CN104194347A - Preparation method for low-temperature-resistant deacidified room-temperature vulcanized silicone rubber - Google Patents
Preparation method for low-temperature-resistant deacidified room-temperature vulcanized silicone rubber Download PDFInfo
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Abstract
The invention relates to a preparation method for room-temperature vulcanized silicone rubber. The method comprises the following steps: (1) mixing octamethyl cyclotetrasiloxane and hexaethyl cyclotrisiloxane, heating, adding a catalyst, polymerizing, adding water, stirring, adding a neutralizer, heating, and boiling at low temperature to obtain alpha, omega-dihydroxyl polydimethyl diethylsiloxane; (2) adding the alpha, omega-dihydroxyl polydimethyl diethylsiloxane and white carbon black respectively, uniformly mixing, performing heat treatment, and cooling to room temperature to prepare a mixture; (3) stirring the mixture, and adding a cross-linking agent for reaction to prepare low-temperature-resistant deacidified room-temperature vulcanized silicone rubber. The low-temperature-resistant deacidified room-temperature vulcanized silicone rubber prepared by the preparation method is stable and has an excellent mechanical property and low temperature resistance.
Description
Technical field
The present invention relates to a kind of preparation method of room temperature vulcanized silicone rubber, specifically a kind of preparation method of low temperature resistant depickling type room temperature vulcanized silicone rubber, belongs to specialty elastomer production technical field.
Background technology
Prepared by room temperature vulcanized silicone rubber simple, easy to use, of a great variety, widely applicable, can in-place mo(u)lding etc. advantage, be therefore widely used in the fields such as building, electronics, automobile as sizing agent, sealing agent, in-place forming material etc.Along with the deep development in these fields, the performance of room temperature glue is had higher requirement, especially at aerospace field, require rubber item to there is excellent resistance to low temperature.Two important factors that affect rubber low temperature resistance performance are glass transition and crystallization.In all rubber kinds, silicon rubber has minimum second-order transition temperature (T
g), be the best rubber of lower temperature resistance.But the regularity of silicon rubber molecular chain causes silicon rubber crystallization under certain low temperature, has limited silicon rubber in the more application in low temperature field.
The employing copolymerization methods such as Babu have synthesized polydimethyldiphenylsiloxane.Due to adding of copolymerization units, destroy the regularity of polysiloxane molecule chain, this polysiloxane is non-crystalline polymer.But adding of phenyl, make the T of this polysiloxane
graise.In the time that phenyl content in polymkeric substance is 9%, T
gbe only-108 DEG C, and along with the increase of phenyl content, the T of polymkeric substance
gobviously raise.
Brewer etc. have synthesized the poly-diethyl diphenyl siloxane of a series of different phenyl contents.Characterize through DSC, in the time that phenyl content is 8%, polysiloxane is non-crystalline polymer, and T
gfor-127 DEG C.But because ethyl content in this polymkeric substance is very high, the production cost of this polymkeric substance is obviously increased, be unfavorable for applying.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of low temperature resistant depickling type room temperature vulcanized silicone rubber.Silicon rubber low temperature performance excellent prepared by the method, and reduced the production cost of such silicon rubber.
