CN102532548A - Low-temperature-resisting crude silicon rubber - Google Patents
Low-temperature-resisting crude silicon rubber Download PDFInfo
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- CN102532548A CN102532548A CN2012100090494A CN201210009049A CN102532548A CN 102532548 A CN102532548 A CN 102532548A CN 2012100090494 A CN2012100090494 A CN 2012100090494A CN 201210009049 A CN201210009049 A CN 201210009049A CN 102532548 A CN102532548 A CN 102532548A
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Abstract
The invention discloses a low-temperature-resisting crude silicon rubber which is obtained by polymerizing octamethyl cyclotetrasiloxane (D4), hexaethylcyclotrisiloxane (D3Et), 2,4,6,8-tetravinyl-2,4,6,8-tetramethylcyclotetrasiloxane (D4Vi), a catalyst and an accelerating agent and then heating, removing small molecular low-boiling-point substances in materials in vacuum and cooling to room temperature. According to the invention, the low-temperature-resisting crude silicon rubber product disclosed by the invention is stable, the glass transition temperature (Tg) of the rubber is low and is not crystallized at low temperature; polymerization process is simple and does not need a solvent, and the high-molecular-weight low-temperature-resisting crude silicon rubber can be obtained through severely controlling reaction conditions in short reaction time; and the rubber is high in yield, controllable in molecular weight, simple in posttreatment and easy to produce in a large scale.
Description
Technical field
The invention belongs to the preparation technology field of macromolecular compound, specifically a kind of low temperature resistant raw-silastic continuously and preparation method thereof.
Background technology
Zylox has many uniquenesses and excellent performance; Low etc. like high-low temperature resistant, insulation, hydrophobic, good weatherability, good permeability and compression deformation rate, make in fields such as aerospace, chemical industry, machinery, weaving, building, traffic, medical medicine, agriculturals to have obtained using widely.
Rubber is as a kind of Material Used, and its use value is its elasticity.But along with human scientific-technical progress; The exploration spatial deeply especially needs to use in space exploration under very low temperature, to keep elasticity and sealing property, and the rubber item of works better for a long time; And general rubber does not have use value; Therefore prepare the rubber item of anti-very low temperature, not only have important Research Significance, and have important and practical meanings.The winter hardiness of Zylox is relevant with its second-order transition temperature and low temperature crystallization property.The second-order transition temperature (Tg) of YSR 3286 (PDMS) is-125 ℃, and gathering di-ethyl siloxane (PDES) is the ZGK 5 with minimum second-order transition temperature (Tg) known today, is-145 ℃.Although the second-order transition temperature of PDMS and PDES (Tg) is very low, PDMS is about-50 ℃, and PDES is about-70 ℃ and 20 ℃, and owing to strong crystallization is followed the string, so their range of application is very limited.On siloxane chain, introducing other link, destroy the regularity of polysiloxane chain, is a kind of effective ways that reduce percent crystallinity.As introduce the phenyl modified ZGK 5 that the phenylbenzene chain link obtains, introduce the ZGK 5 that the aminomethyl phenyl chain link obtains the aminomethyl phenyl modification.
Brewer etc. chain as the modification that gathers di-ethyl siloxane with phenylbenzene silica link or methyl trifluoro propyl silica chain link; Obtain lower glass transition temperatures (Tg) behind the reaction 24h; And non crystallized ethyl copolymerized siloxanes under the low temperature, the molecular weight Mn of product is 1.2 * 10
4～1.8 * 10
4Brewer etc. have also prepared the di-ethyl siloxane of gathering with aminomethyl phenyl or ethylphenyl modification, the copolymerized siloxanes that obtains also have low second-order transition temperature (Tg) and low temperature non-crystallizable, molecular weight Mn is 1.5 * 10
4～2.2 * 10
4Liu etc. have prepared the ethyl copolymerized siloxanes of ternary, quaternary, and the copolymerized siloxanes that obtains has low second-order transition temperature (Tg), and is non-crystallizable under the low temperature, and molecular weight Mn is 2.0 * 10
4～2.1 * 10
4
Although the ZGK 5 of above-mentioned preparation has low second-order transition temperature (Tg), and non-crystallizable under the low temperature, but exist the reaction times long, the problem that the molecular weight of product is lower.
