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Method for preparing polytetrafluoroethylene resin for coating

The technology of polytetrafluoroethylene and phase tetrafluoroethylene is applied in the field of preparation of polytetrafluoroethylene resin, which can solve the problems of ultra-fast polymerization reaction speed, decreased yield, and reduced crystallinity of copolymer, and achieves the promotion of uniform alternating reaction. , The effect of improving construction performance and eliminating performance loss

Active Publication Date: 2011-09-07
ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Chinese Patent Publication No. CN1244556A discloses a quaternary copolymer with chlorotrifluoroethylene as the main body, which introduces carboxyl functional groups, which solves the shortcomings of poor dispersion and wettability of fluorine coating resins when making paint, and is prone to paint defects. It also has the problem of poor alcohol resistance; and in order to effectively reduce the crystallinity of the copolymer, when selecting non-fluorinated vinyl compounds, copolymerization of isomeric vinyl esters and vinyl esters with tetrafluoroethylene, linear carbon-carbon The alternation of the copolymerization components of the main chain can be more evenly distributed on the long chain of the macromolecule, giving uniform solubility, but it is still not very ideal
But it still does not solve the problem of poor solubility (high degree of copolymer crystallinity) of the fluorine-containing monomer copolymer, and the solid content is low, the hardness of the coating film is poor, and the gloss is low
[0006] Chinese Patent Publication No. CN101323653A discloses a coating resin, which uses vinyl tertiary carbonate (VV9, VV10) as a comonomer to alternately polymerize with tetrafluoroethylene; in addition, it is also pointed out in the patent application that in tetrafluoroethylene When ethylene-type fluorocarbon coating resin is polymerized, since the reaction between vinyl acetate itself is much faster than the reaction speed between vinyl acetate and tetrafluoroethylene, it is difficult to realize the alternate polymerization between two different monomers, which affects the It is made of fluorine-containing paint coating film aging resistance
However, if the reaction temperature is too high and the temperature rise rate is too fast, the yield will decrease, and the obtained product will turn yellow and the color will deepen; on the other hand, if the reaction temperature is too high and the temperature rise rate is too fast, the decomposition rate of the initiator will increase sharply. , will make the polymerization reaction speed super fast and out of control, the chain termination reaction will be accelerated, the molecular weight of the product (film-forming resin) will decrease, and the viscosity of the product resin will be extremely low, resulting in various disadvantages in the preparation of coatings

Method used

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  • Method for preparing polytetrafluoroethylene resin for coating

Examples

Experimental program
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Effect test

Embodiment 1

[0032] 1) Add 66kg of mixed solvent of butyl acetate and 24kg of methyl isobutyl ketone, 44kg of vinyl acetate, 8kg of allyl alcohol, and 2.5kg of undecylenic acid into the polymerization reactor; cool the reactor to 15°C, and evacuate And replace with nitrogen 3 to 4 times;

[0033] 2) When the vacuum degree in the kettle reaches 0.095MPa, add gas-phase tetrafluoroethylene monomer until the pressure in the kettle rises by 0.03MPa (gauge pressure), and analyze the oxygen content. When the oxygen content in the kettle system is ≤ 30ppm, it is qualified; Azodiisobutyronitrile was dissolved in butyl acetate to make a dilute solution with a concentration of 4% by weight, and the above-mentioned solution was pumped into the reactor with a constant flow rate of 4L / h with a metering pump, and then the agitator was started;

[0034] 3) Raise the temperature and pressure of the reactor to the first constant point, that is, the temperature is 65±1°C, and the pressure is 0.9±0.05MPa (gau...

Embodiment 2

[0045] Add each polymerizable monomer according to the amount shown in Table 1, and carry out the polymerization reaction according to the preparation method of Example 1, wherein, during the polymerization process, the initiator is continuously added at a constant flow rate of 5 L / h. When the temperature and pressure of the reactor rise to the first constant point, the temperature is 55±1°C, and the pressure is 1.0±0.05MPa (gauge pressure); when the amount of additional tetrafluoroethylene monomer is consumed to about 1 / 3, the reactor The temperature and pressure rise to the second constant point, the temperature is 70±1°C, and the pressure is 1.5±0.05MPa (gauge pressure); when the amount of additional tetrafluoroethylene monomer is consumed to about 2 / 3, the temperature and pressure of the reactor Rising to the third constant point, the temperature is 80±1°C, the pressure is 2.0±0.05MPa (gauge pressure), when the amount of tetrafluoroethylene monomer added is the rated amount...

Embodiment 3

[0047] The polymerized monomers were added in the amounts shown in Table 1, and the preparation process was the same as in Example 1. The performance test of the prepared product was performed, and the results are shown in Table 1.

[0048] Table 1 Formula and performance test (unit: kg)

[0049]

[0050] As can be seen from Table 1, the polytetrafluoroethylene resin for coatings prepared by the method of the present invention is colorless and transparent in appearance, between 3 ± 0.5 in chroma, high in fluorine content, and excellent in solubility to solvents. According to the fluorine content of the resin, products with different fluorine content can be provided according to the market demand of different application fields of the resin, and the application development of the potential market can be broadened.

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Abstract

The invention provides a method for preparing polytetrafluoroethylene resin for coating. Gas phase tetrafluoroethylene, vinyl acetate, undecylenic acid and allyl alcohol are taken as polymerization monomers for performing polymerization, an initiating agent is continuously added in the whole polymerization process, and polymerization is performed under an isothermal isobaric condition. The methodfor preparing the polytetrafluoroethylene resin for coating provided by the invention can promote the vinyl acetate and the tetrafluoroethylene to uniformly and alternately react, thereby preparing the polytetrafluoroethylene resin for coating with good solubility, high fluorine content and resistance to chemical corrosion; the prepared resin is colorless and transparent and is improved from matte gloss to high gloss to fully embody the color of the coated film; and performance loss of the resin caused by introduction of exogenous impurities is eliminated, the coated film has recoatability, and the workability is greatly improved. The polymerization process is stable and can meet the requirements of industry scalization.

Description

technical field [0001] The invention relates to a preparation method of polytetrafluoroethylene resin, in particular to a preparation method of alternate polymerization resin of tetrafluoroethylene and vinyl acetate. Background technique [0002] Polytetrafluoroethylene resin for coatings refers to the chain segment linear polymer material containing tetrafluoroethylene as the main film-forming material. The macromolecular chain segment or end of this material has hydroxyl, carboxyl or ester comonomers. Compared with other fluorine-containing olefins and other fluorine-containing monomers, the fluorine content of tetrafluoroethylene monomer ranks first. The fluorine-containing resin for coatings prepared by using tetrafluoroethylene monomer has high fluorine content. Compared with coatings prepared from other fluorine-containing vinyl resins, it has better weather resistance, corrosion resistance, and solvent resistance. [0003] Different fluorine-containing monomers have ...

Claims

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Application Information

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IPC IPC(8): C08F214/26C08F218/08C08F210/14C08F216/08C09D127/18
Inventor 张建新胡显权何炯姚权卫
Owner ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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