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Method for synthesizing fluorine-silicon-oxygen polymer body through anion ring-opening polymerization and reactive extrusion

An anionic ring-opening and polymerization technology, which is applied in the field of polymer polymerization, can solve the problems that the initiator system cannot respond to the use of extrusion technology, and achieve the effect of good industrialization prospects, high quality and stable quality

Active Publication Date: 2012-05-30
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, during reactive extrusion, the residence time in the extruder is only a few minutes, and the polymerization reaction must be completed
Therefore, the initiator system used in the usual kettle polymerization process cannot be used in reactive extrusion technology

Method used

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  • Method for synthesizing fluorine-silicon-oxygen polymer body through anion ring-opening polymerization and reactive extrusion
  • Method for synthesizing fluorine-silicon-oxygen polymer body through anion ring-opening polymerization and reactive extrusion

Examples

Experimental program
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Effect test

Embodiment 1

[0030] The trifluoropropyltrimethylcyclotrisiloxane monomer that has been purified to meet the polymerization requirements of the present invention is heated to 35-40°C. The mass ratio of trifluoropropyltrimethylcyclotrisiloxane / sodium hydroxide is 50:1, protected by argon, and prepolymerized at 120°C for 30 minutes to prepare the sodium silanolate initiator, and according to the volume ratio of 20 / 3 Add trifluoropropyltrimethylcyclotrisiloxane to dilute the initiator. There are 5 feed inlets on the twin-screw extruder, which are respectively located in the first, second, third, fourth, and eighth barrel sections, which are the feed inlets for the above-mentioned monomers in turn, and the accelerator dimethyl sulfoxide Feed inlet, sodium silanolate initiator feed inlet, methyl vinyl cyclotetrasiloxane feed inlet, chloropentamethyldisiloxane feed inlet; under the delivery of metering pump, the refined The monomer, accelerator, and initiator are input into the twin-screw extrud...

Embodiment 2

[0035] The trifluoropropyltrimethylcyclotrisiloxane monomer that has been purified to meet the polymerization requirements of the present invention is heated to 35-40°C. The mass ratio of trifluoropropyltrimethylcyclotrisiloxane / sodium hydroxide is 50:1, protected by argon, and prepolymerized at 120°C for 30 minutes to prepare the sodium silanolate initiator, and according to the volume ratio of 20 / 3 Add trifluoropropyltrimethylcyclotrisiloxane to dilute the initiator. There are 5 feeding ports on the twin-screw extruder, which are respectively located in the first, second, third, fifth, and eighth screw barrel sections, which are the above-mentioned monomer feeding ports in turn, and the accelerator ethyl acetate feed Inlet, sodium silanolate initiator inlet, hexamethylcyclotrisiloxane and methylvinylcyclotetrasiloxane mixed monomer inlet, trimethylchlorosilane inlet; delivery in metering pump Next, the refined monomers, accelerators, and initiators are input into the twin-s...

Embodiment 3

[0040] Heating the mixed monomers of trifluoropropyltrimethylcyclotrisiloxane and octamethylcyclotetrasiloxane in an equimolar ratio required by the polymerization of the present invention to 35-40°C. The mass ratio of trifluoropropyltrimethylcyclotrisiloxane / sodium hydroxide is 50:1, protected by argon, and prepolymerized at 120°C for 30 minutes to prepare the sodium silanolate initiator, and according to the volume ratio of 20 / 3 Add trifluoropropyltrimethylcyclotrisiloxane to dilute the initiator. There are 4 feed inlets on the twin-screw extruder, which are respectively located in the first, second, third, fourth, and eighth screw barrel sections, which are the feed inlets for the above-mentioned mixed monomers in turn, and the accelerator ethyl acetate feed inlet. Feed port, sodium silanolate initiator feed port, methyl vinyl cyclotetrasiloxane feed port, chloropentamethyldisiloxane feed port; under the delivery of the metering pump, the refined single The body, accelerat...

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Abstract

The invention relates to a method for synthesizing a fluorine-silicon-oxygen polymer body through anion ring-opening polymerization and reactive extrusion, which comprises the following steps of: putting a monomer, an initiating agent, a polarity regulator, a vinyl cyclic monomer, and an end capping agent into different screw sections of a screw extruder to perform polymerization; and performing decompression to remove decomposition products and by-products of the polarity regulator and the initiating agent to obtain different types of fluorinated polysiloxane polymers. Compared with the prior art, the method adopts a reactive extrusion technique to shorten the production cycle to a few minutes without complex solvent separation and purification. The method has the advantages of high efficiency, small energy consumption, low cost, no pollution, continuous production and high and stable quality, simultaneously can obtain copolymers with different structures, and has good social benefits and economic benefits and very good industrial prospects.

Description

technical field [0001] The invention relates to a polymer polymerization method, in particular to a fluorosilicone polymer bulk anion ring-opening polymerization reaction extrusion synthesis method. Background technique [0002] Fluorosilicone polymers, such as trifluoropropyltrimethylcyclotrisiloxane anionic ring-opening polymerization can synthesize poly2,4,6-trifluoropropyl 2,4,6, which has better performance than polysiloxane - Trimethylcyclotrisiloxane (PMTFPS). PMTFPS not only has unique low surface energy, low glass transition temperature, excellent heat resistance, weather resistance and other properties, but also the introduction of fluorine-containing groups can effectively solve the shortcomings of polysiloxanes that are not resistant to oil and organic solvents. It can be made into fluorosilicone elastomers, sealing substrates and high-performance low surface energy antifouling coatings, and used as a copolymer composition to improve the surface properties of po...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/24C08G77/06C08G77/44
Inventor 郑安呐杨鹏管涌危大福高亚娟李书召胡福增王书忠
Owner EAST CHINA UNIV OF SCI & TECH
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