CN110144044A - A kind of no-solvent type methyl silicon resin and its manufacture craft - Google Patents
A kind of no-solvent type methyl silicon resin and its manufacture craft Download PDFInfo
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- CN110144044A CN110144044A CN201910427009.3A CN201910427009A CN110144044A CN 110144044 A CN110144044 A CN 110144044A CN 201910427009 A CN201910427009 A CN 201910427009A CN 110144044 A CN110144044 A CN 110144044A
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- solvent type
- silicon resin
- type methyl
- methyl silicon
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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
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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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- Silicon Polymers (AREA)
Abstract
The invention belongs to no-solvent type methyl silicon resin manufacture technology fields, in particular a kind of no-solvent type methyl silicon resin, in terms of mass percentage, including water 5%-30%, methyltrimethoxysilane 30%-100%, methyltriethoxysilane 30%-100%, dimethyldimethoxysil,ne 0%-60%, dimethyl diethoxysilane 0%-60%, methyl silicate 0%-60%, silester 0%-60% and catalyst 0%-1%；The present invention is by the no-solvent type methyl silicon resin of above-mentioned mass percentage family planning output, and production technology is generated without waste water, and product is solvent-free, and hardness is high, can use catalyst room temperature curing, offer convenience to enterprise's production and sales.
Description
Technical field
The invention belongs to no-solvent type methyl silicon resin manufacture technology fields, and in particular to a kind of no-solvent type methyl silicon tree
Rouge and its manufacture craft.
Background technique
Solvent-free silicone resin is a kind of without solvent type silicone resin, nontoxic to the human body without heavy metal and aromatic hydrocarbon solvent
Evil effect, the environment-friendly type macromolecule material that no coupling product generates when solidification；
But existing solvent-free silicone resin, in production, fabrication cycle is troublesome, and solvent-free silicone resin obtained is hard
It spends low, it is not possible to use catalyst room temperature curing, make troubles to enterprise's production and sales.
Summary of the invention
To solve the problems mentioned above in the background art.The present invention provides a kind of no-solvent type methyl silicon resin and its
Manufacture craft has the characteristics that hardness is high, catalyst room temperature can be used cured.
To achieve the above object, the invention provides the following technical scheme: a kind of no-solvent type methyl silicon resin, with quality hundred
Divide content meter, including water 5%-30%, methyltrimethoxysilane 30%-100%, methyltriethoxysilane 30%-
100%, dimethyldimethoxysil,ne 0%-60%, dimethyl diethoxysilane 0%-60%, methyl silicate 0%-60%,
Silester 0%-60% and catalyst 0%-1%.
As a kind of no-solvent type methyl silicon resin optimal technical scheme of the invention, the methyltrimethoxysilane is
A kind of organic compound, the crosslinking agent and fiberglass surface treating agent for being mainly used as room temperature vulcanized silicone rubber are moulded with enhancing
The outer reason agent of bed of material laminate.
As a kind of no-solvent type methyl silicon resin optimal technical scheme of the invention, the methyltriethoxysilane is used
In rubber, pharmaceutical sector, it is used as organosilicon macromolecule raw material.
As a kind of no-solvent type methyl silicon resin optimal technical scheme of the invention, the dimethyldimethoxysil,ne
It is used primarily in organic siliconresin and makees modifying agent, organic silicon compounded rubber stock constitution controller and chain extender.
As a kind of no-solvent type methyl silicon resin optimal technical scheme of the invention, the dimethyl diethoxy silicon
Alkane, colourless transparent liquid, be mainly used for silicon rubber preparation in constitution controller, organosilicon product synthesis in chain extender and silicon
Oily synthesis material.
As a kind of no-solvent type methyl silicon resin optimal technical scheme of the invention, the quanmethyl silicate is colourless
Prescribed liquid, has unstable in the presence of moisture, can gradually decomposite silica in air.
As a kind of no-solvent type methyl silicon resin optimal technical scheme of the invention, silester silicon at normal temperature
Sour tetra-ethyl ester is colourless or light yellow clear liquid, hydrolysis can occur with water, generate silica sol.
As a kind of no-solvent type methyl silicon resin optimal technical scheme of the invention, the catalyst is hydrochloric acid.
As a kind of no-solvent type methyl silicon resin optimal technical scheme of the invention, in terms of mass percentage, including
Water 20%, methyltrimethoxysilane 60%, methyltriethoxysilane 60%, dimethyldimethoxysil,ne 30%, diformazan
Base diethoxy silane 30%, methyl silicate 30%, silester 30% and catalyst 0.5%.
