CN103694082A - Method for purifying tetrafluoro propanol - Google Patents
Method for purifying tetrafluoro propanol Download PDFInfo
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- CN103694082A CN103694082A CN201310613589.8A CN201310613589A CN103694082A CN 103694082 A CN103694082 A CN 103694082A CN 201310613589 A CN201310613589 A CN 201310613589A CN 103694082 A CN103694082 A CN 103694082A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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Abstract
The invention discloses a method for purifying tetrafluoro propanol. The method comprises the following steps: (1) rectifying crude tetrafluoro propanol in a first rectification tower to obtain a distillate and a tower bottom liquid, and sending the tower bottom liquid into a second rectification tower for vacuum distillation; (2) circulating a tower bottom liquid of the second rectification tower back to the inlet of the first rectification tower; (3) sending a distillate from the second rectification tower into a third rectification tower for atmospheric rectification to obtain a distillate and a tower bottom liquid; (4) sending the tower bottom liquid from the third rectification tower into a fourth rectification tower for atmospheric rectification to obtain a distillate and a tower bottom liquid, circulating the tower bottom liquid back to the inlet of the first rectification tower, adjusting the pH value of the distillate to 7-10 with alkaline substances and sending the distillate into a fifth rectification tower; and (5) recycling the tower bottom liquid of the fifth rectification tower back to the inlet of the first rectification tower, and collecting the distillate from the fifth rectification tower to obtain the tetrafluoro propanol product. The invention has the advantages of good product quality, simple process, green and environment-friendliness.
Description
Technical field
The invention belongs to C3-Fluoroalcohol technical field, be specifically related to a kind of method of purification of C3-Fluoroalcohol.
Background technology
C3-Fluoroalcohol have do not fire, nontoxic, non-corrosiveness and good oilness, be a kind of novel containing fluorous solvent, because its solvability is good, gasification rate fast, low toxin, be widely used as the pigment solvent of CD-R/DVD-R; Also be widely used in medicine, agricultural chemicals, dyestuff, fine-chemical intermediate, photograph color the make up the difference processing aid of agent, fabric finishing agent, fluorine resin, FFKM and the clean-out system of electronic product.C3-Fluoroalcohol has remarkable cleaning performance as clean-out system, has its important purposes in microelectronics and photoelectronics, and it without destruction, is a kind of substitute of fluorine Lyons clean-out system of excellence to atmospheric layer.But the value segments such as medicine, electronics are high to the purity requirement of C3-Fluoroalcohol, and general requirement is more than 99.95%.
The method of suitability for industrialized production C3-Fluoroalcohol is as follows at present:
First methyl alcohol and initiator are added to reaction system, then by adding tetrafluoroethylene monomer, the system stagnation pressure of making remains on a preset value, carries out telomerization.Reaction is undertaken by following formula:
nCF
2=CF
2+CH
30H→H(CF
2CF
2)
nCH
20H
After reaction finishes, the crude product obtaining is the mixture of the telomeric alcohol of different polymerization degree, and wherein, the telomeric alcohol of n=1 is C3-Fluoroalcohol.In the product that the method obtains, major part is the telomeric alcohol of n≤4, but still the telomeric alcohol that contains a certain amount of n >=3, and in some situation, the content of these unwanted telomeric alcohols is up to 30%.
In addition, carry out as stated above telomerization, in product, also remain undecomposed initiator.Along with the difference of its kind and consumption, difference is generally 0.2%-2.0% to the residual quantity of initiator.These residual initiators can decompose in follow-up treating process, generate fluorine-containing ether material, as tetrafluoro propyl group tertbutyl ether, octafluoro amyl group tertbutyl ether etc., and aldehydes nonsaturation impurity, as formaldehyde, tetrafluoro propionic aldehyde, trifluoro propionic aldehyde, octafluoro valeral etc., these impurity are owing to forming azeotrope or Azeotrope-like with C3-Fluoroalcohol, be difficult to remove by rectifying separation, to have influence on the purity of C3-Fluoroalcohol, limited it and at electronics, medicine etc., product purity has been required the application in high field.
