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Purification method of 3,3,4,4,5,5-hexafluorocyclopentene
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A technology of hexafluorocyclopentene and a purification method, which is applied in the field of purification of chemical products
Active Publication Date: 2017-08-25
BEIJING YUJI SCI & TECH +1
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But up to now, there is no report about extracting and rectifying separation to reduce c-HCFO-1426 content to obtain high-purity c-HFO-1436
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Embodiment 1
[0033] Using an extractive rectification tower with a diameter of 100mm equipped with an ε-ring packing, the c-HFO-1436 product containing 5.0% c-HCFO-1426 (mass percentage) is passed through an extractive distillation column operating at an absolute pressure of about 0.1 MPa. Distillation tower for processing. The c-HFO-1436 / c-HCFO-1426 mixture is added from the bottom of the rectification tower, the extractant (a mixture of o-dichlorobenzene and hexyl acetate with a mass ratio of 4:1) is added from the middle of the tower, and the extractive rectification tower The kettle temperature is controlled at about 110°C, and the reflux ratio is about 10. The gas phase components were extracted from the top of the tower, and the fraction at 70-71°C was collected to obtain the c-HFO-1436 product. The collected c-HFO-1436 product was analyzed by gas chromatography, and the results are shown in Table 2.
Embodiment 2
[0035] The same operation as in Example 1, except that the extractant was changed to a mixture of o-dichlorobenzene and hexyl acetate at a mass ratio of 2:1, the results are shown in Table 2.
Embodiment 3
[0037] The same operation as in Example 1, except that the extractant was changed to a mixture of o-dichlorobenzene and hexyl acetate at a mass ratio of 1:1, the results are shown in Table 2.
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Abstract
The invention relates to a purification method of 3,3,4,4,5,5-hexafluorocyclopentene, and belongs to the field of chemical synthesis. The purification method of 3,3,4,4,5,5-hexafluorocyclopentene is characterized in that a material contains a 1-chloro-3,3,4,4,5,5-hexafluorocyclopentene impurity, the method is an extraction and rectification method, a mixture containing chlorobenzene or 1,2-dichlorohexafluorocyclopentene and liquid acetate with the boiling point being higher than 100DEG C is adopted as an extractant, a mass ratio of the chlorobenzene or 1,2-dichlorohexafluorocyclopentene to the acetate is 4:1-1:2, and a mass ratio of the extractant to the material is 1-20:1. The special mixed extractant is adopted in the invention, the content of 1-chloro-3,3,4,4,5,5-hexafluorocyclopentene in the extracted, rectified and purified product is smaller than 0.10%, and the extractant residual amount is smaller than 50ppm, so the 3,3,4,4,5,5-hexafluorocyclopentene product accords with practical requirements.
Description
technical field [0001] The present invention relates to a kind of purification method of 3,3,4,4,5,5-hexafluorocyclopentene, especially relate to from 3,3,4,4,5,5-hexafluorocyclopentene (hereinafter referred to as c -HFO-1436) and 1-chloro-3,3,4,4,5,5-hexafluorocyclopentene (hereinafter referred to as c-HCFO-1426) mixture, which belongs to the chemical industry Product purification technology field. Background technique [0002] 3,3,4,4,5,5-Hexafluorocyclopentene (c-HFO-1436) does not contain chlorine and has no damaging effect on the atmospheric ozone layer. Alternatives to hydrochlorofluorocarbons (HCFCs) and are used in cleaning agents. However, in all these applications, the purity of c-HFO-1436 is required to be above 99.9%. However, in several current production methods of c-HFO-1436, according to different synthetic routes, 1,2-dichlorohexafluorocyclopentene (c-CFO-416), 1-chloro- 3,3,4,4,5,5-hexafluorocyclopentene (c-HCFO-1426) and other by-products. These by-pr...
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