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A kind of amino-terminated fluorine-containing acrylate prepolymer and preparation method thereof

An acrylate and prepolymer technology, which is applied in the field of amino-terminated fluorine-containing acrylate prepolymers and its preparation, can solve the problems of expensive fluorine-containing polymers, difficulty in modifying other polymers, and poor solubility. Excellent hydrophobic and oleophobic properties, excellent hydrophobic properties, and low production cost

Inactive Publication Date: 2019-02-01
国科广化(南雄)新材料研究院有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, fluoropolymers have disadvantages such as high price, poor solubility, difficult processing, and poor compatibility with other polymers.
[0003] When fluoropolymers are used in practice, their limitations are mainly reflected in: (1) The solubility of fluoropolymers and solvents is very poor, and it is difficult to find suitable compatible solvents; (2) Fluoropolymers and other polymers Poor material compatibility, it is difficult to achieve the purpose of modifying other polymers by means of physical blending or compounding; (3) Although fluorine-containing polymers can reach a temporary compatible state with other polymers in a suitable compatible solvent , but with the volatilization of the solvent or the cross-linking and curing of other polymers, the fluoropolymers tend to separate to the surface, making it difficult to retain for a long time

Method used

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  • A kind of amino-terminated fluorine-containing acrylate prepolymer and preparation method thereof
  • A kind of amino-terminated fluorine-containing acrylate prepolymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Preparation of amino-terminated fluorine-containing acrylate prepolymer: Add 20 parts by mass of hexafluorobutyl methacrylate and 40 parts by mass of N,N-dimethylformamide into a container, raise the temperature to 60°C, add 1.5 parts by mass Cystamine hydrochloride, 0.6 parts by mass of azobisisobutyronitrile, stirred and reacted for 8 hours, added triethylamine to make the pH = 8, then added 0.8 parts by mass of formaldehyde solution with a mass concentration of 37%, and stirred thoroughly for 1 hour to obtain terminal The amino fluorine-containing acrylate prepolymer solution is obtained by distilling off the solvent under reduced pressure to obtain an amino-terminated fluorine-containing acrylate prepolymer. The polymer number average molecular weight M was measured by permeation gel chromatography (GPC) n for 3280.

Embodiment 2

[0025] Preparation of amino-terminated fluorine-containing acrylate prepolymer: Add 40 parts by mass of trifluoroethyl methacrylate and 80 parts by mass of N,N-dimethylformamide into a container, heat up to 60°C, add 4 parts by mass of mercapto Ethylamine, 0.8 parts by mass of azobisisobutyronitrile, stirred and reacted for 9 hours, added triethylamine to make the pH = 8, added 2 parts by mass of formaldehyde solution with a mass concentration of 38%, and stirred thoroughly for 0.5 hours to obtain Fluorine acrylate prepolymer solution, the solvent is distilled off under reduced pressure to obtain an amino-terminated fluorine-containing acrylate prepolymer. The polymer number average molecular weight M was measured by permeation gel chromatography (GPC) n for 3480.

Embodiment 3

[0027] Preparation of amino-terminated fluorine-containing acrylate prepolymer: Add 30 parts by mass of dodecafluoroheptyl methacrylate and 60 parts by mass of N,N-dimethylformamide into a container, raise the temperature to 110°C, and add 0.6 parts by mass of Mercaptoethylamine, 0.1 parts by mass of azobisisobutyronitrile, stirred and reacted for 9 hours, diisopropylethylamine was added to make the pH = 8, and 1.5 parts by mass of formaldehyde solution with a mass concentration of 40% was added, and after fully stirred for 2 hours, the obtained The amino-terminated fluorine-containing acrylate prepolymer solution is obtained by distilling off the solvent under reduced pressure to obtain the amino-terminated fluorine-containing acrylate prepolymer. The polymer number average molecular weight M was measured by permeation gel chromatography (GPC) n for 2040.

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Abstract

The invention discloses an amino end fluorinated acrylate prepolymer and a preparation method thereof. The preparation method comprises the following steps: adding 20-40 parts of by mass of a fluorine-containing monomer and 40-80 parts by mass of a solvent into a container; heating to 60-110 DEG C, adding 0.6-4 parts by mass of an amino-containing chain transfer agent and 0.1-0.8 part by mass of an initiator, performing a stirring reaction for 6-9 hours, adding a pH adjusting agent, adjusting the pH value to be 8, further adding 0.8-2 parts by mass of a formaldehyde solution, sufficiently stirring for 0.5-2 hours so as to obtain an amino end fluorinated acrylate prepolymer solution, and performing reduced pressure distillation so as to remove a solvent, thereby obtaining the amino end fluorinated acrylate prepolymer. The amino end fluorinated acrylate prepolymer disclosed by the invention is prepared by adding the amino-containing chain transfer agent and a free radical to initialize a fluorine-containing monomer reaction, the reaction is simple, and the preparation cost is low.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to an amino-terminated fluorine-containing acrylate prepolymer and a preparation method thereof. Background technique [0002] The fluorine-carbon bonds are large and tightly arranged, which can effectively prevent the exposure of carbon atoms and carbon chains, so fluoropolymers exhibit excellent chemical stability, water resistance, high temperature resistance and corrosion resistance. Therefore, organic fluoropolymers can be widely used in the fields of release agents, tank linings, photovoltaic backsheets, decorations, and pharmaceutical blister packaging. However, fluoropolymers have disadvantages such as high price, poor solubility, difficult processing, and poor compatibility with other polymers. [0003] When fluoropolymers are used in practice, their limitations are mainly reflected in: (1) The solubility of fluoropolymers and solvents is very poor, and it is difficult to...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F120/22C08F2/38
CPCC08F2/38C08F120/22
Inventor 刘伟区林展聪王政芳
Owner 国科广化(南雄)新材料研究院有限公司