CN101225015B - Monochloropentafluoroethane and pentafluoroethane secondary extraction technology - Google Patents
Monochloropentafluoroethane and pentafluoroethane secondary extraction technology Download PDFInfo
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- CN101225015B CN101225015B CN2008100138980A CN200810013898A CN101225015B CN 101225015 B CN101225015 B CN 101225015B CN 2008100138980 A CN2008100138980 A CN 2008100138980A CN 200810013898 A CN200810013898 A CN 200810013898A CN 101225015 B CN101225015 B CN 101225015B
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Abstract
The invention discloses a re-extraction process for chloropentafluoroethane and pentafluoroethane, belonging to the technical field of pentafluoroethane, comprising a processing step that the chloropentafluoroethane is essentially removed from the crude pentafluoroethane with chloropentafluoroethane via extraction and distillation. The re-extraction process for chloropentafluoroethane and pentafluoroethane is characterized in that: through a re-extraction for the top of the distillation column, chloropentafluoroethane essentially free of chloropentafluoroethane is acquired from the crude chloropentafluoroethane at the top of the extraction and distillation column, and a mixture of the chloropentafluoroethane and extraction solvent is gained at the bottom of the column; high-concentration chloropentafluoroethane is acquired through distillation; the extraction solvent is applied for recycle use; any one or mixture of any two from nitroethane, isohexane, n-hexane, and nitromethane serves as the extraction solvent; the reflux ratio for the re-extraction distillation is between two and six. The re-extraction distillation is carried out for the extracted and distilled crude matters at the column, and high purity R115 and R125 are acquired, thereby the enrichment problems of R115 in the system are solved.
Description
Technical field
The invention belongs to the pentafluoride ethane technical field, be specifically related to an a kind of chloropentafluoroethane and pentafluoride ethane reextraction technology.
Background technology
At pentafluoride ethane (HFC-125, abbreviation R125) in the production, can produce a chloropentafluoroethane (CFC-115, be called for short R115), and HFC-125 is when using as refrigeration agent, and the content of CFC-115 must be lower than 0.5%, during particularly use in cryogenic refrigeration agent composition field, wish that HFC-125 has low-down CFC-115 content, is about 100ppm usually.In treating process, HFC-125 and CFC-115 can form azeotropic mixture, only depend on the conventional distillation technology to be difficult to thorough separation.In the industry, usually adopt extraction rectification technique, promptly add solvent as extraction agent in mixed solution, wherein a component is dissolved in extraction agent, strengthened the relative volatility of two components in the raw material, the system that makes azeotrope or boiling point differ very little still can separate with rectificating method.
At present, Da Jin, Dupont aspect in this regard all carried out further investigation, the patent (number of applying for a patent CN95195569.1 as the acquisition in 1997 of Daikin Industrial Co., Ltd, name is called: the manufacture method of pentafluoride ethane), promptly provide the method for effectively being isolated HFC-125 by the mixture of HFC-125 and CFC-115.Promptly be to use the dichloro pentafluoropropane, zellon, methyl alcohol, ethanol, propyl alcohol, butanols, five fluorine propyl alcohol, C3-Fluoroalcohol, acetone, hexanaphthene, pentamethylene, trieline, tetracol phenixin, octane, the oil benzoline, sherwood oil, diethyl ether, Nitromethane 99Min. is made extraction agent, the mixture that will contain HFC-125 and CFC-115 formation carries out extractive distillation, generate the HFC-125 of high density, obtain CFC-115 as overhead product, obtain the mixture of HFC-125 and extraction agent as the residual thing of tower, this mixture is by distillation, extraction agent is separated with HFC-125, this extraction agent is re-used in extractive distillation.
Publication number is that the Chinese patent of CN1295995A discloses a kind of method of separating the purification pentafluoride ethane by extracting rectifying from C2ClF5/pentafluoride ethane mixture, it is characterized in that using pimelinketone, acetonitrile, Nitromethane 99Min., mix ketone or pure ester mixture as extraction agent, enrichment the extraction liquid of pentafluoride ethane must make with extra care pentafluoride ethane as tower bottoms through simple distillation.
