CN107082882A - A kind of preparation method of methacryloxypropyl silane polymer - Google Patents
A kind of preparation method of methacryloxypropyl silane polymer Download PDFInfo
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- CN107082882A CN107082882A CN201710391908.3A CN201710391908A CN107082882A CN 107082882 A CN107082882 A CN 107082882A CN 201710391908 A CN201710391908 A CN 201710391908A CN 107082882 A CN107082882 A CN 107082882A
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- methacryloxypropyl silane
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- silane polymer
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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
- C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
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Abstract
The invention discloses a kind of preparation method of methacryloxypropyl silane polymer, this method comprises the following steps：Methacryloxypropyl silane is put into reactor；Glacial acetic acid is continuously added in reactor, stirring is sufficiently mixed it；Draw deionized water at the uniform velocity to instill in reactor, 15min completion of dropping, reacted under the conditions of 120 DEG C, the by-product carbinol of generation is distilled off；Added in product of distillation in sodium carbonate or sodium acid carbonate and residual acid, be sufficiently stirred for after 15 30min suction filtration and collect filtrate, obtain product.The invention discloses a kind of synthetic method of methacryloxypropyl silane polymer, methanol is removed by distilling, it is ensured that react and carried out to positive direction, while the chain for generating methacryloxypropyl silane polymer is longer, when product is combined with organic polymer, adhesion is stronger.
Description
Technical field
The invention belongs to polymer synthesis techniques field, more particularly to a kind of methacryloxypropyl silane polymer
Preparation method.
Background technology
(methyl) acrylic ester monomer has active double bond, can be in radical initiator and ultraviolet light, electron beam
Under solidify to form a class there is poly- (methyl) the acrylate polymeric material of good film forming, cementability and weatherability, and
Si-C, Si-O bond energy of organosilicon polymer are high, possess excellent resistance to ag(e)ing, high temperature resistant, radiation hardness and chemical stability etc.
Feature, additionally with nontoxic and good water repelling anti-fouling, electric insulation and physiological inertia.
According to the structure of organosilicon in molecule, (methyl) acryloyl-oxy radical siloxane can be divided into side chain type and end (methyl) third
Alkene acyl-oxygen fundamental mode and ring-type (methyl) acryloyl-oxy radical siloxane, are joined directly together between acyloxy and silicon atom or by alkyl phase
Even；(methyl) acryloxy silane or siloxanes minor comonomer and (first are divided into according to the big I of organosiloxane repeat unit
Base) acryloxy polysiloxane macromonomer, the number of function base (methyl) acryloxy wherein on silicone molecules chain
Can be one, two and two or more.
Current working condition, due to that can be produced when alkoxy is hydrolyzed in generation methacryloxypropyl silane polymer process
By-product carbinol, influence reaction is carried out to positive direction, causes polymerization efficiency low.
The content of the invention
It is an object of the invention to provide a kind of preparation method of methacryloxypropyl silane polymer, pass through distillation
Remove methanol, it is ensured that react and carried out to positive direction, when product is combined with organic polymer, adhesion is stronger.
The present invention is achieved by the following technical solutions：
A kind of preparation method of methacryloxypropyl silane polymer, this method comprises the following steps：
S1, by methacryloxypropyl silane put into reactor in；
S2, continuously add glacial acetic acid in reactor, stirring is sufficiently mixed it；
S3, absorption deionized water are at the uniform velocity instilled in reactor, 15min completion of dropping, are reacted under the conditions of 120 DEG C, generation
By-product carbinol is distilled off；
Added in S4, product of distillation in sodium carbonate or sodium acid carbonate and residual acid, be sufficiently stirred for after 15-30min suction filtration simultaneously
Filtrate is collected, product is obtained.
Reaction equation is as follows：
Further, the glacial acetic acid addition is the 1-3% of methacryloxypropyl silane mass fraction.
Further, the deionized water addition is the 3-6% of methacryloxypropyl silane mass fraction.
Further, the methanol distillation condition is that temperature is 90-120 DEG C, and vacuum is -0.1MPa.
The invention has the advantages that：
The invention discloses a kind of synthetic method of methacryloxypropyl silane polymer, methanol is removed by distilling,
Ensure that reaction is carried out to positive direction, while the chain for generating methacryloxypropyl silane polymer is longer, product and organic high score
When son is combined, adhesion is stronger.
Embodiment
Technical scheme in the 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, those of ordinary skill in the art
The all other embodiment obtained under the premise of creative work is not made, belongs to the scope of protection of the invention.
Embodiment 1
S1, by 480g methacryloxypropyl silanes put into equipped with agitator, thermometer, discharge nozzle tri- mouthfuls of 500mL burning
In bottle；
S2, continuously add 4.8g glacial acetic acids in three-necked flask, stirring 5min is sufficiently mixed it；
S3, absorption deionized water 14.4g are at the uniform velocity instilled in three-necked flask, 15min completion of dropping, are reacted under the conditions of 120 DEG C,
The by-product carbinol of generation is distilled off in 90 DEG C under the conditions of -0.1MPa；
Added in S4, product of distillation in sodium carbonate and residual acid, be sufficiently stirred for after 15min suction filtration and collect filtrate, obtain
Product, yield is 94%.
