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Large-steric-hindrance structure perfluoromacromolecule modifier and preparation method thereof

A technology of large steric hindrance and macromolecules, which is applied in the field of perfluorinated macromolecular modifiers and preparations with large steric hindrance structures, and can solve problems such as performance degradation of modified products, defluorination of fluorine atoms, and influence on the use of modifiers. Achieve the effect of increasing the action time, improving the performance of the polymer, and being easy to industrial production

Inactive Publication Date: 2019-06-11
SOUTHWEST JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the preparation of fluoropolymers usually adopts two different routes, one is through the polymerization of perfluoromonomers, and the other is through the modification of polymers by fluorination; for the polymerization of perfluoromonomers In general, it is easy to be enriched on the surface of the blend, resulting in a decrease in the properties of the modified product; while the method of modifying and modifying by adding fluorine atoms, the main disadvantage is that the fluorine atoms will be defluorinated during actual use, which affects Modifier use

Method used

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  • Large-steric-hindrance structure perfluoromacromolecule modifier and preparation method thereof
  • Large-steric-hindrance structure perfluoromacromolecule modifier and preparation method thereof
  • Large-steric-hindrance structure perfluoromacromolecule modifier and preparation method thereof

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preparation example Construction

[0027] A preparation method of a perfluorinated macromolecular modifier with a large steric hindrance structure, comprising the following steps:

[0028] Step 1: Dissolve 30 parts of perfluoro-tert-butanol in toluene, add acrylic acid, add 5-10 parts of cation exchange resin, and add 5-10 parts of imidazolium salt ion solution, mix completely, and react at 60°C Obtain fluorine-containing acrylate monomer in 40 minutes; wherein the amount of acrylic acid is greater than the amount of perfluoro-tert-butanol;

[0029] Step 2: Add 10 parts of azobisisobutyronitrile to the solution obtained in step 1, and heat until the solution is refluxed. After the solution becomes turbid, add polymerization inhibitor ST-2, and stop heating;

[0030] Step 3: Put the mixed solution obtained in step 2 to stand for stratification, remove the lower layer solution, and the upper layer solution can be reused after vacuum rotary evaporation;

[0031] Step 4: Chromatographic separation, the desired pro...

Embodiment 1

[0044] Follow the steps below to prepare a branched fluorine-containing modifier for polymers:

[0045] (1) To prepare fluorine-containing monomer, dissolve 3 parts of perfluoro-tert-butanol in toluene solution, add 5 parts of acrylic acid, 0.5 part of cation exchange resin, and 0.5 part of imidazolium salt ionic liquid, mix well and heat the mixed solution to 60 °C, react for 40 minutes, and obtain fluorine-containing acrylate monomer after fully reacting.

[0046] (2) Polymerization of fluorine-containing monomers, add 1 part of azobisisobutyronitrile to the mixed solution prepared in step (1), heat the solution to reflux, react until the solution becomes turbid, add polymerization inhibitor ST-2, stop heating.

[0047] (3) Preliminary purification, the mixed solution is left to stand for stratification, the lower layer solution is taken out of the separatory funnel, and the upper layer solution can be reused after vacuum rotary evaporation.

[0048] (4) The mixed solution...

Embodiment 2

[0052] Follow the steps below to prepare a branched fluorine-containing modifier for polymers:

[0053] (1) To prepare fluorine-containing monomers, dissolve 3 parts of perfluoro-tert-butanol in toluene solution, add 5 parts of acrylic acid, 1 part of cation exchange resin, and 1 part of imidazolium salt ionic liquid, mix well and heat the mixed solution to 60 °C, react for 40 minutes, and obtain fluorine-containing acrylate monomer after fully reacting.

[0054] (2) Polymerization of fluorine-containing monomers, add 1 part of azobisisobutyronitrile to the mixed solution prepared in step (1), heat the solution to reflux, react until the solution becomes turbid, add polymerization inhibitor ST-2, stop heating.

[0055] (3) Preliminary purification, the mixed solution is left to stand for stratification, the lower layer solution is taken out of the separatory funnel, and the upper layer solution can be reused after vacuum rotary evaporation.

[0056] (4) The mixed solution in...

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Abstract

The invention discloses a large-steric-hindrance structure perfluoromacromolecule modifier and a preparation method thereof. The preparation method comprises the following steps: step 1: dissolving 30parts of perfluoro-tert-butanol in toluene, adding acrylic acid, adding 5-10 parts of cation exchange resin, adding 5-10 parts of imidazolium salt ion solution, and conducting full mixing and full reaction to obtain a fluorine-containing acrylate monomer, wherein the amount of the acrylic acid is greater than the amount of the perfluoro-tert-butanol; step 2: adding 10 parts of azobisisobutyronitrile to the solution obtained in the step 1, conducting heating for refluxing of the solution, adding a polymerization inhibitor when the solution becomes turbid, and stopping heating; step 3: conducting standing for layering of the mixed solution obtained in the step 2, and getting a lower-layer solution; and step 4: conducting chromatographic separation and purification, so as to obtain a desiredproduct. According to the invention, the action time of the modifier in the polymer is increased, and the polymer performance is improved; and the preparation method is simple in process control, strong in anti-crystallization enrichment, and easy for industrial production. .

Description

technical field [0001] The invention relates to the technical field of modifiers and preparations, in particular to a perfluorinated macromolecular modifier with a large steric hindrance structure and a preparation method. Background technique [0002] Many functions of polymer materials often need to be expressed through the surface of the material, so the research on the surface properties of polymer materials has attracted widespread attention; in order to improve the performance of polymers, coating materials, etc., surface modification There are a lot of methods, but many methods have complex process conditions, which are easy to cause side reactions, and will lead to the destruction of the material itself; adding surface modifiers to achieve surface modification, simple process, and wide application range have become the focus of research in recent years. [0003] Fluorine-containing polymer is a surface modifier that has been studied more in recent years. Due to the s...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/653C08F220/24C08F230/08C08G77/442
Inventor 张林樊小强蔡振兵朱旻昊陈多礼严涵
Owner SOUTHWEST JIAOTONG UNIV