CN112812571A - Fireproof and arc-resistant silicon rubber, preparation method thereof and fireproof and arc-resistant adhesive tape - Google Patents
Fireproof and arc-resistant silicon rubber, preparation method thereof and fireproof and arc-resistant adhesive tape Download PDFInfo
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- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
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Abstract
The invention relates to the technical field of silicone rubber, in particular to fireproof and arc-resistant silicone rubber, a preparation method thereof and a fireproof and arc-resistant adhesive tape, which comprise the following raw materials in parts by weight: 70-75 parts of methyl vinyl silicone rubber A, 15-25 parts of methyl vinyl silicone rubber B, 0-0.5 part of platinum complex flame retardant, 35-40 parts of fumed silica, 5-10 parts of vinyl silicone oil, 8-12 parts of structure control agent, 1-5 parts of silane coupling agent, 20-30 parts of aluminum hydroxide, 35-55 parts of filler, 1-5 parts of magnesium oxide and 1-1.5 parts of cross-linking agent. The fireproof and arc-resistant silicon rubber is light and thin, has good flame retardance, fire resistance, compressive strength and arc resistance, is simple in preparation method, and the fireproof and arc-resistant adhesive tape prepared by using the fireproof and arc-resistant silicon rubber has good fireproof flame retardance, arc resistance, corrosion resistance and mechanical strength, can avoid greater loss and potential safety hazards caused by fire, and improves the practicability of the fireproof and arc-resistant adhesive tape.
Description
Technical Field
The invention relates to the technical field of silicone rubber, and particularly relates to fireproof and arc-resistant silicone rubber, a preparation method thereof and a fireproof and arc-resistant adhesive tape.
Background
At present, most power supply lines do not adopt flame-retardant cables, so that the power supply lines need to be subjected to enhanced fireproof treatment; even if a small part of power supply lines adopt flame-retardant cables, the flame-retardant cables have serious aging phenomenon, so that the fire-proof treatment of the lines needs to be enhanced; in the cable and cable arrangement dense place where the fault is easy to occur and the place where the fire hazard exists, the fire prevention treatment needs to be strengthened so as to reduce the transmission of the electric arc.
However, the above problems are limited by the fire-proof and arc-resistant materials, construction and other reasons, so that at present, no good solution is available, and in order to avoid causing greater loss and potential safety hazards, it is urgently needed to develop a fire-proof and arc-resistant adhesive tape with better performance.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide the fireproof and anti-electric-arc silicon rubber which is light and thin, has good flame retardance, fire resistance, compressive strength and electric-arc resistance, can maintain the electric-arc resistance of the fireproof and anti-electric-arc silicon rubber to be as long as the service life of a cable, and can reduce the shrinkage rate, the width of grinding marks, the abrasion and the production cost of a fireproof and anti-electric-arc silicon rubber product by compounding the raw materials.
The invention also aims to provide a preparation method of the fireproof and arc-resistant silicon rubber, which is simple, convenient to operate and control, stable in quality, high in production efficiency, low in production cost and capable of realizing large-scale industrial production.
Still another object of the present invention is to provide a fire-proof and arc-resistant adhesive tape, which has excellent fire-proof and flame-retardant properties, arc resistance, corrosion resistance and mechanical strength, maintains the same life as that of a cable, forms a fire-proof wall with low smoke during combustion, can self-extinguish, does not spread flame, can avoid greater loss and potential safety hazard caused by fire, can rapidly recover power supply after an accident, and improves the practicability of the fire-proof and arc-resistant adhesive tape.
The purpose of the invention is realized by the following technical scheme: the fireproof and arc-resistant silicon rubber comprises the following raw materials in parts by weight:
the methyl vinyl silicone rubber A has the vinyl content of 0.02-0.10 percent and the molecular weight of 60-70 ten thousand; the methyl vinyl silicone rubber has a vinyl content of 0.14-0.18% and a molecular weight of 55-65 ten thousand; the vinyl silicone oil has a vinyl molar content of 3-10%.
