CN107903633B - Mixing silicone rubber and preparation method thereof - Google Patents
Mixing silicone rubber and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of silicone rubber, and discloses mixed silicone rubber which comprises the following components in parts by weight: 100 parts of rubber master batch, 0.5-3 parts of titanium dioxide, 1-10 parts of an anti-aging auxiliary agent, 1-6 parts of a flame-retardant mixture, 3-12 parts of quartz powder, 1-8 parts of diatomite and 1-8 parts of a solvent-resistant auxiliary agent. The invention aims to provide the mixed silicone rubber which has obviously enhanced long-term aging resistance, flame retardance, oil resistance, solvent resistance, water immersion breakdown voltage resistance and mechanical properties, achieves better effect and can meet the requirements of the new energy automobile cable industry, and the preparation method thereof.
Description
Technical Field
The invention relates to the field of silicone rubber, in particular to mixed silicone rubber and a preparation method thereof.
Background
The automobile is one of the symbols of modern industrial civilization, is also an important engine for promoting economic development of one country, and further reflects the comprehensive national strength level of one country. At the end of the 20 th century, with the gradual depletion of global petroleum resources, the increasingly serious atmospheric environmental pollution and the prominent greenhouse effect, the sustainable development of human society and economy is influenced. In recent years, with the progress of science and technology, the research and development and application of electric vehicles, hybrid electric vehicles and fuel cell electric vehicles, which are the ultimate goals of energy conservation, environmental protection and safety, have become the key points of the development of the automobile industry of all countries around the world. The development of new energy automobile industry is actively carried out in countries such as the united states, germany and japan. Governments and automobile companies generally recognize that energy conservation and emission reduction are the main directions of future automobile technology development, and the development of new energy automobile industry is the best way to solve the problem. From the perspective of national strategy, the development of new energy automobile industry can reduce the dependence of China on petroleum resources, ensure the national security of China, protect the environment of China, maintain the sustainable development of economy, and realize the rapid growth of economy and the successful transformation of industry. From the development of the automobile industry, the rapid development of the new energy automobile industry is an irreversible trend.
New energy automobile cable belongs to special cable, and the technical level requirement is relatively high. For example, charging of an electric vehicle requires a charging cable to connect the vehicle and a power supply, and the cable is a relatively critical part of a charging system and directly affects the charging safety of the electric vehicle. The charging cable is used as a current carrier for connecting the electric automobile and the charging pile, so that safety problems always need to be concerned by people, information transmission between the electric automobile and the charging pile needs to be carried out, and charging needs to be controlled. The cable is exposed outdoors for a long time, and various severe natural environments can be encountered in the use process, including large day and night temperature difference change, sunlight irradiation, weathering, humidity, acid rain, freezing, seawater and the like, and the natural environments can seriously affect the service life and the service performance of the charging cable, even reduce the reliability and the safety of the charging cable, and cause property loss and personal injury. Therefore, on the basis of ensuring excellent insulating property, the insulating material has excellent performances of water resistance, acid and alkali resistance, aging resistance, oil resistance, weather resistance, low smoke, flame retardance, environmental protection, harmlessness and the like. Because the use is flexible, the phenomena of artificial bending, twisting, dragging and the like are difficult to avoid, and the mechanical damage is very easy to cause; meanwhile, the charging cable may be soaked by an acid-base solution artificially, so that the performance of the cable material is affected, and the charging cable is damaged. Therefore, excellent flexibility, bending flexibility, abrasion resistance and mechanical properties are required.
At present, polyurethane, silicon rubber, ethylene propylene rubber, chlorinated polyethylene rubber and the like are mainly used as materials of insulation and sheaths on new energy automobile cables. The polyurethane material has the best strength and wear resistance, but is also harder and has poorer elasticity; the ethylene propylene rubber material has the allowable working temperature of (-40 to +150 ℃), is a saturated nonpolar material, has very high chemical resistance, low temperature resistance, ozone resistance and oil resistance, and also has excellent water resistance, hot water vapor resistance, electric insulation performance and the like, but the heat resistance is not good enough; chlorinated polyethylene rubber materials have good heat resistance, aging resistance, flame resistance, ozone resistance and tear resistance, but the elasticity, processability, oil resistance and the like of the chlorinated polyethylene rubber materials are poor; the silicon rubber material has very good cold resistance and heat resistance, can be used for a long time within the range of (-50 to +250 ℃) and also can keep the elasticity of rubber, has very good hydrophobicity, electrical insulation property, fatigue resistance, ozone resistance and impact resistance, can also be used for a long time under sunlight exposure, but has poor tensile property, insufficient elongation, difficult sheet falling of mixed materials and higher price.
On the whole, the silicon rubber has excellent comprehensive performance, so that the silicon rubber is widely applied to new energy automobile cables, and particularly the cables with higher requirements on high and low temperature resistance. However, the performance of general silicone rubber materials cannot completely meet the use requirements of new energy cables, the safe operation and the service life of the new energy cables cannot be guaranteed, and the defects are mainly reflected in the combination of important performances of the silicone rubber, such as long-term aging resistance, oil resistance, solvent resistance, water immersion breakdown voltage resistance, flame retardance, mechanical performance and the like. The silicon rubber material at the present stage can have high tearing strength and good flame retardant property, but the material with high tearing strength has poor performances such as long-term aging resistance, acid and alkali resistance, oil resistance, solvent resistance, wear resistance, water immersion breakdown voltage resistance and the like; meanwhile, the material with good flame retardant property has poor long-term aging resistance. Therefore, the long-term aging resistance, flame retardancy, mechanical properties (especially tear resistance), acid and alkali resistance, oil resistance, voltage resistance, impact resistance, solvent resistance and other properties of the silicone rubber must be improved and balanced by some technical means to meet the industrial requirements.
