CN101157801A - Highly ripping-resistant high temperature sulfidation silicon rubber and method for making same - Google Patents
Highly ripping-resistant high temperature sulfidation silicon rubber and method for making same Download PDFInfo
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Abstract
The invention relates to a high anti-tearing and high temperature vulcanized silicon rubber, which is made through mixing and vulcanization of peroxide vulcanization agent and a combination which uses methylvinyl silicone rubber as base adhesive. The combination, according to weight proportion, comprises 100 of methylvinyl silicone rubber with low vinyl content, 1 to 30 of hydroxyl silicone oil, 0.1 to 3 of inner mold release agent, 15 to 80 of reinforcement agent, 1 to 10 of methylvinyl silicone rubber with high vinyl content and 1 to 10 of hydrogen-containing silicone oil; wherein, the vinyl molar content of the low vinyl-content methyvinyl silicone rubber is 0.01 percent to 0.15 percent; the vinyl molar content of the high vinyl-content methylvinyl silicone rubber is 1 percent to 10 percent. The invention has the advantages that the high vinyl-content methylvinyl silicon rubber is added into the methylvinyl silicone rubber, leading unsymmetrical concentration-crosslinking or one place multiple crosslinking to be formed during sulfuration period and the silicone rubber to generate so large resistance at the place that the rubber is difficult to be torn. In addition, the broken and tensile strength of vulcanized silicon rubber products is up to 8.5 MPa, and the tear strength is up to 45 N/mm.
Description
Technical field
The present invention relates to a kind of highly ripping-resistant high temperature sulfidation silicon rubber and preparation method thereof, make rubber composition, make highly ripping-resistant high temperature sulfidation silicon rubber through sulfuration by the methyl vinyl silicone rubber of different contents of ethylene is mediated.
Background technology
High-temperature silicon disulfide rubber is one of most important organosilicon product.The raw material of preparation high-temperature silicon disulfide rubber have usually methyl vinyl silicone rubber (abbreviation rubber), reinforced filling, antistructurizing agent and each analog assistant through kneading, mixing and filter and make.It has good resistant of high or low temperature, UV resistant, radiation hardness, weather-proof, electrical isolation, high ventilative, physiology inertia, low compression set and resistance to fatigue etc., therefore, silicon rubber has obtained using widely at aspects such as Aeronautics and Astronautics, electric, light industry, machinery, building, chemical industry, medical science, daily necessities.In recent years, along with the continuous development and progress of science and technology, people are also more and more higher to the requirement of silicon rubber, and the high-temperature silicon disulfide rubber that exploitation has special purpose is significant.
As everyone knows, the tear strength of common silicon rubber is not fine, and usually the tear strength of producing with precipitated silica is at 15N/mm, thermal silica produce at 20N/mm, as long as a very little tearing port is arranged in the goods, goods will be torn with very little power.The goods that some is had relatively high expectations, as electric wire and cable jacket, common silicon rubber such as joint can't satisfy.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of highly ripping-resistant high temperature sulfidation silicon rubber, by the methyl vinyl silicone rubber of different content vinyl is mediated, utilize reinforced filling, improvement crosslinking method and special process to improve the tearing toughness of high-temperature silicon disulfide rubber.
A further object of the present invention provides a kind of preparation method at above-mentioned prescription highly ripping-resistant high temperature sulfidation silicon rubber.
The present invention solves the problems of the technologies described above the technical scheme of being taked: a kind of highly ripping-resistant high temperature sulfidation silicon rubber, form by the composition and the mixing sulfuration of peroxide vulcanizing agent that with methyl vinyl silicone rubber are basic glue, wherein, the methyl vinyl silicone rubber structural formula is:
Described composition comprises by weight:
A component low vinyl content methyl vinyl silicone rubber 100
B component hydroxy silicon oil 1～30
C component inner pattern releasing agent applicable 0.1～3
D component strengthening agent 15～80
E component high-vinyl-content methyl vinyl silicone rubber 1～10
F component containing hydrogen silicone oil 0.1～3
Wherein, described low vinyl content methyl vinyl silicone rubber molecular weight is: 400,000～800,000, the vinyl molar content is: 0.01～0.15%, and the vinyl molar content comprises a kind of in 0.01,0.02,0.03,0.04,0.05,0.06,0.07,0.08,0.09,0.1,0.11,0.12,0.13,0.14,0.15%; Described high-vinyl-content methyl vinyl silicone rubber molecular weight is: 400,000～800,000, and the vinyl molar content is 1～10%, the vinyl molar content comprises a kind of in 1,2,3,4,5,6,7,8,9,10%.