" separation method of HFC-125 and CFC-115 " (Lou Fangbiao " fine chemistry industry " the 23rd the 8th phase of volume of August in 2006) carries out organic acid, alcohols, ester class, ketone, ethers, nitrile and alkanes (comprising halogenated alkane and Nitromethane 99Min.); Starve and compare and test.The concrete kind of the extraction agent of its open test has: acetate, ethanol, propyl carbinol, ethyl acetate, butylacetate, mixed ester, acetone, pimelinketone, mixed ketone, ether, acetonitrile, Nitromethane 99Min., normal hexane, hexanaphthene, trifluorobichloroethane, methylene dichloride, a fluorine ethylene dichloride, ethanol mix ester.The result shows, the best results that acetone, pimelinketone, Nitromethane 99Min., acetonitrile, mixed ketone and ethanol mix ester.
" extracting and refining of fluoric ether " (Korea S celebrating " Zhejiang chemical industry " article numbering in 2004: 1006-4184 (2004) 09-0020-02) also disclose similar extraction agent and disclose the boiling range of extracting rectifying.Its relevant content is quoted at this.
No matter above-mentioned prior art still is the data that obtain in the suitability for industrialized production as laboratory test data, though can obtain meeting the HFC-125 product of quality standard, cat head CFC-115 content can't further separate less than 10%.This material is the recirculation enrichment in system, has both influenced the HFC-125 purification, can't deviate to meet the CFC-115 of commodity purity requirement again from system, and general enterprise can only regularly deviate from these mixtures and give it up from system, cause the waste of the energy and resource.
Summary of the invention
To isolate content too low for the CFC-115 that solves the mixture extraction rectifying of HFC-125 and CFC-115 in the prior art, can't continue isolating problem, the applicant carries out repetition test and screening on the prior art basis, develop compound extraction agent, has solved the problems referred to above.
The following technical scheme of the concrete employing of the present invention:
An a kind of chloropentafluoroethane and pentafluoride ethane reextraction technology, comprise that the pentafluoride ethane crude product that includes a chloropentafluoroethane obtains not containing in essence the processing step of the pentafluoride ethane of a chloropentafluoroethane through one-time extractive rectification, it is characterized in that, the chloropentafluoroethane crude product that described one-time extractive rectification cat head produces is through reextraction rectifying, obtain not containing in essence the pentafluoride ethane of a chloropentafluoroethane by the reextraction rectifying tower top, obtain the mixture of the extraction agent of a chloropentafluoroethane and reextraction rectifying at the bottom of the tower, described mixture through distill high density one chloropentafluoroethane, the extraction agent of reextraction rectifying recycles; The extraction agent of described reextraction rectifying is the one or any two kinds mixture in nitroethane, nitroethyl alcohol, isohexane, normal hexane or the nitropropane; The reflux ratio of described reextraction rectifying is 2～6;
The consumption of the extraction agent of reextraction rectifying of the present invention is: a chloropentafluoroethane and extraction agent add according to weight ratio 1: 2～6;
The purity that can access of this technical scheme is that 99.8% pentafluoride ethane and purity are 99.5% 1 chloropentafluoroethane.
The technology of one-time extractive rectification of the present invention is same as the prior art.
Compared with prior art, beneficial effect of the present invention is:
1) the present invention has finished separating fully of R-115 and R-125, and has reached purity requirement separately respectively; Product HFC-125 purity of the present invention is 99.8%, and the purity of byproduct CFC-115 can reach 99.55;
2) extraction agent of the present invention can be increased to the relative volatility of R125 and R115 about 2.7 in reextraction rectifying, and this just can finish separating of R115 and R125 smoothly.
Description of drawings
Fig. 1 is the process flow diagram of prior art;
Fig. 2 is the process flow diagram of the embodiment of the invention.
Among the figure, 1 is the one-time extractive rectification tower, and 2 is the R125 rectifying tower, and 3 is the reextraction rectifying tower, and 4 is the R115 rectifying tower, and 5 is condenser, and 6 is reboiler, and 7 is the R125 storage tank, and 8 is R115 crude product storage tank, and 9 is the R115 storage tank.
Embodiment
Comparative Examples (prior art)
As shown in Figure 1, the R125 crude product is added by one-time extractive rectification tower 1 middle part, extraction agent is by adding near one-time extractive rectification tower 1 top, the impurity material of enrichment is flowed out by cat head, the bottom stream material is extraction agent and product, this material enters R125 rectifying tower 2, and qualified product R125 is refluxed by R125 rectifying tower 2 tops and obtains, and R125 rectifying tower 2 bottoms obtain the extraction agent that can recycle.
The cat head impurity material of prior art also can add the R125 crude product and recycle.
