CN106674524A - Preparation method of alkoxy-terminated polydimethylsiloxane - Google Patents
Preparation method of alkoxy-terminated polydimethylsiloxane Download PDFInfo
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- CN106674524A CN106674524A CN201611256502.6A CN201611256502A CN106674524A CN 106674524 A CN106674524 A CN 106674524A CN 201611256502 A CN201611256502 A CN 201611256502A CN 106674524 A CN106674524 A CN 106674524A
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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
- C08G77/38—Polysiloxanes modified by chemical after-treatment
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of 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; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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Abstract
The invention belongs to the field of a high-molecular material, and specifically provides a preparation method of alkoxy-terminated polydimethylsiloxane. The preparation method comprises: uniformly mixing hydroxyl-terminated polysiloxane, silsesquioxane having at least three alkoxy groups, and an end-capping reaction catalyst in the protection of vacuum or inert gas and performing an end-capping reaction at 0-100 DEG C for 0.5-24 h to obtain alkoxy-terminated polydimethylsiloxane. The preparation method is simple in steps and operation, mild in reaction conditions, easy to achieve and control, and suitable for massive popularization and production in the industry. The obtained alkoxy-terminated polydimethylsiloxane is not prone to condense in a storage process, is stable and reliable in quality, and long in preservation period, and can further improve the stability of hydroxyl silicone oil and high temperature resistance of silicone rubber.
Description
Technical field
The invention belongs to polymeric material field, and in particular to a kind of preparation side of alkoxy end-capped polydimethylsiloxane
Method.
Background technology
End group for hydroxyl linear polydimethylsiloxane-, be a kind of oily liquids, and the characteristics of with methyl-silicone oil.And
And, low viscous hydroxy silicon oil is the superior structural controlling agent in silicone rubber processing, can replace diphenyl silanediol, simplifies work
Skill, improves processing performance, is also used as fabric, leather, the waterproof of paper, soft and release treatment agent.
But, the terminal hydroxy group of the polydimethylsiloxane has reactivity, is difficult during storage and transport
Preserve, easily affect quality because condensation reaction terminal hydroxy group occurs.
Therefore, for stability is improved, shelf life of products is extended, it is ensured that from the point of view of product quality, do not changing poly-
On the premise of dimethyl siloxane this function, the active end in traditional polydimethylsiloxane is converted to into inertia end, is
One important Research Thinking.Thus, how could be quick, easy and stable prepare is a kind of using the replacement of inertia end
The polydimethylsiloxane at traditional hydroxyl activity end is technical problem urgently to be resolved hurrily.
The content of the invention
In order to solve the problems referred to above of prior art presence, the invention provides a kind of alkoxy end-capped polydimethylsiloxanes
The preparation method of alkane, what the preparation method can be quick, easy and stable prepares alkoxy end-capped polydimethylsiloxanes
Alkane, the alkoxy end-capped polydimethylsiloxane obtained by preparation is blocked by alkoxyl, and contracting is not susceptible to during storage
Close, the more stable reliability of product quality, preserve the shelf-life longer.
The technical solution adopted in the present invention is:
The preparation method of a kind of alkoxy end-capped polydimethylsiloxane of the present invention, comprises the steps:
S1, dispensing
Component A:Hydroxy-end capped polysiloxanes;
Component B:Silsesquioxane with least 3 alkoxyls;
Component C:End capping reaction catalyst;
S2, by component A, component B and component C under the conditions of vacuum or inert gas shielding mix homogeneously, obtain batch mixing;
S3, batch mixing is placed under 0~100 DEG C and inert gas shielding carry out end alkoxy groupization original position end capping reaction, obtain
To alkoxy end-capped polydimethylsiloxane.
Wherein:
The structural formula of the hydroxy-end capped polysiloxanes of component A is:
The structural formula of component B is R1 a-CH2CH2Si(OR2)4-a, wherein, R2It is the alkyl with 1~8 carbon atom,
A is 0 or 1.