Summary of the invention
To the deficiency of prior art, it is short that technical problem to be solved by this invention provides a kind of preparation time, low temperature resistant raw-silastic continuously that molecular weight is high and preparation method thereof.
Low temperature resistant raw-silastic continuously according to the invention is characterized in that, the structure of said rubber is:
Make by following method:
(1), gets octamethylcyclotetrasiloxane (D in weight part
4) 10-90 part, Hexaethyl cyclotrisiloxane (D
3 Et) 10-90 part, tetramethyl-tetrem thiazolinyl cyclotetrasiloxane (D
4 Vi) 1～100 part, 0.0001～2 part of catalyzer, 0～1 part of promotor;
Wherein: described catalyzer is Lithium Hydroxide MonoHydrate, sodium hydroxide, Pottasium Hydroxide, cesium hydroxide, TMAH, perhaps the silicon alkoxide of these materials; Described promotor is polyoxyethylene glycol, DMSO 99.8MIN., crown ether, cave ether, polyethers, THF, N, dinethylformamide, ketone, acetonitrile or oil of mirbane;
(2) polymerization is preceding with octamethylcyclotetrasiloxane (D
4) and Hexaethyl cyclotrisiloxane (D
3 Et) at 30～70 ℃, the 0.5～3h that dewaters under 1～100kPa reduced pressure feeds drying nitrogen then and is warming up to 80～180 ℃, adds tetramethyl-tetrem thiazolinyl cyclotetrasiloxane (D
4 Vi), catalyzer, promotor, polymerization, reaction 1-4h;
(3) after the finishing polymerization, be warming up to 180～220 ℃, under vacuum state, remove the small molecules low-boiling-point substance in the material, the time is 1～3h, is cooled to discharging after the room temperature then, obtains low temperature resistant raw-silastic continuously.
Above-mentioned low temperature resistant raw-silastic continuously preferred embodiment is: step (1) is in weight part, said octamethylcyclotetrasiloxane (D
4) be 30-80 part, said Hexaethyl cyclotrisiloxane (D
3 Et) be 20-70 part, said tetramethyl-tetrem thiazolinyl cyclotetrasiloxane (D
4 Vi) be 2～60 parts, said catalyzer is 0.001～1.5 part, said promotor is 0～1 part.
The preferred Pottasium Hydroxide of above-mentioned catalyzer, cesium hydroxide, TMAH, perhaps their silicon alkoxide.
The preferred said promotor of above-mentioned promotor is polyoxyethylene glycol, crown ether, cave ether or polyethers.
Above-mentioned low temperature resistant raw-silastic continuously preferred embodiment is: step (2) is said with octamethylcyclotetrasiloxane (D
4) and Hexaethyl cyclotrisiloxane (D
3 Et) at 50～70 ℃, the 1～2h that dewaters under 10～20kPa reduced pressure feeds drying nitrogen then and is warming up to 90～170 ℃, adds tetramethyl-tetrem thiazolinyl cyclotetrasiloxane (D
4 Vi), catalyzer, promotor, polymerization, reaction 2～4h.
Above-mentioned low temperature resistant raw-silastic continuously preferred embodiment is: the said temperature of step (3) is 200 ℃.
Low temperature resistant raw-silastic continuously product of the present invention is stable, and (Tg) is low for second-order transition temperature, and be non-crystallizable under the low temperature; And polymerization technique is simple, need not solvent, can obtain the low temperature resistant raw-silastic continuously of high-molecular weight through strictness control reaction conditions in the time at shorter reaction; Productive rate is high; Molecular weight is controlled, and aftertreatment is simple, is prone to large-scale production.
Description of drawings
The DSC curve of Fig. 1 rubber raw rubber (Thermogram of record when differential scanning calorimetry is measured).
Embodiment
Embodiment 1
With 400g octamethylcyclotetrasiloxane (D
4) and 77g Hexaethyl cyclotrisiloxane (D
3 Et) join be furnished with stirring rod, N
2In the reactor drum of conduit and TM, at 60 ℃, the 2h that dewaters under the reduced pressure feeds drying nitrogen then and is warming up to 130 ℃, adds 2.58g tetramethyl-tetrem thiazolinyl cyclotetrasiloxane (D
4 Vi) and 3.99g Pottasium Hydroxide silicon alkoxide, beginning polymerization, reaction 2h.Polyreaction continues to be warming up to 200 ℃ after accomplishing, and under vacuum state, removes the small molecules low-boiling-point substance in the material, and the time is 1h, is cooled to the room temperature discharging, obtains low temperature resistant raw-silastic continuously.Measure ethyl content, contents of ethylene, molecular weight and distribution thereof and the fugitive constituent of product, the result lists in table 1, and the DSC of low temperature resistant raw-silastic continuously lists in Fig. 1.