Embodiment
As shown in Figure 2, the R125 crude product is added by one-time extractive rectification tower 1 middle part, and extraction agent is by adding near one-time extractive rectification tower 1 top; The bottom stream material is extraction agent and product, and this material enters R125 rectifying tower 2, and qualified product R125 is refluxed by R125 rectifying tower 2 tops and obtains, and R125 rectifying tower 2 bottoms obtain the extraction agent that can recycle.Above-mentioned process is an one-time extractive rectification.
The impurity material collection of one-time extractive rectification tower 1 cat head enrichment is added by reextraction rectifying tower 3 middle parts in R115 crude product storage tank 8, and extraction agent is by adding near reextraction rectifying tower 3 tops; Reextraction rectifying tower 3 cats head obtain qualified R125 product, enter R125 storage tank 7, and the R125 in the storage tank 7 gets qualified product through molecular sieve dehydration; Obtain to such an extent that R115 and extraction agent must mix material and enter R115 rectifying tower 4 middle parts at the bottom of reextraction rectifying tower 3 towers, after the rectifying, R115 rectifying tower 4 tops obtain qualified R115 product, enter R115 storage tank 9; The extraction agent of R115 rectifying tower 4 bottoms recycles.Said process is reextraction rectifying.
The extraction agent of secondary rectifying is the one or any two kinds mixture in nitroethane, nitroethyl alcohol, isohexane, normal hexane or the nitropropane; The reflux ratio of reextraction rectifying is 2～6; According to pentafluoride ethane or a chloropentafluoroethane and extraction agent weight ratio 1: 2～6 interpolation extraction agents.
The purity of the product R125 of present embodiment is 99.8%, and the purity of byproduct R115 is 99.5%.
Claims (1)
1. chloropentafluoroethane and pentafluoride ethane reextraction technology, comprise that the pentafluoride ethane crude product that includes a chloropentafluoroethane obtains not containing in essence the processing step of the pentafluoride ethane of a chloropentafluoroethane through one-time extractive rectification, it is characterized in that, the chloropentafluoroethane crude product that described one-time extractive rectification cat head produces is through reextraction rectifying, obtain not containing in essence the pentafluoride ethane of a chloropentafluoroethane by the reextraction rectifying tower top, obtain the mixture of the extraction agent of a chloropentafluoroethane and reextraction rectifying at the bottom of the tower, described mixture through distill high density one chloropentafluoroethane, the extraction agent of reextraction rectifying recycles; The extraction agent of described reextraction rectifying is the one or any two kinds mixture in nitroethane, nitroethyl alcohol, isohexane, normal hexane or the nitropropane; The reflux ratio of described reextraction rectifying is 2～6;
The consumption of the extraction agent of described reextraction rectifying is: a chloropentafluoroethane and extraction agent add according to weight ratio 1: 2～6;
The purity of described high density one chloropentafluoroethane is 99.5%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008100138980A CN101225015B (en) | 2008-01-25 | 2008-01-25 | Monochloropentafluoroethane and pentafluoroethane secondary extraction technology |
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| CN2008100138980A CN101225015B (en) | 2008-01-25 | 2008-01-25 | Monochloropentafluoroethane and pentafluoroethane secondary extraction technology |
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| CN101225015A CN101225015A (en) | 2008-07-23 |
| CN101225015B true CN101225015B (en) | 2011-07-20 |
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| CN109053366B (en) * | 2018-09-18 | 2019-10-11 | 福建省清流县东莹化工有限公司 | A kind of purifying process of a chloropentafluoroethane |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1295995A (en) * | 1999-11-10 | 2001-05-23 | 浙江省化工研究院 | Process for purifying pentafluoroethane |
| CN100999438A (en) * | 2007-01-04 | 2007-07-18 | 西安近代化学研究所 | Purification method of pentafluoro ethane |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1295995A (en) * | 1999-11-10 | 2001-05-23 | 浙江省化工研究院 | Process for purifying pentafluoroethane |
| CN100999438A (en) * | 2007-01-04 | 2007-07-18 | 西安近代化学研究所 | Purification method of pentafluoro ethane |
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Inventor after: Ming Wenyong Inventor after: Duan Qi Inventor after: Liu Dong Inventor after: Wang Ruiying Inventor after: Yan Yi Inventor before: Shi Wenyong Inventor before: Duan Qi Inventor before: Liu Dong Inventor before: Wang Ruiying Inventor before: Yan Yi |
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Free format text: CORRECT: INVENTOR; FROM: SHI WENYONG DUAN QI LIU DONG WANG RUIYING YAN YI TO: MING WENYONG DUAN QI LIU DONG WANG RUIYING YAN YI |