Dominant mechanism of the present invention is to have added the high-vinyl-content methyl vinyl silicone rubber in common methyl vinyl silicone rubber, makes it produce interrupted " concentrating crosslinked " or " how crosslinked a place is " when sulfuration.Because the vinyl in the high-vinyl-content methyl vinyl silicone rubber is caused by superoxide easily, so C glue place of arrival has just formed highly cross-linked " strong point ".When the sulphurated siliastic goods that add the high-vinyl-content methyl vinyl silicone rubber are torn, at a touch on " strong point ", just be subjected to bigger resistance, stress is disperseed, be difficult to tear.Tear some breaches exactly, also can only cause " the multichain joint is torn ", can not cause catastrophic destruction, thereby improve the tear strength of sulphurated siliastic goods greatly.
On the basis of such scheme, described low vinyl content methyl vinyl silicone rubber molecular weight preferred 500,000～700,000, further preferred 55,0000～65,0000, the too small meeting of molecular weight causes composition intensity on the low side, and the sizing material operability is poor, and molecular weight crosses conference and causes and eat the strengthening agent difficulty, and production efficiency is low; At least contain two vinyl in this component, vinyl molar content preferred 0.03～0.1%.
Described hydroxy silicon oil structural formula is as follows:
Wherein, a is 1～30 integer, and is further preferred 2～15, and the viscosity of this hydroxy silicon oil under 25 ℃ is 10～50cps, and optimum amount is 4.5～10 parts.Hydroxy silicon oil is as the organopolysiloxane constitution controller, and add-on is too much, causes product to be clamminess, demoulding difficulty, and add-on is very few, and then product is short storage period, easily structurizing, poor in processability.
Described hydroxy silicon oil with measuring can be: 4.5,4.7,5,5.3,5.5,5.8,6,6.2,6.5,6.6,6.8,7,7.2,7.5,7.7,8,8.3,8.5,8.7,9,9.2,9.5,9.6,10.
Described inner pattern releasing agent applicable is the stearate compounds, comprises Zinic stearas, calcium stearate, and a kind of or its combination in the barium stearate, consumption is generally 0.1～3 part, preferred 0.1～1 part.With measuring can be: 0.1,0.13,0.16,0.17,0.18,0.19,0.2,0.21,0.22,0.23,0.24,0.27,0.3,0.32,0.35,0.38,0.4,0.45,0.5,0.6,0.7,0.8,0.9,1.0.
Described strengthening agent is that specific surface area is not less than 150m
2The gas-phase silica of/g, preferred 25～70 parts of consumption, the best is 35～60 parts, specifically can be: 35,38,40,42,45,46,47,48,50,52,55,60.
A-200, A-380 that gas-phase silica such as German Degussa company produce, V-15, N20, T-30, T-40 that Germany Wacker company produces, QS-102, QS-20, QS-30, the QS-40 of day Bender mountain company production, EH-5, M-5 etc. that U.S. Cabot company produces.
On the basis of such scheme, described high-vinyl-content methyl vinyl silicone rubber molecular weight preferred 450,000～700,000, further preferred 500,000～600,000; At least contain two vinyl in this component, the vinyl molar content is preferred 4～10%, and when contents of ethylene was very few, the tearing toughness of rubber composition of the present invention was low, and add-on is big, easy embrittlement behind the rubber vulcanization, and hardness raises, and tear strength descends on the contrary.
High-vinyl-content methyl vinyl silicone rubber consumption is generally 1～10 part, specifically can be: 1,1.5,2,2.5,3,3.5,4,4.5,5,5.5,6,6.5,7,7.5,8,8.5,9,9.5,10.
Described containing hydrogen silicone oil structural formula is as follows:
The main purpose that containing hydrogen silicone oil adds is anti-yellow, improves tearing toughness, improves tensile strength, the hydrogen content of containing hydrogen silicone oil is generally 0.1～1.5%, preferred hydrogen content 0.8～1.5%, and hydrogen content is low excessively, then tearing toughness is low, and hydrogen base molar content specifically can be: 0.8,0.9,1.0,1.1,1.2,1.3,1.4,1.5%.
The consumption of containing hydrogen silicone oil is 0.1～3 part, specifically can be: 0.1,0.2,0.3,0.4,0.45,0.5,0.55,0.6,0.75,0.8,0.85,0.9,0.95,1.0,1.1,1.2,1.3,1.4,1.5,1.6,1.8,2.0,2.2,2.4,2.6,2.8,3.0.
