CN104803823A - Trifluoromethane preparation method - Google Patents
Trifluoromethane preparation method Download PDFInfo
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- CN104803823A CN104803823A CN201410033204.5A CN201410033204A CN104803823A CN 104803823 A CN104803823 A CN 104803823A CN 201410033204 A CN201410033204 A CN 201410033204A CN 104803823 A CN104803823 A CN 104803823A
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- trifluoromethane
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Abstract
The present invention provides a trifluoromethane (HFC-23) preparation method, wherein trichloromethane and hydrofluoric acid react under the effect of a catalyst to prepare the trifluoromethane, and the catalyst is zinc chloride. With the preparation method of the present invention, the trifluoromethane (HFC-23) conversion rate can be significantly improved.
Description
Technical field
The present invention relates to a kind of preparation method of trifluoromethane.
Background technology
Fluoroform, i.e. trifluoromethane (HFC-23) are a kind of chemical formulas is CHF
3organic compound, be the one of haloform.Be colourless gas under normal temperature, molecular weight is 70.01g/mol.
Trifluoromethane (HFC-23) is byproduct when manufacturing Teflon, and organism carries out to trifluoroacetic acid the trifluoromethane (HFC-23) that decarboxylic reaction also can produce trace.Trifluoromethane (HFC-23) can be used as refrigeration agent or fire-fighting medium uses.
Summary of the invention
The invention provides the preparation method of a kind of trifluoromethane (HFC-23), under the effect of catalyzer, react obtained by trichloromethane and hydrogen fluoride, wherein said catalyzer is zinc chloride.
In the present invention, described reaction is carried out under pressure is 6-60bars.
In the present invention, the temperature of described reaction is carry out between 75-76 degree.
In the present invention, the temperature of described reaction is 75.5 degree and carries out.
In the present invention, in described raw material, trichloromethane and hydrofluoric mol ratio are 1:1.5-2:1.
In the present invention, the mol ratio of described zinc chloride and raw material total content is 1:20-1:15.
In the present invention, the described reaction times is 2-2.2 hour.
Adopt the present invention to prepare the method for trifluoromethane (HFC-23), the transformation efficiency of product can be significantly improved.
Embodiment
Below the embodiment of the present invention is described in detail, but does not limit the present invention.
The reaction of following embodiment is carry out in the autoclave of 0.5L at a volume, and be made up of stainless steel, comprise the devices such as stirring, this device comprises the device such as pressure tester and thermometer, and arranges opening for feed and exhaust etc.
Preparation embodiment 1
Catalyzer according to following table recipe ratio joins in autoclave simultaneously, with the oxygen in nitrogen replacement still, add raw material again and carry out addition reaction, temperature of reaction 75 DEG C, pressure is 20bars, 2 hours reaction times, crude product underpressure distillation desolvation after reaction, recycled solvent, continues underpressure distillation and obtains final product.
The proportioning raw materials of table 1 embodiment of the present invention 1 and comparative example 1-2
Effect example 1
In autoclave, adopt the proportioning in above-mentioned processing condition and table 1, carry out the preparation of trifluoromethane (HFC-23), the yield of gained trifluoromethane (HFC-23) and the time required for reaction to terminal.
The effect data of table 2 comparative example 1-2 and the embodiment of the present invention 1
Ginseng sees the above table the effect data of 2, can find, in the process preparing trifluoromethane (HFC-23), when the mole number of catalyzer is identical, employing zinc chloride can significantly improve the yield that trifluoromethane (HFC-23) transforms, and then improves the utilization ratio of raw material widely.
Preparation embodiment 2
Join in autoclave according to the catalyzer of following table recipe ratio, with the oxygen in nitrogen replacement still, then add raw material and carry out addition reaction, pressure is 20bars, 2 hours reaction times, crude product underpressure distillation desolvation after reaction, recycled solvent, continues underpressure distillation and obtains final product.
