CN105837824A - A preparing method of a carboxyl-containing long-chain alkyl siloxane dispersion - Google Patents

A preparing method of a carboxyl-containing long-chain alkyl siloxane dispersion Download PDF

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Publication number
CN105837824A
CN105837824A CN201610216059.3A CN201610216059A CN105837824A CN 105837824 A CN105837824 A CN 105837824A CN 201610216059 A CN201610216059 A CN 201610216059A CN 105837824 A CN105837824 A CN 105837824A
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Prior art keywords
chain alkyl
carboxyl
alkyl silicone
components
prepared
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CN201610216059.3A
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Chinese (zh)
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张耀忠
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Individual
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Individual
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Priority to CN201610216059.3A priority Critical patent/CN105837824A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/42Block-or graft-polymers containing polysiloxane sequences
    • C08G77/44Block-or graft-polymers containing polysiloxane sequences containing only polysiloxane sequences
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F299/00Macromolecular compounds obtained by interreacting polymers involving only carbon-to-carbon unsaturated bond reactions, in the absence of non-macromolecular monomers
    • C08F299/02Macromolecular compounds obtained by interreacting polymers involving only carbon-to-carbon unsaturated bond reactions, in the absence of non-macromolecular monomers from unsaturated polycondensates
    • C08F299/08Macromolecular compounds obtained by interreacting polymers involving only carbon-to-carbon unsaturated bond reactions, in the absence of non-macromolecular monomers from unsaturated polycondensates from polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04Polysiloxanes
    • C08G77/38Polysiloxanes modified by chemical after-treatment
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09GPOLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00Polishing compositions

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • General Chemical & Material Sciences (AREA)
  • Silicon Polymers (AREA)

Abstract

A preparing method of a carboxyl-containing long-chain alkyl siloxane dispersion is disclosed. The dispersion is prepared through adopting a long-chain alkyl siloxane component and a carboxyl silane component. The prepared dispersion is high in purity, good in product stability and wide in application range.

Description

A kind of preparation method containing carboxyl chain alkyl silicone dispersion
Technical field
The present invention relates to polymeric material field, be specifically related to a kind of preparation method containing carboxyl chain alkyl silicone dispersion.
Background technology
The chain alkyl silicone dispersion containing carboxyl is group composition important in automotive coatings polishing agent, and the automotive polish VOC content that it is prepared is relatively low, and has high gloss, good pollution resistance and perception, preferable sense of touch performance.
Summary of the invention
Present invention aim at, it is provided that a kind of preparation method containing carboxyl chain alkyl silicone dispersion, the technical solution adopted in the present invention is:
A kind of preparation method containing carboxyl chain alkyl silicone dispersion, it is characterised in that it is prepared from carboxyl silicon components emulsion reaction by chain alkyl silicone components.
Further, described chain alkyl silicone components is prepared from by following steps:
A: join in reactor by 1 part of a-alkene, under nitrogen protection, is heated to 80 DEG C;
B: be slowly dropped into 1 part of containing hydrogen silicone oil, after 1-1.5h dropping, rises high-temperature to 120 DEG C;
C: being slowly dropped into isopropyl alcohol solution of chloroplatinic acid, 0.5-1h dropping is complete, insulation reaction 15h;
D: after reaction terminates, decompression is distilled off unreacted a-alkene, and processes through charcoal absorption, final acquisition chain alkyl silicone components.
Further, described carboxyl silicon components is prepared from by following steps:
A: by 12 parts of octamethylcy-clotetrasiloxanes, 1 part of r-the third amino methyl diethoxy silane, 5 parts of methyl dimethoxy epoxide dodecyl silane and 0.1 part of catalyst join in reactor, and oil bath is heated to 110 DEG C;
B: by 25 part 1,3,5-trimethyl cyclotrisiloxane are slowly added in reactor in 1h, and stirring makes it fully react 4h, then rise high-temperature to 150 DEG C, isothermal reaction 1h;
C: decompression is distilled off unreacted low-boiling-point substance, is cooled to 75 DEG C, is subsequently adding 0.8 part of maleic anhydride, continues reaction 1h, finally gives carboxyl silicon components.
The present invention provides the benefit that relative to prior art: the preparation method containing carboxyl chain alkyl silicone dispersion of the present invention, chain alkyl silicone components is used to be prepared from carboxyl silicon components, the dispersion purity prepared is high, and product stability is good, applied range.
Detailed description of the invention
Below with reference to embodiment, the design of the present invention and the technique effect of generation are clearly and completely described, to be completely understood by the purpose of the present invention, feature and effect.Obviously; described embodiment is a part of embodiment of the present invention rather than whole embodiment, based on embodiments of the invention; other embodiments that those skilled in the art is obtained on the premise of not paying creative work, belong to the scope of protection of the invention.
Embodiment 1: a kind of preparation method containing carboxyl chain alkyl silicone dispersion, it is characterised in that its
It is prepared from carboxyl silicon components emulsion reaction by chain alkyl silicone components.
Further, described chain alkyl silicone components is prepared from by following steps:
A: join in reactor by 1 part of a-alkene, under nitrogen protection, is heated to 80 DEG C;
B: be slowly dropped into 1 part of containing hydrogen silicone oil, after 1-1.5h dropping, rises high-temperature to 120 DEG C;
C: being slowly dropped into isopropyl alcohol solution of chloroplatinic acid, 0.5-1h dropping is complete, insulation reaction 15h;
D: after reaction terminates, decompression is distilled off unreacted a-alkene, and processes through charcoal absorption, final acquisition chain alkyl silicone components.
Further, described carboxyl silicon components is prepared from by following steps:
A: by 12 parts of octamethylcy-clotetrasiloxanes, 1 part of r-the third amino methyl diethoxy silane, 5 parts of methyl dimethoxy epoxide dodecyl silane and 0.1 part of catalyst join in reactor, and oil bath is heated to 110 DEG C;
B: by 25 part 1,3,5-trimethyl cyclotrisiloxane are slowly added in reactor in 1h, and stirring makes it fully react 4h, then rise high-temperature to 150 DEG C, isothermal reaction 1h;
C: decompression is distilled off unreacted low-boiling-point substance, is cooled to 75 DEG C, is subsequently adding 0.8 part of maleic anhydride, continues reaction 1h, finally gives carboxyl silicon components.
Above the better embodiment of the present invention is illustrated, but the invention is not limited to described embodiment, those of ordinary skill in the art also can make all equivalent modifications or replacement on the premise of spirit of the present invention, and modification or the replacement of these equivalents are all contained in the application claim limited range.