Described peroxide vulcanizing agent comprises 2,4-dichlorobenzoperoxide, dicumyl peroxide, 2,5-dimethyl-2,5 di-t-butyl hexane peroxide, a kind of or its combination in the di-t-butyl peroxide.The vulcanizing agent consumption is 0.1～5 part during with composition 100 weight parts, and preferred 0.3～1 part, consumption is very few, vulcanizes insufficiently, and consumption is too much, vulcanizes too fastly, makes product generation over cure easily, and product performance descend.Vulcanizing agent with measuring can be: 0.3,0.35,0.4,0.45,0.5,0.55,0.6,0.65,0.7,0.75,0.8,0.9,1.0.
The invention provides a kind of preparation method of highly ripping-resistant high temperature sulfidation silicon rubber, comprise the steps:
The first step: low vinyl content methyl vinyl silicone rubber, hydroxy silicon oil, inner pattern releasing agent applicable were mediated 5～10 minutes;
Second step: divides and drop into strengthening agent for 3～5 times, mediate evenly fully, the kneading temperature is not higher than 80 ℃, is kneaded into to drop into strengthening agent again after a glob of at every turn, all adds and finally be kneaded into discharging when a glob of up to strengthening agent;
The 3rd step: with the mixture of step 2 in Banbury mixer 150～180 ℃ carry out mixing thermal treatment 1～4 hour, it mainly is to allow antistructurizing agent fully react with strengthening agent, strengthening agent can be dispersed in the methyl vinyl silicone rubber well, better play and improve tension and the effect of tearing toughness ground;
The 4th step: with obtaining bin aging 1～2 hour in the step 3, be cooled to below 120 ℃, in mill, be no less than thin-pass three times, thin-pass thickness 0.5～1mm, thin-pass 3～5 times makes rubber unvulcanizate;
The 5th step: the rubber unvulcanizate that step 4 is obtained is cooled to below 50 ℃, mediates with containing hydrogen silicone oil, high-vinyl-content methyl vinyl silicone rubber, mediates temperature and is not higher than 80 ℃, and the kneading time is no less than 30 minutes, discharging;
The 6th step: after anti-refining in the mill, filter on the rubber extruding filter, filter screen order number is not less than 200 orders, makes rubber composition;
The 7th step: rubber composition and vulcanizing agent that step 6 obtains is mixing, vulcanize, make silicon rubber, sulfidation adopts the step up cure of national standard, and one step cure is to vulcanize 5 minutes down at 175 ℃, and post vulcanization is to vulcanize 4 hours down at 200 ℃;
The invention has the beneficial effects as follows:
Utilization has added the novel method of high-vinyl-content methyl vinyl silicone rubber in common methyl vinyl silicone rubber, make silicon rubber when sulfuration, produce interrupted " concentrating crosslinked " or " how crosslinked a place is ", " strong point " that forms makes silicon rubber produce big resistance at this place, be difficult to tear, can not cause big destruction even if produced the breach page or leaf, the tensile strength of pulling apart of sulphurated siliastic goods reaches 8.5MPa, and tear strength reaches 45N/mm (right-angle tearing).
Embodiment
Embodiment 1
The preparation technology of highly ripping-resistant high temperature sulfidation silicon rubber of the present invention is as follows:
The first step: with molecular weight 600,000, low vinyl content methyl vinyl silicone rubber 100 weight parts of vinyl molar content 0.06%, inner pattern releasing agent applicable Zinic stearas 0.2 weight part, 25 ℃ of viscosity 20cps, antistructurizing agent hydroxy silicon oil 9.6 weight parts of hydroxy radical content 8.0% drop in the kneader and mediated 10 minutes;
Second step: the T-40 white carbon black of 48 weight parts divided to put in the kneader for 5 times mediate, temperature is controlled at below 80 ℃, to mediating evenly fully;
The 3rd step: change in the Banbury mixer mixture of step 2 over to 150～180 ℃ and carry out mixing thermal treatment 3 hours;
The 4th step: with the bin aging that obtains in the step 3 1～2 hour, be cooled to below 120 ℃, in mill, carry out thin-pass, thin-pass thickness 0.5～1mm, thin-pass 5 times makes rubber unvulcanizate;
The 5th step: the rubber unvulcanizate that step 4 is obtained is cooled to below 50 ℃, the rubber unvulcanizate weighing also drops in the kneader again, add 25 ℃ of viscosity 15cps, containing hydrogen silicone oil 0.75 weight part and the molecular weight 550000 of hydrogen base content 1.5%, C glue 4.5 weight parts of vinyl molar content 8.0% are proceeded to mediate, and mediate temperature and are not higher than 80 ℃, 40 minutes kneading time, discharging;
The 6th step: after back mixing in the mill, filter on the rubber extruding filter, filter screen 250 orders make rubber composition (I);
The 7th step: rubber composition (I) 100 weight parts that step 6 is obtained, in the 150mm mill, add 0.55 part 2,5-dimethyl-2,5 di-t-butyl peroxides China hexane vulcanizing agent mixes, in the compression molding agent composition is being obtained the one step cure test piece in sulfuration under 175 ℃ after 5 minutes, in 200 ℃ high temperature oven, carry out simultaneously obtaining behind 4 hours the post vulcanization test piece of post vulcanization, make highly ripping-resistant high temperature sulfidation silicon rubber.(following examples are all according to national testing standards such as GB/T531-1999, GB/T529-1999 GB/T528-1998)
Embodiment 2
Change the T-40 white carbon black among the embodiment 1 into the N20 white carbon black, the hydroxy silicon oil of adding changes 7.2 weight parts into, and all the other are all identical with embodiment 1, obtains rubber composition (II).
