CN105885050A - Method for preparing greenhouse vulcanized methyl silicone rubber - Google Patents
Method for preparing greenhouse vulcanized methyl silicone rubber Download PDFInfo
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- CN105885050A CN105885050A CN201610394784.XA CN201610394784A CN105885050A CN 105885050 A CN105885050 A CN 105885050A CN 201610394784 A CN201610394784 A CN 201610394784A CN 105885050 A CN105885050 A CN 105885050A
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- silicone rubber
- room temperature
- methyl silicone
- temperature cure
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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
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses greenhouse vulcanized methyl silicone rubber. By selecting a specific end-capping reagent and a special curing cross-linking agent, product curing is accelerated, viscidity and long-time storage oxidation resistance are improved, process parameters are optimized, the yield of unit time is increased, side reactions and byproducts are reduced, and product purity and yield are increased.
Description
Technical field
The present invention relates to silicone rubber synthesis technical field, especiallyItsRelate to the preparation method of a kind of methyl silicone rubber at room temperature cure.
Background technology
Room temperature vulcanized sili cone rubber, is called for short RTV, refers to that being not required to heat is at room temperature a vulcanizable class silicone rubber.Room temperature vulcanized silicone rubber is that a kind of end group contains hydroxyl, or the silicone rubber of acetoxyl group, and molecular weight is relatively low, the most thick fluid.This kind of rubber adds appropriate reinforcing filler, vulcanizing agent and catalyst, or can at room temperature be vulcanized and elastomer-forming by after the water function in air.After sulfuration completely at aspects such as thermostability, tolerance to cold, dielectric properties all very well, only its mechanical strength is more relatively low, can be used for casting and applying sizing material.
Methyl silicone rubber at room temperature cure, it is called for short 107 glue or RTV-107, it is to prepare one pack system and the basic material of Double-component room-temperature vulcanization type silicone rubber, it also is used as electronic devices and components and the adhering and sealing of molectron, protection against the tide, shockproof and insulant, substantial increase and the lifting of building class along with skyscraper, building sealant raw materials requirement is gradually increased, and the demand of 107 glue also rolls up.
Methyl silicone rubber at room temperature cure the most on the market, hardening time is fast not, and viscosity is relatively low, and long-term storage is apt to deteriorate.
Summary of the invention
In view of this, the present invention proposes that a kind of hardening time is fast, viscosity big and the preparation method of long-term storage stay-in-grade methyl silicone rubber at room temperature cure.
The technical scheme is that and be achieved in that: the preparation method of a kind of methyl silicone rubber at room temperature cure, comprise the following steps,
S1, is warming up to 120 DEG C by dimethicone, end-capping reagent, cure-crosslinking agent, adds catalyst, stirs；
S2,120-125 DEG C of polyreaction 4h；
S3, adds water degraded, regulates reactant liquor viscosity；
S4, oil bath is warming up to when 170 DEG C start to be evacuated to-0.85～-0.1MPa, is continuously heating to 230 DEG C；
S5, detects product viscosity, and addition water adjustment product viscosity, to 6000～10000mPa s, natural cooling, obtains methyl silicone rubber at room temperature cure.
On the basis of above technical scheme, it is preferred that in described step S1, each constituent mass number is as follows:
On the basis of above technical scheme, it is preferred that in described step S1, catalyst uses KOH, LiOH, Me4NOH or Bu4POH。
On the basis of above technical scheme, it is preferred that one or more during end-capping reagent is phosphoric acid, sulfonic acid, dicarboxylic acids, dibasic acid anhydride, binary acyl chlorides or lactone in described step S1.
On the basis of above technical scheme, it is preferred that in described step S1, cure-crosslinking agent uses tetraethyl orthosilicate, ethyl polysilicate or methyl triethyl silicane.
On the basis of above technical scheme, it is preferred that described dimethicone, D3+D4+D5+D6 >=99.8%, D4 >=80%.
On the basis of above technical scheme, it is preferred that described step S1 and S2 are at N2Carry out under protective atmosphere.
The methyl silicone rubber at room temperature cure of the present invention has the advantages that relative to prior art
(1) by selecting specific end-capping reagent and cure-crosslinking agent, accelerate product solidification, promote viscosity and long-term storage antioxygenic property；
(2) Optimizing Process Parameters, improves yield in unit time, reduces side reaction and by-product, improves product purity and recovery rate.
Detailed description of the invention
Below in conjunction with embodiment of the present invention, the technical scheme in embodiment of the present invention is clearly and completely described, it is clear that described embodiment is only a part of embodiment of the present invention rather than whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art are obtained under not making creative work premise, broadly fall into the scope of protection of the invention.
