Purifying method for propanol tetrafluoride

A technology of tetrafluoropropanol and a purification method, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problem of the quality decline of discs, the inability to use tetrafluoropropanol as a pharmaceutical intermediate, and the difficulty in achieving high purity. and other problems to achieve the effect of easy removal

Inactive Publication Date: 2005-10-19
ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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AI Technical Summary

Problems solved by technology

Although the above method can be used to remove the above-mentioned ether impurities, it is difficult to remove unsaturated aldehyde impurities such as formaldehyde, tetrafluoropropionaldehyde, trifluoropropionaldehyde, octafluorovaleraldehyde, etc. Alcohol content is low, it is difficult to achieve a high purity of more than 99%
[0012] The methods described in the above-mentioned prior art are all difficult to completely remove the impurities in tetrafluoropropanol, so that the purity of tetrafluoropropanol cannot rise to a high level of more than 99.9%.
When this low-purity tetrafluoropropanol is used to produce CD-R / DVD-R discs for recording electronic information, the quality of the discs will be reduced and the quality will be reduced.
In the field of pharmaceutical synthesis, this tetrafluoropropanol containing ether and aldehyde impurities cannot be used to produce pharmaceutical intermediates

Method used

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  • Purifying method for propanol tetrafluoride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 2

[0047] Repeat the operation process of Example 1. When the pressure drop reaches 150, do not lower the temperature of the reactor, but instead raise the temperature, and at the same time, intermittently add tetrafluoroethylene monomer for 3 times during the heating process, until the temperature is raised to 140°C, and kept at this temperature for 1 hour . Cool the reaction kettle to room temperature and discharge. The reaction mixture was analyzed for residual initiator levels below the detection limit.

[0048] At room temperature, 80 g of sodium thiosulfate was added to the reaction crude product.

[0049] The reaction mixture was purified and fractionated to obtain tetrafluoropropanol with a purity of more than 99.5%, and the calculated yield was 89.3%.

[0050] During the refining process, the collected tetrafluoropropanol fractions with a purity of more than 99.99% accounted for about 22.7% of the total tetrafluoropropanol collected.

Embodiment 3-6

[0052] Repeat the operation process of Example 2. Only different initiators or acid absorbing agents are used in different embodiments, and different reaction conditions are adopted according to the different initiators used. In the later stage of the reaction, different ways of adding tetrafluoroethylene monomer are adopted, the added amount is different, and the added stabilizer is also different. The specific situation is as follows:

[0053] Table 3-6 List of responses

[0054]

[0055] Note: TFE, TFP, DTBP, and IPP are English abbreviations for tetrafluoroethylene, tetrafluoropropanol, di-tert-butyl peroxide, and diisopropyl peroxydicarbonate, respectively.

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Abstract

The present invention discloses propanol tetrafluoride purifying method and is especially method of eliminating residual initiator and active impurity from telomerized coarse alcohol product obtained through the intermittent telomerization between ethylene tetrafluoride and methanol. After telomerization to produce telomerized coarse alcohol product, the reaction temperature is raised to 50-180 deg.c, more ethylene tetrafluoride monomer is further led into the reactor, and after maintaining the temperature for 0.5-5 hr, stabilizer is added to form neutral or weak alkali mixture. Then, the mixture is rectified continuously at normal pressure, residual methanol is recovered, and the intermediate fractions are eliminated, so as to obtain propanol tetrafluoride with purity as high as 99.9 %.

Description

technical field [0001] The invention relates to a method for purifying tetrafluoropropanol, in particular to a method for removing residual initiators and active impurities from crude telomer alcohol obtained through intermittent telomerization of tetrafluoroethylene and methanol. Background technique [0002] Tetrafluoropropanol is non-flammable, non-toxic, non-corrosive and excellent lubricity. It is a new type of fluorine-containing solvent. Because of its good solubility, fast gasification speed and low toxicity, it is widely used as CD- R / DVD-R pigment solvent; also widely used in pharmaceuticals, pesticides, dyes, fine chemical intermediates, photographic color fillers, fabric finishing agents, fluorine-containing resins, processing aids for perfluororubber and cleaning agents for electronic products . As a cleaning agent, it has excellent cleaning performance and has important uses in microelectronics and optoelectronics. It has no destructive effect on the atmospher...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/80C07C31/38
Inventor 张在利曾子敏陈立义李斌吴长根徐世章孙凌云
Owner ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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