Embodiment 3
Change the T-40 white carbon black among the embodiment 1 into the V-15 white carbon black, the hydroxy silicon oil of adding changes 6.2 weight parts into, and all the other are all identical with embodiment 1, obtains rubber composition (III).
Table 1 is asked for an interview in its performance perameter contrast.
Table 1
| Project | The mechanical property of one step cure (testing again after placing 2Hr under the room temperature after one section) | ||
| Composition (I) | Composition (II) | Composition (III) | |
| Hardness (ShoreA) | 61 | 58 | 56 |
| Tensile strength (Mpa) | 8.9 | 8.5 | 7.3 |
| Tensile yield (%) | 520 | 560 | 584 |
| Tear strength (N/mm) | 46.4 | 41.5 | 38.5 |
| Setafter break (%) | 12 | 15 | 16 |
| The mechanical property of post vulcanization (testing again after placing 16Hr under the room temperature after two sections) | |||
| Hardness (ShoreA) | 64 | 61 | 59 |
| Tensile strength (Mpa) | 9.1 | 8.7 | 7.2 |
| Tensile yield (%) | 507 | 545 | 566 |
| Tear strength (N/mm) | 45.2 | 40.6 | 37.2 |
| Setafter break (%) | 10 | 12 | 14 |
Specific surface area by the visible gas-phase silica that uses of table 1 is big more, and its tear strength and stretching are emphasized just big more, and it is more higher that product hardness is also wanted accordingly.
Embodiment 4
The preparation technology of highly ripping-resistant high temperature sulfidation silicon rubber of the present invention is as follows:
The first step: with molecular weight 600,000, low vinyl content methyl vinyl silicone rubber 100 weight parts of vinyl molar content 0.08%, inner pattern releasing agent applicable Zinic stearas 0.2 weight part, 25 ℃ of viscosity 20cps, antistructurizing agent hydroxy silicon oil 7.5 weight parts of hydroxy radical content 8.0% drop into pre-the kneading 10 minutes in the kneader;
Second step: the QS-20 white carbon black of 50 weight parts divided to put in the kneader for 5 times mediate, temperature is controlled at below 80 ℃, to mediating evenly fully;
The 3rd step: change in the Banbury mixer mixture of step 2 over to 150～180 ℃ and carry out mixing thermal treatment 3 hours;
The 4th step: with the bin aging that obtains in the step 3 1～2 hour, be cooled to below 120 ℃, in mill, carry out thin-pass, thin-pass thickness 0.5～1mm, thin-pass 5 times makes rubber unvulcanizate;
The 5th step: the rubber unvulcanizate that step 4 is obtained is cooled to below 50 ℃, weighing also drops in the kneader again, add 25 ℃ of viscosity 15cps, containing hydrogen silicone oil 0.75 weight part and the molecular weight 550000 of hydrogen base content 1.5%, C glue 4.5 weight parts of vinyl molar content 8.0% are proceeded to mediate, and mediate temperature and are not higher than 80 ℃, 40 minutes kneading time, discharging;
The 6th step: after back mixing in the mill, filter on the rubber extruding filter, filter screen 250 orders make rubber composition (IV);
The 7th step: rubber composition (IV) 100 weight parts that step 6 is obtained, in the 150mm mill, add 0.55 part 2,5-dimethyl-2,5 di-t-butyl hexane peroxide vulcanizing agents mix, in the compression molding agent composition is being obtained the one step cure test piece in sulfuration under 175 ℃ after 5 minutes, in 200 ℃ high temperature oven, carry out simultaneously obtaining behind 4 hours the post vulcanization test piece of post vulcanization, make highly ripping-resistant high temperature sulfidation silicon rubber.
