CN106279697A - A kind of low viscosity vinyl silicone oil and preparation method thereof - Google Patents
A kind of low viscosity vinyl silicone oil and preparation method thereof Download PDFInfo
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- CN106279697A CN106279697A CN201610704338.4A CN201610704338A CN106279697A CN 106279697 A CN106279697 A CN 106279697A CN 201610704338 A CN201610704338 A CN 201610704338A CN 106279697 A CN106279697 A CN 106279697A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
- C08G77/08—Preparatory processes characterised by the catalysts used
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/32—Post-polymerisation treatment
- C08G77/34—Purification
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on 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; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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Abstract
The invention discloses a kind of low viscosity vinyl silicone oil and preparation method thereof, the preparation method of this low viscosity vinyl silicone oil comprises the following steps: 1) dimethyl siloxane mixed methylcyclosiloxane is carried out evacuation and takes off low, adds acid and carries out pre-treatment；2) add base catalyst and tetramethyl divinyl disiloxane, fully react；3) to step 2) product carry out except matchmaker, remove base catalyst, then evacuation take off low, obtain low viscosity vinyl silicone oil.The low viscosity vinyl silicone oil water white transparency of the present invention, viscosity is only 80～90cps, product yield reaches more than 93%, and storage stability is good, and the double-component casting glue using the low viscosity vinyl silicone oil of the present invention to make has that viscosity is low, levelling is effective, the hardness advantage such as suitably.The preparation method of the present invention is simple to operate, and production cost is low, it is easy to carry out industrialized production.
Description
Technical field
The present invention relates to a kind of low viscosity vinyl silicone oil and preparation method thereof.
Background technology
The stable in properties of low viscosity vinyl silicone oil, volatile matter is low, is to prepare add-on type liquid silicon rubber, organosilicon embedding
The primary raw material of material, silicone rubber etc..At present, on the market the viscosity of low viscosity vinyl-terminated silicone fluid be concentrated mainly on 200～
, easily there are the problems such as excessive, the poor fluidity of viscosity when making dual composition addition type liquid casting glue in 300cps, and yield is relatively simultaneously
Low, the low-molecular-weight of abjection is many, affects benefit.
Therefore, it is necessary to develop the vinyl silicone oil that a kind of viscosity is lower.
Summary of the invention
It is an object of the invention to provide a kind of low viscosity vinyl silicone oil and preparation method thereof.
The technical solution used in the present invention is:
The preparation method of a kind of low viscosity vinyl silicone oil, comprises the following steps:
1) dimethyl siloxane mixed methylcyclosiloxane is carried out evacuation and take off low, add acid and carry out pre-treatment；
2) add base catalyst and tetramethyl divinyl disiloxane, fully react；
3) to step 2) product carry out except matchmaker, remove base catalyst, then evacuation take off low, obtain low viscosity vinyl
Silicone oil.
Described dimethyl siloxane mixed methylcyclosiloxane, acid, base catalyst, the consumption of tetramethyl divinyl disiloxane
Ratio is 1L:(2～10) g:(2～10) g:(8～30) g.
Described acid is at least one in sulphuric acid, hydrochloric acid, oxalic acid, acetic acid.
Described base catalyst is prepared by the following method and obtains: by dimethyl siloxane mixed methylcyclosiloxane, inorganic base
The methanol solution of methanol solution and Tetramethylammonium hydroxide 1:(0.01 in mass ratio～0.02): (0.03～0.1) adds reaction
Still, room temperature～60 DEG C of evacuation dehydrations 1～4h, then it is warming up to 100～120 DEG C of evacuation dehydrations 2～3h；Described inorganic base is hydrogen
At least one in sodium oxide, potassium hydroxide, calcium hydroxide, barium hydroxide, rubidium hydroxide, Cesium hydrate.；Described inorganic base
The mass fraction of methanol solution is 40～60%；The mass fraction of the methanol solution of described Tetramethylammonium hydroxide be 20～
30%.
Step 1) described in evacuation take off and low carry out at 10～80 DEG C, the time is 0.5～2h.
Step 2) described in the temperature of reaction be 80～150 DEG C, the response time is 2～5h.
Step 3) described in carry out at 140～160 DEG C except matchmaker, the time is 0.5～2h.