Disclosure of Invention
In order to solve the defects that the existing silicon rubber cannot well balance the long-term aging resistance, flame retardance, oil resistance, solvent resistance, soaking breakdown voltage resistance, mechanical performance and the like, the mixed silicon rubber which obviously enhances the long-term aging resistance, flame retardance, oil resistance, solvent resistance, soaking breakdown voltage resistance and mechanical performance, achieves better effects and can meet the requirements of the new energy automobile cable industry and the preparation method thereof are provided. The specific scheme is as follows: the mixing silicone rubber is characterized by comprising the following components in parts by weight:
100 parts of rubber master batch, 0.5-3 parts of titanium dioxide, 1-10 parts of an anti-aging auxiliary agent, 1-6 parts of a flame-retardant mixture, 3-12 parts of quartz powder, 1-8 parts of diatomite and 1-8 parts of a solvent-resistant auxiliary agent;
the rubber compound masterbatch I comprises the following components in parts by weight:
100 parts of methyl vinyl silicone rubber, 40-53 parts of fumed silica, 3-15 parts of hydrophobic treatment type white carbon black, 1-8 parts of low-viscosity vinyl silicone resin, 10-15 parts of a structural control agent, 0.1-1 part of vinyl triethoxysilane and 0.1-0.5 part of a release agent;
the methyl vinyl silicone rubber consists of 80-88 parts of methyl vinyl silicone rubber with the molecular weight of 60-80 ten thousand and the vinyl molar content of 0.03-0.05%, 6-17 parts of methyl vinyl silicone rubber with the molecular weight of 60-80 ten thousand and the vinyl molar content of 0.08-0.23%, and 2-6 parts of methyl vinyl silicone rubber with the molecular weight of 60-80 ten thousand and the vinyl molar content of 1.0-5.0%.
The low-viscosity vinyl silicon resin in the scheme refers to vinyl silicon resin with the kinematic viscosity of 30-120CS and the vinyl content of 3.5-5.5%.
In the mixed silicone rubber, the flame-retardant mixture consists of the following components in parts by weight:
100 parts of silicone rubber master batch, 0.8-1.5 parts of triazole compound, 0.5-1 part of release agent and 3-5 parts of platinum compound;
the second silicone rubber master batch consists of the following components in parts by weight:
80-88 parts of vinyl-terminated methyl vinyl silicone rubber with the molecular weight of 60-80 ten thousand and the vinyl molar content of 0.03-0.05 percent, 5-17 parts of methyl-terminated methyl vinyl silicone rubber with the molecular weight of 60-80 ten thousand and the vinyl molar content of 0.08-0.23 percent, 0.5-2 parts of methyl-terminated methyl vinyl silicone rubber with the molecular weight of 60-80 ten thousand and the vinyl molar content of 1.0-4.0 percent, 27-35 parts of gas phase white carbon black, 2-5 parts of dimethyl diethoxysilane, 1-3.5 parts of hexamethyldisilazane, 0.5-2 parts of vinyl silicone oil with the dynamic viscosity of 9000-13000 mPa.s and the vinyl content of 0.3-0.5 percent, 0.02-0.08 part of tetramethyl divinyl disilazane, 0.5-2 parts of purified water and 0.5-0.8 part of release agent.
It should be noted that: the flame retardant mechanism of the flame retardant mixture of the present invention is: the platinum compound causes the side chain organic group of the silicon rubber to generate cross-linking reaction at high temperature through catalysis, and improves the cross-linking density, thereby improving the thermal stability of the silicon rubber molecules and preventing the silicon rubber molecules from being further decomposed; but also is beneficial to increasing the content of residues after combustion, promoting the formation of a ceramic layer, further isolating air and extinguishing flame; therefore, the cross-linked structure generated by the platinum compound in the combustion process greatly inhibits the thermal degradation of the flame-retardant silicone rubber material, and plays a flame-retardant role. When the platinum compound flame retardant is used alone in the silicone rubber, only little or no flame retardant effect can be generated; however, when the platinum compound flame retardant is used in combination with carbon black, various metal oxides, hydroxides, carbonates, triazole compounds, silicone resins, etc., the flame retardancy of silicone rubber can be significantly improved.
In the above-mentioned compounded silicone rubber, the triazole-based compound is one of benzotriazole, 1-methyltriazole, 5, 6-dimethyltriazole and 2-phenylbenzotriazole.
In the mixed silicone rubber, the platinum compound consists of the following components in parts by weight: 0.8-2 parts of platinum complex and 10-25 parts of tetramethyl divinyl silazane.
In the above mixed silicone rubber, the release agent in the first mixed rubber masterbatch and the second silicone rubber masterbatch is one or more of stearic acid, zinc stearate, calcium stearate, magnesium stearate and aluminum stearate.
In the above mixed silicone rubber, the anti-aging auxiliary agent is one or a combination of cerium oxide, cerium acetate, cerium oxalate, cerium sulfate, cerium nitrate and cerium carbonate; in the above mixed silicone rubber, the solvent-resistant assistant is a composition of calcium silicate and magnesium oxide, wherein the calcium silicate accounts for 70-80% of the total weight, and the magnesium oxide accounts for 20-30% of the total weight.
In the above-mentioned mixed silicone rubber, the BET specific surface areas of the fumed silica and the hydrophobic treatment type fumed silica are both 150-380m2/g。
In the mixed silicone rubber, the structural control agent consists of the following components in parts by weight: the adhesive has the viscosity of 20-50 mpa.s, 2-6 parts of hydroxy silicone oil with the mass content of 3-11% of hydroxyl, 20-50 mpa.s, 2-4 parts of vinyl hydroxy silicone oil with the mass content of 5-9% of vinyl and the mass content of 3-7% of hydroxyl, 2-5 parts of diphenyl dimethoxy silane, 1-3 parts of hexamethyldisilazane and 0-1.5 parts of purified water.
Meanwhile, the invention also discloses a preparation method of the mixing silicone rubber, which comprises the following steps: the rubber compound masterbatch I and all other raw materials are put into a kneader and mixed for 0.5 to 2 hours, and the temperature of the rubber material in the whole processing process in the kneader is less than or equal to 100 ℃.
In the preparation method of the mixed silicone rubber, the preparation method of the first rubber master batch comprises the following steps: firstly, putting methyl vinyl silicone rubber, hexamethyldisilazane and purified water into a kneader for pretreatment, then putting other raw materials for multiple times and uniformly stirring, then heating to 160 ℃, mixing for 2-3h, cooling to 100 ℃ or below, and taking out the kneader to obtain the rubber compound masterbatch I.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the invention, by selecting the appropriate raw rubber with low and medium vinyl content, using the appropriate fumed silica and the structural control agent with good aging resistance effect, excellent mechanical properties, especially tear strength, are obtained;
(2) according to the invention, by adding a small amount of different aging-resistant materials, the short-term and long-term aging resistance of the rubber material is obviously improved under the condition of not reducing the mechanical property;
(3) according to the invention, a small amount of platinum complex composition is added, and a small amount of titanium dioxide, triazole compound and appropriate anti-aging material are matched, so that the flame retardant property of the silicone rubber is obviously improved on the basis of not reducing the mechanical property and the anti-aging property;
(4) according to the invention, a small amount of proper release agent is added, so that the processing performance of the rubber compound is obviously improved on the basis of basically not reducing the mechanical performance, the aging resistance and the flame retardant performance.