Embodiment 5
All the other are all identical with embodiment 2, just change the QS-20 white carbon black add-on among the embodiment 2 into 30 parts, add hydroxy silicon oil and change 4.5 weight parts into, obtain rubber composition (V).
Embodiment 6
All the other are all identical with embodiment 2, just change the QS-20 white carbon black add-on among the embodiment 2 into 40 parts, add hydroxy silicon oil and change 6.0 weight parts into, obtain rubber composition (VI).
Embodiment 7
All the other are all identical with embodiment 2, just change the QS-20 white carbon black add-on among the embodiment 2 into 60 parts, add hydroxy silicon oil and change 9.0 weight parts into, obtain rubber composition (VII).
Table 2 is asked for an interview in its performance perameter contrast.
Table 2
| Project | The mechanical property of one step cure (testing again after placing 2Hr under the room temperature after one section) | |||
| Composition (IV) | Composition (V) | Composition (VI) | Composition (VII) | |
| Hardness (ShoreA) | 59 | 41 | 48 | 65 |
| Tensile strength (Mpa) | 7.8 | 7.2 | 7.6 | 7.3 |
| Tensile yield (%) | 620 | 875 | 780 | 450 |
| Tear strength (N/mm) | 42.1 | 28.6 | 35.2 | 32.5 |
| Setafter break (%) | 15 | 16 | 16 | 10 |
| The mechanical property of post vulcanization (testing again after placing 16Hr under the room temperature after two sections) | ||||
| Hardness (ShoreA) | 63 | 44 | 52 | 69 |
| Tensile strength (Mpa) | 7.6 | 6.8 | 7.3 | 6.9 |
| Tensile yield (%) | 601 | 816 | 725 | 398 |
| Tear strength (N/mm) | 41.1 | 27.5 | 33.6 | 29.8 |
| Setafter break (%) | 12 | 14 | 14 | 8 |
By table 2 as seen, the tear strength of the gas-phase silica weight part of adding its composition in the time of 50 parts is best, adds too much or very few, and tear strength is descended.
Comparative Examples
The preparation technology of highly ripping-resistant high temperature sulfidation silicon rubber of the present invention is as follows:
The first step: with 600,000 molecular weight, low vinyl content methyl vinyl silicone rubber 100 weight parts of vinyl molar content 0.05%, inner pattern releasing agent applicable Zinic stearas 0.2 weight part, 25 ℃ of viscosity 20cps, antistructurizing agent hydroxy silicon oil 10 weight parts of hydroxy radical content 8.0% drop into pre-the kneading 10 minutes in the kneader;
Second step: the T-40 white carbon black of 50 weight parts divided to put into for 5 times eat powder in the kneader, temperature is controlled at below 80 ℃, and is complete to eating powder;
The 3rd step: will eat sizing material that powder finishes and change in the Banbury mixer 150～180 ℃ over to and carry out mixing thermal treatment 3 hours;
The 4th step: parked 1～2 hour, and be cooled to back below 120 ℃ and in mill, carry out thin-pass, thin-pass thickness 0.5～1mm, thin-pass 5 times makes rubber unvulcanizate;
The 5th step: park and be cooled to below 50 ℃, the rubber unvulcanizate weighing that the 4th step was obtained also drops in the kneader again, add 25 ℃ of viscosity 15cps, containing hydrogen silicone oil 0.75 weight part of hydrogen base content 1.5% (in 100 parts of rubber unvulcanizates), mediate, mediate temperature and be not higher than 80 ℃, 40 minutes kneading time;
The 6th step: discharging, on the rubber extruding filter, filtering after the back mixing in the mill, filter screen 250 orders make rubber composition (VIII);
The 7th step: with 100 parts of the 6th rubber compositions that obtain of step, in the 150mm mill, add 0.55 part 2,5-dimethyl-2,5 di-t-butyl peroxides China hexane vulcanizing agent mixes, in the compression molding agent composition is being obtained the one step cure test piece in sulfuration under 175 ℃ after 5 minutes, in 200 ℃ high temperature oven, carry out simultaneously obtaining behind 4 hours the post vulcanization test piece of post vulcanization, make silicon rubber.
Embodiment 8
All the other are all identical with Comparative Examples, just add molecular weight 550000 in comparative example step five, and C glue 2.0 weight parts of vinyl molar content 8.0% obtain rubber composition (IX).
Embodiment 9
All the other are all identical with Comparative Examples, just add molecular weight 550000 in comparative example step five, and C glue 4.5 weight parts of vinyl molar content 8.0% obtain rubber composition (X).