A kind of production method of no-solvent type methyl silicon resin, includes the following steps:
S1, methyltrimethoxysilane 60%, methyltriethoxysilane 60%, dimethyldimethoxysil,ne
30%, dimethyl diethoxysilane 30%, methyl silicate 30%, silester 30% and catalyst 0.5% are placed into reaction
40min-60min is stirred with the speed of 300r/min-400r/min in kettle, and passes through 0 DEG C of -70 DEG C of heat preservation；
S2, heat preservation -8 hours 0 hour after, water 20% is added dropwise to reaction kettle；
S3, then 0 DEG C -70 DEG C keep the temperature -8 hours 0 hour；
S4, reaction kettle is opened, heating distills out methanol, ethyl alcohol；
S5, curing in -8 hours 0 hour is finally kept the temperature at 8 DEG C -180 DEG C, obtain no-solvent type methyl silicon resin.
Compared with prior art, the beneficial effects of the present invention are: the present invention passes through above-mentioned mass percentage family planning output
No-solvent type methyl silicon resin, production technology generates without waste water, and product is solvent-free, and hardness is high, can use catalyst case
Temperature solidification, offers convenience to enterprise's production and sales.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment 1
A kind of no-solvent type methyl silicon resin, in terms of mass percentage, including water 5%, methyltrimethoxysilane
30%, methyltriethoxysilane 30%, dimethyldimethoxysil,ne 20%, dimethyl diethoxysilane 20%, silicic acid
Methyl esters 20%, silester 20% and catalyst 0.2%.
A kind of production method of no-solvent type methyl silicon resin, includes the following steps:
S1, methyltrimethoxysilane 30%, methyltriethoxysilane 30%, dimethyldimethoxysil,ne
20%, dimethyl diethoxysilane 20%, methyl silicate 20%, silester 20% and catalyst 0.2% are placed into reaction
40min is stirred with the speed of 300r/min in kettle, and passes through 20 DEG C of heat preservations；
S2, heat preservation 2 hours after, water 5% is added dropwise to reaction kettle；
S3, then 20 DEG C keep the temperature 2 hours；
S4, reaction kettle is opened, heating distills out methanol, ethyl alcohol；
S5, curing in 2 hours is finally kept the temperature at 8 DEG C, obtain no-solvent type methyl silicon resin.
As a kind of optional embodiment of the present invention, the methyltrimethoxysilane is a kind of organic compound, mainly
The outer reason agent of crosslinking agent and fiberglass surface treating agent and reinforced plastics laminate as room temperature vulcanized silicone rubber.
As a kind of optional embodiment of the present invention, the methyltriethoxysilane is used for rubber, pharmaceutical sector, as having
Machine polymeric silicon raw material.
As a kind of optional embodiment of the present invention, the dimethyldimethoxysil,ne is used primarily in organic siliconresin work
Modifying agent, organic silicon compounded rubber stock constitution controller and chain extender.
As a kind of optional embodiment of the present invention, the dimethyl diethoxysilane, colourless transparent liquid is main to use
In silicon rubber preparation in constitution controller, organosilicon product synthesis in chain extender and silicone oil synthesis material.
As a kind of optional embodiment of the present invention, the quanmethyl silicate is colourless transparent liquid, in the presence of having moisture
It is unstable, silica can be gradually decomposited in air.
As a kind of optional embodiment of the present invention, tetraethyl orthosilicate is colourless or pale yellow to the silester at normal temperature
Color transparency liquid can occur hydrolysis with water, generate silica sol.
As a kind of optional embodiment of the present invention, the catalyst is hydrochloric acid.
Embodiment 2
A kind of no-solvent type methyl silicon resin, in terms of mass percentage, including water 20%, methyltrimethoxysilane
60%, methyltriethoxysilane 60%, dimethyldimethoxysil,ne 30%, dimethyl diethoxysilane 30%, silicic acid
Methyl esters 30%, silester 30% and catalyst 0.5%.
A kind of production method of no-solvent type methyl silicon resin, includes the following steps:
S1, methyltrimethoxysilane 60%, methyltriethoxysilane 60%, dimethyldimethoxysil,ne
30%, dimethyl diethoxysilane 30%, methyl silicate 30%, silester 30% and catalyst 0.5% are placed into reaction
50min is stirred with the speed of 350r/min in kettle, and passes through 35 DEG C of heat preservations；
S2, heat preservation 4 hours after, water 20% is added dropwise to reaction kettle；
S3, then 35 DEG C keep the temperature 4 hours；
S4, reaction kettle is opened, heating distills out methanol, ethyl alcohol；
S5, curing in 4 hours is finally kept the temperature at 90 DEG C, obtain no-solvent type methyl silicon resin.
