CN111517937B - Purification method of hexachloroacetone - Google Patents
Purification method of hexachloroacetone Download PDFInfo
- Publication number
- CN111517937B CN111517937B CN202010344242.8A CN202010344242A CN111517937B CN 111517937 B CN111517937 B CN 111517937B CN 202010344242 A CN202010344242 A CN 202010344242A CN 111517937 B CN111517937 B CN 111517937B
- Authority
- CN
- China
- Prior art keywords
- hexachloroacetone
- pentachloroacetone
- crude product
- adsorption column
- purifying
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- DOJXGHGHTWFZHK-UHFFFAOYSA-N Hexachloroacetone Chemical compound ClC(Cl)(Cl)C(=O)C(Cl)(Cl)Cl DOJXGHGHTWFZHK-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000000746 purification Methods 0.000 title abstract description 4
- RVSIFWBAGVMQKT-UHFFFAOYSA-N 1,1,1,3,3-pentachloropropan-2-one Chemical compound ClC(Cl)C(=O)C(Cl)(Cl)Cl RVSIFWBAGVMQKT-UHFFFAOYSA-N 0.000 claims abstract description 64
- 238000001179 sorption measurement Methods 0.000 claims abstract description 61
- 239000012043 crude product Substances 0.000 claims abstract description 40
- 239000003463 adsorbent Substances 0.000 claims abstract description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 15
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 14
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 7
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 7
- 239000000741 silica gel Substances 0.000 claims description 5
- 229910002027 silica gel Inorganic materials 0.000 claims description 5
- 238000005470 impregnation Methods 0.000 claims description 2
- 239000012798 spherical particle Substances 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 13
- 239000000126 substance Substances 0.000 abstract description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 13
- 239000002808 molecular sieve Substances 0.000 description 13
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 9
- 238000011049 filling Methods 0.000 description 9
- 238000004817 gas chromatography Methods 0.000 description 9
- 238000005086 pumping Methods 0.000 description 9
- 238000009835 boiling Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 4
- 238000004821 distillation Methods 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 239000011800 void material Substances 0.000 description 3
- HEDRZPFGACZZDS-MICDWDOJSA-N Trichloro(2H)methane Chemical compound [2H]C(Cl)(Cl)Cl HEDRZPFGACZZDS-MICDWDOJSA-N 0.000 description 2
- 230000003321 amplification Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/79—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The invention relates to a method for purifying hexachloroacetone, belonging to the technical field of organic chemical purification. According to the method, according to different adsorption selectivity of the adsorbent to pentachloroacetone and hexachloroacetone, pentachloroacetone impurities in the crude product of hexachloroacetone are removed to obtain hexachloroacetone with the pentachloroacetone content of less than 0.2wt%.
Description
Technical Field
The invention relates to a method for purifying hexachloroacetone, belonging to the technical field of organic chemical purification.
Background
Hexachloroacetone is a commonly used fine chemical intermediate and is mainly applied to medicines, pesticides and organic chemicals. Hexachloroacetone is prepared by direct chlorination of acetone, and a plurality of byproducts are generated in the synthesis process, mainly pentachloroacetone and acetone polycondensed chloride. Wherein, the boiling point of the acetone condensed chloride is close to 300 ℃, the difference between the boiling point of the acetone condensed chloride and the boiling point of hexachloroacetone is larger than 203 ℃, and the acetone condensed chloride can be removed by a reduced pressure distillation method; pentachloroacetone and hexachloroacetone have similar structures and physical and chemical properties, and are difficult to remove. Because the difference between the boiling point (192 ℃) of the pentachloroacetone and the hexachloroacetone is small, the difference between the pentachloroacetone and the hexachloroacetone is within 5 ℃ under the condition of reduced pressure distillation (less than or equal to 2 KPa), the pentachloroacetone is not completely separated from the hexachloroacetone, and the content of the pentachloroacetone after the reduced pressure distillation is still more than 2.0 percent. As hexachloroacetone has high boiling point, easy decomposition and strong corrosivity, the rectification method is very difficult.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for purifying hexachloroacetone, which is characterized in that pentachloroacetone impurities in a hexachloroacetone crude product are removed according to different adsorption selectivity of an adsorbent to pentachloroacetone and hexachloroacetone to obtain hexachloroacetone with the pentachloroacetone content of less than 0.2wt%.
The purpose of the invention is realized by the following technical scheme.