Embodiment 2
With 400g octamethylcyclotetrasiloxane (D
4) and 77g Hexaethyl cyclotrisiloxane (D
3 Et) join be furnished with stirring rod, N
2In the reactor drum of conduit and TM, at 60 ℃, the 2h that dewaters under the reduced pressure feeds drying nitrogen then and is warming up to 130 ℃, adds 3.23g tetramethyl-tetrem thiazolinyl cyclotetrasiloxane (D
4 Vi) and 3.99g Pottasium Hydroxide silicon alkoxide, beginning polymerization, reaction 2h.Polyreaction continues to be warming up to 200 ℃ after accomplishing, and under vacuum state, removes the small molecules low-boiling-point substance in the material, and the time is 1h, is cooled to the room temperature discharging, obtains low temperature resistant raw-silastic continuously.Measure ethyl content, contents of ethylene, molecular weight and distribution thereof and the fugitive constituent of product, the result lists in table 1.
Embodiment 3
With 400g octamethylcyclotetrasiloxane (D
4) and 460g Hexaethyl cyclotrisiloxane (D
3 Et) join be furnished with stirring rod, N
2In the reactor drum of conduit and TM, at 60 ℃, the 2h that dewaters under the reduced pressure feeds drying nitrogen then and is warming up to 130 ℃, adds 3.87g tetramethyl-tetrem thiazolinyl cyclotetrasiloxane (D
4 Vi) and 6.72g Pottasium Hydroxide silicon alkoxide, beginning polymerization, reaction 2h.Polyreaction continues to be warming up to 200 ℃ after accomplishing, and under vacuum state, removes the small molecules low-boiling-point substance in the material, and the time is 1h, is cooled to the room temperature discharging, obtains low temperature resistant raw-silastic continuously.Measure ethyl content, contents of ethylene, molecular weight and distribution thereof and the fugitive constituent of product, the result lists in table 1.
Embodiment 4
With 400g octamethylcyclotetrasiloxane (D
4) and 250g Hexaethyl cyclotrisiloxane (D
3 Et) join be furnished with stirring rod, N
2In the reactor drum of conduit and TM, at 60 ℃, the 2h that dewaters under the reduced pressure feeds drying nitrogen then and is warming up to 130 ℃, adds 3.87g tetramethyl-tetrem thiazolinyl cyclotetrasiloxane (D
4 Vi) and 8.96g Pottasium Hydroxide silicon alkoxide, beginning polymerization, reaction 2h.Polyreaction continues to be warming up to 200 ℃ after accomplishing, and under vacuum state, removes the small molecules low-boiling-point substance in the material, and the time is 1h, is cooled to the room temperature discharging, obtains low temperature resistant raw-silastic continuously.Measure ethyl content, contents of ethylene, molecular weight and distribution thereof and the fugitive constituent of product, the result lists in table 1.
Embodiment 5
With 400g octamethylcyclotetrasiloxane (D
4) and 77g Hexaethyl cyclotrisiloxane (D
3 Et) join be furnished with stirring rod, N
2In the reactor drum of conduit and TM, at 60 ℃, the 2h that dewaters under the reduced pressure feeds drying nitrogen then and is warming up to 90 ℃, adds 2.58g tetramethyl-tetrem thiazolinyl cyclotetrasiloxane (D
4 Vi), 6.48g TMAH silicon alkoxide and 1.43g polyoxyethylene glycol, beginning polymerization, reaction 2h.Polyreaction continues to be warming up to 150 ℃ after accomplishing, and keeps 1h.Be warming up to 200 ℃ at last again, under vacuum state, remove the small molecules low-boiling-point substance in the material, the time is 1h, is cooled to the room temperature discharging, obtains low temperature resistant raw-silastic continuously.Measure ethyl content, contents of ethylene, molecular weight and distribution thereof and the fugitive constituent of product, the result lists in table 1.