R in component B1For cage structure, the space structure formula of component B is as follows:
In the space structure formula of component B:Cage structure is R1, one of R is-CH2CH2Si(OR2)4-a, remaining R
It is methyl.
The end capping reaction catalyst is mixture, hydroxylamine derivative, the alkali metal hydrogen of organic amine, carboxylic metallic salt and amine
The combination of one or more in oxide, organolithium, Bronsted acid, lewis acid and phosphate ester acid.
In order to further improve reaction efficiency and speed, preferred response parameter:Component A, component B and described
The mol ratio of component C is followed successively by 100:5-15:0.1-10.In S2, component A, component B and component C are added in high speed dispersor
It is uniformly mixed, the rotating speed of the stirring is 200-3000r/min, and mixing time is 1-30min.After stirring in S2
The viscosity number of the batch mixing for arriving is 18000-19000mPas.In S2, the vacuum of the vacuum is 0.08-0.099MPa.S2 and
In S3, the noble gases are argon or helium.
The viscosity number of the alkoxy end-capped polydimethylsiloxane obtained in the present invention is 19000-20000mPas, is glued
Degree change is little, it is easy to control, and operates and easy to use.
Based on above technical scheme, beneficial effects of the present invention are:
First, preparation method step succinct, easy to operate (only needing to be sufficiently mixed each raw material) of the invention, and
And reaction condition (0~100 DEG C can react) is gentle, be easily achieved and control, the response time is controlled in 0.5~24h, is fitted
In the production of industrial large-scale promotion.
Secondly, the preparation method of the present invention using the silsesquioxane with least 3 alkoxyls as hydroxy silicon oil (i.e.
Component A polysiloxanes in the present invention) end-capping reagent, hydroxy-end capped polysiloxanes not only can with silsesquioxane end-blocking in situ
The stability of hydroxy silicon oil is effectively improved, and the combination of hydroxy silicon oil and silsesquioxane can also improve the resistance to of silicone rubber
High-temperature behavior.
3rd, the alkoxy end-capped polydimethylsiloxane that preparation method of the invention is prepared, during storage not
Easily it is condensed, the more stable reliability of product quality, preserves the shelf-life longer.
4th, the alkoxy end-capped polydimethylsiloxane viscosity B coefficent that the preparation method of the present invention is prepared is little, can
It is widely used in the full-automatic big production of single-component de-alcoholized room temperature vulcanized organosilicon sealing material.
5th, in component B, R1It is the cage modle polysilsesquioxane with cage structure.The cage modle polysilsesquioxane
Cage modle frame structure cause it that there is good dielectricity and optical property, in terms of toughness reinforcing, cage modle polysilsesquioxane is received
Rice corpuscles can terminate the development at micro-crack tip, and either shear band or strand are rearranged to cause crazing, " cage "
Elasticity can play a part of similar " hoodle ", therefore can also further lift the alkoxy end-capped poly- of present invention preparation
The mechanical toughness of dimethyl siloxane.
Specific embodiment
The present invention is further explained with reference to specific embodiment.
In following examples, the hydroxy-end capped polysiloxanes buying for being adopted wins the limited public affairs of glad chemical science and technology from Guangzhou
Department, the tri-alkoxy silsesquioxane and tetraalkoxy silsesquioxane for being adopted is purchased from Shanghai Mai Ruier chemical technologies to be had
Limit company, end capping reaction catalyst is equally also all ordinary commercial products, and source is no longer repeated one by one.
In following examples:
Component A:Hydroxy-end capped polysiloxanes, structural formula:
Component B:Silsesquioxane with least 3 alkoxyls, structural formula is R1 a-CH2CH2Si(OR2)4-a, wherein, R2
It is the alkyl with 1~8 carbon atom, a is 0 or 1.Component B space structure formula is as follows:
In the space structure formula of component B:Cage structure is R1, one of R is-CH2CH2Si(OR2)4-a, remaining R
It is methyl.