A method for purifying hexachloroacetone, said method comprising the steps of:
and (3) enabling the hexachloroacetone crude product with the temperature of 0-40 ℃ to pass through an adsorption column with the temperature same as that of the hexachloroacetone crude product at the flow rate of 5-40 mm/min, and removing most of pentachloroacetone in the hexachloroacetone crude product according to different adsorption selectivity of the adsorbent to the pentachloroacetone and the hexachloroacetone to obtain the hexachloroacetone with the pentachloroacetone content not more than 0.2wt%.
The adsorbent filled in the adsorption column is a molecular sieve, activated alumina or modified silica gel, and the modified silica gel is silica gel loaded with 5-10 wt% of magnesium sulfate.
The temperature of the hexachloroacetone crude product is preferably 10-20 ℃.
The hexachloroacetone crude product is hexachloroacetone containing pentachloroacetone, and the content of the pentachloroacetone is not more than 3.0wt%, preferably 0.5wt% -1.5 wt%.
The flow rate of the crude hexachloroacetone through the adsorption column is preferably 10 mm/min-15 mm/min.
The adsorbent is preferably spherical particles, and the diameter of the adsorbent is preferably 3 mm-5 mm.
The adsorbent is preferably modified silica gel, the modified silica gel is prepared by an isovolumetric impregnation method, and the silica gel is dried at 100-150 ℃ for not less than 5h after being loaded with magnesium sulfate.
Before use, the adsorbent is dried at 100-200 ℃ for not less than 5h, preferably at 150-200 ℃.
Has the advantages that:
the method removes the pentachloroacetone impurity in the crude product of the hexachloroacetone by utilizing the different adsorption selectivity of the adsorbent to the pentachloroacetone and the hexachloroacetone, has simple operation, low operation temperature, long service life of the adsorbent and easy amplification, can ensure that the content of the pentachloroacetone impurity is not more than 0.2wt percent, and the hexachloroacetone with the pentachloroacetone removed can be used as a raw material for preparing the deuterated chloroform.
Detailed Description
The present invention is further illustrated by the following detailed description, wherein the processes are conventional unless otherwise specified, and the starting materials are commercially available from a public source without further specification.
Example 1
(1) Drying a spherical 5A molecular sieve with the diameter of 3mm at 200 ℃ for 10 hours, and filling the dried molecular sieve into an adsorption column with the inner diameter of 60mm and the volume of 1L, wherein the void ratio of the 5A molecular sieve is 40%;
(2) Keeping the temperature of the adsorption column at 0 ℃, pumping the hexachloroacetone crude product (the content of pentachloroacetone impurities is 0.5 wt%) at 0 ℃ into the adsorption column from bottom to top at the flow rate of 5.5mL/min by using a plunger pump, wherein the flow rate of the hexachloroacetone crude product passing through the adsorption column is 5mm/min, and removing most pentachloroacetone in the hexachloroacetone crude product according to different adsorption selectivity of a 5A molecular sieve to the pentachloroacetone and the hexachloroacetone to obtain the high-purity hexachloroacetone.
As can be seen from the gas chromatography analysis, the content of pentachloroacetone in the high-purity hexachloroacetone is 0.13wt%.
Example 2
(1) Drying spherical beta activated alumina with the diameter of 3mm at 200 ℃ for 10h, and filling the dried spherical beta activated alumina into an adsorption column with the inner diameter of 60mm and the volume of 1L, wherein the porosity of the beta activated alumina is 40%;
(2) Keeping the temperature of the adsorption column at 0 ℃, pumping the hexachloroacetone crude product (the content of pentachloroacetone impurities is 0.5 wt%) with the temperature of 0 ℃ into the adsorption column from bottom to top at the flow rate of 5.5mL/min by using a plunger pump, wherein the flow rate of the hexachloroacetone crude product passing through the adsorption column is 5mm/min, and most of pentachloroacetone in the hexachloroacetone crude product is removed according to different adsorption selectivity of beta activated alumina on the pentachloroacetone and the hexachloroacetone to obtain the high-purity hexachloroacetone.
As can be seen from the gas chromatography analysis, the content of pentachloroacetone in the high-purity hexachloroacetone is 0.18wt%.