In order to improve the purity of C3-Fluoroalcohol, expand its Application Areas, people have carried out large quantity research:
As set forth following purification process in European patent EP 0967193 A2: after C3-Fluoroalcohol telomerization finishes, reacting coarse product is processed with alkali, and then carries out rectifying; Or directly carry out common steaming rectifying after adding alkali mixing.Yet, owing to containing certain density residual initiator in reacting coarse product, will impel the decomposition of these initiators after adding alkali, decompose the free radical producing and cause occurring multiple side reaction, generate and be above-mentionedly difficult to the fluorine-containing ether material that separation is removed, and aldehydes nonsaturation impurity.Although the method still can be removed for unsaturated aldehydes impurity, bad to fluorine-containing ethers separating substances, gained C3-Fluoroalcohol purity is many below 99%.
And for example European patent EP 0968989 A2 has considered the impact of residual initiator for rectifying, has focused on the method for removing residual initiator, as high-temperature decomposition, acid catalyst decomposition method, reductive agent decomposition method, ultraviolet light degradation method and caustic leaching process.Although use above method can remove above-mentioned ethers impurity,, for unsaturated aldehydes impurity, as formaldehyde, tetrafluoro propionic aldehyde, trifluoro propionic aldehyde, octafluoro valeral etc. are difficult to remove, therefore, the content of rectifying gained C3-Fluoroalcohol is on the low side, is difficult to reach more than 99% high purity.
And for example Chinese patent CN1683294A discloses a kind of method of purification of C3-Fluoroalcohol, it is under the prerequisite of initiator and acid-acceptor existence, to carry out after telomerization generation crude telomeric alcoholate at tetrafluoroethylene and methyl alcohol, temperature of reaction is risen to 50-180 ℃, continuation passes into tetrafluoroethylene monomer in reactor, insulation 0.5-5 hour, then add stablizer to form neutrality or weakly alkaline mixture, again this mixture is carried out to normal pressure continuous rectification, first reclaim remaining methyl alcohol, then remove middle runnings, finally can obtain purity is more than 99.9% C3-Fluoroalcohol, weak point is that technique is loaded down with trivial details, in production process, can produce a large amount of waste water, add stablizer oxidation-reduction quality material, easily produce new impurity, increase the difficulty of separating-purifying.
Summary of the invention
The present invention has overcome the defect of prior art, provides that a kind of good product quality, technique are simple, the method for purification of the C3-Fluoroalcohol of environmental protection.
In order to address the above problem, the technical solution used in the present invention is: a kind of method of purification of C3-Fluoroalcohol, comprises the following steps:
(1) thick C3-Fluoroalcohol being inputted in the first rectifying tower, is first rectifying under 60～80 ℃ of conditions at normal pressure and tower top temperature, obtains distillate and tower bottoms, and tower bottoms is inputted to Second distillation column;
(2) controlling Second distillation column tower top temperature is 70～110 ℃, and vacuum tightness is that 15～25KPa carries out rectification under vacuum, obtains distillate and tower bottoms, and by distillate input the 3rd rectifying tower, tower bottoms loops back the first rectifying tower import;
(3) controlling the 3rd rectifying tower tower top temperature is 80～106 ℃, and pressure is that normal pressure carries out rectifying, obtains distillate and tower bottoms, by tower bottoms input the 4th rectifying tower;
(4) controlling the 4th rectifying tower tower top temperature is 107～109 ℃, and pressure is that normal pressure carries out rectifying, obtains distillate and tower bottoms, and tower bottoms is looped back to the first rectifying tower import, and it is 7～10 rear input the 5th rectifying tower that distillate is adjusted to pH value with alkaline matter;
(5) controlling the 5th rectifying tower tower top temperature is 107～109 ℃, and pressure is that normal pressure carries out rectifying, obtains distillate and tower bottoms, and tower bottoms is looped back to the first rectifying tower import, collects distillate and obtains C3-Fluoroalcohol product.
Further:
By recycle after distillate rectifying step (1) Suo Shu.
By recycle after distillate rectifying step (3) Suo Shu.
The described alkaline matter of step (4) is preferably sodium methylate or sodium hydroxide.
In the present invention the first rectifying tower be mainly utilize methyl alcohol in thick C3-Fluoroalcohol and C3-Fluoroalcohol and on a small quantity the different principle of relative volatility of other components carry out rectifying, thereby reclaim the excessive methyl alcohol of not participating in reaction.At normal pressure and tower top temperature, be rectifying under 60～80 ℃ of conditions, obtain distillate and tower bottoms, distillate is thick methyl alcohol, using after its rectifying as the raw material recycle of synthetic C3-Fluoroalcohol.