Step 3) described in evacuation take off and low carry out at 180～200 DEG C, the time is 1～5h.
The invention has the beneficial effects as follows: the low viscosity vinyl silicone oil water white transparency of the present invention, viscosity be only 80～
90cps, product yield reaches more than 93%, and storage stability is good, uses the low viscosity vinyl silicone oil of the present invention to make
Double-component casting glue has that viscosity is low, levelling is effective, the hardness advantage such as suitably.The preparation method of the present invention is simple to operate, raw
Produce low cost, it is easy to carry out industrialized production.
Detailed description of the invention
The preparation method of a kind of low viscosity vinyl silicone oil, comprises the following steps:
1) dimethyl siloxane mixed methylcyclosiloxane is carried out evacuation and take off low, add acid and carry out pre-treatment；
2) add base catalyst and tetramethyl divinyl disiloxane, fully react；
3) to step 2) product carry out except matchmaker, remove base catalyst, then evacuation take off low, obtain low viscosity vinyl
Silicone oil.
Preferably, described dimethyl siloxane mixed methylcyclosiloxane, acid, base catalyst, tetramethyl divinyl two silica
The amount ratio of alkane is 1L:(2～10) g:(2～10) g:(8～30) g.
Preferably, described acid is at least one in sulphuric acid, hydrochloric acid, oxalic acid, acetic acid.
It is further preferred that described acid is oxalic acid.
Preferably, described base catalyst is prepared by the following method and obtains: by dimethyl siloxane mixed methylcyclosiloxane, nothing
The methanol solution of machine alkali and the methanol solution of Tetramethylammonium hydroxide 1:(0.01 in mass ratio～0.02): (0.03～0.1) adds
Enter reactor, room temperature～60 DEG C of evacuation dehydrations 1～4h, then be warming up to 100～120 DEG C of evacuation dehydrations 2～3h；Described inorganic
Alkali is at least one in sodium hydroxide, potassium hydroxide, calcium hydroxide, barium hydroxide, rubidium hydroxide, Cesium hydrate.；Described nothing
The mass fraction of the methanol solution of machine alkali is 40～60%；The mass fraction of the methanol solution of described Tetramethylammonium hydroxide is 20
～30%.
Preferably, step 1) described in evacuation take off and low carry out at 10～80 DEG C, the time is 0.5～2h.
Preferably, step 2) described in the temperature of reaction be 80～150 DEG C, the response time is 2～5h.
Preferably, step 3) described in carry out at 140～160 DEG C except matchmaker, the time is 0.5～2h.
Preferably, step 3) described in evacuation take off and low carry out at 180～200 DEG C, the time is 1～5h.
Below in conjunction with specific embodiment, the present invention is made further explanation and description.
Embodiment 1:
2.5L dimethyl siloxane mixed methylcyclosiloxane is added reactor, and 80 DEG C of constant temperature evacuation take off low 1h, add 10g oxalic acid
Carry out pre-treatment, add 10g base catalyst, after 15min, add 50g tetramethyl divinyl disiloxane, 120 DEG C of constant temperature
3h is reacted in stirring, then constant temperature 140 DEG C carries out 1h and removes matchmaker, and last 180 DEG C of constant temperature take off low 3h, obtain low viscosity vinyl silicone oil.
Embodiment 2:
3L dimethyl siloxane mixed methylcyclosiloxane is added reactor, and 80 DEG C of constant temperature evacuation take off low 0.5h, add 6g oxalic acid
Carrying out pre-treatment, add 6g base catalyst, add 24g tetramethyl divinyl disiloxane after 25min, 80 DEG C of constant temperature stir
Mixing reaction 2h, then constant temperature 140 DEG C carries out 0.5h and removes matchmaker, last 180 DEG C of constant temperature take off low 1h, obtain low viscosity vinyl silicone oil.
Embodiment 3:
2.5L dimethyl siloxane mixed methylcyclosiloxane is added reactor, and 80 DEG C of constant temperature evacuation take off low 2h, add 25g oxalic acid
Carry out pre-treatment, add 25g base catalyst, after 28min, add 75g tetramethyl divinyl disiloxane, 150 DEG C of constant temperature
5h is reacted in stirring, then constant temperature 160 DEG C carries out 2h and removes matchmaker, and last 200 DEG C of constant temperature take off low 5h, obtain low viscosity vinyl silicone oil.