The fireproof and arc-resistant silicon rubber is light and thin, has good flame retardance, fire resistance, compressive strength and arc resistance, can maintain the arc resistance of the fireproof and arc-resistant silicon rubber to be as long as the service life of a cable, and can reduce the shrinkage rate, the width of grinding marks, the abrasion and the production cost of a fireproof and arc-resistant silicon rubber product by compounding the raw materials. The methyl vinyl silicone rubber A and the methyl vinyl silicone rubber B have high molecular weight, long main chain and large intermolecular force, can effectively improve the mechanical strength of the fireproof and arc-resistant silicone rubber, can ensure that the prepared silicone rubber has better comprehensive properties such as hardness, tensile strength, elongation at break, tearing strength and the like by strictly controlling the mixing proportion of the methyl vinyl silicone rubber with low vinyl content and high vinyl content, polysiloxane molecular chains of the silicone rubber are connected into macromolecules with a three-dimensional network structure through branched chains to form crosslinking, the crosslinking density is increased along with the increase of the vinyl content in the vinyl silicone oil, so the vinyl content has influence on the crosslinking density, the hardness, the tearing strength, the tensile strength and the elongation at break of the silicone rubber, for example, the vinyl content is increased, and the tearing strength and the tensile strength of the silicone rubber are increased and then reduced, further increase in crosslink density results in a decrease in the molar mass of molecular chains between crosslinks, resulting in a decrease in the strength of molecular weights between crosslinks; the particle size of the used modified gas-phase white carbon black particles is small, the specific surface area is 200 plus one square meter per gram (300 square meters per gram), the mechanical strength of the silicone rubber can be improved when the modified gas-phase white carbon black particles are dispersed in the silicone rubber, the anti-tracking performance of the silicone rubber can also be improved when the modified gas-phase white carbon black particles are added, the compatibility of the modified gas-phase white carbon black particles and the silicone rubber is better, and the prepared silicone rubber has excellent heat conduction performance, so that the heat generated by electric arc can be dissipated in time, and the tracking resistance of the silicone; the filler adopted in the method can be filled in the thermosetting resin and the thermoplastic resin to enhance the strength of the silicone rubber, so that the strength of the product can be improved, the hardness and the compressive strength of the product can be improved, and the shrinkage rate, the width of grinding marks, the abrasion and the production cost of the product can be reduced; the addition of the vinyl silicone oil can improve the crosslinking density and the thermal aging performance of the silicone rubber, and the electric arc resistance of the silicone rubber is gradually improved along with the increase of the crosslinking density; the structure control agent is used for effectively controlling the structuralization between the rubber compound and the fumed silica during the processing of the silicone rubber, improving the processing performance of the silicone rubber and prolonging the storage period of the rubber material; the content of the aluminum hydroxide has the influence on the electric leakage, mark forming and ablation performance of the silicon rubber material, and the increase of the content of the aluminum hydroxide can obviously improve the internal electric leakage, electric arc resistance and subjectivity of the silicon rubber material; the high-purity magnesium oxide adopted by the method has excellent alkali resistance and electrical insulation property at high temperature, has high thermal expansion coefficient and thermal conductivity and good light transmittance, is widely used as a high-temperature heat-resistant material, is used as a raw material of a light-transmitting ceramic crucible, a substrate and the like in the ceramic field, is used as a filler of a magnetic device, a filler of an insulating material and various carriers in the electrical material and the electrical field, is used as a ceramic substrate which has the thermal conductivity more than 2 times higher than that of aluminum oxide, and has the electrolyte loss of only 1/10 of the aluminum oxide; platinum in the platinum complex flame retardant promotes oxidative degradation on the surface of the silicon rubber in contact with air to form a high cross-linked structure, so that organic groups on the surface are reduced, a noncombustible siloxane film is formed to shield the air, and therefore flame does not spread into the silicon rubber any more and is self-extinguished, and further the comprehensive performance of the fireproof and arc-resistant silicon rubber is improved.
Preferably, the fumed silica is modified fumed silica, and the modified fumed silica is prepared by the following steps:
s1, weighing 25-35 parts of fumed silica and 1-3 parts of potassium hydroxide according to parts by weight, adding into a stirring device, uniformly mixing and stirring, and pretreating at the temperature of 200-300 ℃ for 20-40min to obtain a mixture A for later use;
s2, weighing 5-10 parts of vinyl silane and 8-16 parts of alkyl carbonate according to parts by weight, adding the mixture A obtained in the step S1, stirring and dispersing the mixture A uniformly at the speed of 800r/min and at the temperature of 200-300 ℃ for 60-100min, and then obtaining the modified fumed silica.
The modified fumed silica adopted in the raw materials is prepared by the method, the fumed silica is effectively modified by the method, part of hydroxyl groups of the fumed silica subjected to modification treatment are replaced by organic groups, so that the value of the hydroxyl groups is greatly reduced, the hydrophobic effect of the surface of the fumed silica is better due to the reduction of the hydroxyl group content of the fumed silica, and the hydroxyl group content of the surface of the modified fumed silica is 0.5/nm2The surface ratio is 390m2The/g can play a role in thickening and improving the rheological property in the invention. The vinyl silane adopted in the method can well treat the hydroxyl on the surface of the fumed silica; the alkyl carbonate is used as an organic matter, and provides an organic substituent group for the modification of the fumed silica, so that the modification of the fumed silica is promoted.
Preferably, each part of the structure control agent is at least one of hydroxyl-terminated polydimethylsiloxane, cyclosilazane and diphenylsilanediol. Each part of the silane coupling agent is a mixture of vinyltrimethoxysilane and vinyltriethoxysilane according to the weight ratio of 0.8-1.0: 1.
The structure control agent adopted by the invention is used as the structure control agent in the processing of the silicon rubber, effectively controls the structuralization between the rubber compound and the modified fumed silica, improves the processing performance of the silicon rubber and prolongs the storage period of the rubber material; the adopted silane coupling agent plays a role in connecting inorganic matters and organic matters, can greatly improve the physical and mechanical properties of the reinforced sizing material and improve the wettability and the dispersibility of the modified fumed silica in the sizing material.
Preferably, each part of the filler is a mixture of silicon micropowder, glass fiber powder and boron nitride according to the weight ratio of 3-4:0.3-0.5: 0.5-1.0. Each part of the cross-linking agent is one of hydrogen-containing silicone oil, tetramethyl ethylenediamine and melamine.
The silicon micropowder adopted in the filler is gray or grey powder, has good fire resistance, can improve the fire resistance of the prepared silicon rubber, the adopted glass fiber powder is formed by chopping, grinding and screening specially-drawn continuous glass fiber strands, and is used as a filling reinforcing material to improve the hardness and compressive strength of a product and reduce the shrinkage rate, the width of grinding marks, abrasion and production cost of the product.