As a kind of optional embodiment of the present invention, the methyltrimethoxysilane is a kind of organic compound, mainly
The outer reason agent of crosslinking agent and fiberglass surface treating agent and reinforced plastics laminate as room temperature vulcanized silicone rubber.
As a kind of optional embodiment of the present invention, the methyltriethoxysilane is used for rubber, pharmaceutical sector, as having
Machine polymeric silicon raw material.
As a kind of optional embodiment of the present invention, the dimethyldimethoxysil,ne is used primarily in organic siliconresin work
Modifying agent, organic silicon compounded rubber stock constitution controller and chain extender.
As a kind of optional embodiment of the present invention, the dimethyl diethoxysilane, colourless transparent liquid is main to use
In silicon rubber preparation in constitution controller, organosilicon product synthesis in chain extender and silicone oil synthesis material.
As a kind of optional embodiment of the present invention, the quanmethyl silicate is colourless transparent liquid, in the presence of having moisture
It is unstable, silica can be gradually decomposited in air.
As a kind of optional embodiment of the present invention, tetraethyl orthosilicate is colourless or pale yellow to the silester at normal temperature
Color transparency liquid can occur hydrolysis with water, generate silica sol.
As a kind of optional embodiment of the present invention, the catalyst is hydrochloric acid.
Embodiment 3
A kind of no-solvent type methyl silicon resin, in terms of mass percentage, including water 30%, methyltrimethoxysilane
100%, methyltriethoxysilane 100%, dimethyldimethoxysil,ne 60%, dimethyl diethoxysilane 60%, silicon
Sour methyl esters 60%, silester 60% and catalyst 1%.
A kind of production method of no-solvent type methyl silicon resin, includes the following steps:
S1, methyltrimethoxysilane 100%, methyltriethoxysilane 100%, dimethyldimethoxysil,ne
60%, dimethyl diethoxysilane 60%, methyl silicate 60%, silester 60% and catalyst 1% are placed into reaction kettle
In 60min stirred with the speed of 400r/min, and pass through 70 DEG C of heat preservations；
S2, heat preservation 8 hours after, water 30% is added dropwise to reaction kettle；
S3, then 70 DEG C keep the temperature 8 hours；
S4, reaction kettle is opened, heating distills out methanol, ethyl alcohol；
S5, curing in 8 hours is finally kept the temperature at 180 DEG C, obtain no-solvent type methyl silicon resin.
As a kind of optional embodiment of the present invention, the methyltrimethoxysilane is a kind of organic compound, mainly
The outer reason agent of crosslinking agent and fiberglass surface treating agent and reinforced plastics laminate as room temperature vulcanized silicone rubber.
As a kind of optional embodiment of the present invention, the methyltriethoxysilane is used for rubber, pharmaceutical sector, as having
Machine polymeric silicon raw material.
As a kind of optional embodiment of the present invention, the dimethyldimethoxysil,ne is used primarily in organic siliconresin work
Modifying agent, organic silicon compounded rubber stock constitution controller and chain extender.
As a kind of optional embodiment of the present invention, the dimethyl diethoxysilane, colourless transparent liquid is main to use
In silicon rubber preparation in constitution controller, organosilicon product synthesis in chain extender and silicone oil synthesis material.
As a kind of optional embodiment of the present invention, the quanmethyl silicate is colourless transparent liquid, in the presence of having moisture
It is unstable, silica can be gradually decomposited in air.
As a kind of optional embodiment of the present invention, tetraethyl orthosilicate is colourless or pale yellow to the silester at normal temperature
Color transparency liquid can occur hydrolysis with water, generate silica sol.
As a kind of optional embodiment of the present invention, the catalyst is hydrochloric acid.
In summary: no-solvent type methyl silicon resin of the present invention by above-mentioned mass percentage family planning output, production
Technique is generated without waste water, and product is solvent-free, and hardness is high, can be used catalyst room temperature curing, be brought to enterprise's production and sales
It is convenient.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (10)
1. a kind of no-solvent type methyl silicon resin, which is characterized in that in terms of mass percentage, including water 5%-30%, methyl
Trimethoxy silane 30%-100%, methyltriethoxysilane 30%-100%, dimethyldimethoxysil,ne 0%-60%,
Dimethyl diethoxysilane 0%-60%, methyl silicate 0%-60%, silester 0%-60% and catalyst 0%-1%.