Embodiment 4:
2.5L dimethyl siloxane mixed methylcyclosiloxane is added reactor, and 60 DEG C of constant temperature evacuation take off low 1h, add 19.65g
Oxalic acid carries out pre-treatment, adds 19.65g base catalyst, adds 55g tetramethyl divinyl disiloxane after 30min,
4h are reacted in 130 DEG C of constant temperature stirrings, then constant temperature 150 DEG C carries out 1.5h and removes matchmaker, and last 190 DEG C of constant temperature take off low 4h, obtain low viscosity second
Thiazolinyl silicone oil.
Test case 1:
The low viscosity vinyl silicone oil of embodiment 1～4 preparation is carried out performance test, its performance test data such as table 1 institute
Show.
The performance test data of the low viscosity vinyl silicone oil of table 1 embodiment 1～4
| Performance indications | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Silicon oil viscosity (cps) | 80 | 90 | 85 | 83 |
| Outward appearance | Water white transparency | Water white transparency | Transparent slightly yellow | Water white transparency |
| Yield (%) | 95 | 94 | 93 | 94 |
Test case 2:
Prepare double-component casting glue with the low viscosity vinyl silicone oil of embodiment 1～4 for raw material, respectively obtain double-component and fill
Sealing 1～4, the performance test data of double-component casting glue 1～4 is as shown in table 2.
The composition of double-component casting glue is as follows:
Component A (mass parts): vinyl silicone oil: 200 parts；Filler: 500～600 parts；Containing hydrogen silicone oil: 20～40 parts；
B component (mass parts): vinyl silicone oil: 220～240 parts；Inhibitor: 0.03～0.05 part；Catalyst 0.2～
0.4 part.
The performance test data of table 2 double-component casting glue 1～4
As shown in Table 1: the low viscosity vinyl silicone oil water white transparency of the present invention, viscosity is low, only 80～90cps, yield
Reach more than 93%, want high 5～10% compared with traditional handicraft formula.
As shown in Table 2: use the present invention low viscosity vinyl silicone oil make double-component casting glue have viscosity low, stream
Flat effective, the hardness advantage such as suitably.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by above-described embodiment
Limit, the change made under other any spirit without departing from the present invention and principle, modify, substitute, combine, simplify,
All should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (9)
1. the preparation method of a low viscosity vinyl silicone oil, it is characterised in that: comprise the following steps:
1) dimethyl siloxane mixed methylcyclosiloxane is carried out evacuation and take off low, add acid and carry out pre-treatment；
2) add base catalyst and tetramethyl divinyl disiloxane, fully react；
3) to step 2) product carry out except matchmaker, remove base catalyst, then evacuation take off low, obtain low viscosity vinyl silicon
Oil.
Preparation method the most according to claim 1, it is characterised in that: described dimethyl siloxane mixed methylcyclosiloxane, acid, alkali
Property catalyst, the amount ratio of tetramethyl divinyl disiloxane are 1L:(2～10) g:(2～10) g:(8～30) g.
Preparation method the most according to claim 1, it is characterised in that: described acid is in sulphuric acid, hydrochloric acid, oxalic acid, acetic acid
At least one.
Preparation method the most according to claim 1, it is characterised in that: described base catalyst is prepared by the following method
Obtain: by the methanol solution of dimethyl siloxane mixed methylcyclosiloxane, the methanol solution of inorganic base and Tetramethylammonium hydroxide by quality
Than 1:(0.01～0.02): (0.03～0.1) adds reactor, room temperature～60 DEG C of evacuation dehydrations 1～4h, then is warming up to 100
～120 DEG C of evacuation dehydrations 2～3h；Described inorganic base is sodium hydroxide, potassium hydroxide, calcium hydroxide, barium hydroxide, hydroxide
At least one in rubidium, Cesium hydrate.；The mass fraction of the methanol solution of described inorganic base is 40～60%；Described tetramethyl hydrogen
The mass fraction of the methanol solution of amine-oxides is 20～30%.
Preparation method the most according to claim 1, it is characterised in that: the evacuation described in step 1) takes off low at 10～80 DEG C
Under carry out, the time is 0.5～2h.