(5) According to the invention, a small amount of proper low-viscosity vinyl silicone resin, diatomite, calcium silicate and magnesium oxide are added, and a proper amount of titanium dioxide and an anti-aging auxiliary agent are matched, so that the oil resistance and the solvent resistance of the rubber compound are obviously improved on the basis of not reducing the mechanical property, the anti-aging property and the flame retardant property.
(6) According to the invention, by adding a small amount of proper kinds of quartz powder, the friction resistance of the rubber compound is obviously improved on the basis of not reducing the mechanical property, the aging resistance and the flame resistance.
(7) According to the invention, the appropriate type and amount of fumed silica and hydrophobic treated silica are matched, so that the hydrophobicity and the breakdown voltage performance of the rubber compound are obviously improved on the basis of not reducing the mechanical performance, the aging resistance and the flame retardant performance.
(8) According to the characteristics of different materials, the preparation method of the invention adopts a two-step method, so that the most excellent comprehensive performance can be obtained by the aid of the process, the preparation cost is low, and the production efficiency is improved.
(9) The invention has the most outstanding innovation point of balancing the mechanical property, the aging resistance, the flame retardant property, the oil resistance, the solvent resistance, the soaking breakdown voltage resistance and the processing property. Because of the mechanical propertiesThe tear strength, the aging resistance, the flame retardant property, the oil resistance, the solvent resistance and the soaking breakdown voltage resistance are in a certain contradiction relationship, and the processing property, the aging resistance, the flame retardant property and the hydrophobic property are also in contradiction; especially if the density is required to be less than or equal to 1.25g/cm3Therefore, the flame retardance can not be improved by adding a large amount of conventional powder raw materials, and even if the flame retardance is improved by using a certain amount of platinum complex, too much flame-retardant powder can not be matched, so that the difficulty in improving the flame retardance is greatly increased; meanwhile, the performances of oil resistance, solvent resistance and breakdown voltage resistance after soaking can be improved to a certain extent, and the performances such as tear strength and the like can not be improved by adding a large amount of powder. Therefore, the innovation point realizes the comprehensive optimization of mechanical property, aging resistance, flame retardant property, oil resistance, solvent resistance, water immersion breakdown voltage resistance and processability by the comprehensive means of (1) to (8), and meets the requirements of new energy automobile cables on materials.
Detailed Description
The technical solution of the present invention will be described in further detail with reference to the following embodiments, but the present invention is not limited thereto.
Example 1
1. The formula of the rubber compound (parts by weight): 100 parts of rubber master batch, 0.5 part of titanium dioxide, 2 parts of an anti-aging auxiliary agent, 1.5 parts of a flame-retardant mixture, 3 parts of quartz powder, 2 parts of diatomite and 1 part of a solvent-resistant auxiliary agent.
In this embodiment, the anti-aging auxiliary agent is one of cerium oxide, cerium acetate, cerium oxalate, cerium sulfate, cerium nitrate and cerium carbonate, and the selection of the above-mentioned cerium compound does not significantly affect the application effects of embodiments 1 to 8, and in this embodiment, cerium oxide is selected;
in this example, the formulation of the flame retardant mixture is:
100 parts of silicone rubber master batch, 0.8-1.5 parts of triazole compound, 0.5-1 part of release agent and 3-5 parts of platinum compound; in practical applications, the data selection in this range does not significantly affect the application effects of examples 1-8. Specifically, in this embodiment, two 100 parts of silicone rubber masterbatch, 1 part of triazole compound, 1 part of mold release agent, and 4 parts of platinum compound, wherein the platinum compound is prepared from 1.2: 15 platinum complex and tetramethyldivinylsilazane. The release agent is selected from zinc stearate, and the triazole compound is 5, 6-dimethyl triazole.
The formula of the silicone rubber master batch II is as follows:
the high-performance silicone rubber comprises 60-80 ten thousand of vinyl-terminated methyl vinyl silicone rubber with the molecular weight of 0.03-0.05 percent, 60-80 ten thousand of methyl-terminated methyl vinyl silicone rubber with the molecular weight of 0.08-0.23 percent, 60-80 ten thousand of methyl-terminated methyl vinyl silicone rubber with the molecular weight of 1.0-4.0 percent, 60-80 ten thousand of methyl-terminated methyl vinyl silicone rubber with the molecular weight of 5-9.5 percent, white carbon black prepared by a gas phase method, dimethyl diethoxy silane, hexamethyldisilazane, 9000-13000 mPa.s of dynamic viscosity, 0.3-0.5 percent of vinyl silicone oil with the vinyl content, tetramethyl divinyl disilazane, purified water and a mold release agent.
It should be noted that the molecular weight, ethylene molar content and viscosity of the above raw materials are selected within the above ranges, which do not significantly affect the application effects of examples 1 to 8, and the weight ratio is 60 to 80 ten thousand, and the vinyl terminated methyl vinyl silicone rubber with 0.03 to 0.05% of vinyl molar content: methyl terminated methyl vinyl silicone rubber with molecular weight of 60-80 ten thousand and vinyl molar content of 0.08-0.23%: methyl terminated methyl vinyl silicone rubber with molecular weight of 60-80 ten thousand and vinyl molar content of 1.0-4.0%: methyl-terminated methyl vinyl silicone rubber with molecular weight of 60-80 ten thousand and vinyl molar content of 5-9.5%: white carbon black by a gas phase method: dimethyl diethoxysilane: hexamethyldisilazane: vinyl silicone oil with dynamic viscosity of 9000-13000 mPa.s and vinyl content of 0.3-0.5%: tetramethyldivinyldisilazane: purified water: the weight ratio of the release agent is 80-88: 5-17: 1-4: 0.5-2: 27-35: 2-5: 1-3.5: 0.5-2: 0.02-0.08: 0.5-2: 0.5-0.8; in this example and examples 2-8, selecting values within the above weight ratio ranges does not produce significant performance variation, for example: 84: 12: 3: 1: 30: 3: 2.5: 1: 0.05: 1: 0.7; or 80: 17: 1: 2: 27: 5: 1: 2: 0.02: 2: 0.8 or 87: 7: 4: 2: 35: 2: 3.5: 0.5: 0.08: 0.5: 0.8. no matter what choice is made, no obvious influence is caused on the actual application effect. In this embodiment, the weight ratio is selected from 84: 12: 3: 1: 30: 3: 2.5: 1: 0.05: 1: 0.7.
the preparation method of the silicone rubber master batch II comprises the following steps: firstly putting the methyl vinyl silicone rubber into a kneader, then putting other raw materials for multiple times, uniformly stirring the raw materials, then heating to 160 ℃, mixing for 2-3h, cooling to 100 ℃, and taking out the kneader to obtain the rubber compound masterbatch II.