The invention also provides a preparation method of the fireproof and arc-resistant silicon rubber, which comprises the following steps:
1) adding the methyl vinyl silicone rubber A into a vacuum kneader according to parts by weight, kneading for 4-8min, dividing the fumed silica into five equal parts, adding one part of the fumed silica into the kneader, adding one fifth of the total amount of the structure control agent, stirring for 15-30min, adding the rest fumed silica for four times, heating to 95-105 ℃ after agglomeration for rubber mixing, refining for 50-70min under the vacuum condition of- (0.07-0.08) MPa during rubber mixing, discharging, and cooling the rubber for open refining to obtain base rubber for later use;
2) adding methyl vinyl silicone rubber B into a vacuum kneader according to parts by weight, adding one tenth of the total amount of the raw materials of aluminum hydroxide, a filling agent, magnesium oxide and a platinum complex flame retardant into the kneader, uniformly mixing and stirring, adding vinyl silicone oil, and one fifth of the total amount of the raw materials of a structure control agent and a silane coupling agent, stirring for about 15-25min, then adding the rest of aluminum hydroxide, the filling agent, the magnesium oxide, the platinum complex flame retardant, the structure control agent and the silane coupling agent, agglomerating, heating to 95-105 ℃ for rubber mixing, refining for 50-70min under the vacuum condition of- (0.07-0.08) MPa during rubber mixing, discharging, cooling the rubber, and milling to obtain powder rubber for later use;
3) mixing and milling the base rubber obtained in the step 1) and the powder rubber obtained in the step 2) uniformly, putting the mixture into a filter to be filtered by a 145-plus-155-mesh filter screen, and standing for 8-12 hours to obtain mixed rubber for later use;
4) vulcanizing the mixed rubber in an open mill, adding a cross-linking agent and 0.1-0.5 part of a vulcanizing agent, uniformly mixing in an open mill, and rolling to obtain the fireproof and arc-resistant silicon rubber; the vulcanizing agent is 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide, the vulcanizing temperature is 160-200 ℃, and the vulcanizing time is 6-12 min.
The fireproof and arc-resistant silicon rubber is prepared by adopting the steps, the preparation method is simple, the operation and control are convenient, the quality is stable, the production efficiency is high, and the production cost is low. Wherein, the temperature in the rubber mixing process in the step 1) needs to be strictly controlled to be 95-105 ℃ in the preparation process, if the temperature is too high, the filling effect of the modified fumed silica is not good, the reinforcing effect of the modified fumed silica on the methyl vinyl silicone rubber A and the methyl vinyl silicone rubber B is not favorable, and if the stirring speed is too low, the mutual reinforcing effect between the modified fumed silica and the methyl vinyl silicone rubber A and the methyl vinyl silicone rubber B is also not favorable.
The invention also provides a fireproof and arc-resistant adhesive tape which is prepared by adopting the fireproof and arc-resistant silicon rubber, when the fireproof and arc-resistant adhesive tape is prepared, the fireproof and arc-resistant silicon rubber is firstly placed between a first roller and a second roller of a prepared calender, a piece of glass fiber cloth is inserted between the second roller and a third roller of the calender, the fireproof and arc-resistant silicon rubber is attached to the glass fiber after a machine is started, and then the fireproof and arc-resistant silicon rubber is placed in an oven for vulcanization molding to obtain the calendered cloth; coating glue on the calendered cloth, drying and forming, attaching isolation paper, rolling, and cutting into products with corresponding width specifications to obtain the fireproof and arc-resistant adhesive tape; the glue is organic silicon glue.
The fireproof and arc-resistant adhesive tape prepared from the fireproof and arc-resistant silicon rubber has good fireproof flame retardance, arc resistance, corrosion resistance and mechanical strength, can maintain the arc resistance of the fireproof and arc-resistant adhesive tape to have the same service life as that of a cable, forms low smoke of a fireproof wall during combustion, can be self-extinguished, does not spread flame, can avoid greater loss and potential safety hazard caused by fire, can quickly recover power supply after an accident, and improves the practicability of the fireproof and arc-resistant adhesive tape.
The invention has the beneficial effects that: the fireproof and arc-resistant silicon rubber is light and thin, has good flame retardance, fire resistance, compressive strength and arc resistance, can maintain the same service life of the arc resistance as a cable, and can reduce the shrinkage rate, the width of grinding marks, the abrasion and the production cost of a fireproof and arc-resistant silicon rubber product by compounding the raw materials.
The preparation method of the fireproof and arc-resistant silicon rubber is simple, convenient to operate and control, stable in quality, high in production efficiency, low in production cost and capable of realizing large-scale industrial production.
The fireproof and arc-resistant adhesive tape has good fireproof flame retardance, arc resistance, corrosion resistance and mechanical strength, can maintain the arc resistance of the fireproof and arc-resistant adhesive tape to be as long as the service life of a cable, forms low smoke of a fireproof wall during combustion, can be self-extinguished, does not spread flame, can avoid greater loss and potential safety hazard caused by fire, can quickly recover power supply after an accident, and improves the practicability of the fireproof and arc-resistant adhesive tape.
Detailed Description
The present invention will be further described with reference to the following examples for facilitating understanding of those skilled in the art, and the description of the embodiments is not intended to limit the present invention.
Example 1
The fireproof and arc-resistant silicon rubber comprises the following raw materials in parts by weight:
the methyl vinyl silicone rubber A has a vinyl content of 0.02 percent and a molecular weight of 60 ten thousand; the methyl vinyl silicone rubber has a vinyl content of 0.14% and a molecular weight of 55 ten thousand; the vinyl silicone oil has a vinyl molar content of 3%.
The fumed silica is modified fumed silica, and the modified fumed silica is prepared by the following steps:
s1, weighing 25 parts of fumed silica and 1 part of potassium hydroxide according to parts by weight, adding the fumed silica and the potassium hydroxide into a stirring device, uniformly mixing and stirring, and pretreating at 200 ℃ for 20min to obtain a mixture A for later use;
s2, weighing 5 parts of vinyl silane and 8 parts of alkyl carbonate according to parts by weight, adding the mixture A obtained in the step S1, stirring and dispersing the mixture A uniformly at the speed of 400r/min, and then preserving heat for 60min at the temperature of 200 ℃ to obtain the modified fumed silica.