Embodiment 10
All the other are all identical with Comparative Examples, just add molecular weight 550000 in comparative example step five, and C glue 6.0 weight parts of vinyl molar content 8.0% obtain rubber composition (XI).
Embodiment 11
All the other are all identical with Comparative Examples, just add molecular weight 550000 in comparative example step five, and C glue 8.5 weight parts of vinyl molar content 8.0% obtain rubber composition (XII).
Table 3 is asked for an interview in its performance perameter contrast.
Table 3
| Project | The mechanical property of one step cure (testing again after placing 2Hr under the room temperature after one section) | ||||
| Composition (VIII) | Composition (IX) | Composition (X) | Composition (XI) | Composition (XII) | |
| Hardness (ShoreA) | 53 | 57 | 60 | 64 | 66 |
| Tensile strength (Mpa) | 9.5 | 9.3 | 9.1 | 8.7 | 8.3 |
| Tensile yield (%) | 740 | 685 | 550 | 436 | 360 |
| Tear strength (N/mm) | 30.5 | 36.5 | 46.2 | 32.6 | 26.8 |
| Setafter break (%) | 20 | 16 | 12 | 9 | 8 |
| The mechanical property of post vulcanization (testing again after placing 16Hr under the room temperature after two sections) | |||||
| Hardness (ShoreA) | 54 | 60 | 64 | 67 | 71 |
| Tensile strength (Mpa) | 8.6 | 9.0 | 9.2 | 8.3 | 7.5 |
| Tensile yield (%) | 723 | 635 | 522 | 410 | 326 |
| Tear strength (N/mm) | 28.7 | 35.2 | 45.4 | 31.2 | 25.6 |
| Setafter break (%) | 16 | 13 | 10 | 8 | 6 |
By table three as can be seen, the add-on of C glue has very big influence to tear strength, and optimum weight part of C glue is at 3～5 parts.
Claims (9)
1. a highly ripping-resistant high temperature sulfidation silicon rubber is formed by the composition and the mixing sulfuration of peroxide vulcanizing agent that with methyl vinyl silicone rubber are basic glue, and wherein, described composition comprises by weight:
A component low vinyl content methyl vinyl silicone rubber 100
B component hydroxy silicon oil 1～30
C component inner pattern releasing agent applicable 0.1～3
D component strengthening agent 15～80
E component high-vinyl-content methyl vinyl silicone rubber 1～10
F component containing hydrogen silicone oil 0.1～3
Wherein, described low vinyl content methyl vinyl silicone rubber molecular weight is 400,000～800,000, and the vinyl molar content is 0.01～0.15%; High-vinyl-content methyl vinyl silicone rubber molecular weight is 400,000～800,000, and the vinyl molar content is 1～10%.
2. highly ripping-resistant high temperature sulfidation silicon rubber according to claim 1 is characterized in that: described low vinyl content methyl vinyl silicone rubber molecular weight is 550,000～650,000, and the vinyl molar content is 0.03～0.1%.
3. highly ripping-resistant high temperature sulfidation silicon rubber according to claim 1 is characterized in that: described hydroxy silicon oil structural formula is as follows:
Wherein, a is 1～30 integer, and the viscosity of this hydroxy silicon oil under 25 ℃ is 10～50cps, and optimum amount is 4.5～10 parts.
4. highly ripping-resistant high temperature sulfidation silicon rubber according to claim 1 is characterized in that: described inner pattern releasing agent applicable is the stearate compounds, comprises Zinic stearas, calcium stearate, and a kind of or its combination in the barium stearate, consumption is 0.1～1 part.
5. highly ripping-resistant high temperature sulfidation silicon rubber according to claim 1 is characterized in that: described strengthening agent is that specific surface area is not less than 150m
2The gas-phase silica of/g, add-on are 35～60 parts.
6. highly ripping-resistant high temperature sulfidation silicon rubber according to claim 1 is characterized in that: described high-vinyl-content methyl vinyl silicone rubber molecular weight is 400,000～600,000, and the vinyl molar content is 4～10%.
7. highly ripping-resistant high temperature sulfidation silicon rubber according to claim 1 is characterized in that: the hydrogen base molar content of described containing hydrogen silicone oil is 0.8～1.5%.
8. highly ripping-resistant high temperature sulfidation silicon rubber according to claim 1, it is characterized in that: described peroxide vulcanizing agent comprises 2, the 4-dichlorobenzoperoxide, dicumyl peroxide, 2,5-dimethyl-2,5 di-t-butyl hexane peroxide, a kind of or its combination in the di-t-butyl peroxide, described vulcanizing agent consumption are 0.3～1 part during with composition 100 weight parts.