2. The first formula of the silicone rubber master batch comprises: 87 parts of methyl vinyl silicone rubber with 0.05 percent of vinyl molar content, 8.7 parts of methyl vinyl silicone rubber with 0.08 percent of vinyl molar content, 4.3 parts of methyl vinyl silicone rubber with 3.0 percent of vinyl molar content, 48 parts of fumed silica, 4 parts of hydrophobic treatment type fumed silica, 2 parts of low-viscosity vinyl silicone resin, 14 parts of structural control agent, 0.2 part of vinyl triethoxysilane and 0.2 part of mold release agent.
The molecular weight of the methyl vinyl silicone rubber is 60-80 ten thousand, and as long as the molecular weight is in the molecular weight range of the examples 1-8, the effect is not obviously different, and in the example, the molecular weight is selected to be 70 ten thousand.
Wherein the BET specific surface areas of the fumed silica and the hydrophobic treatment type fumed silica are both 150-380m2(ii) in terms of/g. As long as examples 1 to 8 were within this specific surface area range, the effects were constant without significant difference, and in this example, the specific surface area was selected to be 300m2And about/g.
The formula of the structural control agent is as follows: 20-50 mpa.s of viscosity, 3-11% of hydroxyl group mass content, 20-50 mpa.s of viscosity, 5-9% of vinyl hydroxyl silicone oil with 3-7% of vinyl mass content, diphenyldimethoxysilane, hexamethyldisilazane and purified water; wherein the weight ratio of the hydroxyl silicone oil with the viscosity of 20-50 mpa.s and the hydroxyl mass content of 3-11%, the vinyl hydroxyl silicone oil with the viscosity of 20-50 mpa.s and the vinyl mass content of 5-9% and the hydroxyl mass content of 3-7%, the diphenyl dimethoxysilane, the hexamethyldisilazane and the purified water is 2-6: 2-4: 2-5: 1-3: 0 to 1.5. It should be noted that, in the actual testing process, under the condition that the total amount of the structural control agent is fixed, the structural control agent obtained by using the components in the above-mentioned ranges does not produce obvious difference in the application effects of the embodiments 1 to 8, such as viscosity of 20 to 50mpa.s, hydroxy silicone oil with hydroxy mass content of 3 to 11%, viscosity of 20 to 50mpa.s, vinyl hydroxy silicone oil with vinyl mass content of 5 to 9% and hydroxy mass content of 3 to 7%, diphenyldimethoxysilane, hexamethyldisilazane, and purified water, in a weight ratio of 2: 2: 2: 2: 0.5 or 2: 4: 5: 1: 1.5 or 6: 2: 2: 3: 0.1; the above-mentioned value ranges do not bring about significant changes in the effects of the applications of examples 1 to 8. In the present embodiment, it is preferably in a weight ratio of 2: 2: 2: 2: 0.5. in addition, the viscosity is 20-50 mpa.s, the viscosity of the hydroxyl silicone oil with the hydroxyl mass content of 3-11%, the viscosity of the vinyl hydroxyl silicone oil with the viscosity of 20-50 mpa.s, the viscosity of the vinyl hydroxyl silicone oil with the vinyl mass content of 5-9% and the hydroxyl mass content of 3-7% is controlled to be smaller, and the significant difference in the effects of the embodiments 1-8 cannot be brought by controlling the hydroxyl content and the vinyl content in the ranges, which is specifically: hydroxyl silicone oil with the viscosity of 20-50 mpa.s and the hydroxyl mass content of 8%, and vinyl hydroxyl silicone oil with the viscosity of 20-50 mpa.s, the vinyl mass content of 7% and the hydroxyl mass content of 5%.
The preparation method comprises the following steps: firstly putting raw rubber, hexamethyldisilazane and purified water into a mixing kneader to carry out raw rubber pretreatment, eliminating silicon hydroxyl as much as possible, then putting the rest raw materials in the rubber compound masterbatch I formula into the kneader to be uniformly stirred, wherein the white carbon black needs to be put in 7 times, discharging after mixing, and standing for 5 hours. And then putting the mixed materials into a vacuum kneader to stir and mix rubber, vacuumizing the whole process, heating from the beginning of kneading, carrying out constant temperature treatment for 2 hours at 160 ℃, then discharging when cooling to 80 ℃, and cooling to normal temperature to obtain the rubber compound masterbatch I. And putting the rubber compound masterbatch I and all other raw materials into a kneader together, uniformly stirring, then performing intensive mixing for 0.5h, discharging, and performing an extrusion, filtration and packaging process to obtain the rubber compound silicone rubber product applied to the new energy automobile cable.
The main properties are as follows:
description of the drawings: vulcanizing agent: the additive amount of the bi-component platinum vulcanizing agent is 0.5%/1.6%, and the vulcanizing conditions are as follows: 130 ℃ for 10 min.
Example 2:
1. the formula of the rubber compound is as follows: 100 parts of rubber master batch, 1.5 parts of titanium dioxide, 4 parts of an anti-aging auxiliary agent, 2.5 parts of a flame-retardant mixture, 6 parts of quartz powder, 4 parts of diatomite and 2.5 parts of a solvent-resistant auxiliary agent.