Each part of the structure control agent is hydroxyl-terminated polydimethylsiloxane.
Each part of the silane coupling agent is a mixture of vinyltrimethoxysilane and vinyltriethoxysilane according to the weight ratio of 0.8: 1.
Each part of the filler is a mixture of silicon micropowder, glass fiber powder and boron nitride according to the weight ratio of 3:0.3: 0.5.
Each part of the cross-linking agent is hydrogen-containing silicone oil.
The preparation method of the fireproof and arc-resistant silicon rubber comprises the following steps:
1) adding the methyl vinyl silicone rubber A into a vacuum kneader according to parts by weight, kneading for 4min, dividing the fumed silica into five equal parts, adding one part of the fumed silica into the kneader, adding one fifth of the total amount of the structure control agent into the kneader, stirring for 15min, adding the rest fumed silica into the kneader for four times, heating to 95 ℃ after agglomeration for rubber mixing, refining for 50min under the vacuum condition of-0.07 MPa during rubber mixing, discharging, cooling the rubber, and refining to obtain base rubber for later use;
2) adding methyl vinyl silicone rubber B into a vacuum kneader according to parts by weight, adding one tenth of the total amount of the raw materials of aluminum hydroxide, a filling agent and magnesium oxide into the kneader, uniformly mixing and stirring, adding vinyl silicone oil, and one fifth of the total amount of the raw materials of a structure control agent and a silane coupling agent, stirring for about 15min, then adding the rest of aluminum hydroxide, the filling agent, the magnesium oxide, a platinum complex flame retardant, the structure control agent and the silane coupling agent, heating to 95 ℃ after agglomeration for rubber mixing, refining for 50min under the vacuum condition of-0.07 MPa during rubber mixing, discharging, and cooling and opening to obtain powder rubber for later use;
3) mixing the base rubber obtained in the step 1) and the powder rubber obtained in the step 2), uniformly milling, putting the mixture into a filter, filtering the mixture by using a 145-mesh filter screen, and standing the mixture for 8 hours to obtain mixed rubber for later use;
4) vulcanizing the mixed rubber in an open mill, adding a cross-linking agent and 0.1 part of a vulcanizing agent, uniformly mixing in the open mill, and rolling to obtain the fireproof and arc-resistant silicon rubber; the vulcanizing agent is 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide, the vulcanizing temperature is 160 ℃, and the vulcanizing time is 6 min.
A fireproof and arc-resistant adhesive tape is prepared by adopting the fireproof and arc-resistant silicon rubber, when the fireproof and arc-resistant adhesive tape is prepared, the fireproof and arc-resistant silicon rubber is firstly placed between a first roller and a second roller of a prepared calender, a glass fiber cloth and a second roller and a third roller of the calender are inserted between the first roller and the second roller, the fireproof and arc-resistant silicon rubber is attached to the glass fiber after a machine is started, and then the fireproof and arc-resistant silicon rubber is placed in an oven for vulcanization molding to obtain calendered cloth; coating glue on the calendered cloth, drying and forming, attaching isolation paper, rolling, and cutting into products with corresponding width specifications to obtain the fireproof and arc-resistant adhesive tape; the glue is organic silicon glue.
Example 2
The fireproof and arc-resistant silicon rubber comprises the following raw materials in parts by weight:
the methyl vinyl silicone rubber A has a vinyl content of 0.04% and a molecular weight of 63 ten thousand; the vinyl content of the methyl vinyl silicone rubber is 0.15%, and the molecular weight is 58 ten thousand; the vinyl silicone oil has a vinyl molar content of 4%.
The fumed silica is modified fumed silica, and the modified fumed silica is prepared by the following steps:
s1, weighing 28 parts of fumed silica and 1.5 parts of potassium hydroxide according to parts by weight, adding into a stirring device, uniformly mixing and stirring, and pretreating at 225 ℃ for 25min to obtain a mixture A for later use;
s2, weighing 6 parts of vinyl silane and 10 parts of alkyl carbonate according to parts by weight, adding the mixture A obtained in the step S1, stirring and dispersing the mixture A uniformly at the speed of 500r/min, and then preserving heat for 70min at the temperature of 225 ℃ to obtain the modified fumed silica.
Each part of the structure control agent is hydroxyl-terminated polydimethylsiloxane.
Each part of the silane coupling agent is a mixture of vinyltrimethoxysilane and vinyltriethoxysilane according to the weight ratio of 0.9: 1.
Each part of the filler is a mixture of silicon micropowder, glass fiber powder and boron nitride according to the weight ratio of 3.2:0.35: 0.6.
Each part of the cross-linking agent is hydrogen-containing silicone oil.