In the present invention, Second distillation column is to be mainly to carry out rectification under vacuum under 70～110 ℃ of conditions at vacuum tightness 15～25Pa and tower top temperature, mainly to utilize the C3-Fluoroalcohol principle different from the relative volatility of a small amount of other components to carry out rectifying, the distillate obtaining is thick C3-Fluoroalcohol, entered the 3rd rectifying tower, the high liquid that boils of tower reactor enters the first rectifying tower and recycles.
In the present invention the 3rd rectifying tower be utilize methyl alcohol and C3-Fluoroalcohol and on a small quantity the different principle of relative volatility of other components carry out rectifying, further remove a small amount of methyl alcohol of taking out of in Second distillation column decompression process.At normal pressure and tower top temperature, be rectifying under 80～106 ℃ of conditions, obtain distillate and tower bottoms, distillate is thick methyl alcohol, using after its rectifying as the raw material recycle of synthetic C3-Fluoroalcohol, tower bottoms enters the 4th rectifying tower.
In the present invention, to be mainly the principle of utilizing the trimethyl carbinol and water energy azeotropic generate the trimethyl carbinol etc. by initiator for reaction in telomeric alcohol crude product to the 4th rectifying tower removes, and the general formula of simultaneously removing in thick C3-Fluoroalcohol is H (CF
2cF
2)
ncH
20H(n>=3) telomeric alcohol.Controlling the 4th rectifying tower tower top temperature is 107～109 ℃, and pressure is that normal pressure carries out rectifying, in the input of the thick C3-Fluoroalcohol of distillate and still regulate pH value, be mainly in and the acidic substance in C3-Fluoroalcohol.Tower bottoms is that general formula is H (CF
2cF
2)
ncH
20H(n>=3) telomeric alcohol, is entered the first rectifying tower and is recycled.
In the present invention, the 5th rectifying tower is mainly a small amount of high boiling material of removing in C3-Fluoroalcohol, improves C3-Fluoroalcohol purity.Control 107～109 ℃ of the 5th rectifying tower tower top temperature, pressure is that normal pressure carries out rectifying, obtains distillate and tower bottoms, and distillate is high-purity C3-Fluoroalcohol, packs, and tower bottoms enters the first rectifying tower and recycles.
Compared with prior art, the present invention has the following advantages:
1, good product quality, after purifying, C3-Fluoroalcohol purity, more than 99.96%, reaches as high as 99.99%, can be applicable to electronics, medicine etc. C3-Fluoroalcohol product purity is required to high value segment;
2, technique is simple, adopts conventional distillation operation when obtaining high purity C3-Fluoroalcohol product, has reclaimed again material benzenemethanol, has further reduced production cost;
3, environmental protection, non-wastewater discharge in production process, only needs regularly to reclaim a small amount of high boiling material, has reduced three waste discharge.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
In figure, the first rectifying tower 1, Second distillation column 2, the three rectifying tower 3, the four rectifying tower 4, deacidification still 5, the five rectifying tower 6.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail, but the present invention is not limited only to following examples.
Embodiment 1
A method of purification for C3-Fluoroalcohol, comprises the following steps:
(1) thick C3-Fluoroalcohol being inputted in the first rectifying tower 1, is first rectifying under 60 ℃ of conditions at normal pressure and tower top temperature, obtains distillate and tower bottoms, and distillate is thick methyl alcohol, using after its rectifying as the raw material recycle of synthesizing C3-Fluoroalcohol; Tower bottoms is inputted to Second distillation column 2;
(2) controlling Second distillation column 2 tower top temperatures is 110 ℃, and vacuum tightness is that 15KPa carries out rectification under vacuum, obtains distillate and tower bottoms, and by distillate input the 3rd rectifying tower 3, tower bottoms loops back the first rectifying tower 1 import;
(3) controlling the 3rd rectifying tower 3 tower top temperatures is 80 ℃, and pressure is that normal pressure carries out rectifying, obtains distillate and tower bottoms, and distillate is thick methyl alcohol, using after its rectifying as the raw material recycle of synthesizing C3-Fluoroalcohol; By tower bottoms input the 4th rectifying tower 4;
(4) controlling the 4th rectifying tower 4 tower top temperatures is 107 ℃, and pressure is that normal pressure carries out rectifying, obtains distillate and tower bottoms, tower bottoms is looped back to the first rectifying tower 1 import, by distillate input deacidification still 5, add sodium methylate, adjusting PH is 7 rear input the 5th rectifying tower 6;
(5) controlling the 5th rectifying tower 6 tower top temperatures is 107 ℃, and pressure is that normal pressure carries out rectifying, obtains distillate and tower bottoms, tower bottoms is looped back to the first rectifying tower 1 import, collect distillate and obtain C3-Fluoroalcohol product, sampling gas chromatographic analysis, the results are shown in Table 1.