2. The first formula of the silicone rubber master batch comprises: 87 parts of methyl vinyl silicone rubber with 0.05 percent of vinyl molar content, 8.7 parts of methyl vinyl silicone rubber with 0.08 percent of vinyl molar content, 4.3 parts of methyl vinyl silicone rubber with 3.0 percent of vinyl molar content, 48 parts of fumed silica, 4 parts of hydrophobic treatment type fumed silica, 2 parts of low-viscosity vinyl silicone resin, 14 parts of structural control agent, 0.2 part of vinyl triethoxysilane and 0.2 part of mold release agent.
The preparation method comprises the following steps: firstly putting raw rubber, hexamethyldisilazane and purified water into a mixing kneader to carry out raw rubber pretreatment, eliminating silicon hydroxyl as much as possible, then putting the rest raw materials in the rubber compound masterbatch I formula into the kneader to be uniformly stirred, wherein the white carbon black needs to be put in 7 times, discharging after mixing, and standing for 5 hours. And then putting the mixed materials into a vacuum kneader to stir and mix rubber, vacuumizing the whole process, heating from the beginning of kneading, carrying out constant temperature treatment for 2 hours at 160 ℃, then discharging when cooling to 80 ℃, and cooling to normal temperature to obtain the rubber compound masterbatch I. And putting the rubber compound masterbatch I and all other raw materials into a kneader together, uniformly stirring, then performing intensive mixing for 0.5h, discharging, and performing an extrusion, filtration and packaging process to obtain the rubber compound silicone rubber product applied to the new energy automobile cable.
The main properties are as follows:
description of the drawings: vulcanizing agent: the additive amount of the bi-component platinum vulcanizing agent is 0.5%/1.6%, and the vulcanizing conditions are as follows: 130 ℃ for 10 min.
Example 3:
1. the formula of the rubber compound is as follows: 100 parts of rubber master batch, 1.5 parts of titanium dioxide, 5.0 parts of an anti-aging auxiliary agent, 4 parts of a flame-retardant mixture, 6 parts of quartz powder, 6 parts of diatomite and 3.5 parts of a solvent-resistant auxiliary agent.
2. The first formula of the silicone rubber master batch comprises: 87 parts of methyl vinyl silicone rubber with 0.05 percent of vinyl molar content, 8.7 parts of methyl vinyl silicone rubber with 0.08 percent of vinyl molar content, 4.3 parts of methyl vinyl silicone rubber with 3.0 percent of vinyl molar content, 48 parts of fumed silica, 4 parts of hydrophobic treatment type fumed silica, 2 parts of low-viscosity vinyl silicone resin, 14 parts of structural control agent, 0.2 part of vinyl triethoxysilane and 0.2 part of mold release agent.
The preparation method comprises the following steps: firstly putting raw rubber, hexamethyldisilazane and purified water into a mixing kneader to carry out raw rubber pretreatment, eliminating silicon hydroxyl as much as possible, then putting the rest raw materials in the rubber compound masterbatch I formula into the kneader to be uniformly stirred, wherein the white carbon black needs to be put in 7 times, discharging after mixing, and standing for 5 hours. And then putting the mixed materials into a vacuum kneader to stir and mix rubber, vacuumizing the whole process, heating from the beginning of kneading, carrying out constant temperature treatment for 2 hours at 160 ℃, then discharging when cooling to 80 ℃, and cooling to normal temperature to obtain the rubber compound masterbatch I. And putting the rubber compound masterbatch I and all other raw materials into a kneader together, uniformly stirring, then performing intensive mixing for 0.5h, discharging, and performing an extrusion, filtration and packaging process to obtain the rubber compound silicone rubber product applied to the new energy automobile cable.
The main properties are as follows:
description of the drawings: vulcanizing agent: the additive amount of the bi-component platinum vulcanizing agent is 0.5%/1.6%, and the vulcanizing conditions are as follows: 130 ℃ for 10 min.
Example 4:
1. the formula of the rubber compound is as follows: 100 parts of rubber master batch, 2 parts of titanium dioxide, 7.0 parts of an anti-aging auxiliary agent, 6 parts of a flame-retardant mixture, 9 parts of quartz powder, 6 parts of diatomite and 4 parts of a solvent-resistant auxiliary agent.
2. The first formula of the silicone rubber master batch comprises: 87 parts of methyl vinyl silicone rubber with 0.05 percent of vinyl molar content, 8.7 parts of methyl vinyl silicone rubber with 0.08 percent of vinyl molar content, 4.3 parts of methyl vinyl silicone rubber with 3.0 percent of vinyl molar content, 48 parts of fumed silica, 4 parts of hydrophobic treatment type fumed silica, 2 parts of low-viscosity vinyl silicone resin, 14 parts of structural control agent, 0.2 part of vinyl triethoxysilane and 0.2 part of mold release agent.
The preparation method comprises the following steps: firstly putting raw rubber, hexamethyldisilazane and purified water into a mixing kneader to carry out raw rubber pretreatment, eliminating silicon hydroxyl as much as possible, then putting the rest raw materials in the rubber compound masterbatch I formula into the kneader to be uniformly stirred, wherein the white carbon black needs to be put in 7 times, discharging after mixing, and standing for 5 hours. And then putting the mixed materials into a vacuum kneader to stir and mix rubber, vacuumizing the whole process, heating from the beginning of kneading, carrying out constant temperature treatment for 2 hours at 160 ℃, then discharging when cooling to 80 ℃, and cooling to normal temperature to obtain the rubber compound masterbatch I. And putting the rubber compound masterbatch I and all other raw materials into a kneader together, uniformly stirring, then performing intensive mixing for 0.5h, discharging, and performing an extrusion, filtration and packaging process to obtain the rubber compound silicone rubber product applied to the new energy automobile cable.
The main properties are as follows:
description of the drawings: vulcanizing agent: the additive amount of the bi-component platinum vulcanizing agent is 0.5%/1.6%, and the vulcanizing conditions are as follows: 130 ℃ for 10 min.
Example 5
1. The formula of the rubber compound is as follows: 100 parts of rubber master batch, 0.5 part of titanium dioxide, 2 parts of an anti-aging auxiliary agent, 1.5 parts of a flame-retardant mixture, 3 parts of quartz powder, 2 parts of diatomite and 1 part of a solvent-resistant auxiliary agent.
2. The first formula of the silicone rubber master batch comprises: 80 parts of methyl vinyl silicone rubber with 0.05 percent of vinyl molar content, 16 parts of methyl vinyl silicone rubber with 0.23 percent of vinyl molar content, 4 parts of methyl vinyl silicone rubber with 3.0 percent of vinyl molar content, 41 parts of fumed silica, 8 parts of hydrophobic processing type fumed silica, 8 parts of low-viscosity vinyl silicone resin, 15 parts of structural control agent, 0.5 part of vinyl triethoxysilane and 0.4 part of mold release agent.