Technical scheme of the present invention is as follows:
A preparation method for low temperature resistant depickling type room temperature vulcanized silicone rubber, step is as follows:
(1) by the octamethylcyclotetrasiloxane (D of 100 weight parts
4) and the hexaetcycletrisiloxane (D of 15~200 weight parts
3 et) under the condition of 20~50 revs/min of low whipping speeds, mix 0.1~0.5 hour, then be warming up to 90~170 DEG C, add the catalyzer of 0.0001~10 weight part, under the condition that low whipping speed is 5~20 revs/min, polymerase 10 .5~1 hour, then add the water of 0.001~5 weight part, stir 2~3 hours, add again the neutralizing agent of 0.0001~10 weight part, stir 1~2 hour, be warming up to again 180~200 DEG C, 5~20 revs/min of low whipping speeds, under the condition of pressure 1~10Pa, de-low boiling 0.5~1 hour, make α, alpha, omega-dihydroxy polydimethyl di-ethyl siloxane,
Described catalyzer is lithium hydroxide, sodium hydroxide, potassium hydroxide, cesium hydroxide, Tetramethylammonium hydroxide, or the silicon alkoxide of these materials;
Described neutralizing agent is ethylene chlorhydrin, phosphoric acid, acetic acid, silica-based phosphoric acid ester;
(2) low whipping speed is under the condition of 100~1000 revs/min, the α that adds respectively step (1) to make, alpha, omega-dihydroxy polydimethyl di-ethyl siloxane and white carbon black, α, the weight ratio of alpha, omega-dihydroxy polydimethyl di-ethyl siloxane and white carbon black is 100:(5~40), after mixing, thermal treatment 0.5~2 hour under 70~180 DEG C of conditions, be cooled to room temperature, make mixture;
(3) mixture step (2) being made is that 1~10Pa, rotating speed are under the condition of 100~1000 revs/min at pressure, stir 0.5~1 hour, add linking agent, linking agent and α, the weight ratio of alpha, omega-dihydroxy polydimethyl di-ethyl siloxane is (1~10): 100, continuing at pressure is that 1~10Pa, rotating speed are to stir 0.1~1 hour under the condition of 100~500 revs/min, makes low temperature resistant depickling type room temperature vulcanized silicone rubber;
In described step (3), linking agent is methyl triacetoxysilane, ethyltriacetoxysilane or dimethyl diacetoxy silane.
Preferred according to the present invention, in described step (1), hexaetcycletrisiloxane (D
3 et) weight part is: 20~150, catalyst weight part is: 0.001~6, the weight part of water is: 0.001~2.
Preferred according to the present invention, described α, the structural formula of alpha, omega-dihydroxy polydimethyl di-ethyl siloxane is as follows:
Wherein: m, n are natural number, and n/ (m+n)=0.01~0.99;
Preferred according to the present invention, in described step (2), α, the weight ratio of alpha, omega-dihydroxy polydimethyl di-ethyl siloxane and white carbon black is 100:(10~30).
Preferred according to the present invention, in described step (2), white carbon black is thermal silica and/or precipitated silica.
Preferred according to the present invention, in described step (3), linking agent and α, the weight ratio of alpha, omega-dihydroxy polydimethyl di-ethyl siloxane is (1~7): 100.
Preferred according to the present invention, in described step (3), stir as adopting planetary mixer to stir.
Beneficial effect
1, the low temperature resistant depickling type room temperature vulcanized silicone rubber that prepared by the present invention, product is stable, has excellent mechanical property and low temperature tolerance characteristics;
2, the low temperature resistant depickling type room temperature vulcanized silicone rubber that prepared by the present invention, in ensureing excellent low-temperature performance, has reduced production cost.
3, in the low temperature resistant depickling type room temperature vulcanized silicone rubber that prepared by the present invention, add the amount of linking agent few, the acidic substance that distribute when curing are low, environmentally friendly;
Brief description of the drawings
The thermography curve (DSC) that the differential scanning calorimetry of low temperature resistant depickling type room temperature vulcanized silicone rubber prepared by Fig. 1, the embodiment of the present invention 1 is measured.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is further elaborated, but institute of the present invention protection domain is not limited to this.
In embodiment, the detection method of tensile strength and tensile yield adopts GB/T 528-1998; The detection method of tear strength adopts GB/T529-1999; The detection method of hardness adopts GB/T 531-1999.
Embodiment 1
A preparation method for low temperature resistant depickling type room temperature vulcanized silicone rubber, step is as follows:
(1) by the octamethylcyclotetrasiloxane (D of 100 weight parts
4) and the hexaetcycletrisiloxane (D of 30 weight parts
3 et) join in reactor, start stirring, stirring velocity is at 30 revs/min, after 0.2 hour, be warming up to 130 DEG C, add the potassium hydroxide silicon alkoxide of 2 weight parts, and stirring velocity is reduced to 10 revs/min, after polymerase 10 .5 hour, add the water of 0.05 weight part, after 2 hours, add the ethylene chlorhydrin of 0.02 weight part, after 1 hour, be warming up to 180 DEG C, under the stirring velocity of 10 revs/min, under 1~10Pa pressure, de-low boiling 1 hour, makes α, alpha, omega-dihydroxy polydimethyl di-ethyl siloxane;
(2) low whipping speed is under the condition of 500 revs/min, adds respectively the α of 100 weight parts, the thermal silica of alpha, omega-dihydroxy polydimethyl di-ethyl siloxane and 20 weight parts, after mixing, under 160 DEG C of conditions, thermal treatment 1 hour, is cooled to room temperature, makes mixture;
(3) mixture step (2) being made is that 1~10Pa, rotating speed are under the condition of 300 revs/min at pressure, stir 0.5 hour, add the methyl triacetoxysilane of 3 weight parts, continuing at pressure is that 1~10Pa, rotating speed are to stir 0.1 hour under the condition of 100 revs/min, makes low temperature resistant depickling type room temperature vulcanized silicone rubber.