Embodiment 2
A method of purification for C3-Fluoroalcohol, comprises the following steps:
(1) thick C3-Fluoroalcohol being inputted in the first rectifying tower 1, is first rectifying under 65 ℃ of conditions at normal pressure and tower top temperature, obtains distillate and tower bottoms, and distillate is thick methyl alcohol, using after its rectifying as the raw material recycle of synthesizing C3-Fluoroalcohol; Tower bottoms is inputted to Second distillation column 2;
(2) controlling Second distillation column 2 tower top temperatures is 100 ℃, and vacuum tightness is that 18KPa carries out rectification under vacuum, obtains distillate and tower bottoms, and by distillate input the 3rd rectifying tower 3, tower bottoms loops back the first rectifying tower 1 import;
(3) controlling the 3rd rectifying tower 3 tower top temperatures is 85 ℃, and pressure is that normal pressure carries out rectifying, obtains distillate and tower bottoms, and distillate is thick methyl alcohol, using after its rectifying as the raw material recycle of synthesizing C3-Fluoroalcohol; By tower bottoms input the 4th rectifying tower 4;
(4) controlling the 4th rectifying tower 4 tower top temperatures is 108 ℃, and pressure is that normal pressure carries out rectifying, obtains distillate and tower bottoms, tower bottoms is looped back to the first rectifying tower 1 import, by distillate input deacidification still 5, add sodium methylate, adjusting PH is 8 rear input the 5th rectifying tower 6;
(5) controlling the 5th rectifying tower 6 tower top temperatures is 109 ℃, and pressure is that normal pressure carries out rectifying, obtains distillate and tower bottoms, tower bottoms is looped back to the first rectifying tower 1 import, collect distillate and obtain C3-Fluoroalcohol product, sampling gas chromatographic analysis, the results are shown in Table 1.
Embodiment 3
A method of purification for C3-Fluoroalcohol, comprises the following steps:
(1) thick C3-Fluoroalcohol being inputted in the first rectifying tower 1, is first rectifying under 70 ℃ of conditions at normal pressure and tower top temperature, obtains distillate and tower bottoms, and distillate is thick methyl alcohol, using after its rectifying as the raw material recycle of synthesizing C3-Fluoroalcohol; Tower bottoms is inputted to Second distillation column 2;
(2) controlling Second distillation column 2 tower top temperatures is 90 ℃, and vacuum tightness is that 20KPa carries out rectification under vacuum, obtains distillate and tower bottoms, and by distillate input the 3rd rectifying tower 3, tower bottoms loops back the first rectifying tower 1 import;
(3) controlling the 3rd rectifying tower 3 tower top temperatures is 95 ℃, and pressure is that normal pressure carries out rectifying, obtains distillate and tower bottoms, and distillate is thick methyl alcohol, using after its rectifying as the raw material recycle of synthesizing C3-Fluoroalcohol; By tower bottoms input the 4th rectifying tower 4;
(4) controlling the 4th rectifying tower 4 tower top temperatures is 109 ℃, and pressure is that normal pressure carries out rectifying, obtains distillate and tower bottoms, tower bottoms is looped back to the first rectifying tower 1 import, by distillate input deacidification still 5, add sodium methylate, adjusting PH is 9 rear input the 5th rectifying tower 6;
(5) controlling the 5th rectifying tower 6 tower top temperatures is 108 ℃, and pressure is that normal pressure carries out rectifying, obtains distillate and tower bottoms, tower bottoms is looped back to the first rectifying tower 1 import, collect distillate and obtain C3-Fluoroalcohol product, sampling gas chromatographic analysis, the results are shown in Table 1.