The preparation method comprises the following steps: firstly putting raw rubber, hexamethyldisilazane and purified water into a mixing kneader to carry out raw rubber pretreatment, eliminating silicon hydroxyl as much as possible, then putting the rest raw materials in the rubber compound masterbatch I formula into the kneader to be uniformly stirred, wherein the white carbon black needs to be put in 7 times, discharging after mixing, and standing for 5 hours. And then putting the mixed materials into a vacuum kneader to stir and mix rubber, vacuumizing the whole process, heating from the beginning of kneading, carrying out constant temperature treatment for 2 hours at 160 ℃, then discharging when cooling to 80 ℃, and cooling to normal temperature to obtain the rubber compound masterbatch I. And putting the rubber compound masterbatch I and all other raw materials into a kneader together, uniformly stirring, then performing intensive mixing for 0.5h, discharging, and performing an extrusion, filtration and packaging process to obtain the rubber compound silicone rubber product applied to the new energy automobile cable.
The main properties are as follows:
description of the drawings: vulcanizing agent: the additive amount of the bi-component platinum vulcanizing agent is 0.5%/1.6%, and the vulcanizing conditions are as follows: 130 ℃ for 10 min.
Example 6:
1. the formula of the rubber compound is as follows: 100 parts of rubber master batch, 1.5 parts of titanium dioxide, 4.0 parts of an anti-aging auxiliary agent, 2.5 parts of a flame-retardant mixture, 6 parts of quartz powder, 4 parts of diatomite and 2.5 parts of a solvent-resistant auxiliary agent.
2. The first formula of the silicone rubber master batch comprises: 80 parts of methyl vinyl silicone rubber with 0.05 percent of vinyl molar content, 16 parts of methyl vinyl silicone rubber with 0.23 percent of vinyl molar content, 4 parts of methyl vinyl silicone rubber with 3.0 percent of vinyl molar content, 41 parts of fumed silica, 8 parts of hydrophobic processing type fumed silica, 8 parts of low-viscosity vinyl silicone resin, 15 parts of structural control agent, 0.5 part of vinyl triethoxysilane and 0.4 part of mold release agent.
The preparation method comprises the following steps: the method comprises the steps of firstly putting raw rubber, hexamethyldisilazane and purified water into a mixing internal mixer for raw rubber pretreatment, eliminating silicon hydroxyl as much as possible, then putting the rest raw materials in a rubber compound masterbatch I formula into the internal mixer for uniformly mixing, wherein white carbon black needs to be put in 7 times, discharging after mixing, and standing for 5 hours. And then putting the mixed materials into a vacuum kneader to stir and mix rubber, vacuumizing the whole process, heating from the beginning of kneading, carrying out constant temperature treatment for 2 hours at 160 ℃, then discharging when cooling to 80 ℃, and cooling to normal temperature to obtain the rubber compound masterbatch I. And putting the rubber compound masterbatch I and all other raw materials into an internal mixer together, uniformly stirring, then performing intensive mixing for 0.5h, discharging, and performing extrusion, filtration and packaging procedures to obtain the mixed silicone rubber product applied to the new energy automobile cable.
The main properties are as follows:
description of the drawings: vulcanizing agent: the additive amount of the bi-component platinum vulcanizing agent is 0.5%/1.6%, and the vulcanizing conditions are as follows: 130 ℃ for 10 min.
Example 7:
1. the formula of the rubber compound is as follows: 100 parts of rubber master batch, 1.5 parts of titanium dioxide, 5.0 parts of an anti-aging auxiliary agent, 4 parts of a flame-retardant mixture, 6 parts of quartz powder, 6 parts of diatomite and 3.5 parts of a solvent-resistant auxiliary agent.
2. The first formula of the silicone rubber master batch comprises: 80 parts of methyl vinyl silicone rubber with 0.05 percent of vinyl molar content, 16 parts of methyl vinyl silicone rubber with 0.23 percent of vinyl molar content, 4 parts of methyl vinyl silicone rubber with 3.0 percent of vinyl molar content, 41 parts of fumed silica, 8 parts of hydrophobic processing type fumed silica, 8 parts of low-viscosity vinyl silicone resin, 15 parts of structural control agent, 0.5 part of vinyl triethoxysilane and 0.4 part of mold release agent.
The preparation method comprises the following steps: firstly putting raw rubber, hexamethyldisilazane and purified water into a mixing kneader to carry out raw rubber pretreatment, eliminating silicon hydroxyl as much as possible, then putting the rest raw materials in the rubber compound masterbatch I formula into the kneader to be uniformly stirred, wherein the white carbon black needs to be put in 7 times, discharging after mixing, and standing for 5 hours. And then putting the mixed materials into a vacuum kneader to stir and mix rubber, vacuumizing the whole process, heating from the beginning of kneading, carrying out constant temperature treatment for 2 hours at 160 ℃, then discharging when cooling to 80 ℃, and cooling to normal temperature to obtain the rubber compound masterbatch I. And putting the rubber compound masterbatch I and all other raw materials into a kneader together, uniformly stirring, then performing intensive mixing for 0.5h, discharging, and performing an extrusion, filtration and packaging process to obtain the rubber compound silicone rubber product applied to the new energy automobile cable.
The main properties are as follows:
description of the drawings: vulcanizing agent: the additive amount of the bi-component platinum vulcanizing agent is 0.5%/1.6%, and the vulcanizing conditions are as follows: 130 ℃ for 10 min.
Example 8:
1. the formula of the rubber compound is as follows: 100 parts of rubber master batch, 2 parts of titanium dioxide, 7.0 parts of an anti-aging auxiliary agent, 6 parts of a flame-retardant mixture, 9 parts of quartz powder, 6 parts of diatomite and 4 parts of a solvent-resistant auxiliary agent.
2. The first formula of the silicone rubber master batch comprises: 80 parts of methyl vinyl silicone rubber with 0.05 percent of vinyl molar content, 16 parts of methyl vinyl silicone rubber with 0.23 percent of vinyl molar content, 4 parts of methyl vinyl silicone rubber with 3.0 percent of vinyl molar content, 41 parts of fumed silica, 8 parts of hydrophobic processing type fumed silica, 8 parts of low-viscosity vinyl silicone resin, 15 parts of structural control agent, 0.5 part of vinyl triethoxysilane and 0.4 part of mold release agent.