The DSC curve (differential scanning calorimetry is surveyed the Thermogram of time recording) of low temperature resistant depickling type room temperature vulcanized silicone rubber as shown in Figure 1; Performance is as shown in table 1.
Embodiment 2
A preparation method for low temperature resistant depickling type room temperature vulcanized silicone rubber, step is as follows:
(1) by the octamethylcyclotetrasiloxane (D of 100 weight parts
4) and the hexaetcycletrisiloxane (D of 30 weight parts
3 et) join in reactor, start stirring, stirring velocity is at 30 revs/min, after 0.2 hour, be warming up to 130 DEG C, add the potassium hydroxide silicon alkoxide of 2 weight parts, and stirring velocity is reduced to 10 revs/min, after polymerase 10 .5 hour, add the water of 0.05 weight part, after 2 hours, add the ethylene chlorhydrin of 0.02 weight part, after 1 hour, be warming up to 180 DEG C, under the stirring velocity of 10 revs/min, under 1~10Pa pressure, de-low boiling 1 hour, makes α, alpha, omega-dihydroxy polydimethyl di-ethyl siloxane;
(2) low whipping speed is under the condition of 500 revs/min, adds respectively the α of 100 weight parts, the precipitated silica of alpha, omega-dihydroxy polydimethyl di-ethyl siloxane and 20 weight parts, after mixing, under 160 DEG C of conditions, thermal treatment 1 hour, is cooled to room temperature, makes mixture;
(3) mixture step (2) being made is that 1~10Pa, rotating speed are under the condition of 300 revs/min at pressure, stir 0.5 hour, add the methyl triacetoxysilane of 5 weight parts, continuing at pressure is that 1~10Pa, rotating speed are to stir 0.1 hour under the condition of 100 revs/min, makes low temperature resistant depickling type room temperature vulcanized silicone rubber.Its performance is as shown in table 1.
Embodiment 3
A preparation method for low temperature resistant depickling type room temperature vulcanized silicone rubber, step is as follows:
(1) by the octamethylcyclotetrasiloxane (D of 100 weight parts
4) and the hexaetcycletrisiloxane (D of 30 weight parts
3 et) join in reactor, start stirring, stirring velocity is at 30 revs/min, after 0.2 hour, be warming up to 130 DEG C, add the potassium hydroxide silicon alkoxide of 2 weight parts, and stirring velocity is reduced to 10 revs/min, after polymerase 10 .5 hour, add the water of 0.05 weight part, after 2 hours, add the ethylene chlorhydrin of 0.02 weight part, after 1 hour, be warming up to 180 DEG C, under the stirring velocity of 10 revs/min, under 1~10Pa pressure, de-low boiling 1 hour, makes α, alpha, omega-dihydroxy polydimethyl di-ethyl siloxane;
(2) low whipping speed is under the condition of 500 revs/min, adds respectively the α of 100 weight parts, the thermal silica of alpha, omega-dihydroxy polydimethyl di-ethyl siloxane and 20 weight parts, after mixing, under 160 DEG C of conditions, thermal treatment 1 hour, is cooled to room temperature, makes mixture;
(3) mixture step (2) being made is that 1~10Pa, rotating speed are under the condition of 300 revs/min at pressure, stir 0.5 hour, add the methyl triacetoxysilane of 7 weight parts, continuing at pressure is that 1~10Pa, rotating speed are to stir 0.1 hour under the condition of 100 revs/min, makes low temperature resistant depickling type room temperature vulcanized silicone rubber.Its performance is as shown in table 1.
