Supercharge Your Innovation With Domain-Expert AI Agents!

Preparation method of E-1,1,1,4,4,4-hexafluoro-2-butene

A technology of butene and Z-1, applied in the field of E-HFO-1336mzz, can solve the problems of runaway reaction, easy gasification, difficult safe operation, etc., and achieve the effects of easy raw materials, high conversion rate and easy reaction

Active Publication Date: 2018-11-02
泉州宇极新材料科技有限公司
View PDF10 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0021] The above-mentioned prior art has the following problems: firstly, the raw materials of the first route are not easy to obtain, and the liquid phase method is adopted, a large amount of solvent is used, and a large amount of waste liquid and waste solid are produced; secondly, the raw materials of the second route are not easy to obtain, and the yield is low. Second, the yield of the third route is low; the fourth route is not only low in yield, but also easily produces a large amount of waste liquid and waste solid; the yield of the fifth route is too low; the sixth route Mid-ultraviolet irradiation is difficult to control, and the yield is low; the yield of ultraviolet irradiation in the seventh route is too low, and the method of using aluminum chlorofluoride as a catalyst is also difficult to control, Z-1, 1, 1, 4, 4, 4 - The boiling point of hexafluoro-2-butene is 33-33.5°C (760mmHg), which is very close to the reaction temperature (10°C to 24°C). It is easy to gasify and cause the reaction to go out of control. The above liquid phase method is difficult to achieve large-scale continuous production. E -1,1,1,4,4,4-hexafluoro-2-butene
The sulfur tetrafluoride used in the eighth route is a highly toxic substance, which is difficult to handle safely, and the yield of the target product is low

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
  • Preparation method of E-1,1,1,4,4,4-hexafluoro-2-butene
  • Preparation method of E-1,1,1,4,4,4-hexafluoro-2-butene
  • Preparation method of E-1,1,1,4,4,4-hexafluoro-2-butene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] 10 ml of commercially available activated carbon (Shirasagi C2x7 / 12 activated carbon, Osaka Gas Chemicals Co. Ltd.) was charged into a tubular reactor made of Inconium alloy with an inner diameter of 1 / 2 inch and a length of 30 cm. The reaction conditions are as follows: the reaction temperature is raised to 400° C., the contact time of Z-1,1,1,4,4,4-hexafluoro-2-butene is 15 s, and the reaction pressure is 0.1 MPa. After running for 10 hours, the reaction product was collected and heated, and the gas phase organic phase was taken for GC analysis. The reaction result is: the conversion rate of Z-1,1,1,4,4,4-hexafluoro-2-butene is 99.5%, E-1,1,1,4,4,4-hexafluoro-2 - The selectivity to butene was 98.8%.

Embodiment 2

[0049] The catalyst AlF that 10 milliliters of above-mentioned methods are prepared is filled in the tubular reactor made of Incon alloy of inner diameter 1 / 2 inch, long 30cm 3 . The reaction conditions are as follows: the reaction temperature is raised to 400° C., the contact time of Z-1,1,1,4,4,4-hexafluoro-2-butene is 15 s, and the reaction pressure is 0.1 MPa. After running for 10 hours, the reaction product was collected and heated, and the gas phase organic phase was taken for GC analysis. The reaction result is: the conversion rate of Z-1,1,1,4,4,4-hexafluoro-2-butene is 99.3%, E-1,1,1,4,4,4-hexafluoro-2 - The selectivity to butene was 98.4%.

Embodiment 3

[0051] The catalyst AlF that 10 milliliters of above-mentioned methods are prepared is filled in the tubular reactor made of Incon alloy of inner diameter 1 / 2 inch, long 30cm 3 . The reaction conditions are as follows: the reaction temperature is raised to 300° C., the contact time of Z-1,1,1,4,4,4-hexafluoro-2-butene is 15 s, and the reaction pressure is 0.1 MPa. After running for 10 hours, the reaction product was collected and heated, and the gas phase organic phase was taken for GC analysis. The reaction result is: the conversion rate of Z-1,1,1,4,4,4-hexafluoro-2-butene is 73.1%, E-1,1,1,4,4,4-hexafluoro-2 - The selectivity to butene was 99.2%.

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 preparation method of E-1,1,1,4,4,4-hexafluoro-2-butene. The preparation method comprises the following step: in the presence of a catalyst, performing an isomerization reaction on Z-1,1,1,4,4,4-hexafluoro-2-butene to obtain the E-1,1,1,4,4,4-hexafluoro-2-butene, wherein the catalyst is activated carbon or metal fluoride. By the technical method provided by the invention,a raw material is easy to obtain, the conversion rate is high, and the reaction is easy to control; a reaction mixture is purified by distillation, a product is obtained on the tower top and can be further purified, and the raw material in a tower kettle can be recycled into a reactor, so that continuous mass production of the E-1,1,1,4,4,4-hexafluoro-2-butene is achieved.

Description

technical field [0001] The present invention relates to a gas phase preparation of E-1,1,1,4,4,4-hexafluoro-2-butene (E-HFO-1336mzz), in particular to a kind of Z-1,1,1,4 , 4,4-hexafluoro-2-butene (Z-HFO-1336mzz) as a raw material, in the presence of a catalyst isomerization reaction to obtain E-HFO-1336mzz method. Background technique [0002] Up to now, various documents have disclosed eight routes for the synthesis of E-1,1,1,4,4,4-hexafluoro-2-butene. [0003] The first route is the elimination method. Literature [A.I.Burmakov, L.A.Motnyak, B.V.Kunshenko, L.A.Alekseeva, L.M.Yagupolskii, Journal of Organic Chemistry USSR (English Translation), 1980,16,1204-1209.] reported 1,1,1,4,4,4-6 Fluorobutan-2-ol is eliminated in the presence of sulfur tetrafluoride to obtain E-1,1,1,4,4,4-hexafluoro-2-butene, Z-1,1,1,4,4 , 4-hexafluoro-2-butene and 1,1,1,2,4,4,4-heptafluorobutane, wherein, E-1,1,1,4,4,4-hexafluoro-2 - The yield of butene was only 37%. See reaction (1) for the ...

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
IPC IPC(8): C07C17/358C07C21/18
CPCC07B2200/09C07C17/358C07C21/18
Inventor 张呈平董利张妮贾晓卿权恒道
Owner 泉州宇极新材料科技有限公司
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More