Reaction equation is as follows：
Embodiment 2
S1, by 480g methacryloxypropyl silanes put into equipped with agitator, thermometer, discharge nozzle tri- mouthfuls of 500mL burning
In bottle；
S2, continuously add 10g glacial acetic acids in three-necked flask, stirring 10min is sufficiently mixed it；
S3, absorption deionized water 28.8g are at the uniform velocity instilled in three-necked flask, 15min completion of dropping, are reacted under the conditions of 120 DEG C,
The by-product carbinol of generation is distilled off in 100 DEG C under the conditions of -0.1MPa；
Added in S4, product of distillation in sodium acid carbonate and residual acid, be sufficiently stirred for after 30min suction filtration and collect filtrate, obtain
To product, yield is 93%.
Embodiment 3
S1, by 480g methacryloxypropyl silanes put into equipped with agitator, thermometer, discharge nozzle tri- mouthfuls of 500mL burning
In bottle；
S2, continuously add 14.4g glacial acetic acids in three-necked flask, stirring 8min is sufficiently mixed it；
S3, absorption deionized water 20g are at the uniform velocity instilled in three-necked flask, 15min completion of dropping, are reacted under the conditions of 120 DEG C, raw
Into by-product carbinol in 120 DEG C, be distilled off under the conditions of -0.1MPa；
Added in S4, product of distillation in sodium carbonate and residual acid, be sufficiently stirred for after 20min suction filtration and collect filtrate, obtain
Product, yield is 95%.
Above content is only citing made for the present invention and explanation, and affiliated those skilled in the art are to being retouched
The specific embodiment stated is made various modifications or supplement or substituted using similar mode, without departing from invention or super
More scope defined in the claims, all should belong to protection scope of the present invention.
Claims (4)
1. a kind of preparation method of methacryloxypropyl silane polymer, it is characterised in that this method comprises the following steps：
S1, by methacryloxypropyl silane put into reactor in；
S2, continuously add glacial acetic acid in reactor, stirring is sufficiently mixed it；
S3, absorption deionized water are at the uniform velocity instilled in reactor, 15min completion of dropping, are reacted under the conditions of 120 DEG C, the by-product of generation
Thing methanol is distilled off；
Added in S4, product of distillation in sodium carbonate or sodium acid carbonate and residual acid, be sufficiently stirred for after 15-30min suction filtration and collect
Filtrate, obtains product.
Reaction equation is as follows：
2. a kind of preparation method of methacryloxypropyl silane polymer according to claim 1, it is characterised in that：Institute
State the 1-3% that glacial acetic acid addition is methacryloxypropyl silane mass fraction.
3. a kind of preparation method of methacryloxypropyl silane polymer according to claim 1, it is characterised in that：Institute
State the 3-6% that deionized water addition is methacryloxypropyl silane mass fraction.
4. a kind of preparation method of methacryloxypropyl silane polymer according to claim 1, it is characterised in that：Institute
Stating methanol distillation condition is, temperature is 90-120 DEG C, and vacuum is -0.1MPa.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710391908.3A CN107082882A (en) | 2017-05-27 | 2017-05-27 | A kind of preparation method of methacryloxypropyl silane polymer |
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| CN201710391908.3A CN107082882A (en) | 2017-05-27 | 2017-05-27 | A kind of preparation method of methacryloxypropyl silane polymer |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101353479A (en) * | 2007-07-27 | 2009-01-28 | 德古萨有限责任公司 | Siloxane oligomer, preparation and use thereof |
| CN102604105A (en) * | 2012-02-29 | 2012-07-25 | 安徽硅宝翔飞有机硅新材料有限公司 | Preparation method of aminosilane polymer |
| CN103214509A (en) * | 2013-03-25 | 2013-07-24 | 中科院广州化学有限公司 | Cubic eight-methacryloyloxy silsesquioxane crystal and preparation method thereof |
-
2017
- 2017-05-27 CN CN201710391908.3A patent/CN107082882A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101353479A (en) * | 2007-07-27 | 2009-01-28 | 德古萨有限责任公司 | Siloxane oligomer, preparation and use thereof |
| CN102604105A (en) * | 2012-02-29 | 2012-07-25 | 安徽硅宝翔飞有机硅新材料有限公司 | Preparation method of aminosilane polymer |
| CN103214509A (en) * | 2013-03-25 | 2013-07-24 | 中科院广州化学有限公司 | Cubic eight-methacryloyloxy silsesquioxane crystal and preparation method thereof |
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Application publication date: 20170822 |
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