CN107987790A - A kind of silicone polyether base rubber of low viscosity and preparation method thereof - Google Patents
A kind of silicone polyether base rubber of low viscosity and preparation method thereof Download PDFInfo
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- CN107987790A CN107987790A CN201711307009.7A CN201711307009A CN107987790A CN 107987790 A CN107987790 A CN 107987790A CN 201711307009 A CN201711307009 A CN 201711307009A CN 107987790 A CN107987790 A CN 107987790A
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- base rubber
- silicone polyether
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- molar part
- low viscosity
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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
- C09J183/10—Block or graft copolymers containing polysiloxane sequences
- C09J183/12—Block or graft copolymers containing polysiloxane sequences containing polyether sequences
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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
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/46—Block-or graft-polymers containing polysiloxane sequences containing polyether sequences
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- Polymers & Plastics (AREA)
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Abstract
Silicone polyether base rubber the invention discloses a kind of low viscosity and preparation method thereof, after being polymerize by the polysiloxanes of end si-h bond and the polyethers progress hydrosilylation of end alkenyl, and obtains after carrying out hydrosilylation end-blocking with alkenyl alkoxy silane;During preparation, the polyethers of 1 molar part end alkenyl is sequentially added in the reactor, the polysiloxanes of the end si-h bond of 1.01 ~ 2 molar parts, 0.005 ~ 0.1 molar part catalyst, 0 ~ 100 molar part solvent, after when reaction 1 ~ 24 is small at 0 DEG C ~ 100 DEG C, add 2.02 ~ 4 molar part alkenyl alkoxy silanes continue hydrosilylation addition reaction 1 ~ 24 it is small when after, it is purified, be dried to obtain silicone polyether base rubber.The base rubber of the preparation of the present invention viscosity is low, water-tolerant, and technique used is close with the technique of original MS base rubbers, there is good industrialization prospect.
Description
Technical field
The invention belongs to organic gel field, more particularly to a kind of silicone polyether base rubber of low viscosity and its preparation side
Method, specifically obtains a kind of polysiloxanes of alkoxysilyl group end-blocking and the segmented copolymer of polyethers.
Background technology
Fluid sealant is widely used in metal, glass, and timber, silicone resin, add sulphur silicon rubber, ceramics, natural and synthetic fibers,
And the bonding of many paint frostings.Polyurethane sealant cures containing free isocyanates and is also easy to produce bubble.Silicone
Fluid sealant tearing strength is low, covering with paint property is poor, easily pollutes building materials.Silane modified polyether seal glue (MS glue) is a kind of to hold silane
Base polyethers is high-performance environment-friendly fluid sealant prepared by basic polymer.MS glue has the advantages of polyurethane and silicone sealant concurrently, gram
Shortcoming has been taken, there is excellent mechanical strength, covering with paint property, resistance to soiling, and isocyanate-free and organic solvent in product, be domestic
The main direction of development of outer novel elastic fluid sealant.
The base rubber technology of preparing of MS glue is based on KANEKA and the technology of two companies of WACKER exploitation.Wherein, with
The base rubber of KANEKA has relatively low viscosity and preferable mechanical property.KANEKA is using allyl polyether through chain extension, pi-allyl
After halogen end-blocking, then with hydrogen siloxane hydrosilylation addition reaction is carried out to block.
This case will carry out the chain extension of hydrosilylation addition reaction using the polysiloxanes opposite end alkenyl polyether of end si-h bond, into
One step reduces the viscosity of base rubber, improves the water resistance of base rubber.
The content of the invention
Silicone polyether base rubber the object of the present invention is to provide a kind of low viscosity and preparation method thereof.
To achieve the above object, there is provided following technical scheme:
A kind of silicone polyether base rubber of low viscosity, it is characterised in that:Silicone polyether base rubber is by end si-h bond
Polysiloxanes with holding the polyethers of alkenyl to carry out after hydrosilylation polymerize, olefinic recycle base alkoxy silane carries out Si―H addition reaction
Obtained after reaction end-blocking.
The preparation method of the corresponding silicone polyether base rubber for preparing said structure, comprises the following steps:
The polyethers of 1 molar part end alkenyl, the poly- silica of the end si-h bond of 1.01~2 molar parts are sequentially added in the reactor
Alkane, 0.005~0.1 molar part catalyst, 0~100 molar part solvent, at 0 DEG C~100 DEG C react 1~24 it is small when after, then add
Enter 2.02~4 molar part alkenyl alkoxy silanes continue hydrosilylation addition reaction 1~24 it is small when after, it is purified, dry
To silicone polyether base rubber.