Example 3
(1) Drying spherical modified silica gel (prepared by an isometric immersion method, the magnesium sulfate loading is 5wt%, and the drying temperature and time are 150 ℃ and 10 hours) with the diameter of 3mm at 200 ℃ for 10 hours, and filling the dried spherical modified silica gel into an adsorption column with the inner diameter of 60mm and the volume of 1L, wherein the porosity of the modified silica gel is 40%;
(2) Keeping the temperature of the adsorption column at 0 ℃, pumping the hexachloroacetone crude product (the content of pentachloroacetone impurities is 0.5 wt%) at 0 ℃ into the adsorption column from bottom to top at the flow rate of 5.5mL/min by using a plunger pump, wherein the flow rate of the hexachloroacetone crude product passing through the adsorption column is 5mm/min, and removing most pentachloroacetone in the hexachloroacetone crude product according to different adsorption selectivity of modified silica gel to pentachloroacetone and hexachloroacetone to obtain high-purity hexachloroacetone.
As can be seen from the gas chromatography analysis, the content of pentachloroacetone in the high-purity hexachloroacetone is 0.08wt%.
Example 4
(1) Drying a spherical 5A molecular sieve with the diameter of 5mm at 100 ℃ for 10h, and filling the dried spherical 5A molecular sieve into an adsorption column with the inner diameter of 60mm and the volume of 1L, wherein the void ratio of the 5A molecular sieve is 40%;
(2) Keeping the temperature of the adsorption column at 40 ℃, pumping the hexachloroacetone crude product (the content of pentachloroacetone impurities is 3.0 wt%) with the temperature of 40 ℃ into the adsorption column from bottom to top at the flow rate of 44mL/min by using a plunger pump, wherein the flow rate of the hexachloroacetone crude product passing through the adsorption column is 40mm/min, and most of pentachloroacetone in the hexachloroacetone crude product is removed according to the different adsorption selectivity of a 5A molecular sieve to the pentachloroacetone and the hexachloroacetone, so that the high-purity hexachloroacetone is obtained.
As can be seen from gas chromatography analysis, the content of pentachloroacetone in the high-purity hexachloroacetone is 0.16wt%.
Example 5
(1) Drying spherical beta activated alumina with the diameter of 5mm at 100 ℃ for 10h, and filling the dried spherical beta activated alumina into an adsorption column with the inner diameter of 60mm and the volume of 1L, wherein the porosity of the beta activated alumina is 40%;
(2) Keeping the temperature of the adsorption column at 40 ℃, pumping the hexachloroacetone crude product (the content of pentachloroacetone impurities is 3.0 wt%) with the temperature of 40 ℃ into the adsorption column from bottom to top at the flow rate of 44mL/min by using a plunger pump, wherein the flow rate of the hexachloroacetone crude product passing through the adsorption column is 40mm/min, and removing most pentachloroacetone in the hexachloroacetone crude product according to different adsorption selectivity of beta activated alumina on pentachloroacetone and hexachloroacetone to obtain high-purity hexachloroacetone.
As can be seen from the gas chromatography analysis, the content of pentachloroacetone in the high-purity hexachloroacetone is 0.20wt%.
Example 6
(1) Drying spherical modified silica gel (prepared by an isometric immersion method, the magnesium sulfate loading capacity is 5wt%, and the drying temperature and time are 150 ℃ and 10 hours) with the diameter of 5mm at 100 ℃ for 10 hours, and filling the spherical modified silica gel into an adsorption column with the inner diameter of 60mm and the volume of 1L, wherein the porosity of the modified silica gel is 40%;
(2) Keeping the temperature of the adsorption column at 40 ℃, pumping the hexachloroacetone crude product (the content of pentachloroacetone impurities is 3.0 wt%) with the temperature of 40 ℃ into the adsorption column from bottom to top at the flow rate of 44mL/min by using a plunger pump, wherein the flow rate of the hexachloroacetone crude product passing through the adsorption column is 40mm/min, and most of pentachloroacetone in the hexachloroacetone crude product is removed according to different adsorption selectivity of modified silica gel on pentachloroacetone and hexachloroacetone to obtain high-purity hexachloroacetone.
As can be seen from the gas chromatography analysis, the content of pentachloroacetone in the high-purity hexachloroacetone is 0.11wt%.