Preparation method the most according to claim 1, it is characterised in that: step 2) described in the temperature of reaction be 80～150
DEG C, the response time is 2～5h.
Preparation method the most according to claim 1, it is characterised in that: entering at 140～160 DEG C except matchmaker described in step 3)
OK, the time is 0.5～2h.
Preparation method the most according to claim 1, it is characterised in that: the evacuation described in step 3) takes off low 180～200
Carrying out at DEG C, the time is 1～5h.
9. the low viscosity vinyl silicone oil that in claim 1～8 prepared by method described in any one.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610704338.4A CN106279697B (en) | 2016-08-22 | 2016-08-22 | A kind of low viscosity vinyl silicone oil and preparation method thereof |
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| CN201610704338.4A CN106279697B (en) | 2016-08-22 | 2016-08-22 | A kind of low viscosity vinyl silicone oil and preparation method thereof |
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| CN106279697A true CN106279697A (en) | 2017-01-04 |
| CN106279697B CN106279697B (en) | 2019-06-25 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108359098A (en) * | 2018-02-26 | 2018-08-03 | 广州盛泰诺新材料科技有限公司 | A kind of vinyl silicone oil and preparation method thereof |
| CN112280039A (en) * | 2020-10-20 | 2021-01-29 | 浙江润禾有机硅新材料有限公司 | Preparation method of ultralow-viscosity vinyl silicone oil |
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| CN102443173A (en) * | 2011-10-26 | 2012-05-09 | 华南理工大学 | Low-viscosity methyl vinyl silicon oil and preparation method thereof |
| CN103333338A (en) * | 2013-07-11 | 2013-10-02 | 江苏天辰硅材料有限公司 | Vinyl silicone oil and synthetic method thereof |
| CN103881095A (en) * | 2014-02-21 | 2014-06-25 | 东莞新东方科技有限公司 | Preparation method of vinyl silicone oil |
| CN105482121A (en) * | 2015-12-29 | 2016-04-13 | 江苏创景科技有限公司 | Synthesis method of polyvinyl silicon oil |
-
2016
- 2016-08-22 CN CN201610704338.4A patent/CN106279697B/en active Active
Patent Citations (4)
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| CN102443173A (en) * | 2011-10-26 | 2012-05-09 | 华南理工大学 | Low-viscosity methyl vinyl silicon oil and preparation method thereof |
| CN103333338A (en) * | 2013-07-11 | 2013-10-02 | 江苏天辰硅材料有限公司 | Vinyl silicone oil and synthetic method thereof |
| CN103881095A (en) * | 2014-02-21 | 2014-06-25 | 东莞新东方科技有限公司 | Preparation method of vinyl silicone oil |
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Non-Patent Citations (1)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108359098A (en) * | 2018-02-26 | 2018-08-03 | 广州盛泰诺新材料科技有限公司 | A kind of vinyl silicone oil and preparation method thereof |
| CN112280039A (en) * | 2020-10-20 | 2021-01-29 | 浙江润禾有机硅新材料有限公司 | Preparation method of ultralow-viscosity vinyl silicone oil |
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| CN106279697B (en) | 2019-06-25 |
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Effective date of registration: 20191122 Address after: 306a, building 1, Zhuoyue Meilin Central Plaza (North District), Zhongkang Road, Futian District, Shenzhen City, Guangdong Province Patentee after: Shenzhen Sunyes Electronic Manufacturing Holding Co., Ltd. Address before: Two road 518132 in Guangdong Province, Shenzhen Guangming New District Gongming Office No. 2 ocean community. Patentee before: Shenzhen Sunyes New Material Co., Ltd. |
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Address after: 519000 room 300, floor 1, Zone C, building 24, Gangwan 1 science and Technology Innovation Park, No. 1 Jintang Road, Tangjiawan Town, high tech Zone, Zhuhai City, Guangdong Province Patentee after: Xinya electronic manufacturing (Guangdong) Co.,Ltd. Address before: 306a, building 1, Zhuoyue Meilin Central Plaza (North District), Zhongkang Road, Futian District, Shenzhen, Guangdong 518000 Patentee before: SHENZHEN SUNYES ELECTRONIC MANUFACTURING HOLDING Co.,Ltd. |
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