Component C:End capping reaction catalyst.
Embodiment 1:
A kind of preparation method of alkoxy end-capped polydimethylsiloxane is present embodiments provided, step is:By component A,
Component B and component C (component C elects triethylamine as) are according to mol ratio 100:5:0.1 dispensing, is subsequently adding in high speed dispersor in argon
It is uniformly mixed under gas shielded and obtains batch mixing, the rotating speed of stirring is 200r/min, and mixing time is 30min, gained batch mixing
Viscosity number is 18000mPas.After the completion of stirring, under argon protection, batch mixing is placed into 24h under 0 DEG C of environment carries out end
Alkoxylate original position end capping reaction.By quick tiron chemical method inspection end-blocking effect, without viscosity peak phenomenon.
Embodiment 2:
A kind of preparation method of alkoxy end-capped polydimethylsiloxane is present embodiments provided, step is:By component A,
(component C is by triethylamine and zinc methacrylate according to mol ratio for component B (component B is tri-alkoxy silsesquioxane) and component C
1:1 ratio is mixed) according to mol ratio 100:15:10 dispensings, are subsequently adding in high speed dispersor and are stirred under argon protection
Mix mix homogeneously and obtain batch mixing, the rotating speed of stirring is 3000r/min, and mixing time is 1min, and the viscosity number of gained batch mixing is
19000mPa·s.After the completion of stirring, under argon protection, batch mixing is set to 0 into .5h in 100 DEG C of environment decentralizations carries out end alkoxy group
Change end capping reaction in situ.The viscosity number of finally obtained alkoxy end-capped polydimethylsiloxane is 20000mPas.
Embodiment 3:
A kind of preparation method of alkoxy end-capped polydimethylsiloxane is present embodiments provided, step is:By component A,
Component B (component B is tetraalkoxy silsesquioxane) and component C (component C is N- ethylhydroxyl amines) are according to mol ratio 100:10:5
Dispensing, is subsequently adding in high speed dispersor and is uniformly mixed and obtains batch mixing under helium protection, and the rotating speed of stirring is 1500r/
Min, mixing time is 15min, and the viscosity number of gained batch mixing is 18500mPas.After the completion of stirring, under helium protection, will
Batch mixing places 12h under 50 DEG C of environment and carries out end alkoxy groupization original position end capping reaction.It is finally obtained alkoxy end-capped poly-
The viscosity number of dimethyl siloxane is 19000mPas.
Embodiment 4:
A kind of preparation method of alkoxy end-capped polydimethylsiloxane is present embodiments provided, step is:By component A,
Component B (component B is tetraalkoxy silsesquioxane) and component C (component C is Lithium hydrate) are according to mol ratio 100:6:6 match somebody with somebody
Material, is subsequently adding in high speed dispersor and is uniformly mixed and obtains batch mixing under argon protection, and the rotating speed of stirring is 1000r/
Min, mixing time is 10min, and the viscosity number of gained batch mixing is 18000mPas.After the completion of stirring, under argon protection, will
Batch mixing places 5h under 60 DEG C of environment and carries out end alkoxy groupization original position end capping reaction.Finally obtained alkoxy end-capped poly- two
The viscosity number of methylsiloxane is 19000mPas.
Embodiment 5:
A kind of preparation method of alkoxy end-capped polydimethylsiloxane is present embodiments provided, step is:By component A,
Component B (component B is tetraalkoxy silsesquioxane) and component C (component C is n-BuLi) are according to mol ratio 100:9:4 match somebody with somebody
Material, is subsequently adding in high speed dispersor to be uniformly mixed under the vacuum condition of vacuum 0.08MPa and obtains batch mixing, stirring
Rotating speed is 2000r/min, and mixing time is 10min, and the viscosity number of gained batch mixing is 18000mPas.After the completion of stirring, keep
The vacuum condition of vacuum 0.08MPa, batch mixing is placed into 15h under 30 DEG C of environment carries out end alkoxy groupization end-blocking in situ instead
Should.The viscosity number of finally obtained alkoxy end-capped polydimethylsiloxane is 19000mPas.