Example 7
(1) Drying a spherical 5A molecular sieve with the diameter of 3mm at 150 ℃ for 10 hours, and filling the dried molecular sieve into an adsorption column with the inner diameter of 60mm and the volume of 1L, wherein the void ratio of the 5A molecular sieve is 40%;
(2) Keeping the temperature of the adsorption column at 15 ℃, pumping the hexachloroacetone crude product (the content of pentachloroacetone impurities is 1.0 wt%) with the temperature of 15 ℃ into the adsorption column from bottom to top at the flow rate of 16.5mL/min by using a plunger pump, wherein the flow rate of the hexachloroacetone crude product passing through the adsorption column is 15mm/min, and removing most pentachloroacetone in the hexachloroacetone crude product according to different adsorption selectivity of 5A molecular sieves on pentachloroacetone and hexachloroacetone to obtain high-purity hexachloroacetone.
As can be seen from gas chromatography analysis, the content of pentachloroacetone in the high-purity hexachloroacetone is 0.10wt%.
After the adsorption column in this example was used for 150 hours, the pentachloroacetone content in hexachloroacetone after passing through the adsorption column increased to 0.2wt%.
Example 8
(1) Drying spherical beta activated alumina with the diameter of 3mm at 150 ℃ for 10h, and filling the dried spherical beta activated alumina into an adsorption column with the inner diameter of 60mm and the volume of 1L, wherein the porosity of the beta activated alumina is 40%;
(2) Keeping the temperature of the adsorption column at 15 ℃, pumping the hexachloroacetone crude product (the content of pentachloroacetone impurities is 1.0 wt%) with the temperature of 15 ℃ into the adsorption column from bottom to top at the flow rate of 16.5mL/min by using a plunger pump, wherein the flow rate of the hexachloroacetone crude product passing through the adsorption column is 15mm/min, and most of pentachloroacetone in the hexachloroacetone crude product is removed according to different adsorption selectivity of beta activated alumina on the pentachloroacetone and the hexachloroacetone to obtain the high-purity hexachloroacetone.
As can be seen from the gas chromatography analysis, the content of pentachloroacetone in the high-purity hexachloroacetone is 0.14wt%.
After the adsorption column in this example was used for 112 hours, the pentachloroacetone content in hexachloroacetone after passing through the adsorption column increased to 0.2wt%.
Example 9
(1) Drying spherical modified silica gel (prepared by an isometric immersion method, the magnesium sulfate loading is 5wt%, and the drying temperature and time are 150 ℃ and 10 hours) with the diameter of 3mm at 150 ℃ for 10 hours, and filling the dried spherical modified silica gel into an adsorption column with the inner diameter of 60mm and the volume of 1L, wherein the porosity of the modified silica gel is 40%;
(2) Keeping the temperature of the adsorption column at 15 ℃, pumping the hexachloroacetone crude product (the content of pentachloroacetone impurities is 1.0 wt%) with the temperature of 15 ℃ into the adsorption column from bottom to top at the flow rate of 16.5mL/min by using a plunger pump, wherein the flow rate of the hexachloroacetone crude product passing through the adsorption column is 15mm/min, and most of pentachloroacetone in the hexachloroacetone crude product is removed according to different adsorption selectivity of modified silica gel on pentachloroacetone and hexachloroacetone to obtain high-purity hexachloroacetone.
As can be seen from gas chromatography analysis, the content of pentachloroacetone in the high-purity hexachloroacetone is 0.06wt%.
After the adsorption column in this example was used for 641h, the pentachloroacetone content in hexachloroacetone after passing through the adsorption column increased to 0.2wt%.
In summary, the above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A method for purifying hexachloroacetone is characterized by comprising the following steps: the method comprises the following steps of,
the temperature is 0 o C~40 o C, enabling the crude product of the hexachloroacetone to pass through an adsorption column with the temperature being the same as that of the crude product of the hexachloroacetone at the flow rate of 5 mm/min-40 mm/min to obtain the hexachloroacetone with the pentachloroacetone content being not more than 0.2 wt%;
the adsorbent filled in the adsorption column is modified silica gel, and the modified silica gel is silica gel loaded with 5wt% -10 wt% magnesium sulfate; the crude product of hexachloroacetone is hexachloroacetone containing pentachloroacetone, and the content of pentachloroacetone is not more than 3.0 wt%.
2. The method of purifying hexachloroacetone according to claim 1, wherein: the temperature of the hexachloroacetone crude product is 10 o C~20 o C。
3. The method of purifying hexachloroacetone according to claim 1, wherein: the mass fraction of pentachloroacetone in the hexachloroacetone crude product is 0.5-1.5%.