The preparation method of the fireproof and arc-resistant silicon rubber comprises the following steps:
1) adding the methyl vinyl silicone rubber A into a vacuum kneader according to parts by weight, kneading for 5min, dividing the fumed silica into five equal parts, adding one part of the fumed silica into the kneader, adding one fifth of the total amount of the structure control agent into the kneader, stirring for 18min, adding the rest fumed silica into the kneader for four times, heating to 98 ℃ after agglomeration for rubber mixing, refining for 55min under the vacuum condition of-0.073 MPa during rubber mixing, discharging, cooling the rubber, and refining to obtain base rubber for later use;
2) adding methyl vinyl silicone rubber B into a vacuum kneader according to parts by weight, adding one tenth of the total amount of the raw materials of aluminum hydroxide, a filling agent, magnesium oxide and a platinum complex flame retardant into the kneader, uniformly mixing and stirring, adding vinyl silicone oil, and one fifth of the total amount of the raw materials of a structure control agent and a silane coupling agent, stirring for about 18min, then adding the rest of aluminum hydroxide, the filling agent, the magnesium oxide, the platinum complex flame retardant, the structure control agent and the silane coupling agent, heating to 98 ℃ after agglomeration for rubber mixing, refining for 55min under the vacuum condition of-0.073 MPa during rubber mixing, discharging, cooling the rubber, and refining to obtain rubber powder for later use;
3) mixing and milling the base rubber obtained in the step 1) and the powder rubber obtained in the step 2) uniformly, putting the mixture into a filter to filter the mixture by a 148-mesh filter screen, and standing the mixture for 9 hours to obtain mixed rubber for later use;
4) vulcanizing the mixed rubber in an open mill, adding a cross-linking agent and 0.2 part of a vulcanizing agent, uniformly mixing in the open mill, and rolling to obtain the fireproof and arc-resistant silicon rubber; the vulcanizing agent is 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide, the vulcanizing temperature is 170 ℃, and the vulcanizing time is 7 min.
A fireproof and arc-resistant adhesive tape is prepared by adopting the fireproof and arc-resistant silicon rubber, when the fireproof and arc-resistant adhesive tape is prepared, the fireproof and arc-resistant silicon rubber is firstly placed between a first roller and a second roller of a prepared calender, a glass fiber cloth and a second roller and a third roller of the calender are inserted between the first roller and the second roller, the fireproof and arc-resistant silicon rubber is attached to the glass fiber after a machine is started, and then the fireproof and arc-resistant silicon rubber is placed in an oven for vulcanization molding to obtain calendered cloth; coating glue on the calendered cloth, drying and forming, attaching isolation paper, rolling, and cutting into products with corresponding width specifications to obtain the fireproof and arc-resistant adhesive tape; the glue is organic silicon glue.
Example 3
The fireproof and arc-resistant silicon rubber comprises the following raw materials in parts by weight:
the methyl vinyl silicone rubber A has a vinyl content of 0.06% and a molecular weight of 65 ten thousand; the methyl vinyl silicone rubber has a vinyl content of 0.16% and a molecular weight of 60 ten thousand; the vinyl silicone oil has a vinyl molar content of 6%.
The fumed silica is modified fumed silica, and the modified fumed silica is prepared by the following steps:
s1, weighing 30 parts of fumed silica and 2 parts of potassium hydroxide according to parts by weight, adding the fumed silica and the potassium hydroxide into a stirring device, uniformly mixing and stirring, and pretreating at 250 ℃ for 30min to obtain a mixture A for later use;
s2, weighing 8 parts of vinyl silane and 12 parts of alkyl carbonate according to parts by weight, adding the mixture A obtained in the step S1, stirring and dispersing the mixture A uniformly at the speed of 600r/min, and then preserving heat for 800min at the temperature of 250 ℃ to obtain the modified fumed silica.
Each part of the structure control agent is hydroxyl-terminated polydimethylsiloxane.
Each part of the silane coupling agent is a mixture of vinyltrimethoxysilane and vinyltriethoxysilane according to the weight ratio of 0.9: 1.
Each part of the filler is a mixture of silicon micropowder, glass fiber powder and boron nitride according to the weight ratio of 3.5:0.4: 0.8.
Each part of the cross-linking agent is hydrogen-containing silicone oil.
The preparation method of the fireproof and arc-resistant silicon rubber comprises the following steps:
1) adding the methyl vinyl silicone rubber A into a vacuum kneader according to parts by weight, kneading for 6min, dividing the fumed silica into five equal parts, adding one part of the fumed silica into the kneader, adding one fifth of the total amount of the structure control agent into the kneader, stirring for 23min, adding the rest fumed silica into the kneader for four times, heating to 100 ℃ after agglomeration for rubber mixing, refining for 60min under the vacuum condition of-0.05 MPa during rubber mixing, discharging, cooling the rubber, and refining to obtain base rubber for later use;
2) adding methyl vinyl silicone rubber B into a vacuum kneader according to parts by weight, adding one tenth of the total amount of the raw materials of aluminum hydroxide, a filling agent, magnesium oxide and a platinum complex flame retardant into the kneader, uniformly mixing and stirring, adding vinyl silicone oil, and one fifth of the total amount of the raw materials of a structure control agent and a silane coupling agent, stirring for about 20min, then adding the rest of aluminum hydroxide, the filling agent, the magnesium oxide, the platinum complex flame retardant, the structure control agent and the silane coupling agent, heating to 100 ℃ after agglomeration for rubber mixing, refining for 60min under the vacuum condition of-0.075 MPa during rubber mixing, discharging, cooling the rubber, and refining to obtain rubber powder for later use;
3) mixing and milling the base rubber obtained in the step 1) and the powder rubber obtained in the step 2) uniformly, putting the mixture into a filter to filter the mixture by a 150-mesh filter screen, and standing the mixture for 10 hours to obtain mixed rubber for later use;
4) vulcanizing the mixed rubber in an open mill, adding a cross-linking agent and 0.3 part of a vulcanizing agent, uniformly mixing in the open mill, and rolling to obtain the fireproof and arc-resistant silicon rubber; the vulcanizing agent is 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide, the vulcanizing temperature is 180 ℃, and the vulcanizing time is 9 min.