Claims (3)

1. the preparation method containing carboxyl chain alkyl silicone dispersion, it is characterised in that it is prepared from carboxyl silicon components emulsion reaction by chain alkyl silicone components.
Preparation method containing carboxyl chain alkyl silicone dispersion the most according to claim 1, it is characterised in that described chain alkyl silicone components is prepared from by following steps:
A: join in reactor by 1 part of a-alkene, under nitrogen protection, is heated to 80 DEG C;
B: be slowly dropped into 1 part of containing hydrogen silicone oil, after 1-1.5h dropping, rises high-temperature to 120 DEG C;
C: being slowly dropped into isopropyl alcohol solution of chloroplatinic acid, 0.5-1h dropping is complete, insulation reaction 15h;
D: after reaction terminates, decompression is distilled off unreacted a-alkene, and processes through charcoal absorption, final acquisition chain alkyl silicone components.
Preparation method containing carboxyl chain alkyl silicone dispersion the most according to claim 1, it is characterised in that described carboxyl silicon components is prepared from by following steps:
A: by 12 parts of octamethylcy-clotetrasiloxanes, 1 part of r-the third amino methyl diethoxy silane, 5 parts of methyl dimethoxy epoxide dodecyl silane and 0.1 part of catalyst join in reactor, and oil bath is heated to 110 DEG C;
B: by 25 part 1,3,5-trimethyl cyclotrisiloxane are slowly added in reactor in 1h, and stirring makes it fully react 4h, then rise high-temperature to 150 DEG C, isothermal reaction 1h;
C: decompression is distilled off unreacted low-boiling-point substance, is cooled to 75 DEG C, is subsequently adding 0.8 part of maleic anhydride, continues reaction 1h, finally gives carboxyl silicon components.
CN201610216059.3A 2016-04-10 2016-04-10 A preparing method of a carboxyl-containing long-chain alkyl siloxane dispersion Pending CN105837824A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610216059.3A CN105837824A (en) 2016-04-10 2016-04-10 A preparing method of a carboxyl-containing long-chain alkyl siloxane dispersion

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610216059.3A CN105837824A (en) 2016-04-10 2016-04-10 A preparing method of a carboxyl-containing long-chain alkyl siloxane dispersion

Publications (1)

Publication Number Publication Date
CN105837824A true CN105837824A (en) 2016-08-10

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101104693A (en) * 2006-07-14 2008-01-16 戈尔德施米特股份公司 Straight-chain carboxyl group functional organic siloxane derivative and use thereof
CN101402734A (en) * 2008-11-11 2009-04-08 宁波润禾化学工业有限公司 Process for producing long-chain alkyl-phenyl modified silicone oil
CN102336912A (en) * 2010-07-21 2012-02-01 宁波晨光纺织助剂有限公司 Silicone oil emulsion with multiple functional groups and preparation method thereof
CN102627773A (en) * 2012-03-19 2012-08-08 江苏飞翔化工股份有限公司 Polyoxyethylene fatty alcohol ether-siloxane copolymer and its preparation method and use
JP5015994B2 (en) * 2009-04-02 2012-09-05 信越化学工業株式会社 Organopolysiloxane, process for producing the same, and cosmetic composition containing the organopolysiloxane
CN102757646A (en) * 2011-04-22 2012-10-31 信越化学工业株式会社 Silicone microemulsion composition

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101104693A (en) * 2006-07-14 2008-01-16 戈尔德施米特股份公司 Straight-chain carboxyl group functional organic siloxane derivative and use thereof
CN101402734A (en) * 2008-11-11 2009-04-08 宁波润禾化学工业有限公司 Process for producing long-chain alkyl-phenyl modified silicone oil
JP5015994B2 (en) * 2009-04-02 2012-09-05 信越化学工業株式会社 Organopolysiloxane, process for producing the same, and cosmetic composition containing the organopolysiloxane
CN102336912A (en) * 2010-07-21 2012-02-01 宁波晨光纺织助剂有限公司 Silicone oil emulsion with multiple functional groups and preparation method thereof
CN102757646A (en) * 2011-04-22 2012-10-31 信越化学工业株式会社 Silicone microemulsion composition
CN102627773A (en) * 2012-03-19 2012-08-08 江苏飞翔化工股份有限公司 Polyoxyethylene fatty alcohol ether-siloxane copolymer and its preparation method and use

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Application publication date: 20160810