Embodiment 4
A preparation method for low temperature resistant depickling type room temperature vulcanized silicone rubber, step is as follows:
(1) by the octamethylcyclotetrasiloxane (D of 100 weight parts
4) and the hexaetcycletrisiloxane (D of 15 weight parts
3 et) join in reactor, start stirring, stirring velocity is at 30 revs/min, after 0.2 hour, be warming up to 110 DEG C, add the cesium hydroxide silicon alkoxide of 2 weight parts, and stirring velocity is reduced to 10 revs/min, after polymerase 10 .5 hour, add the water of 0.05 weight part, after 2 hours, add the ethylene chlorhydrin of 0.02 weight part, after 1 hour, be warming up to 180 DEG C, under the stirring velocity of 10 revs/min, under 1~10Pa pressure, de-low boiling 1 hour, makes α, alpha, omega-dihydroxy polydimethyl di-ethyl siloxane;
(2) low whipping speed is under the condition of 500 revs/min, adds respectively the α of 100 weight parts, the precipitated silica of alpha, omega-dihydroxy polydimethyl di-ethyl siloxane and 10 weight parts, after mixing, under 160 DEG C of conditions, thermal treatment 1 hour, is cooled to room temperature, makes mixture;
(3) mixture step (2) being made is that 1~10Pa, rotating speed are under the condition of 300 revs/min at pressure, stir 0.5 hour, add the ethyltriacetoxysilane of 5 weight parts, continuing at pressure is that 1~10Pa, rotating speed are to stir 0.1 hour under the condition of 100 revs/min, makes low temperature resistant depickling type room temperature vulcanized silicone rubber.Its performance is as shown in table 1.
Embodiment 5
A preparation method for low temperature resistant depickling type room temperature vulcanized silicone rubber, step is as follows:
(1) by the octamethylcyclotetrasiloxane (D of 100 weight parts
4) and the hexaetcycletrisiloxane (D of 200 weight parts
3 et) join in reactor, start stirring, stirring velocity is at 30 revs/min, after 0.2 hour, be warming up to 130 DEG C, add the potassium hydroxide silicon alkoxide of 2 weight parts, and stirring velocity is reduced to 10 revs/min, after polymerase 10 .5 hour, add the water of 0.05 weight part, after 2 hours, add the silica-based phosphoric acid ester of 0.02 weight part, after 1 hour, be warming up to 180 DEG C, under the stirring velocity of 10 revs/min, under 1~10Pa pressure, de-low boiling 1 hour, makes α, alpha, omega-dihydroxy polydimethyl di-ethyl siloxane;
(2) low whipping speed is under the condition of 500 revs/min, adds respectively the α of 100 weight parts, the thermal silica of alpha, omega-dihydroxy polydimethyl di-ethyl siloxane and 40 weight parts, after mixing, under 160 DEG C of conditions, thermal treatment 1 hour, is cooled to room temperature, makes mixture;
(3) mixture step (2) being made is that 1~10Pa, rotating speed are under the condition of 300 revs/min at pressure, stir 0.5 hour, add the methyl triacetoxysilane of 10 weight parts, continuing at pressure is that 1~10Pa, rotating speed are to stir 0.1 hour under the condition of 100 revs/min, makes low temperature resistant depickling type room temperature vulcanized silicone rubber.Its performance is as shown in table 1.
Embodiment 6
A preparation method for low temperature resistant depickling type room temperature vulcanized silicone rubber, step is as follows:
(1) by the octamethylcyclotetrasiloxane (D of 100 weight parts
4) and the hexaetcycletrisiloxane (D of 30 weight parts
3 et) join in reactor, start stirring, stirring velocity is at 30 revs/min, after 0.2 hour, be warming up to 130 DEG C, add the potassium hydroxide silicon alkoxide of 2 weight parts, and stirring velocity is reduced to 10 revs/min, after polymerase 10 .5 hour, add the water of 0.1 weight part, after 3 hours, add the acetic acid of 0.02 weight part, after 1 hour, be warming up to 180 DEG C, under the stirring velocity of 10 revs/min, under 1~10Pa pressure, de-low boiling 1 hour, makes α, alpha, omega-dihydroxy polydimethyl di-ethyl siloxane;
(2) low whipping speed is under the condition of 500 revs/min, adds respectively the α of 100 weight parts, the precipitated silica of alpha, omega-dihydroxy polydimethyl di-ethyl siloxane and 20 weight parts, after mixing, under 160 DEG C of conditions, thermal treatment 1 hour, is cooled to room temperature, makes mixture;
(3) mixture step (1) being made is that 1~10Pa, rotating speed are under the condition of 300 revs/min at pressure, stir 0.5 hour, add the methyl triacetoxysilane of 1 weight part, continuing at pressure is that 1~10Pa, rotating speed are to stir 0.1 hour under the condition of 150 revs/min, makes low temperature resistant depickling type room temperature vulcanized silicone rubber.Its performance is as shown in table 1.
