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A kind of star comb polyether organosilicon copolymer and preparation method thereof

A technology of polyether silicone and star-shaped comb, which is applied in ether preparation, organic chemistry, and alkylene oxide preparation of ether, etc. It can solve problems such as wide molecular weight distribution, uncontrollable branching structure, complex process, etc., and meet the reaction conditions Mild, good application prospects, simple process effect

Active Publication Date: 2017-01-11
JIANGSU MAYSTA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] There are certain technical problems in the preparation methods of organosilicon or silicon-containing star-shaped copolymers in the above-mentioned prior art: the patents with publication numbers CN1105036A, CN103539944A and CN1738866A all use divinylbenzene or dienes to produce star-shaped branched structures , but its branched structure is not controllable, the preparation of star structure is diverse, and the molecular weight distribution is very wide
A large amount of organic solvents are used in the above-mentioned preparation process, which produces a large amount of waste liquid, which is easy to pollute the environment; meanwhile, the reaction is mainly active polymerization such as atom transfer radical polymerization or RAFT polymerization and post-treatment is required, the process is relatively complicated, and industrialization is very difficult. and pose a huge security risk

Method used

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  • A kind of star comb polyether organosilicon copolymer and preparation method thereof
  • A kind of star comb polyether organosilicon copolymer and preparation method thereof
  • A kind of star comb polyether organosilicon copolymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Add 26.48g of allyl alcohol, 120.55g of ethylene oxide and 52.97g of propylene oxide into the reactor, in the presence of 0.87g KOH catalyst, pressure ≤0.4Mpa, reaction temperature 120℃, react for 5h to obtain allyl Base polyether

[0028] (2) Add 16.01g of 1,7-octadiene and 83.99g of heptamethyltrisiloxane into the reactor, in the presence of 6ppm chloroplatinic acid catalyst and 13ppm N,N ethylenediamine promoter, heating at normal pressure To 100-110°C, react for 4 hours to obtain the star copolymer initiator.

[0029] (3) The octamethylcyclotetrasiloxane, tetramethylcyclotetrasiloxane and star copolymer initiator are reacted at 80℃ for 5h under the action of sulfuric acid to obtain hydrogen-containing polymethylsiloxane star A copolymer in which the molar ratio between octamethylcyclotetrasiloxane, tetramethylcyclotetrasiloxane and the star copolymer initiator is 10:3:1.

[0030] (4) Add 128.51g of hydrogen-containing polymethylsiloxane star copolymer and 171.49g of ...

Embodiment 2

[0035] (1) Add 11.86g of allyl alcohol, 116.97g of ethylene oxide and 71.17g of propylene oxide into the reactor, in the presence of 0.94g of KOH catalyst, pressure ≤0.4Mpa, reaction temperature of 120℃, react for 5h to obtain allyl Base polyether

[0036] (2) Add 17.68g of 1,8-nonadiene and 82.32g of heptamethyltrisiloxane into the reactor. In the presence of 6ppm chloroplatinic acid catalyst and 12ppm dimethylaniline co-catalyst, heat at normal pressure to 110 React at -120°C for 4h to obtain the star copolymer initiator.

[0037] (3) The octamethylcyclotetrasiloxane, tetramethylcyclotetrasiloxane and star copolymer initiator are reacted at 80℃ for 5h under the action of sulfuric acid to obtain hydrogen-containing polymethylsiloxane star A copolymer in which the molar ratio between octamethylcyclotetrasiloxane, tetramethylcyclotetrasiloxane and the star copolymer initiator is 17:3:1.

[0038] (4) Add 100.13g of hydrogen-containing polymethylsiloxane star copolymer and 199.87g of ...

Embodiment 3

[0043] (1) Add 10.30g of allyl alcohol, 148.49g of ethylene oxide and 41.21g of propylene oxide into the reactor. In the presence of 0.95g of KOH catalyst, the pressure is ≤0.4Mpa, the reaction temperature is 120°C, and the reaction time is 5h to obtain the alkene Propyl polyether

[0044] (2) Add 19.30g of 1,9-decadiene and 80.70g of heptamethyltrisiloxane into the reactor, add 10ppm chloroplatinic acid catalyst and 20ppm N,N dimethylformamide catalyst, and heat up to 110-120°C, react for 4h to obtain the star copolymer initiator.

[0045] (3) The octamethylcyclotetrasiloxane, tetramethylcyclotetrasiloxane and star copolymer initiator are reacted at 80℃ for 5h under the action of sulfuric acid to obtain hydrogen-containing polymethylsiloxane star A copolymer in which the molar ratio of octamethylcyclotetrasiloxane, tetramethylcyclotetrasiloxane and star copolymer initiator is 25:4:1.

[0046] (4) Add 94.76g of hydrogen-containing polymethylsiloxane star copolymer and 205.24g of al...

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Abstract

The invention discloses a starlike pectinate polyether-organosilicone copolymer. A branch point (starlike copolymer initiator) in the copolymer is composed of alkadiene and heptamethyltrisiloxane, which are connected by a silicon-carbon bond; a branched chain is a polysiloxane chain and is connected to the branch point by a silicon-oxygen-silicon chain; a side chain is a polyether chain and is connected to the polysiloxane chain by the silicon-carbon bond. The starlike pectinate polyether-organosilicone copolymer disclosed by the invention has a structure with the structural formula I described in the description, wherein in the structural formula I, the value of x is 7-20, R is a structure with a structural formula II described in the description, and in the structural formula II, the value of m is 10-40, the value of n is 1-8, the value of a is 4-30, the value of b is 0-10, the value of m+n is 11-48, and the value of a+b is 4-40.

Description

Technical field [0001] The invention relates to a preparation method of a polyether organosilicon copolymer, and more specifically to a star comb-shaped polyether organosilicon copolymer and a preparation method thereof. Background technique [0002] Polyether silicone copolymer is a comb-type copolymer with siloxane as the main chain and polyether as the side chain. Among them, siloxane is the hydrophobic group, so that the product has low surface tension and excellent chemical stability and electrical insulation. , Anti-aging and other properties; polyether as a hydrophilic group makes the product have good surface activity. By changing the type, quantity and location of the introduced polyether, the hydrophilicity and lipophilicity of the copolymer can be effectively adjusted to obtain different properties such as foam stabilization, defoaming, lubrication, and emulsification. [0003] In recent years, the rapid development of polymerization technology has provided a variety of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/46C08G77/50C08G77/06C08G65/28C07C41/03C07C43/178
Inventor 唐雄峰孙宇沈杰陈天鹏
Owner JIANGSU MAYSTA CHEM
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