4. The method for purifying hexachloroacetone according to claim 1, wherein: the flow rate of the crude hexachloroacetone through the adsorption column is 10 mm/min-15 mm/min.
5. The method of purifying hexachloroacetone according to claim 1, wherein: the adsorbent is spherical particles.
6. The method of purifying hexachloroacetone according to claim 5, wherein: the diameter of the adsorbent is 3mm to 5mm.
7. The method for purifying hexachloroacetone according to claim 1, wherein: the modified silica gel is prepared by an isovolumetric impregnation method, and magnesium sulfate is loaded on the silica gel and then the silica gel is 100 DEG o C~150 o Drying under C to be not less than 5h.
8. The method of purifying hexachloroacetone according to claim 1, wherein: the adsorbent is used before 100 o C~200 o Drying at C is not less than 5h.
9. The method for purifying hexachloroacetone according to claim 1, wherein: the adsorbent is used before 150 deg.C o C~200 o Drying at C is not less than 5h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010344242.8A CN111517937B (en) | 2020-04-27 | 2020-04-27 | Purification method of hexachloroacetone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010344242.8A CN111517937B (en) | 2020-04-27 | 2020-04-27 | Purification method of hexachloroacetone |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111517937A CN111517937A (en) | 2020-08-11 |
| CN111517937B true CN111517937B (en) | 2022-12-09 |
Family
ID=71903291
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010344242.8A Active CN111517937B (en) | 2020-04-27 | 2020-04-27 | Purification method of hexachloroacetone |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111517937B (en) |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA842873A (en) * | 1970-05-26 | S. Chu Arthur | Purification of perhaloacetones | |
| JPS5781433A (en) * | 1980-11-11 | 1982-05-21 | Central Glass Co Ltd | Purification of hexafluoroacetone |
| US5523499A (en) * | 1992-03-10 | 1996-06-04 | E. I. Du Pont De Nemours And Company | Purification of hexafluoroethane products |
| CN102076645A (en) * | 2008-07-03 | 2011-05-25 | 阿克马法国公司 | Process for the purification of 2, 3, 3, 3-tetrafluoro-1-propene (hfo-1234yf) |
| CN102558538A (en) * | 2011-12-28 | 2012-07-11 | 湖南大学 | Deep purification method of hexafluropropylene oxide |
| CN103910599A (en) * | 2013-01-06 | 2014-07-09 | 中化蓝天集团有限公司 | Ultra-high purity hexafluoroethane preparation method |
| CN103936547A (en) * | 2014-04-30 | 2014-07-23 | 上海杰视医疗科技有限公司 | Perfluorooctane purification method |
| CN105327676A (en) * | 2014-08-11 | 2016-02-17 | 浙江蓝天环保高科技股份有限公司 | Modified adsorbent and application of same in preparation of ultra-pure hexafluoroethane |
| CN106631692A (en) * | 2016-11-16 | 2017-05-10 | 中央硝子株式会社 | Method for producing hexafluoroisopropanol and fluoromethyl hexafluoroisopropyl ether (sevoflurane) |
| CN109761776A (en) * | 2018-12-29 | 2019-05-17 | 中国船舶重工集团公司第七一八研究所 | A kind of method of purification of hexachloroacetone |
| CN109970509A (en) * | 2017-12-27 | 2019-07-05 | 浙江蓝天环保高科技股份有限公司 | A kind of method of purification of technical grade perfluoroethane |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB0031303D0 (en) * | 2000-12-21 | 2001-01-31 | Ici Plc | Process for the purification of fluoromethyl hexafluoroisopropyl ether |
-
2020
- 2020-04-27 CN CN202010344242.8A patent/CN111517937B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA842873A (en) * | 1970-05-26 | S. Chu Arthur | Purification of perhaloacetones | |
| JPS5781433A (en) * | 1980-11-11 | 1982-05-21 | Central Glass Co Ltd | Purification of hexafluoroacetone |
| US5523499A (en) * | 1992-03-10 | 1996-06-04 | E. I. Du Pont De Nemours And Company | Purification of hexafluoroethane products |
| CN102076645A (en) * | 2008-07-03 | 2011-05-25 | 阿克马法国公司 | Process for the purification of 2, 3, 3, 3-tetrafluoro-1-propene (hfo-1234yf) |
| CN102558538A (en) * | 2011-12-28 | 2012-07-11 | 湖南大学 | Deep purification method of hexafluropropylene oxide |