The preparation method comprises the following steps: firstly putting raw rubber, hexamethyldisilazane and purified water into a mixing kneader to carry out raw rubber pretreatment, eliminating silicon hydroxyl as much as possible, then putting the rest raw materials in the rubber compound masterbatch I formula into the kneader to be uniformly stirred, wherein the white carbon black needs to be put in 7 times, discharging after mixing, and standing for 5 hours. And then putting the mixed materials into a vacuum kneader to stir and mix rubber, vacuumizing the whole process, heating from the beginning of kneading, carrying out constant temperature treatment for 2 hours at 160 ℃, then discharging when cooling to 80 ℃, and cooling to normal temperature to obtain the rubber compound masterbatch I. And putting the rubber compound masterbatch I and all other raw materials into a kneader together, uniformly stirring, then performing intensive mixing for 0.5h, discharging, and performing an extrusion, filtration and packaging process to obtain the rubber compound silicone rubber product applied to the new energy automobile cable.
The main properties are as follows:
description of the drawings: vulcanizing agent: the additive amount of the bi-component platinum vulcanizing agent is 0.5%/1.6%, and the vulcanizing conditions are as follows: 130 ℃ for 10 min.
Comparative example 1
1. The formula of the rubber compound is as follows: 100 parts of rubber master batch, 0.5 part of titanium dioxide, 0.5 part of anti-aging auxiliary agent, 1.5 parts of flame-retardant mixture, 3 parts of quartz powder, 0 part of diatomite and 0 part of solvent-resistant auxiliary agent.
2. The first formula of the silicone rubber master batch comprises: 87 parts of methyl vinyl silicone rubber with 0.03 percent of vinyl molar content, 8.7 parts of methyl vinyl silicone rubber with 0.23 percent of vinyl molar content, 4.3 parts of methyl vinyl silicone rubber with 5.0 percent of vinyl molar content, 53 parts of fumed silica, 0 part of hydrophobic treatment type fumed silica, 0 part of low-viscosity vinyl silicone resin, 15 parts of structural control agent, 0.2 part of vinyl triethoxysilane and 0.2 part of mold release agent.
The preparation method comprises the following steps: firstly putting raw rubber, hexamethyldisilazane and purified water into a mixing kneader to carry out raw rubber pretreatment, eliminating silicon hydroxyl as much as possible, then putting the rest raw materials in the rubber compound masterbatch I formula into the kneader to be uniformly stirred, wherein the white carbon black needs to be put in 7 times, discharging after mixing, and standing for 5 hours. And then putting the mixed materials into a vacuum kneader to stir and mix rubber, vacuumizing the whole process, heating from the beginning of kneading, carrying out constant temperature treatment for 2 hours at 160 ℃, then discharging when cooling to 80 ℃, and cooling to normal temperature to obtain the rubber compound masterbatch I. And putting the rubber compound masterbatch I and all other raw materials into a kneader together, uniformly stirring, then performing intensive mixing for 0.5h, discharging, and performing an extrusion, filtration and packaging process to obtain the rubber compound silicone rubber product applied to the new energy automobile cable.
The main properties are as follows:
description of the drawings: vulcanizing agent: the additive amount of the bi-component platinum vulcanizing agent is 0.5%/1.6%, and the vulcanizing conditions are as follows: 130 ℃ for 10 min.
The above description is only exemplary of the invention, and any modification, equivalent replacement, and improvement made within the spirit and scope of the present invention should be considered within the scope of the present invention.
Claims (7)
1. The mixing silicone rubber is characterized by comprising the following components in parts by weight:
100 parts of rubber master batch, 0.5-3 parts of titanium dioxide, 1-10 parts of an anti-aging auxiliary agent, 1-6 parts of a flame-retardant mixture, 3-12 parts of quartz powder, 1-8 parts of diatomite and 1-8 parts of a solvent-resistant auxiliary agent;
the rubber compound masterbatch I comprises the following components in parts by weight:
100 parts of methyl vinyl silicone rubber, 40-53 parts of fumed silica, 3-15 parts of hydrophobic treatment type fumed silica, 1-8 parts of low-viscosity vinyl silicon resin, 10-15 parts of a structural control agent, 0.1-1 part of vinyl triethoxysilane and 0.1-0.5 part of a release agent;
the methyl vinyl silicone rubber consists of 80-88 parts of methyl vinyl silicone rubber with the molecular weight of 60-80 ten thousand and the vinyl molar content of 0.03-0.05%, 6-17 parts of methyl vinyl silicone rubber with the molecular weight of 60-80 ten thousand and the vinyl molar content of 0.08-0.23%, and 2-6 parts of methyl vinyl silicone rubber with the molecular weight of 60-80 ten thousand and the vinyl molar content of 1.0-5.0%;
the solvent-resistant auxiliary agent is a composition of calcium silicate and magnesium oxide, wherein the calcium silicate accounts for 70-80% of the total weight, and the magnesium oxide accounts for 20-30% of the total weight; the anti-aging auxiliary agent is one or a combination of cerium oxide, cerium acetate, cerium oxalate, cerium sulfate, cerium nitrate and cerium carbonate; the flame-retardant mixture comprises the following components in parts by weight: 100 parts of silicone rubber master batch, 0.8-1.5 parts of triazole compound, 0.5-1 part of release agent and 3-5 parts of platinum compound;
the second silicone rubber master batch consists of the following components in parts by weight:
80-88 parts of vinyl-terminated methyl vinyl silicone rubber with the molecular weight of 60-80 ten thousand and the vinyl molar content of 0.03-0.05 percent, 5-17 parts of methyl-terminated methyl vinyl silicone rubber with the molecular weight of 60-80 ten thousand and the vinyl molar content of 0.08-0.23 percent, 0.5-2 parts of methyl-terminated methyl vinyl silicone rubber with the molecular weight of 60-80 ten thousand and the vinyl molar content of 1.0-4.0 percent, 27-35 parts of gas phase white carbon black, 2-5 parts of dimethyl diethoxysilane, 1-3.5 parts of hexamethyldisilazane, 0.5-2 parts of vinyl silicone oil with the dynamic viscosity of 9000-13000 mPa.s and the vinyl content of 0.3-0.5 percent, 0.02-0.08 part of tetramethyl divinyl disilazane, 0.5-2 parts of purified water and 0.5-0.8 part of release agent.