Embodiment 6:
A kind of preparation method of alkoxy end-capped polydimethylsiloxane is present embodiments provided, step is:By component A,
(component C is CH for component B (component B is tetraalkoxy silsesquioxane) and component C3COOH) according to mol ratio 100:12:6 match somebody with somebody
Material, is subsequently adding in high speed dispersor to be uniformly mixed under the vacuum condition of vacuum 0.099MPa and obtains batch mixing, stirs
Rotating speed be 1500r/min, mixing time is 13min, and the viscosity number of gained batch mixing is 19000mPas.After the completion of stirring, protect
The vacuum condition of vacuum 0.099MPa is held, batch mixing is placed into 5h under 80 DEG C of environment carries out end alkoxy groupization end-blocking in situ instead
Should.The viscosity number of finally obtained alkoxy end-capped polydimethylsiloxane is 19500mPas.
Embodiment 7:
A kind of preparation method of alkoxy end-capped polydimethylsiloxane is present embodiments provided, step is:By component A,
Component B (component B is tetraalkoxy silsesquioxane) and component C (component C is iron chloride) are according to mol ratio 100:6:0.5 matches somebody with somebody
Material, is subsequently adding in high speed dispersor and is uniformly mixed and obtains batch mixing under argon protection, and the rotating speed of stirring is 800r/min,
Mixing time is 18min, and the viscosity number of gained batch mixing is 18000mPas.After the completion of stirring, under argon protection, by batch mixing
20h is placed under 20 DEG C of environment carries out end alkoxy groupization original position end capping reaction.Finally obtained alkoxy end-capped poly- diformazan
The viscosity number of radical siloxane is 19000mPas.
Embodiment 8:
A kind of preparation method of alkoxy end-capped polydimethylsiloxane is present embodiments provided, step is:By component A,
(component C is by triethylamine, zinc methacrylate and N- ethyl hydroxyls for component B (component B is tetraalkoxy silsesquioxane) and component C
Amine is according to mol ratio 1:1:0.5 ratio is mixed) according to mol ratio 100:15:7 dispensings, in being subsequently adding high speed dispersor
It is uniformly mixed under argon protection and obtains batch mixing, the rotating speed of stirring is 2200r/min, and mixing time is 6min, and gained is mixed
The viscosity number of material is 18000mPas.After the completion of stirring, under argon protection, batch mixing is placed into 6h under 40 DEG C of environment is carried out
End alkoxy groupization original position end capping reaction.The viscosity number of finally obtained alkoxy end-capped polydimethylsiloxane is
19000mPa·s。
In the following performance indications detection carried out to embodiments of the invention 1~8, relevant criterion requirement is satisfied by, is produced
Product are qualified.
Organopolysiloxane viscosity is tested by GB/T10247-2008.By quick tiron chemical method, inspection end-blocking effect
Really.By JY/T007-1996 superconducting pulse Fourier-transform nuclear magnetic resonance spectral method general rules, polysiloxanes end sense is characterized
Change situation.
The present invention is not limited to above-mentioned preferred forms, and anyone can show that other are various under the enlightenment of the present invention
The product of form, however, make any change in its details, it is every with technical scheme identical or similar to the present application,
It is within the scope of the present invention.
Claims (10)
1. a kind of preparation method of alkoxy end-capped polydimethylsiloxane, it is characterised in that comprise the steps:
S1, dispensing
Component A:Hydroxy-end capped polysiloxanes;
Component B:Silsesquioxane with least 3 alkoxyls;
Component C:End capping reaction catalyst;
S2, by component A, component B and component C under the conditions of vacuum or inert gas shielding mix homogeneously, obtain batch mixing;
S3, batch mixing is placed under 0~100 DEG C and inert gas shielding carry out end alkoxy groupization original position end capping reaction, obtain alkane
Epoxide blocks polydimethylsiloxane.
