CN102603471A - Production method of p-trifluoromethyl chlorobenzene - Google Patents
Production method of p-trifluoromethyl chlorobenzene Download PDFInfo
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- CN102603471A CN102603471A CN2012100386900A CN201210038690A CN102603471A CN 102603471 A CN102603471 A CN 102603471A CN 2012100386900 A CN2012100386900 A CN 2012100386900A CN 201210038690 A CN201210038690 A CN 201210038690A CN 102603471 A CN102603471 A CN 102603471A
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- chlorine
- chlorination
- chloro benzo
- benzo trifluoride
- working method
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Abstract
The invention discloses a production method of p-trifluoromethyl chlorobenzene, which comprises the following steps: adding p-chlorotoluene in a chlorinating reactor, introducing chlorine gas to perform chlorination at 90-100 DEG C for 16-20 hours, and performing aeration to remove hydrogen chloride after the chlorination is finished, and obtaining p-chlorotrichlorotoluene; and adding obtained p-chlorotrichlorotoluene into a high pressure fluorinating reactor, introducing HF, performing fluoridation at 100 DEG C and under a pressure of 1.5MPa for 6-8 hours, and obtaining p-trifluoromethyl chlorobenzene. The production method of trifluoromethyl chlorobenzene disclosed by the invention is simple and convenient, and easy to operate, and the product content after rectification is up to over 99.5%.
Description
Technical field
The present invention relates to a kind of working method of p-chloro benzo trifluoride-99.
Background technology
The working method of existing p-chloro benzo trifluoride-99 is complicated, and the product yield is low, and finished product content is low.
Summary of the invention
The object of the present invention is to provide a kind of easy to operate, the working method of the high p-chloro benzo trifluoride-99 of finished product content.
Technical solution of the present invention is:
A kind of working method of p-chloro benzo trifluoride-99 is characterized in that: comprise the following steps:
(1) chlorination: 4-Chlorotoluene 99.5 is added chlorination tank, feed chlorine and under 90 ~ 100 ℃, carry out chlorination 16 ~ 20 hours, after chlorination finished, aeration removed de-chlorine hydride, obtains the chlorine benzenyl trichloride;
(2) fluoridize: what will obtain adds high pressure to the chlorine benzenyl trichloride and fluoridizes still, feeds HF, 1.5MPa, 100 ℃ of following fluoridations 6 ~ 8 hours, obtains p-chloro benzo trifluoride-99.
The mol ratio of 4-Chlorotoluene 99.5 and chlorine is 1:3 ~ 3.5 in the step (1).
Mol ratio to chlorine benzenyl trichloride and HF in the step (2) is 1:3.2.
The p-chloro benzo trifluoride-99 that step (2) obtains is also through rectification process.
The inventive method is easy, and is easy to operate, and the product content after the rectifying reaches more than 99.5%.
Below in conjunction with embodiment the present invention is described further.
Embodiment
A kind of working method of p-chloro benzo trifluoride-99 comprises the following steps:
(1) chlorination: 4-Chlorotoluene 99.5 is added chlorination tank, feed chlorine and under 90 ~ 100 ℃, carry out chlorination 16 ~ 20 hours, after chlorination finished, aeration removed de-chlorine hydride, obtains the chlorine benzenyl trichloride;
(2) fluoridize: what will obtain fluoridizes still to chlorine benzenyl trichloride adding high pressure; Feed HF,, obtain p-chloro benzo trifluoride-99 1.5MPa, 100 ℃ of following fluoridations 6 ~ 8 hours; The blowing that reduces pressure then carries out rectifying and obtains p-chloro benzo trifluoride-99 content and reach the finished product more than 99.5% after the drying.
The mol ratio of 4-Chlorotoluene 99.5 and chlorine is 1:3 ~ 3.5 (routine 1:3,1::3.2,1:3.5) in the step (1).
Mol ratio to chlorine benzenyl trichloride and HF in the step (2) is 1:3.2.
