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Preparation method of fluorine-containing soap-free emulsion repellent

A soap-free emulsion and protective agent technology, which is applied in the production of coatings and bulk chemicals, can solve the problems of high energy consumption, prone to violent polymerization, and non-flammability, so as to improve the yield and purity and avoid the phenomenon of violent polymerization , the effect of improving production efficiency

Active Publication Date: 2015-08-26
SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Many enterprises have adopted the water system, but found that the water system also has many disadvantages, for example: the emulsifier and other impurities are used in the suspension and emulsion polymerization methods, so it is difficult to obtain high-purity polymers; the drying process of the product consumes a lot of energy; the production A large amount of waste water is produced in the process, which needs to be treated, etc., and the improvement of the water system to the environment is minimal, so it is necessary to find an environmentally friendly and clean solvent
[0004] Supercritical carbon dioxide has the characteristics of chemical inertness, low toxicity, non-flammability, easy recovery, and easy realization of critical state. At present, there are many domestic researches on supercritical extraction and supercritical synthesis of non-fluoropolymers. In terms of synthesis of fluoropolymers It is very few, and the experiment found that in the carbon dioxide medium, the polymerization heat of the polymerization reaction is not easy to export, and the phenomenon of violent polymerization is easy to occur.

Method used

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  • Preparation method of fluorine-containing soap-free emulsion repellent
  • Preparation method of fluorine-containing soap-free emulsion repellent
  • Preparation method of fluorine-containing soap-free emulsion repellent

Examples

Experimental program
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Effect test

Embodiment 1

[0021] (1) Mix the composite initiation system composed of polytetrafluoroethylene, azobisisobutyronitrile and azobisisoheptanonitrile at a mass ratio of 1:0.05, wherein the composite initiation system includes azobisisobutyronitrile, azo The mass ratio of diisoheptanonitrile is 1:0.5, then add water, then add 2-methyl methacrylate, the ratio of the added quality to polytetrafluoroethylene is 1:10, add 2-methyl methacrylate The speed is one drop per second, and finally adjust the pH of the mixed solution to 3, control the temperature to 80°C, and stir for 1 hour to obtain the mixed solution A, wherein the water added is 10% of the solution mass before adjusting the pH;

[0022] (2) Under the protection of nitrogen atmosphere, the redox system composed of mixed liquid A, styrene, dihydrocarbon peroxide and tertiary amine fatty acid ferrous salt, and hydroquinone are mixed and then added to the reaction in the presence of supercritical carbon dioxide medium Polymerization is car...

Embodiment 2

[0024] (1) Mix the composite initiation system composed of polyhexafluoroethylene, dimethyl azobisisobutyrate and azobisisobutyronitrile at a mass ratio of 1:0.05, wherein the composite initiation system contains azobisisobutyronitrile The mass ratio of dimethyl methacrylate and azobisisobutyronitrile is 1: 2, then add water, then add 2-ethyl methacrylate, the ratio of the added quality to polyhexafluoroethylene is 1: 10, add 2 - The speed of ethyl methacrylate is one drop per second, and finally adjust the pH of the mixed solution to 7, and control the temperature to 80°C, stir and react for 1 hour to obtain mixed solution A, wherein the water added is 10% of the solution quality before pH adjustment %;

[0025] (2) Under the protection of a nitrogen atmosphere, mix the mixed solution A, n-butyl acrylate, the oil-soluble initiator as a redox system composed of dihydrocarbon peroxide and cuprous naphthenate, and mix tert-butyl quinone and add organic Carry out polyreaction in...

Embodiment 3

[0027] (1) Mix polyhexafluoropropylene oxide and water-soluble initiators such as azobisisobutyronitrile and azobisisoheptanonitrile in a mass ratio of 1:0.05, and the two substances in the composite initiation system The mass ratio is 1:1.5, then add water, then add 4-methylstyrene, the ratio of the added quality to polyhexafluoropropylene oxide is 1:10, and the speed of adding 4-methylstyrene is per second One drop, finally adjust the pH of the mixed solution to 6, control the temperature to 80°C, stir and react for 1 hour to obtain the mixed solution A, wherein the water added is 10% of the mass of the solution before adjusting the pH;

[0028] (2) Under the protection of a nitrogen atmosphere, mix the mixed solution A, isooctyl acrylate, the oil-soluble initiator is a redox system composed of dihydrocarbon peroxide and tertiary amine fatty acid ferrous salt, and add copper naphthenate. Carry out polymerization reaction in the reactor that supercritical carbon dioxide mediu...

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Abstract

The invention discloses a preparation method of a fluorine-containing soap-free emulsion repellent, and relates to the technical field of fluorine-containing emulsion repellent preparation, in particular to a preparation method of an environment-friendly fluorine-containing composite emulsion repellent. The preparation method of the fluorine-containing soap-free emulsion repellent comprises the following steps that (1) a fluorine-containing polymer, a water-soluble initiator and a polymer monomer react to form a mixed solution A; and (2) the mixed solution A, the polymer monomer B, an oil-soluble initiator and a polymerization inhibitor are added to a closed reaction kettle with a supercritical carbon dioxide medium for a polymerization reaction under nitrogen atmosphere protection, and supercritical extraction is adopted after reaction completion to form a product. The method overcomes the defect that a solvent is difficultly cleaned up; the obtained product is good in stability; the yield and the purity of the generated fluorine-containing polymer are significantly increased and improved; flash polymerization is avoided; and the production efficiency is improved.

Description

technical field [0001] The invention relates to the technical field of preparation of a fluorine-containing emulsion protective agent, in particular to a preparation method of an environment-friendly fluorine-containing soap-free emulsion protective agent. Background technique [0002] Fluorine-containing polymers refer to a class of polymers in which the hydrogen atoms on the carbon chain are fully or partially replaced by fluorine atoms. Since the fluorine atoms have strong electronegative properties, after replacing the hydrogen atoms on the organic carbon chain, the perfluoroalkyl The group endows fluorocarbon polymers with very low surface free energy, and acrylate copolymers containing fluorocarbon chains have high surface activity, high oxygen permeability, water and oil resistance, and high chemical resistance, thus endowing paper, leather, fabrics, The surface of rough media such as stone is waterproof, oil-proof and anti-fouling. [0003] In industrial production,...

Claims

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Application Information

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IPC IPC(8): C08F259/08C08F283/06C08F212/08C08F220/14C08F220/18C08F212/12C08F4/40C09D151/00C09D151/08
CPCY02P20/54
Inventor 王青杨东元刘世川李霁阳许磊
Owner SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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