Embodiment 1
The preparation method of the methyl silicone rubber at room temperature cure of the present embodiment, each constituent mass number is as follows:
Concrete preparation process is as follows:
1, equipment operation situation is checked, including water, electricity etc.；
2, it is passed through N2, start vacuum pump and dimethicone, phosphoric acid, tetraethyl orthosilicate pumped in reactor, and to be warming up to still temperature be 120 DEG C；
3, KOH is added, stirring, make catalyst be sufficiently mixed；
4, judging viscosity height during polymerization with eye observation, polymerization time is 4 hours, and temperature is maintained at 120～125 DEG C；
5, add water degraded, regulate reactant liquor viscosity；
6, oil bath is warming up to when 170 DEG C start to be evacuated to-0.85～-0.1MPa, when being continuously heating to 230 DEG C, stops heating up；
7, sampling detection product viscosity, addition water adjustment product viscosity, to 6000～10000mPa s, natural cooling, obtains methyl silicone rubber at room temperature cure.
After testing, methyl silicone rubber at room temperature cure prepared by the present embodiment, hardening time at normal temperatures is 3～5s, and product recovery rate is 83%.
Embodiment 2
The preparation method of the methyl silicone rubber at room temperature cure of the present embodiment, each constituent mass number is as follows:
Concrete preparation process is as follows:
1, equipment operation situation is checked, including water, electricity etc.；
2, it is passed through N2, start vacuum pump and dimethicone, sulfonic acid, ethyl polysilicate pumped in reactor, and to be warming up to still temperature be 120 DEG C；
3, LiOH is added, stirring, make catalyst be sufficiently mixed；
4, judging viscosity height during polymerization with eye observation, polymerization time is 4 hours, and temperature is maintained at 120～125 DEG C；
5, add water degraded, regulate reactant liquor viscosity；
6, oil bath is warming up to when 170 DEG C start to be evacuated to-0.85～-0.1MPa, when being continuously heating to 230 DEG C, stops heating up；
7, sampling detection product viscosity, addition water adjustment product viscosity, to 6000～10000mPa s, natural cooling, obtains methyl silicone rubber at room temperature cure.
After testing, methyl silicone rubber at room temperature cure prepared by the present embodiment, hardening time at normal temperatures is 3～5s, and product recovery rate is 82%.
Embodiment 3
The preparation method of the methyl silicone rubber at room temperature cure of the present embodiment, each constituent mass number is as follows:
Concrete preparation process is as follows:
1, equipment operation situation is checked, including water, electricity etc.；
2, it is passed through N2, start vacuum pump and dimethicone, dicarboxylic acids, methyl triethyl silicane pumped in reactor, and to be warming up to still temperature be 120 DEG C；
3, Me is added4NOH, stirring, make catalyst be sufficiently mixed；
4, judging viscosity height during polymerization with eye observation, polymerization time is 4 hours, and temperature is maintained at 120～125 DEG C；
5, add water degraded, regulate reactant liquor viscosity；
6, oil bath is warming up to when 170 DEG C start to be evacuated to-0.85～-0.1MPa, when being continuously heating to 230 DEG C, stops heating up；
7, sampling detection product viscosity, addition water adjustment product viscosity, to 6000～10000mPa s, natural cooling, obtains methyl silicone rubber at room temperature cure.
After testing, methyl silicone rubber at room temperature cure prepared by the present embodiment, hardening time at normal temperatures is 3～5s, and product recovery rate is 85%.
Embodiment 4
The preparation method of the methyl silicone rubber at room temperature cure of the present embodiment, each constituent mass number is as follows:
Concrete preparation process is as follows:
1, equipment operation situation is checked, including water, electricity etc.；
2, it is passed through N2, start vacuum pump and dimethicone, lactone, methyl triethyl silicane pumped in reactor, and to be warming up to still temperature be 120 DEG C；
3, Bu is added4POH, stirring, make catalyst be sufficiently mixed；
4, judging viscosity height during polymerization with eye observation, polymerization time is 4 hours, and temperature is maintained at 120～125 DEG C；
5, add water degraded, regulate reactant liquor viscosity；
6, oil bath is warming up to when 170 DEG C start to be evacuated to-0.85～-0.1MPa, when being continuously heating to 230 DEG C, stops heating up；
7, sampling detection product viscosity, addition water adjustment product viscosity, to 6000～10000mPa s, natural cooling, obtains methyl silicone rubber at room temperature cure.
After testing, methyl silicone rubber at room temperature cure prepared by the present embodiment, hardening time at normal temperatures is 3～5s, and product recovery rate is 85%.