Embodiment 7
A preparation method for low temperature resistant depickling type room temperature vulcanized silicone rubber, step is as follows:
(1) by the octamethylcyclotetrasiloxane (D of 100 weight parts
4) and the hexaetcycletrisiloxane (D of 30 weight parts
3 et) join in reactor, start stirring, stirring velocity is at 30 revs/min, after 0.2 hour, be warming up to 130 DEG C, add the potassium hydroxide silicon alkoxide of 2 weight parts, and stirring velocity is reduced to 10 revs/min, after polymerase 10 .5 hour, add the water of 0.05 weight part, after 2 hours, add the ethylene chlorhydrin of 0.02 weight part, after 1 hour, be warming up to 180 DEG C, under the stirring velocity of 10 revs/min, under 1~10Pa pressure, de-low boiling 1 hour, makes α, alpha, omega-dihydroxy polydimethyl di-ethyl siloxane;
(2) low whipping speed is under the condition of 500 revs/min, adds respectively the α of 100 weight parts, the thermal silica of alpha, omega-dihydroxy polydimethyl di-ethyl siloxane and 15 weight parts, after mixing, under 160 DEG C of conditions, thermal treatment 1 hour, is cooled to room temperature, makes mixture;
(3) mixture step (2) being made is that 1~10Pa, rotating speed are under the condition of 300 revs/min at pressure, stir 0.5 hour, add the dimethyl diacetoxy silane of 5 weight parts, continuing at pressure is that 1~10Pa, rotating speed are to stir 0.1 hour under the condition of 100 revs/min, makes low temperature resistant depickling type room temperature vulcanized silicone rubber.Its performance is as shown in table 1.
Embodiment 8
A preparation method for low temperature resistant depickling type room temperature vulcanized silicone rubber, step is as follows:
(1) by the octamethylcyclotetrasiloxane (D of 100 weight parts
4) and the hexaetcycletrisiloxane (D of 30 weight parts
3 et) join in reactor, start stirring, stirring velocity is at 30 revs/min, after 0.2 hour, be warming up to 130 DEG C, add the potassium hydroxide silicon alkoxide of 2 weight parts, and stirring velocity is reduced to 10 revs/min, after polymerase 10 .5 hour, add the water of 0.05 weight part, after 2 hours, add the ethylene chlorhydrin of 0.02 weight part, after 1 hour, be warming up to 180 DEG C, under the stirring velocity of 10 revs/min, under 1~10Pa pressure, de-low boiling 1 hour, makes α, alpha, omega-dihydroxy polydimethyl di-ethyl siloxane;
(2) low whipping speed is under the condition of 500 revs/min, add respectively the α of 100 weight parts, the thermal silica of the precipitated silica of alpha, omega-dihydroxy polydimethyl di-ethyl siloxane, 10 weight parts and 10 weight parts, after mixing, thermal treatment 1 hour under 160 DEG C of conditions, be cooled to room temperature, make mixture;
(3) mixture step (1) being made is that 1~10Pa, rotating speed are under the condition of 300 revs/min at pressure, stir 0.5 hour, add the methyl triacetoxysilane of 5 weight parts, continuing at pressure is that 1~10Pa, rotating speed are to stir 0.1 hour under the condition of 100 revs/min, makes low temperature resistant depickling type room temperature vulcanized silicone rubber.Its performance is as shown in table 1.