The proportioning raw materials of table 3 embodiment of the present invention 1-3 and comparative example 3-5
Effect example 2
In autoclave, adopt the proportioning in above-mentioned processing condition and table 1, carry out the preparation of trifluoromethane (HFC-23), the yield of gained trifluoromethane (HFC-23) and the time required for reaction to terminal.
The effect data of table 2 comparative example 3-5 and embodiment of the present invention 1-3
Ginseng sees the above table the effect data of 2, can find, in the process preparing trifluoromethane (HFC-23), when the mole number of catalyzer is identical, when temperature of reaction rises to 75 degree, the yield that trifluoromethane (HFC-23) transforms can be significantly improved, 75.5 degree time, very large leap is achieved in yield, therefore, contriver by experiment, have found the ideal temperature of this reaction between 75-76 degree, the best is 75.5 degree, when lower than 75 degree, the transformation efficiency of reaction is not good, when higher than 76 degree, transformation efficiency change is little, but the waste of the energy can be caused.
Be described in detail specific embodiments of the invention above, but it is just as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and substituting also all among category of the present invention.Therefore, equalization conversion done without departing from the spirit and scope of the invention and amendment, all should contain within the scope of the invention.
Claims (7)
1. a preparation method for trifluoromethane, under the effect of catalyzer, react obtained by trichloromethane and hydrogen fluoride, wherein said catalyzer is zinc chloride.
2. the method for claim 1, is characterized in that, described reaction is carried out under pressure is 6-60bars.
3. the method for claim 1, is characterized in that, the temperature of described reaction is carry out between 75-76 degree.
4. method as claimed in claim 3, it is characterized in that, the temperature of described reaction is 75.5 degree and carries out.
5. the method for claim 1, is characterized in that: in described raw material, trichloromethane and hydrofluoric mol ratio are 1:1.5-2:1.
6. the method for claim 1, is characterized in that: the mol ratio of described zinc chloride and raw material total content is 1:20-1:15.
7. the method for claim 1, is characterized in that, the described reaction times is 2-2.2 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410033204.5A CN104803823A (en) | 2014-01-24 | 2014-01-24 | Trifluoromethane preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410033204.5A CN104803823A (en) | 2014-01-24 | 2014-01-24 | Trifluoromethane preparation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104803823A true CN104803823A (en) | 2015-07-29 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410033204.5A Pending CN104803823A (en) | 2014-01-24 | 2014-01-24 | Trifluoromethane preparation method |
Country Status (1)
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| CN (1) | CN104803823A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114502527A (en) * | 2019-10-18 | 2022-05-13 | 鲁南贝特制药有限公司 | Synthetic method of sevoflurane |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3258500A (en) * | 1959-08-17 | 1966-06-28 | Du Pont | Process for fluorinating halohydro-carbons |
| CN1078172A (en) * | 1992-02-26 | 1993-11-10 | 帝国化学工业公司 | fluorination catalyst and fluorination process |
| JPH10306046A (en) * | 1997-05-08 | 1998-11-17 | Showa Denko Kk | Purification of trifluoromethane |
| CN103012052A (en) * | 2012-12-17 | 2013-04-03 | 南京信息工程大学 | Method for preparing trifluoromethane |
-
2014
- 2014-01-24 CN CN201410033204.5A patent/CN104803823A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3258500A (en) * | 1959-08-17 | 1966-06-28 | Du Pont | Process for fluorinating halohydro-carbons |
| CN1078172A (en) * | 1992-02-26 | 1993-11-10 | 帝国化学工业公司 | fluorination catalyst and fluorination process |
| JPH10306046A (en) * | 1997-05-08 | 1998-11-17 | Showa Denko Kk | Purification of trifluoromethane |
| CN103012052A (en) * | 2012-12-17 | 2013-04-03 | 南京信息工程大学 | Method for preparing trifluoromethane |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114502527A (en) * | 2019-10-18 | 2022-05-13 | 鲁南贝特制药有限公司 | Synthetic method of sevoflurane |
| CN114502527B (en) * | 2019-10-18 | 2024-06-14 | 鲁南贝特制药有限公司 | Synthesis method of sevoflurane |
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Application publication date: 20150729 |
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