2. The compounded silicone rubber according to claim 1, wherein the triazole-based compound is one of benzotriazole, 1-methyltriazole, 5, 6-dimethyltriazole and 2-phenylbenzotriazole.
3. The compounded silicone rubber of claim 1, wherein the release agent in the first rubber compound masterbatch and the second silicone rubber masterbatch is one or more of stearic acid, zinc stearate, calcium stearate, magnesium stearate, and aluminum stearate.
4. The mixing silicone rubber according to claim 1, wherein the BET specific surface areas of the fumed silica and the hydrophobic-treated fumed silica are both 150-380m2/g。
5. The mixing silicone rubber according to claim 1, wherein the structural control agent comprises the following components in parts by weight: the adhesive has the viscosity of 20-50 mpa.s, 2-6 parts of hydroxy silicone oil with the mass content of 3-11% of hydroxyl, 20-50 mpa.s, 2-4 parts of vinyl hydroxy silicone oil with the mass content of 5-9% of vinyl and the mass content of 3-7% of hydroxyl, 2-5 parts of diphenyl dimethoxy silane, 1-3 parts of hexamethyldisilazane and 0-1.5 parts of purified water.
6. The method for producing the mixed silicone rubber according to any one of claims 1 to 5, characterized in that the method comprises: the rubber compound masterbatch I and all other raw materials are put into a kneader and mixed for 0.5 to 2 hours, and the temperature of the rubber material in the whole processing process in the kneader is less than or equal to 100 ℃.
7. The method for producing the mixed silicone rubber according to claim 5, characterized in that the method comprises: the rubber compound masterbatch I and all other raw materials are put into a kneader and mixed for 0.5-2h, and the temperature of the rubber material in the whole processing process in the kneader is less than or equal to 100 ℃;
the preparation method of the rubber compound masterbatch I comprises the following steps: firstly, putting methyl vinyl silicone rubber, hexamethyldisilazane and purified water into a kneader for pretreatment, then putting other raw materials for multiple times and uniformly stirring, then heating to 160 ℃, mixing for 2-3h, cooling to 100 ℃ or below, and taking out the kneader to obtain the rubber compound masterbatch I.
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| CN110551395A (en) * | 2018-05-30 | 2019-12-10 | 厦门明钜科技有限公司 | formula and preparation method of extrusion type mixing silicone rubber |
| CN108727830A (en) * | 2018-06-15 | 2018-11-02 | 苏州速传导热电子材料科技有限公司 | A kind of high tenacity flame-retarded heat-conducting silica gel piece and preparation method thereof |
| CN109467938A (en) * | 2018-10-29 | 2019-03-15 | 镇江亿维硅材料科技有限公司 | A kind of resistance oil silicone rubber rubber compound and preparation method thereof |
| CN109701087B (en) * | 2018-12-20 | 2021-07-23 | 新安天玉有机硅有限公司 | Silicone rubber master batch, silicone rubber and preparation method thereof |
| CN109880373A (en) * | 2019-01-21 | 2019-06-14 | 广州科系维新材料有限公司 | A kind of additive and preparation method thereof applied to transparent flame-retarding silicon rubber |
| CN109957251B (en) * | 2019-03-21 | 2021-07-20 | 江西双龙硅材料科技有限公司 | Preparation method of rubber compound |
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| CN110128832A (en) * | 2019-05-13 | 2019-08-16 | 新安天玉有机硅有限公司 | A kind of cold shrink sleeve anti creepage trace silicon rubber and preparation method thereof |
| CN111019353A (en) * | 2019-11-26 | 2020-04-17 | 东莞市朗晟材料科技有限公司 | High-breakdown-voltage-resistant silica gel for electric wire, and preparation method and use method thereof |
| CN111363365B (en) * | 2020-03-24 | 2022-03-11 | 新安天玉有机硅有限公司 | Ultra-high pressure and high temperature resistant mixed silicone rubber and preparation method thereof |
| CN111253687B (en) * | 2020-03-24 | 2021-04-09 | 山东大学 | Blended rubber of silicon rubber and ethylene propylene diene monomer and preparation method thereof |
| CN111875968A (en) * | 2020-07-17 | 2020-11-03 | 东莞市朗晟材料科技有限公司 | Flame-retardant silicone rubber for low-pressure sealing and preparation method thereof |
| CN113088091B (en) * | 2021-03-23 | 2023-01-03 | 新安天玉有机硅有限公司 | High-temperature mixed silicone rubber for rail transit vehicle cables and preparation method thereof |
| CN113881396A (en) * | 2021-11-23 | 2022-01-04 | 东莞市高酷纳米科技有限公司 | Preparation of high-performance flame-retardant heat-conducting adhesive in electronic industry |
| CN114316605A (en) * | 2021-12-31 | 2022-04-12 | 东莞市正安有机硅科技有限公司 | Transparent flame-retardant silicone rubber and preparation method thereof |
| CN115679722B (en) * | 2022-10-09 | 2024-01-26 | 东莞市科多有机硅材料有限公司 | High-elasticity liquid silk-screen silicone rubber and preparation method thereof |
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| JP4440517B2 (en) * | 2002-05-07 | 2010-03-24 | 信越化学工業株式会社 | Room temperature curable organopolysiloxane composition and parts using the composition as an adhesive |
| JP2006182911A (en) * | 2004-12-27 | 2006-07-13 | Dow Corning Toray Co Ltd | Composition for flame-retardant silicone rubber, flame-retardant silicone rubber composition and flame-retardant silicone rubber |
| CN104761910A (en) * | 2015-04-03 | 2015-07-08 | 新安天玉有机硅有限公司 | Rubber compound for two-stage low-compression-set-free sealing strips and preparation method and applications thereof |
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Inventor after: Pan Hanxin Inventor after: Cheng Yangjie Inventor after: Chen Guizhong Inventor after: Wen Guanyun Inventor after: Tao Jiang Inventor after: Huang Wending Inventor before: Pan Hanxin Inventor before: Cheng Yangjie Inventor before: Chen Guizhong Inventor before: Wen Guanyun Inventor before: Tao Jiang Inventor before: Huang Wending |