A fireproof and arc-resistant adhesive tape is prepared by adopting the fireproof and arc-resistant silicon rubber, when the fireproof and arc-resistant adhesive tape is prepared, the fireproof and arc-resistant silicon rubber is firstly placed between a first roller and a second roller of a prepared calender, a glass fiber cloth and a second roller and a third roller of the calender are inserted between the first roller and the second roller, the fireproof and arc-resistant silicon rubber is attached to the glass fiber after a machine is started, and then the fireproof and arc-resistant silicon rubber is placed in an oven for vulcanization molding to obtain calendered cloth; coating glue on the calendered cloth, drying and forming, attaching isolation paper, rolling, and cutting into products with corresponding width specifications to obtain the fireproof and arc-resistant adhesive tape; the glue is organic silicon glue.
Example 4
The fireproof and arc-resistant silicon rubber comprises the following raw materials in parts by weight:
the methyl vinyl silicone rubber A has a vinyl content of 0.08% and a molecular weight of 68 ten thousand; the vinyl content of the methyl vinyl silicone rubber is 0.178%, and the molecular weight is 63 ten thousand; the vinyl silicone oil has a vinyl molar content of 8%.
The fumed silica is modified fumed silica, and the modified fumed silica is prepared by the following steps:
s1, weighing 33 parts of fumed silica and 2.5 parts of potassium hydroxide according to parts by weight, adding the fumed silica and the potassium hydroxide into a stirring device, uniformly mixing and stirring, and pretreating at 275 ℃ for 35min to obtain a mixture A for later use;
s2, weighing 9 parts of vinyl silane and 14 parts of alkyl carbonate according to parts by weight, adding the mixture A obtained in the step S1, stirring and dispersing the mixture A uniformly at the speed of 700r/min, and then preserving heat for 90min at 275 ℃ to obtain the modified fumed silica.
Each part of the structure control agent is hydroxyl-terminated polydimethylsiloxane.
Each part of the silane coupling agent is a mixture of vinyltrimethoxysilane and vinyltriethoxysilane according to the weight ratio of 0.95: 1.
Each part of the filler is a mixture of silicon micropowder, glass fiber powder and boron nitride according to the weight ratio of 3.8:0.45: 0.8.
Each part of the cross-linking agent is hydrogen-containing silicone oil.
The preparation method of the fireproof and arc-resistant silicon rubber comprises the following steps:
1) adding the methyl vinyl silicone rubber A into a vacuum kneader according to parts by weight, kneading for 7min, dividing the fumed silica into five equal parts, adding one part of the fumed silica into the kneader, adding one fifth of the total amount of the structure control agent into the kneader, stirring for 26min, adding the rest fumed silica into the kneader for four times, heating to 103 ℃ after agglomeration for rubber mixing, refining for 65min under the vacuum condition of-0.078 MPa during rubber mixing, discharging, cooling the rubber, and refining to obtain base rubber for later use;
2) adding methyl vinyl silicone rubber B into a vacuum kneader according to parts by weight, adding one tenth of the total amount of the raw materials of aluminum hydroxide, a filling agent, magnesium oxide and a platinum complex flame retardant into the kneader, uniformly mixing and stirring, adding vinyl silicone oil, and one fifth of the total amount of the raw materials of a structure control agent and a silane coupling agent, stirring for about 23min, then adding the rest of aluminum hydroxide, the filling agent, the magnesium oxide, the platinum complex flame retardant, the structure control agent and the silane coupling agent, heating to 103 ℃ after agglomeration for rubber mixing, refining for 65min under the vacuum condition of-0.078 MPa during rubber mixing, discharging, cooling the rubber, and milling to obtain rubber powder for later use;
3) mixing and milling the base rubber obtained in the step 1) and the powder rubber obtained in the step 2) uniformly, putting the mixture into a filter to filter the mixture through a 125-mesh filter screen, and standing the mixture for 11 hours to obtain mixed rubber for later use;
4) vulcanizing the mixed rubber in an open mill, adding a cross-linking agent and 0.4 part of a vulcanizing agent, uniformly mixing in the open mill, and rolling to obtain the fireproof and arc-resistant silicon rubber; the vulcanizing agent is 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide, the vulcanizing temperature is 190 ℃, and the vulcanizing time is 10 min.
A fireproof and arc-resistant adhesive tape is prepared by adopting the fireproof and arc-resistant silicon rubber, when the fireproof and arc-resistant adhesive tape is prepared, the fireproof and arc-resistant silicon rubber is firstly placed between a first roller and a second roller of a prepared calender, a glass fiber cloth and a second roller and a third roller of the calender are inserted between the first roller and the second roller, the fireproof and arc-resistant silicon rubber is attached to the glass fiber after a machine is started, and then the fireproof and arc-resistant silicon rubber is placed in an oven for vulcanization molding to obtain calendered cloth; coating glue on the calendered cloth, drying and forming, attaching isolation paper, rolling, and cutting into products with corresponding width specifications to obtain the fireproof and arc-resistant adhesive tape; the glue is organic silicon glue.
Example 5
The fireproof and arc-resistant silicon rubber comprises the following raw materials in parts by weight:
the methyl vinyl silicone rubber A has a vinyl content of 0.10% and a molecular weight of 70 ten thousand; the methyl vinyl silicone rubber has a vinyl content of 0.18% and a molecular weight of 65 ten thousand; the vinyl silicone oil has a vinyl molar content of 10%.
