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Starlike pectinate polyether-organosilicone copolymer and preparation method thereof

A technology of polyether silicone and star-shaped comb, which is applied in the fields of ether preparation, organic chemistry, and alkylene oxide preparation of ether, etc. It can solve the problems of uncontrollable branching structure, complex process, wide molecular weight distribution, etc., and achieve good application The effect of prospect, simple process flow and mild reaction conditions

Active Publication Date: 2015-03-25
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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  • Starlike pectinate polyether-organosilicone copolymer and preparation method thereof
  • Starlike pectinate polyether-organosilicone copolymer and preparation method thereof
  • Starlike pectinate polyether-organosilicone 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 of KOH catalyst, the pressure is ≤0.4Mpa, the reaction temperature is 120°C, and the reaction is 5h to obtain allyl base polyether;

[0028] (2) 16.01g of 1,7-octadiene and 83.99g of heptamethyltrisiloxane were added to the reactor, and in the presence of 6ppm chloroplatinic acid catalyst and 13ppm N, N ethylenediamine co-catalyst, the temperature was raised under normal pressure To 100-110°C, react for 4 hours to obtain a star-shaped copolymer initiator.

[0029] (3) React octamethylcyclotetrasiloxane, tetramethylcyclotetrasiloxane and star copolymer starter at 80°C for 5 hours under the action of sulfuric acid to obtain hydrogen-containing polymethylsiloxane star Copolymer, wherein the molar ratio between octamethylcyclotetrasiloxane, tetramethylcyclotetrasiloxane and star copolymer starter is 10:3:1.

[0030] (4) Add 128.51 g of hydrog...

Embodiment 2

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

[0036] (2) 17.68g of 1,8-nonadiene and 82.32g of heptamethyltrisiloxane were added to the reactor, and in the presence of 6ppm chloroplatinic acid catalyst and 12ppm dimethylaniline cocatalyst, the temperature was raised to 110 React at -120°C for 4 hours to obtain a star-shaped copolymer initiator.

[0037] (3) React octamethylcyclotetrasiloxane, tetramethylcyclotetrasiloxane and star copolymer starter at 80°C for 5 hours under the action of sulfuric acid to obtain hydrogen-containing polymethylsiloxane star Copolymer, wherein the molar ratio between octamethylcyclotetrasiloxane, tetramethylcyclotetrasiloxane and star copolymer starter is 17:3:1.

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

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 is 5h to obtain ene Propyl polyether;

[0044] (2) 19.30g of 1,9-decadiene and 80.70g of heptamethyltrisiloxane are added to the reactor, and at 10ppm chloroplatinic acid catalyst and 20ppm N, N dimethylformamide catalyst, heating at normal pressure to 110-120°C, react for 4 hours to obtain a star-shaped copolymer initiator.

[0045] (3) React octamethylcyclotetrasiloxane, tetramethylcyclotetrasiloxane and star copolymer starter at 80°C for 5 hours under the action of sulfuric acid to obtain hydrogen-containing polymethylsiloxane star Copolymer, wherein the molar ratio between octamethylcyclotetrasiloxane, tetramethylcyclotetrasiloxane and star copolymer starter is 25:4:1.

[0046] (4) 94.76g of hydrogen-containing polymethylsiloxane star copolym...

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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 silicone copolymer, in particular to a star comb polyether silicone copolymer and a preparation method thereof. Background technique [0002] Polyether silicone copolymer is a comb copolymer with siloxane as the main chain and polyether as the side chain, in which siloxane is used as 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, so that the product has a good surface activity. By changing the type, quantity and location of the polyether introduced, the hydrophilic and lipophilic properties 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 provides a variety of methods and me...

Claims

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Application Information

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Patent Type & Authority Applications(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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