Claims (4)
1. the working method of a p-chloro benzo trifluoride-99 is characterized in that: comprise the following steps:
(1) chlorination: 4-Chlorotoluene 99.5 is added chlorination tank, feed chlorine and under 90 ~ 100 ℃, carry out chlorination 16 ~ 20 hours, after chlorination finished, aeration removed de-chlorine hydride, obtains the chlorine benzenyl trichloride;
(2) fluoridize: what will obtain adds high pressure to the chlorine benzenyl trichloride and fluoridizes still, feeds HF, 1.5MPa, 100 ℃ of following fluoridations 6 ~ 8 hours, obtains p-chloro benzo trifluoride-99.
2. the working method of p-chloro benzo trifluoride-99 according to claim 1 is characterized in that: the mol ratio of 4-Chlorotoluene 99.5 and chlorine is 1:3 ~ 3.5 in the step (1).
3. the working method of p-chloro benzo trifluoride-99 according to claim 1 and 2, it is characterized in that: the mol ratio to chlorine benzenyl trichloride and HF in the step (2) is 1:3.2.
4. the working method of p-chloro benzo trifluoride-99 according to claim 1 and 2, it is characterized in that: the p-chloro benzo trifluoride-99 that step (2) obtains is also through rectification process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100386900A CN102603471A (en) | 2012-02-21 | 2012-02-21 | Production method of p-trifluoromethyl chlorobenzene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100386900A CN102603471A (en) | 2012-02-21 | 2012-02-21 | Production method of p-trifluoromethyl chlorobenzene |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102603471A true CN102603471A (en) | 2012-07-25 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012100386900A Pending CN102603471A (en) | 2012-02-21 | 2012-02-21 | Production method of p-trifluoromethyl chlorobenzene |
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| CN (1) | CN102603471A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102746109A (en) * | 2012-08-01 | 2012-10-24 | 山东道可化学有限公司 | Preparation method of 4-Chlorobenzotrifluoride |
| CN109574863A (en) * | 2017-09-28 | 2019-04-05 | 安徽省庆云医药股份有限公司 | A kind of synthetic method of -4 ' of 2- amino-fluoro- benzophenone |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1967244A (en) * | 1932-08-31 | 1934-07-24 | Kinetic Chemicals Inc | Production of organic fluorine compounds |
| JPS615033A (en) * | 1984-06-16 | 1986-01-10 | Tokuyama Soda Co Ltd | Preparation of trifluoromethyl benzal chloride or derivative thereof |
| US4825014A (en) * | 1981-09-03 | 1989-04-25 | Daikin Kogyo Co., Ltd. | Process for preparing chlorotrifluoromethylbenzene |
-
2012
- 2012-02-21 CN CN2012100386900A patent/CN102603471A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1967244A (en) * | 1932-08-31 | 1934-07-24 | Kinetic Chemicals Inc | Production of organic fluorine compounds |
| US4825014A (en) * | 1981-09-03 | 1989-04-25 | Daikin Kogyo Co., Ltd. | Process for preparing chlorotrifluoromethylbenzene |
| JPS615033A (en) * | 1984-06-16 | 1986-01-10 | Tokuyama Soda Co Ltd | Preparation of trifluoromethyl benzal chloride or derivative thereof |
Non-Patent Citations (3)
| Title |
|---|
| 于兆源: "对氯三氟甲基苯的合成研究", 《农药》, no. 4, 30 April 1984 (1984-04-30), pages 13 - 15 * |
| 袁志明: "对氯三氟甲苯的合成工艺的改进", 《精细化工中间体》, vol. 32, no. 2, 9 May 2002 (2002-05-09), pages 46 - 47 * |
| 马英高: "对氯三氟甲苯合成工艺的进展", 《辽宁化工》, no. 4, 28 August 1980 (1980-08-28), pages 34 - 41 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102746109A (en) * | 2012-08-01 | 2012-10-24 | 山东道可化学有限公司 | Preparation method of 4-Chlorobenzotrifluoride |
| CN109574863A (en) * | 2017-09-28 | 2019-04-05 | 安徽省庆云医药股份有限公司 | A kind of synthetic method of -4 ' of 2- amino-fluoro- benzophenone |
| CN109574863B (en) * | 2017-09-28 | 2021-09-14 | 安徽省庆云医药股份有限公司 | Synthesis method of 2-amino-4' -fluoro-benzophenone |
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Application publication date: 20120725 |