The fumed silica is modified fumed silica, and the modified fumed silica is prepared by the following steps:
s1, weighing 35 parts of fumed silica and 3 parts of potassium hydroxide according to parts by weight, adding the fumed silica and the potassium hydroxide into a stirring device, uniformly mixing and stirring, and pretreating at 300 ℃ for 40min to obtain a mixture A for later use;
s2, weighing 10 parts of vinyl silane and 16 parts of alkyl carbonate according to parts by weight, adding the mixture A obtained in the step S1, stirring and dispersing the mixture A uniformly at the speed of 800r/min, and then preserving heat for 100min at the temperature of 300 ℃ to obtain the modified fumed silica.
Each part of the structure control agent is hydroxyl-terminated polydimethylsiloxane.
Each part of the silane coupling agent is a mixture of vinyltrimethoxysilane and vinyltriethoxysilane according to the weight ratio of 1.0: 1.
Each part of the filler is a mixture of silicon micropowder, glass fiber powder and boron nitride according to the weight ratio of 4:0.5: 1.0.
Each part of the cross-linking agent is hydrogen-containing silicone oil.
The preparation method of the fireproof and arc-resistant silicon rubber comprises the following steps:
1) adding the methyl vinyl silicone rubber A into a vacuum kneader according to parts by weight, kneading for 8min, dividing the fumed silica into five equal parts, adding one part of the fumed silica into the kneader, adding one fifth of the total amount of the structure control agent, stirring for 30min, adding the rest fumed silica for four times, agglomerating, heating to 105 ℃ for rubber mixing, refining for 70min under the vacuum condition of-0.08 MPa during rubber mixing, discharging, cooling the rubber, and refining to obtain base rubber for later use;
2) adding methyl vinyl silicone rubber B into a vacuum kneader according to parts by weight, adding one tenth of the total amount of the raw materials of aluminum hydroxide, a filling agent, magnesium oxide and a platinum complex flame retardant into the kneader, uniformly mixing and stirring, adding vinyl silicone oil, and one fifth of the total amount of the raw materials of a structure control agent and a silane coupling agent, stirring for about 25min, then adding the rest of aluminum hydroxide, the filling agent, the magnesium oxide, the platinum complex flame retardant, the structure control agent and the silane coupling agent, heating to 105 ℃ after agglomeration for rubber mixing, refining for 70min under the vacuum condition of-0.08 MPa during rubber mixing, discharging, cooling the rubber, and milling to obtain rubber powder for later use;
3) mixing and milling the base rubber obtained in the step 1) and the powder rubber obtained in the step 2) uniformly, putting the mixture into a filter to filter the mixture by a 155-mesh filter screen, and standing the mixture for 12 hours to obtain mixed rubber for later use;
4) vulcanizing the mixed rubber in an open mill, adding a cross-linking agent and 0.5 part of a vulcanizing agent, uniformly mixing in the open mill, and rolling to obtain the fireproof and arc-resistant silicon rubber; the vulcanizing agent is 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide, the vulcanizing temperature is 200 ℃, and the vulcanizing time is 12 min.
A fireproof and arc-resistant adhesive tape is prepared by adopting the fireproof and arc-resistant silicon rubber, when the fireproof and arc-resistant adhesive tape is prepared, the fireproof and arc-resistant silicon rubber is firstly placed between a first roller and a second roller of a prepared calender, a glass fiber cloth and a second roller and a third roller of the calender are inserted between the first roller and the second roller, the fireproof and arc-resistant silicon rubber is attached to the glass fiber after a machine is started, and then the fireproof and arc-resistant silicon rubber is placed in an oven for vulcanization molding to obtain calendered cloth; coating glue on the calendered cloth, drying and forming, attaching isolation paper, rolling, and cutting into products with corresponding width specifications to obtain the fireproof and arc-resistant adhesive tape; the glue is organic silicon glue.
Comparative example 1
This comparative example differs from example 1 above in that: the white carbon black is not added in the comparative example, and the rest of the content of the comparative example is the same as that of the example 1, and the description is omitted.
Comparative example 2
This comparative example differs from example 3 above in that: in the comparative example, alkyl carbonate is not added in the preparation of the modified fumed silica, and the rest of the comparative example is the same as example 3, and is not described again.
The fire-resistant and arc-resistant silicone rubbers prepared in specific examples 1, 3 and 5 and comparative examples 1 to 2 were respectively subjected to a test of correlation properties, and the test results are shown in table 1:
the test standards of each performance parameter are rebound (GB/T30709-.
TABLE 1
| Item | Example 1 | Example 3 | Example 5 | Comparative example 1 | Comparative example 2 |
| Shore hardness (A) | 75 | 75 | 75 | 52 | 58 |
| Rebound (%) | 44 | 50 | 50 | 33 | 40 |
| Tensile Strength (MPa) | 4 | 6 | 6 | 3.2 | 3.7 |
| Elongation at Break (%) | 220 | 280 | 280 | 200 | 211 |
| Tear Strength (kN/M) | 12 | 15 | 15 | 8 | 10 |
| Volume resistivity, Ω · cm | 2.0×1015 | 2.7×1015 | 2.7×1015 | 1.8×1013 | 2.0×1014 |
| Specific gravity of | 1.48 | 1.53 | 1.53 | 1.22 | 1.36 |
As can be seen from Table 1, the fireproof and arc-resistant silicone rubber prepared in the embodiments 1 and 3 of the invention has excellent mechanical properties, good volume resistivity, hardness and compressive strength, good tear strength, tensile strength, rebound resilience and elongation, and excellent comprehensive properties.