Embodiment 4
A method of purification for C3-Fluoroalcohol, comprises the following steps:
(1) thick C3-Fluoroalcohol being inputted in the first rectifying tower 1, is first rectifying under 75 ℃ of conditions at normal pressure and tower top temperature, obtains distillate and tower bottoms, and distillate is thick methyl alcohol, using after its rectifying as the raw material recycle of synthesizing C3-Fluoroalcohol; Tower bottoms is inputted to Second distillation column 2;
(2) controlling Second distillation column 2 tower top temperatures is 80 ℃, and vacuum tightness is that 23KPa carries out rectification under vacuum, obtains distillate and tower bottoms, and by distillate input the 3rd rectifying tower 3, tower bottoms loops back the first rectifying tower 1 import;
(3) controlling the 3rd rectifying tower 3 tower top temperatures is 100 ℃, and pressure is that normal pressure carries out rectifying, obtains distillate and tower bottoms, and distillate is thick methyl alcohol, using after its rectifying as the raw material recycle of synthesizing C3-Fluoroalcohol; By tower bottoms input the 4th rectifying tower 4;
(4) controlling the 4th rectifying tower 4 tower top temperatures is 107 ℃, and pressure is that normal pressure carries out rectifying, obtains distillate and tower bottoms, tower bottoms is looped back to the first rectifying tower 1 import, by distillate input deacidification still 5, add sodium methylate, adjusting PH is 10 rear input the 5th rectifying tower 6;
(5) controlling the 5th rectifying tower 6 tower top temperatures is 109 ℃, and pressure is that normal pressure carries out rectifying, obtains distillate and tower bottoms, tower bottoms is looped back to the first rectifying tower 1 import, collect distillate and obtain C3-Fluoroalcohol product, sampling gas chromatographic analysis, the results are shown in Table 1.
Embodiment 5
A method of purification for C3-Fluoroalcohol, comprises the following steps:
(1) thick C3-Fluoroalcohol being inputted in the first rectifying tower 1, is first rectifying under 80 ℃ of conditions at normal pressure and tower top temperature, obtains distillate and tower bottoms, and distillate is thick methyl alcohol, using after its rectifying as the raw material recycle of synthesizing C3-Fluoroalcohol; Tower bottoms is inputted to Second distillation column 2;
(2) controlling Second distillation column 2 tower top temperatures is 70 ℃, and vacuum tightness is that 20KPa carries out rectification under vacuum, obtains distillate and tower bottoms, and by distillate input the 3rd rectifying tower 3, tower bottoms loops back the first rectifying tower 1 import;
(3) controlling the 3rd rectifying tower 3 tower top temperatures is 106 ℃, and pressure is that normal pressure carries out rectifying, obtains distillate and tower bottoms, and distillate is thick methyl alcohol, using after its rectifying as the raw material recycle of synthesizing C3-Fluoroalcohol; By tower bottoms input the 4th rectifying tower 4;
(4) controlling the 4th rectifying tower 4 tower top temperatures is 108 ℃, and pressure is that normal pressure carries out rectifying, obtains distillate and tower bottoms, tower bottoms is looped back to the first rectifying tower 1 import, by distillate input deacidification still 5, add sodium hydroxide, adjusting PH is 7 rear input the 5th rectifying tower 6;
(5) controlling the 5th rectifying tower 6 tower top temperatures is 108 ℃, and pressure is that normal pressure carries out rectifying, obtains distillate and tower bottoms, tower bottoms is looped back to the first rectifying tower 1 import, collect distillate and obtain C3-Fluoroalcohol product, sampling gas chromatographic analysis, the results are shown in Table 1.
Table 1 embodiment 1～5 product analysis result
| Embodiment | C3-Fluoroalcohol purity |
| 1 | 99.97% |
| 2 | 99.96% |
| 3 | 99.98% |
| 4 | 99.99% |
| 5 | 99.97% |
Claims (4)
1. a method of purification for C3-Fluoroalcohol, is characterized in that comprising the following steps:
(1) thick C3-Fluoroalcohol being inputted in the first rectifying tower, is first rectifying under 60～80 ℃ of conditions at normal pressure and tower top temperature, obtains distillate and tower bottoms, and tower bottoms is inputted to Second distillation column;
(2) controlling Second distillation column tower top temperature is 70～110 ℃, and vacuum tightness is that 15～25KPa carries out rectification under vacuum, obtains distillate and tower bottoms, and by distillate input the 3rd rectifying tower, tower bottoms loops back the first rectifying tower import;
(3) controlling the 3rd rectifying tower tower top temperature is 80～106 ℃, and pressure is that normal pressure carries out rectifying, obtains distillate and tower bottoms, by tower bottoms input the 4th rectifying tower;
(4) controlling the 4th rectifying tower tower top temperature is 107～109 ℃, and pressure is that normal pressure carries out rectifying, obtains distillate and tower bottoms, and tower bottoms is looped back to the first rectifying tower import, and it is 7～10 rear input the 5th rectifying tower that distillate is adjusted to pH value with alkaline matter;
(5) controlling the 5th rectifying tower tower top temperature is 107～109 ℃, and pressure is that normal pressure carries out rectifying, obtains distillate and tower bottoms, and tower bottoms is looped back to the first rectifying tower import, collects distillate and obtains C3-Fluoroalcohol product.
