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Dipolythiohexafluoroacetone production device and production process

A technology for dimerization of thiohexafluoroacetone and a production device, which is particularly applied in the field of corrosion resistance, can solve the problems of low conversion rate of hexafluoropropylene, difficult waste liquid treatment, low product purity and the like, and achieves durability. and safety guarantee, short reaction time and high product purity

Active Publication Date: 2022-03-01
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Aiming at the problems existing in the prior art, the object of the present invention is to provide a kind of production device and production technology thereof of dimer thiohexafluoroacetone, the present invention adopts Using hexafluoropropylene as raw material, using a tank-type reaction device with a corrosion-resistant coating, and equipped with a green production process such as a temperature controller and a heat exchanger, the durability and safety are guaranteed. After crystallization, water washing and rectification Combined with the purification method used to obtain a dimeric thiohexafluoroacetone product with a yield of more than 95% and a purity of more than 99%, it can effectively solve the high temperature and high pressure requirements in the prior art, high energy consumption, potential safety hazards, waste liquid Difficult handling, low conversion rate of hexafluoropropylene, and low product purity provide an industrialized production process

Method used

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  • Dipolythiohexafluoroacetone production device and production process
  • Dipolythiohexafluoroacetone production device and production process
  • Dipolythiohexafluoroacetone production device and production process

Examples

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Effect test

Embodiment 1

[0034] 1. Dimerized thiohexafluoroacetone production device

[0035] Refer to attached figure 1 , Dimerized thiohexafluoroacetone production device consists of solvent storage tank 1, hexafluoropropylene storage tank 2, catalyst storage tank 3, sulfur raw material storage tank 4, reaction kettle 5, cooling crystallization kettle 6, water washing kettle 7, rectification tower 8. Solvent recovery tank 9, solid recovery tank 10, product storage tank 11;

[0036] The outer wall of the reaction kettle 5 is provided with a heating jacket around the outer wall, a solvent inlet 51, a hexafluoropropylene inlet 52, a catalyst inlet 53, and a sulfur raw material inlet 54 are arranged on the top, an air inlet 55 and an exhaust outlet 56 are arranged on the side, and a A liquid outlet 57 and a solid outlet 58 are provided with a stirring device 59 and a temperature monitoring device 510 inside; the outer wall of the cooling crystallization kettle 6 is provided with a cooling and heating l...

Embodiment 2～5

[0051] In Example 1, step 2) material ratio, preheating temperature in the reactor, hexafluoropropylene ventilation rate, reaction temperature, reaction pressure, reaction time; step 3) crystallization temperature, crystallization time, and washing times are respectively changed into As shown in Table 1, other operations are the same as in Example 1, and the purity and yield of the obtained dimeric thiohexafluoroacetone are shown in Table 1.

[0052] Process synthesis under different equipment and reaction conditions in table 1

[0053]

Embodiment 6

[0055]18L of the cooling residual liquid collected in step 3) of the solvent recovery tank 9 of Example 1 is directly used as a solvent, and 2 L of dimethylformamide is added to make up 20 L as a solvent. Meanwhile, the sulfur solid in the solid recovery tank 10 is heated at 80° C. After drying under vacuum for 4 hours, the obtained 2.0 kg of recovered sulfur was used as part of the sulfur raw material, and 13.30 kg of sublimed sulfur was supplemented as the sulfur raw material. Other operations were the same as in Example 1. The purity of dimeric thiohexafluoroacetone was 99.3%, and the yield was 95.5%. Table 2 shows the impact of recycling times on the yield.

[0056] Table 2 Solvent and the impact of the recycling number of sulfur solids on the product yield

[0057]

[0058] As can be drawn from Table 2, the mechanical application times of solvent and sulfur solid have little effect on the reaction yield, and the solvent and raw materials recovered and reused can be rec...

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Abstract

The invention discloses a dimeric thiohexafluoroacetone production device and a production process, which adopt a kettle type reaction device which takes hexafluoropropylene as a raw material and is provided with a corrosion-resistant coating, and are provided with a temperature controller, a heat exchanger and the like, so that the durability and the safety are guaranteed, and the production efficiency is improved. The dimeric thiohexafluoroacetone product with the yield of 95% or above and the purity of 99% or above is obtained through a purification method combining crystallization, water washing and rectification, and the problems that in the prior art, the requirements for high temperature and high pressure are met, energy consumption is large, potential safety hazards exist, waste liquid treatment is difficult, the conversion rate of hexafluoropropylene is not high, and the purity of the product is low can be effectively solved. The solvent and the sulfur solid recovered after separation and purification can be continuously used for the subsequent preparation process, the conversion rate of the hexafluoropropylene raw material is greatly improved, meanwhile, the treatment cost of the waste liquid is reduced, and the method is simple in process route and device, short in reaction time, high in product purity, environmentally friendly and suitable for industrial application.

Description

(1) Technical field [0001] The invention belongs to the technical field of fine organic fluorine chemistry, and relates to a high-yield, high-purity dimeric thiohexafluoroacetone production device and production process, in particular to a corrosion-resistant reactor as a reactor, reaction raw materials and solvents It can be recycled and reused, and the device and process for producing high-yield and high-purity dimerized thiohexafluoroacetone are produced after high-efficiency purification by the purification method of crystallization, water washing and rectification. (2) Background technology [0002] Dimeric thiohexafluoroacetone (2,2,4,4-tetrakis(trifluoromethyl)-1,3-dithietane) is an important fluorine-containing intermediate, which can be used to prepare hexafluoroacetone and Its hydrates and other fluorine-containing fine chemicals. It is a colorless transparent liquid at room temperature, volatile and has a pungent odor. When the purity is high, a colorless solid c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J19/18B01J19/00B01J4/02B01J4/00B01D9/02B01D3/14C07D331/04
CPCB01J19/18B01J19/0053B01J4/02B01J4/001B01D9/00B01D3/14C07D331/04B01J2219/00006
Inventor 陈爱民刘鹏榕陈亚军陶澄钰李信宋蔚昌
Owner ZHEJIANG UNIV OF TECH
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