Polychlorotrifluoroethylene resin preparation method

The technology of polychlorotrifluoroethylene and chlorotrifluoroethylene is applied in the field of preparation of fluorine-containing polymer materials, which can solve problems such as performance deterioration, pollution, and aggravate PCTFE degradation, and achieve good processability and good heat resistance. Effect

Inactive Publication Date: 2010-02-10
CHANGSHU XINHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] PCTFE is polymerized from chlorotrifluoroethylene (CTFE) as a raw material. In order to obtain PCTFE with sufficient molecular weight to meet the needs of practical applications, a redox initiator system is usually used to polymerize at 0-60 ° C. The oxidant of the initiator system It is persulfate or organic peroxide, and the reducing agent is sodium bisulfite or sodium metabisulfite. The actual polymerization reaction is often more than 30 hours, and the conversion rate of chlorotrifluoroethylene is 60-90%. Although the obtained PCTFE has a strength loss temperature exceeding 260°C (indicating a higher molecular weight), but there are unstable end groups on the molecular chain, which are easily degraded at a processing temperature of 240-280°C, resulting in performance deterioration and severe discoloration
[0006] U.S. Patents US2613202, US2689241 and US5453477 all disclose the preparation of PCTFE, add transition metal ions such as iron ions as accelerato

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0021] Example 1-11:

[0022] The polymerization reaction is carried out in a 10L vertical stainless steel polymerization reactor with stirring. The amount of deionized water, chlorotrifluoroethylene (CTFE), surfactant and initiator, polymerization temperature, polymerization pressure and polymerization time, CTFE conversion rate , The ZST value of PCTFE and the mass loss of the degradability test are shown in Table 1. In Examples 1-11, the surfactant is a perfluorosurfactant, specifically potassium perfluorobutyl sulfonate (KFBS) is used, and the initiator is An organic initiator with a half-life of 0.1-10h at 10-50°C is specifically selected as diisopropyl peroxydicarbonate (IPP).

[0023] After the polymerization reactor is deoxidized, add deionized water and surfactant. The stirring speed of the polymerization reactor is 350n / min. The temperature in the reactor is controlled to the set (designated) temperature, and the porous silica gel adsorption treatment is added. CTFE gas,...

Example Embodiment

[0031] Example 12-14:

[0032] The surfactant potassium perfluorobutyl sulfonate (KFBS) in Examples 1-11 was replaced with ammonium perfluorohexanoate (Example 12), ammonium perfluoroalkyloxonanoate (Example 13) and all Sodium fluorononoxybenzene sulfonate (Example 14), polymerization time, CTFE conversion rate, ZST value of PCTFE and quality value of degradability test are shown in Table 2, and the other conditions are the same as those implemented in Examples 1-11 of Table 1. Examples 1-3, that is, the remaining conditions of Example 12 correspond to Example 1, and the remaining conditions of Example 13 correspond to Example 2 and the remaining conditions of Example 14 correspond to Example 3. The content not mentioned in this embodiment 12-14 is the same as the description of embodiment 1-11.

[0033] Table 2

[0034]

Example Embodiment

[0035] Examples 15-17:

[0036] The initiator diisopropyl peroxydicarbonate (IPP) in Examples 1-11 was replaced with diisobutyryl peroxide (Example 15) and isobutyl peroxide neodecanoate ( Example 16) and diperfluoropropionyl peroxide (Example 17), polymerization time, CTFE conversion rate, PCTFE ZST value and degradability test quality value are shown in Table 3, and other conditions are the same as shown in Table 1. Examples 4-6 in Examples 1-11, namely: the remaining conditions of Example 15 correspond to Example 4, the remaining conditions of Example 16 correspond to Example 5 and the remaining conditions of Example 17 correspond to Example 6. The content not described in Examples 15 to 17 is the same as the description of Examples 1-11.

[0037] table 3

[0038] Example

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PUM

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Abstract

The invention provides a polychlorotrifluoroethylene resin preparation method, belonging to the technical field of the preparation of fluoropolymer material. The method comprises the following steps:firstly purifying polytrifluorochloroethylene, then adopting deionized water as medium and using initiator to performing chlorotrifluoroethylene polymerization in the presence of surfactant and obtaining polychlorotrifluoroethylene resin. The invention has the advantage that the polymerization reaction time is shortened to less than 10h, the conversion rate of chlorotrifluoroethylene reach above 90%, the obtained polychlorotrifluoroethylene resin has good heat resistance and processability and degradation and metachromatism can not appear under the processing temperature of 240-280 DEG C. Therefore, the method can meet the demand of industrialized production.

Description

technical field [0001] The invention belongs to the technical field of preparation of fluorine-containing polymer materials, and in particular relates to a preparation method of polychlorotrifluoroethylene resin. Background technique [0002] Polychlorotrifluoroethylene resin (PCTFE) is a thermoplastic with high added value and high performance. As a high-end product, it is often used in harsh environments where other materials cannot be used. When in contact with liquid oxygen, liquid nitrogen and liquefied natural gas, PCTFE has outstanding anti-brittle properties, excellent gas barrier characteristics, and is not affected by ultraviolet and gamma ray radiation. Among refrigerants, PCTFE has outstanding creep resistance characteristics, so it can be used for load bearing parts contacting refrigerant. [0003] PCTFE can be processed by common processes such as injection molding, extrusion, molding and transfer molding. PCTFE is mainly used to make parts of ultra-cold ref...

Claims

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Application Information

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IPC IPC(8): C08F114/24C08F2/44C08F4/34
Inventor 陶惠平杨斌徐俊德
Owner CHANGSHU XINHUA CHEM
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