| CN103910599A (en) * | 2013-01-06 | 2014-07-09 | 中化蓝天集团有限公司 | Ultra-high purity hexafluoroethane preparation method |
| CN103936547A (en) * | 2014-04-30 | 2014-07-23 | 上海杰视医疗科技有限公司 | Perfluorooctane purification method |
| CN105327676A (en) * | 2014-08-11 | 2016-02-17 | 浙江蓝天环保高科技股份有限公司 | Modified adsorbent and application of same in preparation of ultra-pure hexafluoroethane |
| CN106631692A (en) * | 2016-11-16 | 2017-05-10 | 中央硝子株式会社 | Method for producing hexafluoroisopropanol and fluoromethyl hexafluoroisopropyl ether (sevoflurane) |
| CN109970509A (en) * | 2017-12-27 | 2019-07-05 | 浙江蓝天环保高科技股份有限公司 | A kind of method of purification of technical grade perfluoroethane |
| CN109761776A (en) * | 2018-12-29 | 2019-05-17 | 中国船舶重工集团公司第七一八研究所 | A kind of method of purification of hexachloroacetone |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111517937A (en) | 2020-08-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106349008A (en) | Method for purifying butadiene hexafluoride | |
| CN111517937B (en) | Purification method of hexachloroacetone | |
| EP4194431A1 (en) | Method for refining bio-based crude ethylene glycol | |
| CN113548949B (en) | Production method of 1,1,3-trichloroacetone | |
| US4092403A (en) | Process for the purification of by-product hydrogen chloride streams | |
| CN108126664B (en) | Modified molecular sieve for purifying olefin and method for removing oxygen-containing impurities in olefin by using modified molecular sieve | |
| WO2022022300A1 (en) | Preparation process for phenoxyethanol as cosmetic raw material | |
| CN102643156A (en) | Chloroethane purification process | |
| CN102432427B (en) | Preparation method of medicinal absolute ethyl alcohol | |
| CN113527042B (en) | Production process and production system of cis HFO-1234ze | |
| CN114713209B (en) | Fluoride modified adsorbent and method for purifying crude hexafluoro-1,3-butadiene | |
| JP3240043B2 (en) | Purification method of fluoromethyl-1,1,1,3,3,3-hexafluoroisopropyl ether | |
| CN109970509A (en) | A kind of method of purification of technical grade perfluoroethane | |
| KR20150133789A (en) | Purification method for dichloromethane, and production method for difluoromethane using said purification method | |
| US20060142615A1 (en) | Process for preparing ethanolamine with improved colour | |
| TW201632485A (en) | Process for producing propane, and propane production device | |
| CN112479806A (en) | Separation method of mixture of 2-chloro-3, 3, 3-trifluoropropene and 2-chloro-1, 1,1, 2-tetrafluoropropane | |
| CN112209904A (en) | Method for improving refining and aldehyde-removing efficiency of propylene oxide | |
| KR100668203B1 (en) | Absorbent for removing methanol in ethanol | |
| KR101882588B1 (en) | Method for manufacturing methylethylketone and 2,3-butanediol | |
| CN116393092B (en) | Method for separating and purifying hexafluorobutadiene and efficient adsorbent for separating and purifying hexafluorobutadiene | |
| CN111097512A (en) | Process for preparing propylene oxide | |
| CN114180525A (en) | Separation method of hydrogen chloride/dichloromethane in synthesis of 4-chloroacetoacetic acid ethyl ester | |
| CN113896615B (en) | Method for adsorbing and purifying impurities by using high-purity benzyl chloride | |
| WO2016075033A1 (en) | Process for removing a small-molecule contaminant from a chlorine compound stream |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 056027 No. 17, Exhibition Road, Handan, Hebei Patentee after: 718th Research Institute of China Shipbuilding Corp. Address before: 056027 No. 17, Exhibition Road, Handan, Hebei Patentee before: Handan Purifying Equipment Research Institute |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20231020 Address after: 056027 Hebei Province, Handan city Congtai District Exhibition Road No. 17 Patentee after: Perry Technology Co.,Ltd. Address before: 056027 No. 17, Exhibition Road, Handan, Hebei Patentee before: 718th Research Institute of China Shipbuilding Corp. |