Polymerization inhibitor for tetrafluoroethylene
A technology of polymerization inhibitor and tetrafluoroethylene, which is applied in the preparation of halogenated hydrocarbons, disproportionation separation/purification of halogenated hydrocarbons, organic chemistry, etc., can solve the problem of preventing insufficient performance of polymerization
Active Publication Date: 2008-11-19
DAIKIN IND LTD
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Problems solved by technology
However, here, it is effective for preventing polymerization of TFE in the storage and transportation process, and has insufficient performance for preventing polymerization in the rectification process.
Method used
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Embodiment 1
[0041] 3.88g, 3.78g and 3.85g of silica gel (ヒシビードN, manufactured by Donghae Chemical Co., Ltd.) heat-treated at 150°C for 20 hours were added to three 6.9cm 3 The pressure-resistant container is decompressed and deoxygenated until the oxygen concentration reaches 0.8ppm. Next, a mixed gas (TFE / N) of TFE and nitrogen containing 5.84 molppm, 9.02 molppm and 14.91 molppm of α-terpinene (manufactured by Tokyo Chemical Industry Co., Ltd.) was added at room temperature. 2 =73.2 / 26.8), so that the pressure in the container reaches 0.51MPa. After 24 hours, the container was opened and the weight gain of the silica gel was measured. The results are shown in Table 2.
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The invention provides a polymerization inhibitor preventing the self-polymerization of TFE and not modified to macromolecule body by oxygen in a distillation step, particularly in a rectification step, of TFE. The invention provides a method of distilling tetrafluoroethylene in the presence of the polymerization inhibitor comprising a cyclohexadiene compound of the formula: R<1>-A-R<2>, wherein R<1> is a hydrocarbon group having 1 to 5 carbon atoms, R<2> is a hydrogen atom or a hydrocarbon group having 1 to 5 carbon atoms, and A is a cyclohexadiene ring. The cyclohexadiene compound is preferably alpha-terpinene or gamma-terpinene.
Description
technical field [0001] The present invention relates to a method for preventing clogging caused by self-polymerization of tetrafluoroethylene and a polymer modified product of a polymerization inhibitor in a distillation process of tetrafluoroethylene, particularly in a rectification process. Background technique [0002] In general, it is known that high-purity tetrafluoroethylene (hereinafter referred to as "TFE") is extremely easy to polymerize, and especially when a trace amount of oxygen is contained, it is known to polymerize significantly and sometimes explosively. Therefore, when storing TFE, about 100 to 10,000 ppm of polymerization inhibitors represented by terpenoids are added (US Pat. No. 2,737,533). In addition, it is disclosed that α-pinene, camphor, α-terpinene, D- Terpene mixtures such as limonene, γ-terpinene, p-cumene, terpinene, and rectification methods thereof (US Patent No. 3834996 specification). [0003] However, the polymerization preventing effect...
Claims
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IPC IPC(8): C07C21/185C07C17/386C07C17/42
Inventor 田口麻衣乙井健治高瀬义行斋藤秀哉平贺义之
Owner DAIKIN IND LTD