Table 1
Claims (7)
1. a preparation method for low temperature resistant depickling type room temperature vulcanized silicone rubber, is characterized in that, step is as follows:
(1) by the octamethylcyclotetrasiloxane (D of 100 weight parts
4) and the hexaetcycletrisiloxane (D of 15~200 weight parts
3 et) under the condition of 20~50 revs/min of low whipping speeds, mix 0.1~0.5 hour, then be warming up to 90~170 DEG C, add the catalyzer of 0.0001~10 weight part, under the condition that low whipping speed is 5~20 revs/min, polymerase 10 .5~1 hour, then add the water of 0.001~5 weight part, stir 2~3 hours, add again the neutralizing agent of 0.0001~10 weight part, stir 1~2 hour, be warming up to again 180~200 DEG C, 5~20 revs/min of low whipping speeds, under the condition of pressure 1~10Pa, de-low boiling 0.5~1 hour, make α, alpha, omega-dihydroxy polydimethyl di-ethyl siloxane,
Described catalyzer is lithium hydroxide, sodium hydroxide, potassium hydroxide, cesium hydroxide, Tetramethylammonium hydroxide, or the silicon alkoxide of these materials;
Described neutralizing agent is ethylene chlorhydrin, phosphoric acid, acetic acid, silica-based phosphoric acid ester;
(2) low whipping speed is under the condition of 100~1000 revs/min, the α that adds respectively step (1) to make, alpha, omega-dihydroxy polydimethyl di-ethyl siloxane and white carbon black, α, the weight ratio of alpha, omega-dihydroxy polydimethyl di-ethyl siloxane and white carbon black is 100:(5~40), after mixing, thermal treatment 0.5~2 hour under 70~180 DEG C of conditions, be cooled to room temperature, make mixture;
(3) mixture step (2) being made is that 1~10Pa, rotating speed are under the condition of 100~1000 revs/min at pressure, stir 0.5~1 hour, add linking agent, linking agent and α, the weight ratio of alpha, omega-dihydroxy polydimethyl di-ethyl siloxane is (1~10): 100, continuing at pressure is that 1~10Pa, rotating speed are to stir 0.1~1 hour under the condition of 100~500 revs/min, makes low temperature resistant depickling type room temperature vulcanized silicone rubber;
In described step (3), linking agent is methyl triacetoxysilane, ethyltriacetoxysilane or dimethyl diacetoxy silane.
2. preparation method as claimed in claim 1, is characterized in that, in described step (1), and hexaetcycletrisiloxane (D
3 et) weight part is: 20~150, catalyst weight part is: 0.001~6, the weight part of water is: 0.001~2.
3. preparation method as claimed in claim 1, is characterized in that, described α, and the structural formula of alpha, omega-dihydroxy polydimethyl di-ethyl siloxane is as follows:
Wherein: m, n are natural number, and n/ (m+n)=0.01~0.99.
4. preparation method as claimed in claim 1, is characterized in that, in described step (2), and α, the weight ratio of alpha, omega-dihydroxy polydimethyl di-ethyl siloxane and white carbon black is 100:(10~30).
5. preparation method as claimed in claim 1, is characterized in that, in described step (2), white carbon black is thermal silica and/or precipitated silica.
6. preparation method as claimed in claim 1, is characterized in that, in described step (3), and linking agent and α, the weight ratio of alpha, omega-dihydroxy polydimethyl di-ethyl siloxane is (1~7): 100.
7. preparation method as claimed in claim 1, is characterized in that, in described step (3), stirs as adopting planetary mixer to stir.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105802229A (en) * | 2016-04-12 | 2016-07-27 | 山东东岳有机硅材料有限公司 | Low-temperature-resistant mixed silicone rubber and preparation method thereof |
CN112852291A (en) * | 2021-03-24 | 2021-05-28 | 成都市文物考古工作队 | Preparation method of organic silicon rubber for sealing and protecting ancient ivory |
-
2014
- 2014-09-19 CN CN201410482732.9A patent/CN104194347A/en active Pending
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105802229A (en) * | 2016-04-12 | 2016-07-27 | 山东东岳有机硅材料有限公司 | Low-temperature-resistant mixed silicone rubber and preparation method thereof |
CN105802229B (en) * | 2016-04-12 | 2018-10-09 | 山东东岳有机硅材料股份有限公司 | A kind of low temperature resistant melting silicone rubber and preparation method thereof |
CN112852291A (en) * | 2021-03-24 | 2021-05-28 | 成都市文物考古工作队 | Preparation method of organic silicon rubber for sealing and protecting ancient ivory |
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