9. at the preparation method of the described highly ripping-resistant high temperature sulfidation silicon rubber of one of claim 1 to 8, it is characterized in that comprising the steps:
The first step: low vinyl content methyl vinyl silicone rubber, hydroxy silicon oil, inner pattern releasing agent applicable are mediated;
Second step: divide and drop into strengthening agent 3～5 times, temperature is being mixed below 80 ℃;
The 3rd step: with the mixture of step 2 in Banbury mixer 150～180 ℃ carry out mixing thermal treatment 1～4 hour;
The 4th step: with the bin aging that obtains in the step 3 1～2 hour, be cooled to below 120 ℃, in mill, be no less than thin-pass three times, make rubber unvulcanizate;
The 5th step: the rubber unvulcanizate that step 4 is obtained is cooled to below 50 ℃, proceeds to mediate with containing hydrogen silicone oil, high-vinyl-content methyl vinyl silicone rubber, mediates temperature and is not higher than 80 ℃, and the kneading time is no less than 30 minutes, discharging;
The 6th step: after back mixing in the mill, filter on the rubber extruding filter, filter screen order number is not less than 200 orders, makes the highly ripping-resistant high temperature sulfidation silicon rubber composition;
The 7th step: highly ripping-resistant high temperature sulfidation silicon rubber composition and vulcanizing agent is mixing, and sulfuration makes silicon rubber.
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Cited By (55)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101270261B (en) * | 2008-05-13 | 2010-06-16 | 刘国强 | Ice and snow resistant, anti-corrosion paint and uses thereof |
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| CN101544834B (en) * | 2008-03-25 | 2011-09-28 | 广东标美硅氟新材料有限公司 | Preparation method and application of cold-contraction type power silicone rubber sleeve |
| CN101270261B (en) * | 2008-05-13 | 2010-06-16 | 刘国强 | Ice and snow resistant, anti-corrosion paint and uses thereof |
| CN101531814B (en) * | 2009-04-15 | 2011-05-11 | 天惠有机硅(深圳)有限公司 | Silastic prescription and producing technique thereof |
| CN101538406B (en) * | 2009-04-17 | 2011-06-22 | 天惠有机硅(深圳)有限公司 | Formulation of silastic anti-yellowing vulcanizing agent and preparation method thereof |
| CN101805520A (en) * | 2010-03-19 | 2010-08-18 | 东莞市宏达新材料有限公司 | Silicone self-adhesive formula and preparation method |
| CN101805521A (en) * | 2010-03-19 | 2010-08-18 | 东莞市宏达新材料有限公司 | Antistatic silica gel composition and preparation method thereof |
| CN102243913A (en) * | 2010-05-12 | 2011-11-16 | 深圳市沃尔核材股份有限公司 | Anti-static silicon rubber sleeve and preparation method thereof |
| CN102243913B (en) * | 2010-05-12 | 2014-04-02 | 深圳市沃尔核材股份有限公司 | Anti-static silicon rubber sleeve and preparation method thereof |
| CN102061096A (en) * | 2010-11-18 | 2011-05-18 | 东莞市耀盛硅材料科技有限公司 | Silicon rubber and preparation method thereof |
| CN102070907A (en) * | 2010-12-16 | 2011-05-25 | 平高集团有限公司 | Silicone rubber for composite insulator and preparation method thereof |
| CN102070907B (en) * | 2010-12-16 | 2012-10-31 | 平高集团有限公司 | Silicone rubber for composite insulator and preparation method thereof |
| CN102796382A (en) * | 2011-05-27 | 2012-11-28 | 广东阿尔派新材料股份有限公司 | Intelligent rubber material with reversible temperature color indication function and preparation method thereof |
| CN102796382B (en) * | 2011-05-27 | 2015-12-09 | 广东阿尔派新材料股份有限公司 | Intelligent rubber material of a kind of reversible temperature color instruction and preparation method thereof |
| CN102888120A (en) * | 2012-09-17 | 2013-01-23 | 滁州天成有机硅高分子材料有限公司 | Mixing silicon rubber composition for anti-dynamic fatigue key |
| CN102888119A (en) * | 2012-09-17 | 2013-01-23 | 滁州天成有机硅高分子材料有限公司 | Low-hardness mixing silicone rubber composition and preparation technology thereof |
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| CN103665885B (en) * | 2012-09-24 | 2016-04-27 | 天惠有机硅(深圳)有限公司 | A kind of High tear resistance silicon rubber and preparation method thereof |