The polyethers of so-called end alkenyl, refers to that the polyethers both ends are respectively provided with alkenyl;The polysiloxanes of si-h bond is held, refers to that this is poly-
The both ends of siloxanes are respectively provided with si-h bond.
Preferably, the polyethers is selected from polyethylene glycol, polypropylene glycol, polypropylene oxide, polyethylene oxide, poly- tetrahydrochysene furan
Mutter, the one or more in polybutylene oxide, copolymerization ethylene oxide propylene oxide, copolymerization ethylene oxide tetrahydrofuran, but not office
It is limited to this.
Preferably, the polysiloxanes of described end si-h bond be selected from tetramethyl disiloxane, hexamethyl dihydro trisiloxanes,
Hold the dimethyl silicone polymer of silicon hydrogen, the polymethylphenylsiloxane of end silicon hydrogen, dimethyl silicone polymer-poly- methyl of end silicon hydrogen
One or more in phenyl siloxane, but not limited to this.
Preferably, the catalyst is platinum, ruthenium, palladium class catalyst, selected from chloroplatinic acid, palladium/carbon, platinum/carbon, ruthenium/carbon, four
Divinyl disiloxane complexing platinum (Karstedt catalyst), triphenylphosphine platinum chloride, palladium/Al2O3In one kind or several
Kind, but not limited to this.
Preferably, the solvent be selected from methanol, ethanol, isopropanol, toluene, benzene, chloroform, dichloromethane, tetrahydrofuran,
In dioxane, hexane, ether, ethyl acetate, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide or 1-methyl-2-pyrrolidinone
One or several kinds of mixtures, but not limited to this.
The alkenyl alkoxy silane includes vinyltrimethoxysilane, vinyl methyl dimethoxysilane, alkene
Propyl trimethoxy silicane, vinyltriethoxysilane, but not limited to this.
The beneficial effects of the invention are as follows base rubber viscosity is low, water resistance improves, technique is simple, rapid reaction, high income, steady
The features such as qualitative good, there is good industrialization prospect.
Embodiment
The principle of the present invention is the characteristics of having used for reference the low viscosity of 107 silicone sealant of polysiloxanes, to draw in MS base rubbers
Enter polysiloxanes segment, so that the viscosity of base rubber reduces, water resistance improves, and technique used is close with the technique of original MS base rubbers
And be conducive to integrated process.
The present invention is further illustrated below according to embodiment, and the objects and effects of the present invention will be more apparent.
Embodiment 1:
The polyethylene oxide of 1 molar part end alkenyl is sequentially added in the reactor, and the end si-h bond of 1.01 molar parts gathers
Dimethyl siloxane, 0.005 molar part chloroplatinic acid catalyst, 0 molar part solvent, at 100 DEG C react 24 it is small when after, add
2.02 molar part vinyltrimethoxysilanes continue hydrosilylation addition reaction 24 it is small when after, it is purified, be dried to obtain it is poly-
Polyether silicon base rubber.
Embodiment 2:
The polyethylene oxide of 1 molar part end alkenyl, the poly- diformazan of the end si-h bond of 2 molar parts are sequentially added in the reactor
Radical siloxane, 0.1 molar part chloroplatinic acid catalyst, 100 molar part toluene, at 0 DEG C react 1 it is small when after, add 4 molar parts
Vinyltrimethoxysilane continue hydrosilylation addition reaction 1 it is small when after, it is purified, be dried to obtain silicone polyether base
Glue.
Embodiment 3:
The end si-h bond of 2000,1.05 molar part of polypropylene oxide of 1 molar part end alkenyl is sequentially added in the reactor
Dimethyl silicone polymer, 0.02 molar part Karstedt catalyst, 0.1 molar part toluene, at 40 DEG C react 12 it is small when
Afterwards, add 2.2 molar part vinyl methyl dimethoxysilanes continue hydrosilylation addition reaction 12 it is small when after, through pure
Change, be dried to obtain silicone polyether base rubber.
Spectral analysis of the nuclear magnetic resonance is carried out to product, obtains following result:3.60-3.43(CH2, OCH3),3.43-3.25
(CH),1.13(CH3),0.1(CH3Si)。
Base rubber product physical property:It is yellowish transparent, base rubber viscosity 20000mPa.s when APHA color is 80 or so, 25 DEG C
Left and right.