2. preparation method according to claim 1, it is characterised in that:The structural formula of component B is R1 a-CH2CH2Si
(OR2)4-a, wherein, R2It is the alkyl with 1~8 carbon atom, a is 0 or 1.
3. preparation method according to claim 2, it is characterised in that:R in component B1For cage structure, component B
Space structure formula is as follows:
In the space structure formula of component B:Cage structure is R1, one of R is-CH2CH2Si(OR2)4-a, remaining R is
Methyl.
4. preparation method according to claim 1, it is characterised in that:The end capping reaction catalyst is organic amine, carboxylic acid
The mixture of slaine and amine, hydroxylamine derivative, alkali metal hydroxide, organolithium, Bronsted acid, lewis acid and acid
The combination of one or more in formula phosphate ester.
5. preparation method according to claim 1, it is characterised in that:Component A, component B and component C
Mol ratio is followed successively by 100:5-15:0.1-10.
6. preparation method according to claim 1, it is characterised in that:In S2, component A, component B and component C are added high
It is uniformly mixed in fast dispersion machine, the rotating speed of the stirring is 200-3000r/min, and mixing time is 1-30min.
7. preparation method according to claim 6, it is characterised in that:The viscosity number of the batch mixing obtained after stirring in S2
For 18000-19000mPas.
8. preparation method according to claim 1, it is characterised in that:In S3, the described alkoxy end-capped poly- diformazan for obtaining
The viscosity number of radical siloxane is 19000-20000mPas.
9. preparation method according to claim 1, it is characterised in that:In S2, the vacuum of the vacuum is 0.08-
0.099MPa。
10. preparation method according to claim 1, it is characterised in that:In S2 and S3, the noble gases are argon or helium
Gas.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108219143A (en) * | 2017-12-19 | 2018-06-29 | 杭州之江有机硅化工有限公司 | A kind of preparation method of alkoxy end-capped dimethyl silicone polymer |
CN111333846A (en) * | 2020-04-13 | 2020-06-26 | 新纳奇材料科技江苏有限公司 | Preparation method of single-end alkoxy and single-end methyl polydimethylsiloxane |
CN114230798A (en) * | 2021-11-18 | 2022-03-25 | 杭州四马化工科技有限公司 | Siloxane preparation method and special Venturi ejector |
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CN103897195A (en) * | 2014-03-18 | 2014-07-02 | 江苏科幸新材料股份有限公司 | Method for preparing alkoxy terminated polydimethylsiloxane |
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CN101333227A (en) * | 2007-05-23 | 2008-12-31 | 株式会社普利司通 | Method for making alkoxy-modified silsesquioxanes |
CN103467745A (en) * | 2013-09-03 | 2013-12-25 | 成都硅宝科技股份有限公司 | Preparation method of terminal alkoxy polysiloxane |
CN103897195A (en) * | 2014-03-18 | 2014-07-02 | 江苏科幸新材料股份有限公司 | Method for preparing alkoxy terminated polydimethylsiloxane |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108219143A (en) * | 2017-12-19 | 2018-06-29 | 杭州之江有机硅化工有限公司 | A kind of preparation method of alkoxy end-capped dimethyl silicone polymer |
CN108219143B (en) * | 2017-12-19 | 2019-04-19 | 杭州之江有机硅化工有限公司 | A kind of preparation method of alkoxy end-capped dimethyl silicone polymer |
CN111333846A (en) * | 2020-04-13 | 2020-06-26 | 新纳奇材料科技江苏有限公司 | Preparation method of single-end alkoxy and single-end methyl polydimethylsiloxane |
CN114230798A (en) * | 2021-11-18 | 2022-03-25 | 杭州四马化工科技有限公司 | Siloxane preparation method and special Venturi ejector |
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