As can be seen from the comparison among examples 1, 3 and 5 and comparative examples 1-2, the addition of fumed silica can make the fireproof and arc-resistant silicone rubber have good volume resistivity, hardness, compressive strength, resilience and elongation, and the modification of fumed silica can further improve the volume resistivity, hardness and compressive strength of the fireproof and arc-resistant silicone rubber, and meanwhile, the fireproof and arc-resistant silicone rubber also has good tear strength, tensile strength, resilience and elongation, has excellent comprehensive performance, and has wide market prospect and application value.
The above-described embodiments are preferred implementations of the present invention, and the present invention may be implemented in other ways without departing from the spirit of the present invention.
Claims (10)
1. A fireproof and arc-resistant silicon rubber is characterized in that: the feed comprises the following raw materials in parts by weight:
2. the fire-proof and arc-resistant silicone rubber according to claim 1, wherein: the methyl vinyl silicone rubber A has the vinyl content of 0.02-0.10 percent and the molecular weight of 60-70 ten thousand; the methyl vinyl silicone rubber has a vinyl content of 0.14-0.18% and a molecular weight of 55-65 ten thousand.
3. The fire-proof and arc-resistant silicone rubber according to claim 1, wherein: the fumed silica is modified fumed silica, and the modified fumed silica is prepared by the following steps:
s1, weighing 25-35 parts of fumed silica and 1-3 parts of potassium hydroxide according to parts by weight, adding into a stirring device, uniformly mixing and stirring, and pretreating at the temperature of 200-300 ℃ for 20-40min to obtain a mixture A for later use;
s2, weighing 5-10 parts of vinyl silane and 8-16 parts of alkyl carbonate according to parts by weight, adding the mixture A obtained in the step S1, stirring and dispersing the mixture A uniformly at the speed of 800r/min and at the temperature of 200-300 ℃ for 60-100min, and then obtaining the modified fumed silica.
4. The fire-proof and arc-resistant silicone rubber according to claim 1, wherein: the vinyl silicone oil has a vinyl molar content of 3-10%.
5. The fire-proof and arc-resistant silicone rubber according to claim 1, wherein: each part of the structure control agent is at least one of hydroxyl-terminated polydimethylsiloxane, cyclic silazane and diphenyl silanediol.
6. The fire-proof and arc-resistant silicone rubber according to claim 1, wherein: each part of the silane coupling agent is a mixture of vinyltrimethoxysilane and vinyltriethoxysilane according to the weight ratio of 0.8-1.0: 1.
7. The fire-proof and arc-resistant silicone rubber according to claim 1, wherein: each part of the filler is a mixture of silicon micropowder, glass fiber powder and boron nitride according to the weight ratio of 3-4:0.3-0.5: 0.5-1.0.
8. The fire-proof and arc-resistant silicone rubber according to claim 1, wherein: each part of the cross-linking agent is one of hydrogen-containing silicone oil, tetramethyl ethylenediamine and melamine.
9. A method for preparing a fire-resistant and arc-resistant silicone rubber according to any one of claims 1 to 8, wherein: is prepared by the following steps:
1) adding the methyl vinyl silicone rubber A into a vacuum kneader according to parts by weight, kneading for 4-8min, dividing the fumed silica into five equal parts, adding one part of the fumed silica into the kneader, adding one fifth of the total amount of the structure control agent, stirring for 15-30min, adding the rest fumed silica for four times, heating to 95-105 ℃ after agglomeration for rubber mixing, refining for 50-70min under the vacuum condition of- (0.07-0.08) MPa during rubber mixing, discharging, and cooling the rubber for open refining to obtain base rubber for later use;
2) adding methyl vinyl silicone rubber B into a vacuum kneader according to parts by weight, adding one tenth of the total amount of the raw materials of aluminum hydroxide, a filling agent, magnesium oxide and a platinum complex flame retardant into the kneader, uniformly mixing and stirring, adding vinyl silicone oil, and one fifth of the total amount of the raw materials of a structure control agent and a silane coupling agent, stirring for about 15-25min, then adding the rest of aluminum hydroxide, the filling agent, the magnesium oxide, the platinum complex flame retardant, the structure control agent and the silane coupling agent, agglomerating, heating to 95-105 ℃ for rubber mixing, refining for 50-70min under the vacuum condition of- (0.07-0.08) MPa during rubber mixing, discharging, cooling the rubber, and milling to obtain powder rubber for later use;
3) mixing and milling the base rubber obtained in the step 1) and the powder rubber obtained in the step 2) uniformly, putting the mixture into a filter to be filtered by a 145-plus-155-mesh filter screen, and standing for 8-12 hours to obtain mixed rubber for later use;
4) and (3) vulcanizing the mixed rubber by open milling, adding a cross-linking agent and 0.1-0.5 part of a vulcanizing agent, uniformly mixing, and rolling to obtain the fireproof and arc-resistant silicon rubber.
10. A fireproof and arc-resistant adhesive tape is characterized in that: the fireproof and arc-resistant adhesive tape is prepared from the fireproof and arc-resistant silicone rubber of any one of claims 1 to 8, and is prepared by putting the fireproof and arc-resistant silicone rubber between a first roller and a second roller of a prepared calender, inserting a glass fiber cloth between the second roller and a third roller of the calender, attaching the fireproof and arc-resistant silicone rubber to the glass fiber after starting the machine, and then putting the fireproof and arc-resistant silicone rubber into an oven for vulcanization molding to obtain calendered cloth; and coating glue on the calendered cloth, drying and forming, attaching isolation paper, rolling, and cutting into products with corresponding width specifications to obtain the fireproof and arc-resistant adhesive tape.
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| CN117757271A (en) * | 2023-12-31 | 2024-03-26 | 东莞市朗晟材料科技有限公司 | Flame-retardant fireproof silicon tape and preparation method thereof |
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