2. a kind of no-solvent type methyl silicon resin according to claim 1, it is characterised in that: the methyl trimethoxy oxygroup silicon
Alkane is a kind of organic compound, is mainly used as crosslinking agent and fiberglass surface treating agent and the increasing of room temperature vulcanized silicone rubber
The outer reason agent of strong plastic laminate.
3. a kind of no-solvent type methyl silicon resin according to claim 1, it is characterised in that: the methyltriethoxy silane
Alkane is used for rubber, pharmaceutical sector, is used as organosilicon macromolecule raw material.
4. a kind of no-solvent type methyl silicon resin according to claim 1, it is characterised in that: the dimethylformamide dimethyl oxygroup
Silane is used primarily in organic siliconresin and makees modifying agent, organic silicon compounded rubber stock constitution controller and chain extender.
5. a kind of no-solvent type methyl silicon resin according to claim 1, it is characterised in that: the dimethyl diethoxy
Silane, colourless transparent liquid, be mainly used for silicon rubber preparation in constitution controller, organosilicon product synthesis in chain extender and
Silicone oil synthesis material.
6. a kind of no-solvent type methyl silicon resin according to claim 1, it is characterised in that: the quanmethyl silicate is nothing
Color transparency liquid, has unstable in the presence of moisture, can gradually decomposite silica in air.
7. a kind of no-solvent type methyl silicon resin according to claim 1, it is characterised in that: the silester is in room temperature
Lower tetraethyl orthosilicate is colourless or light yellow clear liquid, hydrolysis can occur with water, generate silica sol.
8. a kind of no-solvent type methyl silicon resin according to claim 1, it is characterised in that: the catalyst is hydrochloric acid.
9. a kind of no-solvent type methyl silicon resin according to claim 1, which is characterized in that in terms of mass percentage,
Including water 20%, methyltrimethoxysilane 60%, methyltriethoxysilane 60%, dimethyldimethoxysil,ne 30%,
Dimethyl diethoxysilane 30%, methyl silicate 30%, silester 30% and catalyst 0.5%.
10. a kind of production method of no-solvent type methyl silicon resin described in -9 any one according to claim 1, feature exist
In including the following steps:
S1, methyltrimethoxysilane 60%, methyltriethoxysilane 60%, dimethyldimethoxysil,ne 30%, two
Methyldiethoxysilane 30%, methyl silicate 30%, silester 30% and catalyst 0.5% be placed into reaction kettle with
The speed of 300r/min-400r/min stirs 40min-60min, and passes through 0 DEG C of -70 DEG C of heat preservation；
S2, heat preservation -8 hours 0 hour after, water 20% is added dropwise to reaction kettle；
S3, then 0 DEG C -70 DEG C keep the temperature -8 hours 0 hour；
S4, reaction kettle is opened, heating distills out methanol, ethyl alcohol；
S5, curing in -8 hours 0 hour is finally kept the temperature at 8 DEG C -180 DEG C, obtain no-solvent type methyl silicon resin.
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| CN201910427009.3A CN110144044A (en) | 2019-05-22 | 2019-05-22 | A kind of no-solvent type methyl silicon resin and its manufacture craft |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111040166A (en) * | 2019-11-28 | 2020-04-21 | 湖北新四海化工股份有限公司 | Environment-friendly moisture-curing silicone resin and preparation method thereof |
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| CN101787133A (en) * | 2010-01-08 | 2010-07-28 | 北京化工大学 | Non-solvent liquid silicone resin and preparation method thereof |
| CN103265702A (en) * | 2013-05-28 | 2013-08-28 | 哈尔滨工业大学 | Preparation method of ultraviolet-resistant and high-temperature-resistant methyl silicone resin |
| CN105585713A (en) * | 2016-03-23 | 2016-05-18 | 衢州市璀璨化工有限公司 | Method for preparing alcohol-solubility methyl silicone resin |
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2019
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|---|---|---|---|---|
| JPH04180926A (en) * | 1990-11-15 | 1992-06-29 | Shin Etsu Chem Co Ltd | Production of polyorganosiloxane resin |
| JPH0598012A (en) * | 1991-10-11 | 1993-04-20 | Shin Etsu Chem Co Ltd | Production of organopolysiloxane resin |
| CN101787133A (en) * | 2010-01-08 | 2010-07-28 | 北京化工大学 | Non-solvent liquid silicone resin and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111040166A (en) * | 2019-11-28 | 2020-04-21 | 湖北新四海化工股份有限公司 | Environment-friendly moisture-curing silicone resin and preparation method thereof |
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