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A kind of fluorine-silicon functional macromonomer containing ethylenic double bond at one end and preparation method thereof

A technology of macromonomer and olefinic double bond, which is applied in the field of fluorine-silicon functional macromonomer containing olefinic double bond at one end and its preparation field, which can solve the problem of less application

Active Publication Date: 2018-07-31
ZHEJIANG SCI-TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The ring-opening of the latter siloxane ring body has two methods: anionic ring-opening polymerization and cationic ring-opening polymerization, while cationic ring-opening polymerization is not as convenient and effective as anionic ring-opening polymerization, and has fewer applications

Method used

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  • A kind of fluorine-silicon functional macromonomer containing ethylenic double bond at one end and preparation method thereof
  • A kind of fluorine-silicon functional macromonomer containing ethylenic double bond at one end and preparation method thereof
  • A kind of fluorine-silicon functional macromonomer containing ethylenic double bond at one end and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) After evacuating the polymerization bottle to high vacuum for 1 hour, add F 3 Monomer (34.3ml, 0.091mol), 40% (Vol) THF (290ml) and n-butyllithium 37.5ml (2.4M n-hexane solution), reacted for 2h to prepare oxyanion initiator lithium silanolate, and then added the remaining F 3 Monomer (343.2ml, 0.909mol) was subjected to ring-opening polymerization reaction for 3h, and then 19.3ml of end-capping agent was added to end-cap for 12h.

[0037] (2) After the product was centrifuged, it was distilled under reduced pressure to remove impurities such as solvents and unreacted monomers, and the product was washed with methanol and dried in a vacuum oven for 24 hours. For products 1 HNMR and gel permeation chromatography (GPC) characterize the structure, molecular weight and distribution of functional macromolecules, in which the gel permeation chromatogram is as follows figure 1 As shown, through the above characterization, it is shown that the product is a structure of fo...

Embodiment 2

[0040] (1) After evacuating the polymerization bottle to high vacuum for 1 hour, add F 3 Monomer (34.3ml, 0.091mol)), 40% (Vol) (290ml) THF and n-butyllithium 37.5ml (2.4M n-hexane solution), reacted for 2h to prepare oxyanion initiator lithium silanolate, and then added the remaining f 3 Monomer (343.2ml, 0.909mol) was subjected to ring-opening polymerization reaction for 3h, and then 21.4ml of end-capping agent was added to end-cap for 12h.

[0041] (2) After the product was centrifuged, it was distilled under reduced pressure to remove impurities such as solvents and unreacted monomers, and the product was washed with methanol and dried in a vacuum oven for 24 hours. For products 1 HNMR and GPC characterize the structure, molecular weight and distribution of functional macromolecules, among which the gel permeation chromatogram is as follows figure 2 As shown, through the above characterization, it is shown that the product has the structure of formula II, n=21.5.

[0...

Embodiment 3

[0044] (1) After evacuating the polymerization bottle to high vacuum for 2 hours, add F 3 Monomer (17.4ml, 0.046mol), 50% (Vol) (405ml) THF and n-butyllithium 18.8ml (2.4M n-hexane solution), reacted for 1h to prepare oxyanion initiator lithium silanolate, and then added the remaining F 3 Monomer (360.2ml, 0.954mol) was subjected to ring-opening polymerization reaction for 3h, and then 9.7ml of end-capping agent was added to end-cap for 12h.

[0045] (2) After the product was centrifuged, it was distilled under reduced pressure to remove impurities such as solvents and unreacted monomers, and the product was washed with methanol and dried in a vacuum oven for 24 hours. For products 1 The structure, molecular weight and distribution of the functional macromolecules were characterized by HNMR and GPC. Through the above characterizations, it was shown that the product had a structure of formula I, n=56.7.

[0046]

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Abstract

The present invention discloses a fluorosilicone functional macromonomer with alkene double bond on single end and a preparation method thereof. The monomer has a structure shown as a formula I or formula II. The fluorosilicone functional macromonomer prepared by the invention can be used in further copolymerization reaction with vinyl monomer, such as styrene and acrylate monomer, and endows the acrylic resin and styrene resin with characteristics of heat resistance, smoothness and weather resistance. The present invention uses an anion ring opening polymerization method for synthesis of a fluorine-containing organosilicon macromonomer with reactive functional group on single end, wherein the macromonomer has clear structure, controllable molecular weight and narrow molecular weight distribution. The macromonomer can be in active controllable polymerization with vinyl monomer to synthesize a block-type graft copolymer with improved physical and chemical properties, and has broad application prospects.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a fluorine-silicon functional macromonomer containing ethylenic double bonds at one end and a preparation method thereof. Background technique [0002] Fluorine-containing polysiloxane refers to the polysiloxane with fluorine atoms in the side chain. At present, the fluorine-containing side chains that are more researched and applied are fluorocarbon groups and fluoroether groups. The earliest polymethyl trifluoropropylene was developed and applied. Polysiloxane (PMTFPS) is a typical representative. The main chain structure of fluorine-containing polysiloxane is a flexible silicone chain, and the side chain is an organic fluorine chain with stable properties and extremely low surface tension. Fluorine atom is the element with the highest electronegativity (4.0). Introducing fluorine-containing groups into polysiloxane to make elastomers and sealants can make them less ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/385C08G77/24
Inventor 易玲敏徐凯黄振架周鸿谢文韬
Owner ZHEJIANG SCI-TECH UNIV
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