Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Conversion method for hexachlorobutadiene

A technology for hexachlorobutadiene and butene, applied in the field of catalytic conversion of hexachlorobutadiene, can solve the problems of inability to recycle, poor thermal stability, low reactivity, etc., and achieves high industrial application prospects and thermal stability. High, low reactivity effects

Inactive Publication Date: 2019-11-01
XIAN MODERN CHEM RES INST
View PDF11 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Hexachlorobutadiene has a boiling point of 210-220°C and has a perchlorodiene structure. Its chemical properties are very stable and it is difficult to carry out chemical reactions. The existing conversion process of hexachlorobutadiene often uses chemical amounts of fluoride and hexachlorobutadiene. Diene reaction, fluoride is a one-time use, can not be recycled, poor industrial applicability
[0005] The key to the reaction between hexachlorobutadiene and anhydrous hydrogen fluoride is the design of the liquid-phase fluorination catalyst system. Due to the existence of the traditional liquid-phase fluorination catalyst antimony pentachloride, the valence state is reduced and deactivated, and the thermal stability is poor. Butadiene has low reactivity and high stability. Therefore, in order to realize the cyclic catalytic reaction of hexachlorobutadiene and anhydrous hydrogen fluoride, it is urgent to develop a liquid-phase fluorination reaction catalyst with high thermal stability, strong acidity and stability. system, patents CN 103193586B and CN 104072333B report a liquid-phase fluorination reaction of hexachlorobutadiene and anhydrous hydrogen fluoride. Although the reaction conversion rate is relatively high, it is difficult to achieve catalytic reaction due to the use of traditional metal antimony catalysts. Circulation, the use of catalysts is disposable, poor economy, and large environmental pollution; patent CN 106008147A reports a gas-phase fluorination reaction of hexachlorobutadiene and anhydrous hydrogen fluoride, although the reaction conversion rate is high, but the product selectivity is poor , short catalyst life, etc.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Conversion method for hexachlorobutadiene
  • Conversion method for hexachlorobutadiene
  • Conversion method for hexachlorobutadiene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 45 grams of alum pentoxide, 50 grams of anhydrous hydrogen fluoride, 20 grams of potassium fluoride and 10 grams of anhydrous sulfuric acid into a 300mL stainless steel belt stirred autoclave. Vacuum to remove excess water.

[0020] Add 52 grams of hexachlorobutadiene and 40 grams of anhydrous hydrogen fluoride into the kettle, then raise the temperature to 150°C for 3-4 hours, control the pressure at 1.5-1.7 MPa, and collect the discharged material with a cold trap.

[0021] The product is detected by NMR, and the data are as follows:

[0022] 1 H NMR (500MHz, CDCl 3 )δ6.64(q,1H,J=6.5Hz);

[0023] 13 C NMR (500MHz, CDCl 3 )δ132.0(qq, J=39.3Hz, J=5.4Hz), 121.9(q, J=37.5Hz), 120.6(q, J=270Hz), 119.1(q, J=272.5Hz);

[0024] 19 F NMR (470MHz, CDCl 3 )δ-71.3(m, CF 3 ),-61.3(m, CF 3 ).

[0025] The above data prove that the product obtained is 2-chloro-1,1,1,4,4,4-hexafluoro-2-butene.

Embodiment 2～8

[0027] Examples 2-8 Prepare 2-chloro-1,1,1,4,4,4-hexafluoro-2-butene according to the same preparation method in Example 1, the difference is that the catalyst in Example 1 is Alum pentoxide, and the ratio of telomerization in Examples 2 to 8 is titanium dioxide, niobium pentoxide, tantalum pentoxide, titanium tetrachloride, alum pentachloride, niobium pentachloride, and tantalum pentachloride. The reaction results of Examples 2-8 are shown in Table 1.

[0028] Table 1 Catalyst Screening

[0029] Example catalyst Conversion rates(%) selectivity (%) 2 TiO 2

Embodiment 9～13

[0031] Examples 9 to 13 were prepared according to the same preparation method in Example 1, 2-chloro-1,1,1,4,4,4-hexafluoro-2-butene, the difference is that the catalyst Agent is potassium fluoride, and in embodiment 9~13, be respectively tripropylamine, tributylphosphine, potassium bisulfate, potassium chlorosulfonate, potassium benzenesulfonate. The reaction results of Examples 9-13 are shown in Table 2.

[0032] Table 2 Screening of catalytic promoters

[0033] Example Catalyst Conversion rates(%) selectivity (%) 9 Tripropylamine 65.1 81.1 10 Tributylphosphine 61.3 72.3 11 Potassium bisulfate 78.2 80.1 12 Potassium chlorosulfonate 80.3 83.0 13 Potassium benzenesulfonate 78.5 73.4

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a catalysis conversion method for a pollutant hexachlorobutadiene. The method comprises the following steps: by taking hexachlorobutadiene and anhydrous hydrogen fluoride as raw materials, and in the presence of a liquid-phase fluorination catalyst and a catalytic addictive, performing synthesis, so as to obtain 2-cholo-1,1,1,4,4,4-hexafluoro-2-butene. The invention provides a green conversion method for pollutants, and mainly aims to catalysis conversion of the hexachlorobutadiene.

Description

technical field [0001] The invention relates to a method for converting pollutants, in particular to the catalytic conversion of hexachlorobutadiene. Background technique [0002] Environmental problems such as water pollution have become one of the challenges of human existence. Hexachlorobutadiene, a by-product produced during the industrial production of perchlorethylene, is one of ten water pollutants and will cause serious damage to water and soil. As human beings pay more and more attention to environmental issues such as water quality, it is urgent to find transformation solutions for such pollutants. [0003] Hexachlorobutadiene has a boiling point of 210-220°C and has a perchlorodiene structure. Its chemical properties are very stable and it is difficult to carry out chemical reactions. The existing conversion process of hexachlorobutadiene often uses chemical amounts of fluoride and hexachlorobutadiene. Diene reaction, fluoride is disposable, cannot be recycled, a...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/21C07C21/18
CPCC07B2200/09C07C17/21C07C21/18
Inventor 赵波吕剑曾纪珺韩升杨志强唐晓博郝志军亢建平李凤仙张伟
Owner XIAN MODERN CHEM RES INST
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com