The foregoing is only the better embodiment of the present invention, not in order to limit the present invention, all within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.
Claims (7)
1. the preparation method of a methyl silicone rubber at room temperature cure, it is characterised in that: comprise the following steps,
S1, is warming up to 120 DEG C by dimethicone, end-capping reagent, cure-crosslinking agent, adds catalyst, stirs；
S2,120-125 DEG C of polyreaction 4h；
S3, adds water degraded, regulates reactant liquor viscosity；
S4, oil bath is warming up to when 170 DEG C start to be evacuated to-0.85～-0.1MPa, is continuously heating to 230 DEG C；
S5, detects product viscosity, and addition water adjustment product viscosity, to 6000～10000mPa s, natural cooling, obtains methyl silicone rubber at room temperature cure.
2. the preparation method of methyl silicone rubber at room temperature cure as claimed in claim 1, it is characterised in that: in described step S1, each constituent mass number is as follows:
3. the preparation method of methyl silicone rubber at room temperature cure as claimed in claim 1, it is characterised in that: in described step S1, catalyst uses KOH, LiOH, Me4NOH or Bu4POH。
4. the preparation method of methyl silicone rubber at room temperature cure as claimed in claim 1, it is characterised in that: one or more during end-capping reagent is phosphoric acid, sulfonic acid, dicarboxylic acids, dibasic acid anhydride, binary acyl chlorides or lactone in described step S1.
5. the preparation method of methyl silicone rubber at room temperature cure as claimed in claim 1, it is characterised in that: in described step S1, cure-crosslinking agent uses tetraethyl orthosilicate, ethyl polysilicate or methyl triethyl silicane.
6. the preparation method of methyl silicone rubber at room temperature cure as claimed in claim 1, it is characterised in that: described dimethicone, D3+D4+D5+D6 >=99.8%, D4 >=80%.
7. the preparation method of methyl silicone rubber at room temperature cure as claimed in claim 1, it is characterised in that: described step S1 and S2 are at N2Carry out under protective atmosphere.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610394784.XA CN105885050A (en) | 2016-06-06 | 2016-06-06 | Method for preparing greenhouse vulcanized methyl silicone rubber |
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| CN201610394784.XA CN105885050A (en) | 2016-06-06 | 2016-06-06 | Method for preparing greenhouse vulcanized methyl silicone rubber |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115785447A (en) * | 2021-09-10 | 2023-03-14 | 山东大学 | Ultralow-viscosity liquid silicone rubber and cross-linking agent and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101768273A (en) * | 2010-01-14 | 2010-07-07 | 湖北大学 | Method for preparing multifunctional or non-functional end group polyorganosiloxane by ring-opening polymerization of cyclosiloxane |
| CN102558563A (en) * | 2011-12-30 | 2012-07-11 | 蓝星化工新材料股份有限公司江西星火有机硅厂 | Preparation method for high-viscosity 107 glue |
| CN102604103A (en) * | 2012-04-11 | 2012-07-25 | 唐山三友硅业有限责任公司 | Preparation method of low volatile matter room temperature vulcanization methyl silicone rubber |
| CN103435807A (en) * | 2013-08-01 | 2013-12-11 | 广东信翼新材料股份有限公司 | Method for preparing odorless and transparent 107 glue at ordinary pressure |
-
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- 2016-06-06 CN CN201610394784.XA patent/CN105885050A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101768273A (en) * | 2010-01-14 | 2010-07-07 | 湖北大学 | Method for preparing multifunctional or non-functional end group polyorganosiloxane by ring-opening polymerization of cyclosiloxane |
| CN102558563A (en) * | 2011-12-30 | 2012-07-11 | 蓝星化工新材料股份有限公司江西星火有机硅厂 | Preparation method for high-viscosity 107 glue |
| CN102604103A (en) * | 2012-04-11 | 2012-07-25 | 唐山三友硅业有限责任公司 | Preparation method of low volatile matter room temperature vulcanization methyl silicone rubber |
| CN103435807A (en) * | 2013-08-01 | 2013-12-11 | 广东信翼新材料股份有限公司 | Method for preparing odorless and transparent 107 glue at ordinary pressure |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115785447A (en) * | 2021-09-10 | 2023-03-14 | 山东大学 | Ultralow-viscosity liquid silicone rubber and cross-linking agent and preparation method thereof |
| CN115785447B (en) * | 2021-09-10 | 2024-02-20 | 山东大学 | Ultralow-viscosity liquid silicone rubber, crosslinking agent thereof and preparation method thereof |
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Application publication date: 20160824 |