2. the method for purification of C3-Fluoroalcohol according to claim 1, is characterized in that recycle after distillate rectifying step (1) Suo Shu.
3. the method for purification of C3-Fluoroalcohol according to claim 1, is characterized in that recycle after distillate rectifying step (3) Suo Shu.
4. the method for purification of C3-Fluoroalcohol according to claim 1, is characterized in that the described alkaline matter of step (4) is sodium methylate or sodium hydroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310613589.8A CN103694082A (en) | 2013-11-26 | 2013-11-26 | Method for purifying tetrafluoro propanol |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310613589.8A CN103694082A (en) | 2013-11-26 | 2013-11-26 | Method for purifying tetrafluoro propanol |
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| Publication Number | Publication Date |
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| CN103694082A true CN103694082A (en) | 2014-04-02 |
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ID=50355776
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| CN201310613589.8A Pending CN103694082A (en) | 2013-11-26 | 2013-11-26 | Method for purifying tetrafluoro propanol |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104016834A (en) * | 2014-06-18 | 2014-09-03 | 山东中氟化工科技有限公司 | Method for recycling fluorine-containing alcohol from residual liquid obtained from tetrafluoropropanol preparation |
| CN109134198A (en) * | 2018-11-08 | 2019-01-04 | 山东科技大学 | A kind of method of separation of extractive distillation tetrafluoropropanol and water azeotropic mixture |
| CN111825528A (en) * | 2020-06-15 | 2020-10-27 | 三明市海斯福化工有限责任公司 | Method for purifying fluorine-containing alcohol |
| CN111875477A (en) * | 2020-08-03 | 2020-11-03 | 岳阳隆兴实业公司 | Azeotropic purification method of o-chlorohydrin |
| CN113979838A (en) * | 2021-08-04 | 2022-01-28 | 浙江巨圣氟化学有限公司 | Method for refining tetrafluoropropanol |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1441763A (en) * | 2000-08-28 | 2003-09-10 | 大金工业株式会社 | Process for producing fluoroalcohol |
| CN1449366A (en) * | 2000-08-24 | 2003-10-15 | 旭硝子株式会社 | Process for producing a fluorinated alcohol |
-
2013
- 2013-11-26 CN CN201310613589.8A patent/CN103694082A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1449366A (en) * | 2000-08-24 | 2003-10-15 | 旭硝子株式会社 | Process for producing a fluorinated alcohol |
| CN1441763A (en) * | 2000-08-28 | 2003-09-10 | 大金工业株式会社 | Process for producing fluoroalcohol |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104016834A (en) * | 2014-06-18 | 2014-09-03 | 山东中氟化工科技有限公司 | Method for recycling fluorine-containing alcohol from residual liquid obtained from tetrafluoropropanol preparation |
| CN104016834B (en) * | 2014-06-18 | 2015-03-25 | 山东中氟化工科技有限公司 | Method for recycling fluorine-containing alcohol from residual liquid obtained from tetrafluoropropanol preparation |
| CN109134198A (en) * | 2018-11-08 | 2019-01-04 | 山东科技大学 | A kind of method of separation of extractive distillation tetrafluoropropanol and water azeotropic mixture |
| CN111825528A (en) * | 2020-06-15 | 2020-10-27 | 三明市海斯福化工有限责任公司 | Method for purifying fluorine-containing alcohol |
| CN111875477A (en) * | 2020-08-03 | 2020-11-03 | 岳阳隆兴实业公司 | Azeotropic purification method of o-chlorohydrin |
| CN113979838A (en) * | 2021-08-04 | 2022-01-28 | 浙江巨圣氟化学有限公司 | Method for refining tetrafluoropropanol |
| CN113979838B (en) * | 2021-08-04 | 2023-09-29 | 浙江巨圣氟化学有限公司 | Method for refining tetrafluoropropanol |
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