Embodiment 4:
Two silicon of tetramethyl of 2000,1.1 molar part of polypropylene oxide of 1 molar part end alkenyl is sequentially added in the reactor
Oxygen alkane, 0.01 molar part Karstedt catalyst, 0.5 molar part dimethylbenzene, at 30 DEG C react 10 it is small when after, add 2.2
Molar part vinyl methyl dimethoxysilane continue hydrosilylation addition reaction 10 it is small when after, it is purified, be dried to obtain it is poly-
Polyether silicon base rubber.
Embodiment 5:
Sequentially add the polyethylene oxide of 1 molar part end alkenyl in the reactor, poly- the two of the end si-h bond of 1.2 molar parts
Methylsiloxane, 0.02 molar part palladium/carbon catalyst, 1 molar part ethyl acetate, at 30 DEG C react 24 it is small when after, add
2.3 molar part allyltrimethoxysilanis continue hydrosilylation addition reaction 24 it is small when after, it is purified, be dried to obtain poly- silicon
Oxygen alkane polyethers base rubber.
Embodiment 6:
The PolyTHF of 1 molar part end alkenyl, the pregnancy of the end si-h bond of 1.2 molar parts are sequentially added in the reactor
Base dihydro trisiloxanes, 0.01 molar part ruthenium/carbon catalyst, 2 molar part toluene, at 40 DEG C react 12 it is small when after, add
2.4 molar part vinyltriethoxysilane continue hydrosilylation addition reaction 12 it is small when after, it is purified, be dried to obtain poly- silicon
Oxygen alkane polyethers base rubber.
Embodiment 7:
The polyethylene oxide of 1 molar part end alkenyl, the poly- first of the end si-h bond of 1.1 molar parts are sequentially added in the reactor
Base phenyl siloxane, 0.15 molar part chloroplatinic acid catalyst, 0.02 molar part toluene, at 100 DEG C react 2 it is small when after, then add
Enter 2.2 molar part vinyl methyl dimethoxysilanes continue hydrosilylation addition reaction 2 it is small when after, it is purified, dry
To silicone polyether base rubber.
Claims (7)
- A kind of 1. silicone polyether base rubber of low viscosity, it is characterised in that:Silicone polyether base rubber is by end si-h bond After polysiloxanes polymerize with the polyethers progress hydrosilylation of end alkenyl, it is anti-that olefinic recycle base alkoxy silane carries out Si―H addition reaction Obtained after should blocking.
- A kind of 2. preparation method of the silicone polyether base rubber of the low viscosity described in claim 1, it is characterised in that:Including with Lower step:Sequentially add the polyethers of 1 molar part end alkenyl in the reactor, the polysiloxanes of the end si-h bond of 1.01~2 molar parts, 0.005~0.1 molar part catalyst, 0~100 molar part solvent, at 0 DEG C~100 DEG C react 1~24 it is small when after, add 2.02~4 molar part alkenyl alkoxy silanes continue hydrosilylation addition reaction 1~24 it is small when after, it is purified, be dried to obtain Silicone polyether base rubber.
- A kind of 3. preparation method of the silicone polyether base rubber of low viscosity as claimed in claim 2, it is characterised in that:It is described Polyethers be selected from polyethylene glycol, polypropylene glycol, polypropylene oxide, polyethylene oxide, PolyTHF, polybutylene oxide, copolymerization One or more in ethylene oxide propylene oxide, copolymerization ethylene oxide tetrahydrofuran.
- A kind of 4. preparation method of the silicone polyether base rubber of low viscosity as claimed in claim 2, it is characterised in that:It is described End si-h bond polysiloxanes be selected from tetramethyl disiloxane, hexamethyl dihydro trisiloxanes, hold silicon hydrogen poly dimethyl silicon One kind in oxygen alkane, the polymethylphenylsiloxane for holding silicon hydrogen, dimethyl silicone polymer-polymethylphenylsiloxane of end silicon hydrogen It is or several.
- A kind of 5. preparation method of the silicone polyether base rubber of low viscosity as claimed in claim 2, it is characterised in that:It is described Catalyst be selected from chloroplatinic acid, palladium/carbon, platinum/carbon, ruthenium/carbon, tetramethyl divinyl disiloxane complexing platinum, triphenylphosphine chlorine Change platinum, palladium/Al2O3In one or more.
