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Preparation method of polychlorotrifluoroethylene resin

A polychlorotrifluoroethylene and trifluorochloroethylene technology, which is applied in the field of fluororesin modification, can solve the problems of unstable product performance, unfavorable post-processing, cumbersome reaction process, etc., and achieves improved strength loss time and mechanical properties, The effect of shortening polymerization time and not easy to degrade and discolor

Active Publication Date: 2017-11-07
SHANDONG HUAXIA SHENZHOU NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, a large amount of organic reagents are used, which is not conducive to post-treatment. At the same time, the reaction process is cumbersome (continuous feeding in stages), and has high requirements for operation.
[0007] Therefore, it is necessary to study a kind of polymerization method of chlorotrifluoroethylene, and prepare polychlorotrifluoroethylene resin with excellent performance in an efficient and environmentally friendly manner, so as to solve the complicated process, long reaction time, The disadvantages of industrial production such as unstable product performance and unfavorable environmental protection

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Accurately weigh 500g of high-purity water in a clean and dry beaker, control the water temperature at 12°C±1°C, weigh 3.2g of potassium dihydrogen phosphate, 5.0g of sodium bisulfite and 7.8g of potassium persulfate into the beaker containing high-purity water, and at the same time Accurately weigh and add 4.8g of sodium dimethyldithiocarbamate, fully stir and mix, transfer the mixed solution to a clean reaction kettle through negative pressure, and use high-purity argon to vacuumize the reaction kettle to remove oxygen. Turn on the magnetic stirrer to 500r / min, connect the reactor to the chlorotrifluoroethylene cylinder, and add 980g of chlorotrifluoroethylene monomer to the reactor. Raise the temperature of the reaction kettle to 30°C, control the reaction temperature to 30°C±1°C, stir and react for 6 hours, stop the reaction, release the pressure, and take out the powdered polychlorotrifluoroethylene resin.

[0035] After washing with high-purity water, drying, and ...

Embodiment 2

[0042]Accurately weigh 650g of high-purity water into a clean and dry beaker, control the water temperature at 12°C±1°C, weigh 5.0g of potassium dihydrogen phosphate, 3.6g of potassium bisulfite and 8g of potassium persulfate into the beaker containing high-purity water, stir well Mix until completely dissolved, at the same time accurately weigh and add 6.0g of sodium dibenzyl dithiocarbamate, transfer the mixed solution to a clean reaction kettle under negative pressure, and use high-purity argon to vacuumize the reaction kettle to remove oxygen. Turn on the magnetic stirrer to 800r / min, connect the reactor to the chlorotrifluoroethylene cylinder, and add 1020g of chlorotrifluoroethylene monomer to the reactor. Raise the temperature of the reactor to 35°C, control the reaction temperature to 35°C±1°C, stir the reaction for 3 hours, stop the reaction, release the pressure, and take out the bead-shaped polychlorotrifluoroethylene resin with a diameter of 1-2 mm.

[0043] After...

Embodiment 3

[0046] Accurately weigh 600g of high-purity water in a clean and dry beaker, control the water temperature at 12°C±1°C, weigh 4.4g of potassium dihydrogen phosphate, 8g of sodium bisulfite and 4.8g of ammonium persulfate into the beaker containing high-purity water, stir well While mixing, accurately weigh and add 6.7g of sodium di-n-butyldithiocarbamate, transfer the mixed solution to a clean reactor by negative pressure, and use high-purity argon to vacuumize the reactor to remove oxygen. Turn on the magnetic stirrer to 300r / min, connect the reactor to the chlorotrifluoroethylene cylinder, and add 850g of chlorotrifluoroethylene monomer to the reactor. Raise the temperature of the reaction kettle to 50°C, control the reaction temperature to 50°C±1°C, stir and react for 7 hours, stop the reaction, release the pressure, and take out the powdered polychlorotrifluoroethylene resin.

[0047] After washing with high-purity water, drying, and weighing to obtain 773g of product, the...

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Abstract

The invention relates to a preparation method of polytrifluorochloroethylene resin and belongs to the technical field of fluororesin modification. According to the preparation method of the polytrifluorochloroethylene resin, a pH buffering agent and a molecular weight modifier are added to a solvent, and trifluorochlor oethylene is triggered to be subjected to a polymerization reaction in the presence of a redox initiator. The preparation method is simple in process, environmentally friendly and moderate in reaction, and saves energy, and the prepared polytrifluorochloroethylene resin has low molecular weight distribution, long strength loss time and stable melt indexes.

Description

technical field [0001] The invention relates to a preparation method of polychlorotrifluoroethylene resin, belonging to the technical field of fluororesin modification. Background technique [0002] Polychlorotrifluoroethylene (PCTFE) is a homopolymer of monomer chlorotrifluoroethylene, the molecular formula is (CF2-CClF)n, it is a transparent resin with low permeability, cold flow resistance, abrasion resistance and radiation resistance , has high mechanical strength and rigidity, and is widely used in coatings, pump valves, packaging materials (films), cables, low-temperature sealing, medical equipment, electronic components, etc. It also plays an irreplaceable role in aerospace and other aspects, and is an important fluorine-containing resin. [0003] Chinese patent application CN 103304712 A discloses a manufacturing method of bead-shaped polychlorotrifluoroethylene resin. The method uses an oil-soluble initiator and an organic dispersant to prepare polychlorotrifluoroe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F114/24C08F2/38C08F2/10C08F4/40
CPCC08F2/10C08F2/38C08F4/40C08F114/24
Inventor 王汉利张琳涵王军
Owner SHANDONG HUAXIA SHENZHOU NEW MATERIAL
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