| CN102899000A (en) * | 2012-11-05 | 2013-01-30 | 江苏天辰硅材料有限公司 | Metal self-adhesive silicone rubber mixture and preparation method thereof |
| CN102876050A (en) * | 2012-11-05 | 2013-01-16 | 江苏天辰硅材料有限公司 | High-temperature vulcanized silicone rubber with ultralow hardness and method for preparing same |
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| CN103467996A (en) * | 2013-08-13 | 2013-12-25 | 天长市荣盛有机硅科技有限公司 | High performance silica gel and preparation method thereof |
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| CN104479365A (en) * | 2014-12-25 | 2015-04-01 | 江苏天辰新材料有限公司 | Preparation method of self-oil-seepingsilicone rubber |
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| CN104530717A (en) * | 2014-12-26 | 2015-04-22 | 江苏天辰新材料有限公司 | Low-tensile-permanent-deformation silicon rubber and manufacturing method thereof |
| CN104559202A (en) * | 2015-01-21 | 2015-04-29 | 宜昌兴之新塑胶电子科技有限公司 | Preparation method of high-tear-resistance silicon compounded rubber |
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| CN105348816A (en) * | 2015-12-15 | 2016-02-24 | 江苏天辰新材料股份有限公司 | High-strength and high-tear-resistance silicon rubber as well as preparation method and application method thereof |
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| CN107523061A (en) * | 2017-07-24 | 2017-12-29 | 安徽超越电缆科技有限公司 | A kind of cracking resistance silicone rubber for cable sheath material |
| CN107523064A (en) * | 2017-10-11 | 2017-12-29 | 惠州市臻晖电子有限公司 | A kind of preparation method of high anti-yellowing containment vessel silica gel material and containment vessel |
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| CN107868472A (en) * | 2017-12-01 | 2018-04-03 | 迈高精细高新材料（深圳）有限公司 | A kind of silicon rubber and preparation method thereof |
| CN108795057A (en) * | 2018-06-25 | 2018-11-13 | 淄博泰康轻工制品有限公司 | A kind of glass silica gel sheath |
| CN108795057B (en) * | 2018-06-25 | 2021-07-27 | 淄博泰康轻工制品有限公司 | Glass silica gel cover |
| CN109111745A (en) * | 2018-07-12 | 2019-01-01 | 江苏雄海智能电气有限公司 | A kind of novel high-strength silicone rubber fireproof preserving and sealing material |
| CN109054388A (en) * | 2018-07-12 | 2018-12-21 | 江苏雄海智能电气有限公司 | A kind of preparation method of high-strength silicone rubber fire retardant anticorrosion sealing material |
| CN108822554A (en) * | 2018-07-23 | 2018-11-16 | 安徽立信橡胶科技有限公司 | A kind of High tear resistance silicon rubber formula |
| CN109354878A (en) * | 2018-08-03 | 2019-02-19 | 华南理工大学 | The duplex metal hydroxide nanometer piece and the preparation method and application thereof of organic ceramic presoma modification |
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| CN111171577A (en) * | 2020-02-10 | 2020-05-19 | 江西蓝星星火有机硅有限公司 | Single-component liquid silicone rubber and preparation method thereof |
| CN111534106A (en) * | 2020-05-27 | 2020-08-14 | 扬州宏远新材料股份有限公司 | Preparation method of medical liquid silicone rubber with high tear strength |
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| CN112521753A (en) * | 2020-12-31 | 2021-03-19 | 东莞市源丰新材料有限公司 | High-tear-resistance high-tensile-strength high-transparency silica gel and preparation method thereof |
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| CN113004702A (en) * | 2021-03-08 | 2021-06-22 | 佛山市天宝利硅工程科技有限公司 | Silicone rubber compound and preparation method thereof |
| CN113429792A (en) * | 2021-04-09 | 2021-09-24 | 苏州歌诗夫新材料有限公司 | High-elongation high-strength precipitation gel material for producing medical negative pressure ball |
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| CN115466516A (en) * | 2022-09-14 | 2022-12-13 | 安徽东爵有机硅有限公司 | High-tear-resistance flame-retardant silicone rubber composition and preparation method thereof |
| CN116690853A (en) * | 2023-08-07 | 2023-09-05 | 山东华夏神舟新材料有限公司 | Fluorosilicone rubber release agent and preparation method and application thereof |
| CN116690853B (en) * | 2023-08-07 | 2023-11-14 | 山东华夏神舟新材料有限公司 | Fluorosilicone rubber release agent and preparation method and application thereof |
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