- A kind of 6. preparation method of the silicone polyether base rubber of low viscosity as claimed in claim 2, it is characterised in that:It is described Solvent be selected from methanol, ethanol, isopropanol, toluene, benzene, chloroform, dichloromethane, tetrahydrofuran, dioxanes, hexane, ether, second It is one or several kinds of mixed in acetoacetic ester, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide or 1-methyl-2-pyrrolidinone Compound.
- A kind of 7. preparation method of the silicone polyether base rubber of low viscosity as claimed in claim 2, it is characterised in that:It is described Alkenyl alkoxy silane be selected from vinyltrimethoxysilane, vinyl methyl dimethoxysilane, pi-allyl trimethoxy One or more in silane, vinyltriethoxysilane.
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109096491A (en) * | 2018-07-06 | 2018-12-28 | 福建拓烯新材料科技有限公司 | A kind of preparation method of Hydrophilicrto polyether silicone oil and the hydrophilic treatment method of glass |
CN109705333A (en) * | 2019-01-09 | 2019-05-03 | 浙江新安化工集团股份有限公司 | A kind of synthetic method of high molecular weight diallyl polyether |
CN111269691A (en) * | 2020-04-13 | 2020-06-12 | 江西省科学院应用化学研究所 | Single-component composite modified polyether sealant and preparation method thereof |
CN111286021A (en) * | 2020-03-31 | 2020-06-16 | 安徽海螺新材料科技有限公司 | Polyether terminated by silyl ether, preparation method thereof and efficient anti-mud water reducer |
EP3666836A1 (en) * | 2018-12-10 | 2020-06-17 | Samsung Electronics Co., Ltd. | Compositions, films comprising cured products of the same, stacked structures comprising the films, and display devices |
CN111440323A (en) * | 2020-05-18 | 2020-07-24 | 烟台德邦科技有限公司 | Synthesis method of alkoxy-terminated organic silicon polyether copolymer and preparation of sealant thereof |
CN112250855A (en) * | 2020-10-16 | 2021-01-22 | 浙江皇马科技股份有限公司 | Synthesis method of vinyl silane terminated modified polyether |
CN114031780A (en) * | 2021-11-05 | 2022-02-11 | 广州集泰化工股份有限公司 | Antistatic silica gel compound and preparation method and application thereof |
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Cited By (11)
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CN109096491A (en) * | 2018-07-06 | 2018-12-28 | 福建拓烯新材料科技有限公司 | A kind of preparation method of Hydrophilicrto polyether silicone oil and the hydrophilic treatment method of glass |
CN109096491B (en) * | 2018-07-06 | 2021-06-08 | 福建拓烯新材料科技有限公司 | Preparation method of hydrophilic polyether silicone oil and hydrophilic treatment method of glass |
EP3666836A1 (en) * | 2018-12-10 | 2020-06-17 | Samsung Electronics Co., Ltd. | Compositions, films comprising cured products of the same, stacked structures comprising the films, and display devices |
US11286350B2 (en) | 2018-12-10 | 2022-03-29 | Samsung Electronics Co., Ltd. | Compositions, films comprising cured products of the same, stacked structures comprising the films, and display devices |
CN109705333A (en) * | 2019-01-09 | 2019-05-03 | 浙江新安化工集团股份有限公司 | A kind of synthetic method of high molecular weight diallyl polyether |
CN111286021A (en) * | 2020-03-31 | 2020-06-16 | 安徽海螺新材料科技有限公司 | Polyether terminated by silyl ether, preparation method thereof and efficient anti-mud water reducer |
CN111286021B (en) * | 2020-03-31 | 2023-03-10 | 安徽海螺材料科技股份有限公司 | Polyether terminated by silyl ether, preparation method thereof and efficient anti-mud water reducer |
CN111269691A (en) * | 2020-04-13 | 2020-06-12 | 江西省科学院应用化学研究所 | Single-component composite modified polyether sealant and preparation method thereof |
CN111440323A (en) * | 2020-05-18 | 2020-07-24 | 烟台德邦科技有限公司 | Synthesis method of alkoxy-terminated organic silicon polyether copolymer and preparation of sealant thereof |
CN112250855A (en) * | 2020-10-16 | 2021-01-22 | 浙江皇马科技股份有限公司 | Synthesis method of vinyl silane terminated modified polyether |
CN114031780A (en) * | 2021-11-05 | 2022-02-11 | 广州集泰化工股份有限公司 | Antistatic silica gel compound and preparation method and application thereof |
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