Preparation method of Z-1,1,1,4,4,4-hexafluoro-2-butene
What is Al technical title?
Al technical title is built by PatSnap Al team. It summarizes the technical point description of the patent document.
A Z-2, Z-1 technology, applied in Z-1, can solve the problems of pollution, corrosion, serious pollution, etc.
Active Publication Date: 2016-10-12
泉州宇极新材料科技有限公司
View PDF8 Cites 22 Cited by
Summary
Abstract
Description
Claims
Application Information
AI Technical Summary
This helps you quickly interpret patents by identifying the three key elements:
Problems solved by technology
Method used
Benefits of technology
Problems solved by technology
There are following defects in these routes: firstly, various literatures do not list the single-pass yield data of Z-1,1,1,4,4,4-hexafluoro-2-butene, and the yields given are generally The sum of the yields of Z-1,1,1,4,4,4-hexafluoro-2-butene and E-1,1,1,4,4,4-hexafluoro-2-butene, generally The yield of Z-1,1,1,4,4,4-hexafluoro-2-butene in the method is very low, while E-1,1,1,4,4,4-hexafluoro-2-butene Alkenes are very high; secondly, 1,2-dichloro-1,1,4,4,4-pentafluorobutane, 2-chloro-1,1,1,4,4,4-hexafluorobutane Or 1,1,1-trifluoro-2-bromo-2-chloroethane is the defect that the raw material price is expensive and difficult to obtain in the route of starting raw material; With 1,1-dichloro-3,3,3-three The coupling route with fluoroethane as the starting material produces a large amount of waste liquid that is difficult to recycle, and the resulting pollution is very serious; the route of hexafluoropropylene as the starting material is relatively long, and hexafluoropropylene is difficult to transport, and there is detonation. The danger of hexachlorobutadiene is that the route of starting raw material is corroded seriously, pollutes serious problem, and wherein the liquid phase system that antimony pentachloride or titanium tetrachloride and HF forms is very strong to the corrosion of equipment, and Pollution is also very serious
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
Click on the blue label to locate the original text in one second.
Reading with bidirectional positioning of images and text.
Smart Image
Examples
Experimental program
Comparison scheme
Effect test
Embodiment 1
[0063] Preparation of fluorination catalyst: Dissolve chromium nitrate in water, add precipitant ammonia water at 60°C, control the pH of the solution between 7.5 and 8.5, make it fully precipitate under stirring conditions, filter the formed slurry, and use Wash with ion water until neutral, then dry at 150°C for 12 hours to obtain chromium hydroxide. According to the mass percentages of tetravalent chromium ions and iron elements being 95% and 5%, the above-mentioned chromium hydroxide and iron hydroxide are uniformly mixed, pressed and molded to obtain a catalyst precursor, and then the catalyst precursor is placed in a nitrogen atmosphere. After calcination at 450°C for 10 hours, activate at 300°C with a mixed gas of hydrogen fluoride and hydrogen at a molar ratio of 10:1 for 10 hours, and at 300°C with a mixed gas atmosphere of chlorine and nitrogen with a molar ratio of 1:10 Oxidation for 12 hours to obtain a fluorination catalyst.
[0064] A tubular reactor made of Inc...
Embodiment 2
[0066] The same operation as in Example 1, the difference is that "according to the mass percentage of tetravalent chromium ion and iron element is 95% and 5%, the chromium hydroxide and iron hydroxide are mixed homogeneously" to "according to the tetravalent The mass percent composition of chromium ion and zinc element is 95% and 5%, chromium hydroxide and zinc hydroxide are mixed " homogeneously ", and the chlorine that oxidizes the catalyst is changed into the oxygen of the amount of equal substance, the result is shown in the table 1.
Embodiment 3
[0068] The same operation as in Example 1, the difference is that the ferric hydroxide in the fluorination catalyst precursor is changed to zinc hydroxide of equal quality and the chlorine gas that is oxidized to the catalyst is changed to the ozone of the amount of the same substance, the results are shown in Table 1.
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
Property
Measurement
Unit
boiling point
aaaaa
aaaaa
boiling point
aaaaa
aaaaa
boiling point
aaaaa
aaaaa
Login to view more
Abstract
The invention relates to a preparation method of Z-1,1,1,4,4,4-hexafluoro-2-butene, belonging to the field of chemical synthesis. The method comprises the following steps of taking hexachlorobutadiene (HCBD) as a raw material, performing gas-phase catalytic chlorination-fluoridation separation to obtain 2,3-dichlorohexafluoro-2-butene, performing liquid-phase dechlorination to obtain hexafluoro-2-butyne, and preparing the Z-1,1,1,4,4,4-hexafluoro-2-butene (Z-HFO-1336mzz) by means of performing gas-phase catalytic hydrogenation, wherein three reactions are included totally. The Z-1,1,1,4,4,4-hexafluoro-2-butene with high selectivity is obtained by means of performing catalytic hydrogenation by adopting the hexafluoro-2-butyne, and meanwhile the product is easily separated from side products and the raw material. The method disclosed by the invention has the advantages that the original raw material is easily obtained, the activity of a catalyst is high, the service life of the catalyst is long, the raw material can be recycled, and the standard of zero emissions is reached.
Description
technical field [0001] The present invention relates to a preparation method of Z-1,1,1,4,4,4-hexafluoro-2-butene (Z-HFO-1336mzz), in particular to a method starting with hexachlorobutadiene Raw materials, chlorofluorination reaction in the presence of fluorination catalyst first, then dechlorination reaction in the presence of zinc powder, and finally hydrogenation in the presence of hydrogenation catalyst to obtain Z-1,1,1,4,4,4-hexa Process for the preparation of fluoro-2-butene. Background technique [0002] Z-1,1,1,4,4,4-hexafluoro-2-butene (Z-HFO-1336mzz), with low greenhouse effect potential (GWP) and zero ozone depletion potential (ODP), It is considered to be an ideal substitute with the most potential to replace 1,1-dichloro-1-fluoroethane (HCFC-141b), and can be used as a refrigerant, blowing agent, fire extinguishing agent, etc. [0003] U.S. Patent US5463150 reported that in sulfolane solvent, 190 ° C, 1,2-dichloro-1,1,4,4,4-pentafluorobutane or 2-chloro-1,1,1...
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
Application Date:The date an application was filed.
Publication Date:The date a patent or application was officially published.
First Publication Date:The earliest publication date of a patent with the same application number.
Issue Date:Publication date of the patent grant document.
PCT Entry Date:The Entry date of PCT National Phase.
Estimated Expiry Date:The statutory expiry date of a patent right according to the Patent Law, and it is the longest term of protection that the patent right can achieve without the termination of the patent right due to other reasons(Term extension factor has been taken into account ).
Invalid Date:Actual expiry date is based on effective date or publication date of legal transaction data of invalid patent.