same manner as in example 1, except that no 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone/carboxyl terminated polybutadiene rubber polycondensate was added.
Comparative example 3
The formula and the preparation method of the environment-friendly cable insulation protective material are the same as those of example 1, except that epoxy-terminated hyperbranched polyphosphate is not added.
Comparative example 4
The present example provides an environment-friendly cable insulation protective material, which has the same formulation and preparation method as example 1, except that nano boron fiber is not added.
The samples of the environment-friendly cable insulation and protection material obtained in the above examples 1 to 5 and comparative examples 1 to 4 were subjected to related performance tests, and the test methods and test results are shown in table 1.
TABLE 1
As can be seen from Table 1, the environment-friendly cable insulation protective material disclosed by the embodiment of the invention has more excellent mechanical properties, flame retardancy and insulation, which are the result of the synergistic effect of the components.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The environment-friendly cable insulation protective material is characterized by comprising the following components in parts by weight: 20-30 parts of 4, 4-diaminodiphenyl sulfide/1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate, 30-50 parts of 3,3' -diamino-4, 4' -difluorodiphenyl sulfone/carboxyl-terminated polybutadiene rubber polycondensate, 3-6 parts of 2,2' -dihydroxy-4, 4' -dimethoxybenzophenone-5, 5' -disulfonic acid, 0.5-1.5 parts of phosphorus pentoxide, 2-4 parts of epoxy-terminated hyperbranched polyphosphate, 1-2 parts of coupling agent, 1-2 parts of vulcanizing agent and 1-3 parts of nano boron fiber.
2. The environment-friendly cable insulation protective material as claimed in claim 1, wherein the coupling agent is at least one of a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH 570.
3. The environment-friendly cable insulation and protection material as claimed in claim 1, wherein the vulcanizing agent is one or more of dibenzoyl peroxide, tetramethylthiuram disulfide, and zinc dibutyldithiocarbamate.
4. The environment-friendly cable insulation and protection material as claimed in claim 1, wherein the preparation method of the 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone/carboxyl-terminated polybutadiene rubber polycondensate comprises the following steps: adding 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone and carboxyl-terminated polybutadiene rubber into a high boiling point solvent, stirring for 15-25 minutes at 35-55 ℃, then adding (1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride) and N-hydroxysuccinimide, continuing to perform heat preservation reaction for 6-8 hours, then precipitating in water, and then placing the precipitated polymer in a vacuum drying oven for drying at 85-95 ℃ to constant weight to obtain the 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone/carboxyl-terminated polybutadiene rubber polycondensate.
5. The environment-friendly cable insulation and protection material as claimed in claim 4, wherein the molar ratio of the 3,3 '-diamino-4, 4' -difluorodiphenyl sulfone, the carboxyl-terminated polybutadiene rubber, the high boiling point solvent, (1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride) and the N-hydroxysuccinimide is 1:1 (6-10) to (0.8-1.2) to 0.5.
6. The environment-friendly cable insulation and protection material as claimed in claim 4, wherein the high boiling point solvent is at least one of dimethylsulfoxide, N-dimethylformamide and N, N-dimethylacetamide.
7. The environment-friendly cable insulation and protection material as claimed in claim 1, wherein the preparation method of the 4, 4-diaminodiphenyl sulfide/1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate comprises the following steps: dissolving 4, 4-diaminodiphenyl sulfide and 1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate in N-methylpyrrolidone to form a solution, adding the solution into a reaction kettle, replacing the air in the kettle with nitrogen or inert gas, then reacting for 3-5 hours at the temperature of 140-160 ℃ under normal pressure, adding a catalyst into the reaction system, heating to the temperature of 230-260 ℃, carrying out polycondensation reaction for 13-18 hours under the pressure of 100-300Pa, cooling to room temperature, adjusting to normal pressure, precipitating in water, washing the precipitated polymer with ethanol for 3-6 times, and drying in a vacuum drying oven at 80-90 deg.C to constant weight to obtain 4, 4-diaminodiphenyl sulfide/1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate.
8. The environment-friendly cable insulation protective material as claimed in claim 7, wherein the catalyst is at least one of thiophosphonate, thiophosphoramide and phosphorous acid; the inert gas is any one of helium, neon and argon; the molar ratio of the 4, 4-diaminodiphenyl sulfide, the 1, 3-bis (3-carboxypropyl) tetramethyldisilane polycondensate, the N-methylpyrrolidone and the catalyst is 1:1 (6-10) to 0.6-1.
9. The environment-friendly cable insulation and protection material as claimed in any one of claims 1 to 8, wherein the preparation method of the environment-friendly cable insulation and protection material comprises the following steps: the components are uniformly mixed according to the parts by weight to form a mixture, and then the mixture is added into a double-screw extruder to be extruded and molded to obtain the environment-friendly cable insulation protective material.
10. The environment-friendly cable insulation protective material as claimed in claim 9, wherein the extrusion molding specifically comprises the following temperature control parameters: the material supply section 165-.
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| CN202010963562.1A CN112048177A (en) | 2020-09-14 | 2020-09-14 | Environment-friendly cable insulation protection material and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114350146A (en) * | 2022-01-06 | 2022-04-15 | 宁波群力紧固件制造有限公司 | High-strength bolt material and preparation method thereof |
| CN116396610A (en) * | 2023-05-22 | 2023-07-07 | 江苏发安建设工程有限公司 | Flame-retardant cable wire material and preparation method thereof |
-
2020
- 2020-09-14 CN CN202010963562.1A patent/CN112048177A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114350146A (en) * | 2022-01-06 | 2022-04-15 | 宁波群力紧固件制造有限公司 | High-strength bolt material and preparation method thereof |
| CN114350146B (en) * | 2022-01-06 | 2024-03-29 | 宁波群力紧固件制造有限公司 | High-strength bolt material and preparation method thereof |
| CN116396610A (en) * | 2023-05-22 | 2023-07-07 | 江苏发安建设工程有限公司 | Flame-retardant cable wire material and preparation method thereof |
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