Embodiment 6
With 400g octamethylcyclotetrasiloxane (D
4) and 77g Hexaethyl cyclotrisiloxane (D
3 Et) join be furnished with stirring rod, N
2In the reactor drum of conduit and TM, at 60 ℃, the 2h that dewaters under the reduced pressure feeds drying nitrogen then and is warming up to 90 ℃, adds 2.58g tetramethyl-tetrem thiazolinyl cyclotetrasiloxane (D
4 Vi), 6.48g TMAH silicon alkoxide and 1.43g crown ether, beginning polymerization, reaction 2h.Polyreaction continues to be warming up to 150 ℃ after accomplishing, and keeps 1h.Be warming up to 200 ℃ at last again, under vacuum state, remove the small molecules low-boiling-point substance in the material, the time is 1h, is cooled to the room temperature discharging, obtains low temperature resistant raw-silastic continuously.Measure ethyl content, contents of ethylene, molecular weight and distribution thereof and the fugitive constituent of product, the result lists in table 1.
Table 1
Claims (6)
1. a low temperature resistant raw-silastic continuously is characterized in that, the structure of said rubber is:
Make by following method:
(1), gets octamethylcyclotetrasiloxane (D in weight part
4) 10-90 part, Hexaethyl cyclotrisiloxane (D
3 Et) 10-90 part, tetramethyl-tetrem thiazolinyl cyclotetrasiloxane (D
4 Vi) 1～100 part, 0.0001～2 part of catalyzer, 0～1 part of promotor;
Wherein: described catalyzer is Lithium Hydroxide MonoHydrate, sodium hydroxide, Pottasium Hydroxide, cesium hydroxide, TMAH, perhaps the silicon alkoxide of these materials; Described promotor is polyoxyethylene glycol, DMSO 99.8MIN., crown ether, cave ether, polyethers, THF, N, dinethylformamide, ketone, acetonitrile or oil of mirbane;
(2) polymerization is preceding with octamethylcyclotetrasiloxane (D
4) and Hexaethyl cyclotrisiloxane (D
3 Et) at 30～70 ℃, the 0.5～3h that dewaters under 1～100kPa reduced pressure feeds drying nitrogen then and is warming up to 80～180 ℃, adds tetramethyl-tetrem thiazolinyl cyclotetrasiloxane (D
4 Vi), catalyzer, promotor, polymerization, reaction 1-4h;
(3) after the finishing polymerization, be warming up to 180～220 ℃, under vacuum state, remove the small molecules low-boiling-point substance in the material, the time is 1～3h, is cooled to discharging after the room temperature then, obtains low temperature resistant raw-silastic continuously.
2. low temperature resistant raw-silastic continuously according to claim 1 is characterized in that, step (1) is in weight part, said octamethylcyclotetrasiloxane (D
4) be 30-80 part, said Hexaethyl cyclotrisiloxane (D
3 Et) be 20-70 part, said tetramethyl-tetrem thiazolinyl cyclotetrasiloxane (D
4 Vi) be 2～60 parts, said catalyzer is 0.001～1.5 part, said promotor is 0～1 part.
3. low temperature resistant raw-silastic continuously according to claim 1 is characterized in that, said catalyzer is a Pottasium Hydroxide, cesium hydroxide, TMAH, perhaps their silicon alkoxide.
4. low temperature resistant raw-silastic continuously according to claim 1 is characterized in that, said promotor is polyoxyethylene glycol, crown ether, cave ether or polyethers.
5. low temperature resistant raw-silastic continuously according to claim 1 is characterized in that, step (2) is said with octamethylcyclotetrasiloxane (D
4) and Hexaethyl cyclotrisiloxane (D
3 Et) at 50～70 ℃, the 1～2h that dewaters under 10～20kPa reduced pressure feeds drying nitrogen then and is warming up to 90～170 ℃, adds tetramethyl-tetrem thiazolinyl cyclotetrasiloxane (D
4 Vi), catalyzer, promotor, polymerization, reaction 2～4h.
6. low temperature resistant raw-silastic continuously according to claim 1 is characterized in that, the said temperature of step (3) is 200 ℃.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103224708A (en) * | 2013-05-17 | 2013-07-31 | 山东大学 | Preparation method of condensed type room temperature vulcanized silicone rubber having low temperature resistance |
| CN103342897A (en) * | 2013-07-29 | 2013-10-09 | 山东大学 | Method for preparing low-temperature resisting addition type room-temperature vulcanized silicone rubber |
| CN103554499A (en) * | 2013-09-29 | 2014-02-05 | 安徽同丰橡塑工业有限公司 | Production technology for heat-vulcanized silicone rubber raw rubber |
| CN105694043A (en) * | 2016-03-11 | 2016-06-22 | 山东大学 | Preparation method of high-molecular-weight poly(methyl ethyl-methyl vinyl) siloxane |
| CN109082123A (en) * | 2018-06-28 | 2018-12-25 | 上海电缆研究所有限公司 | Modified electromagnetic shielding silastic material of graphene and preparation method thereof |
| CN109928989A (en) * | 2019-03-08 | 2019-06-25 | 云南民族大学 | A kind of silanol class organic compound and preparation method |
| CN110484083A (en) * | 2019-07-06 | 2019-11-22 | 谢隆 | A kind of two-component tile grout |
| CN111410745A (en) * | 2019-01-07 | 2020-07-14 | 北京化工大学 | Ultra-low temperature-resistant epoxidized silicone rubber and preparation method thereof |
| CN112080150A (en) * | 2020-10-15 | 2020-12-15 | 浙江迪特西科技有限公司 | Preparation method of gas chromatography sample injection pad |
| CN114774045A (en) * | 2022-04-24 | 2022-07-22 | 宁波西奥东升涂料系统有限公司 | Low-temperature-resistant pouring sealant and preparation method and production equipment thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101838393A (en) * | 2010-04-29 | 2010-09-22 | 山东大学 | Method for synthesizing high-molecular-weight ethyl polysiloxane |
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2012
- 2012-01-12 CN CN 201210009049 patent/CN102532548B/en active Active
Patent Citations (1)
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| CN101838393A (en) * | 2010-04-29 | 2010-09-22 | 山东大学 | Method for synthesizing high-molecular-weight ethyl polysiloxane |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103224708A (en) * | 2013-05-17 | 2013-07-31 | 山东大学 | Preparation method of condensed type room temperature vulcanized silicone rubber having low temperature resistance |
| CN103224708B (en) * | 2013-05-17 | 2015-07-08 | 山东大学 | Preparation method of condensed type room temperature vulcanized silicone rubber having low temperature resistance |
| CN103342897A (en) * | 2013-07-29 | 2013-10-09 | 山东大学 | Method for preparing low-temperature resisting addition type room-temperature vulcanized silicone rubber |
| CN103342897B (en) * | 2013-07-29 | 2016-04-20 | 山东大学 | The preparation method of low temperature resistant addition type room temperature vulcanized silicone rubber |
| CN103554499A (en) * | 2013-09-29 | 2014-02-05 | 安徽同丰橡塑工业有限公司 | Production technology for heat-vulcanized silicone rubber raw rubber |
| CN105694043A (en) * | 2016-03-11 | 2016-06-22 | 山东大学 | Preparation method of high-molecular-weight poly(methyl ethyl-methyl vinyl) siloxane |
| CN109082123A (en) * | 2018-06-28 | 2018-12-25 | 上海电缆研究所有限公司 | Modified electromagnetic shielding silastic material of graphene and preparation method thereof |
| CN111410745A (en) * | 2019-01-07 | 2020-07-14 | 北京化工大学 | Ultra-low temperature-resistant epoxidized silicone rubber and preparation method thereof |
| CN109928989A (en) * | 2019-03-08 | 2019-06-25 | 云南民族大学 | A kind of silanol class organic compound and preparation method |
| CN110484083A (en) * | 2019-07-06 | 2019-11-22 | 谢隆 | A kind of two-component tile grout |
| CN112080150A (en) * | 2020-10-15 | 2020-12-15 | 浙江迪特西科技有限公司 | Preparation method of gas chromatography sample injection pad |
| CN114774045A (en) * | 2022-04-24 | 2022-07-22 | 宁波西奥东升涂料系统有限公司 | Low-temperature-resistant pouring sealant and preparation method and production equipment thereof |
| CN114774045B (en) * | 2022-04-24 | 2023-11-07 | 宁波西奥东升涂料系统有限公司 | Low-temperature-resistant pouring sealant and preparation method and production equipment thereof |
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