CN1027755C - Preparation of camphor with isoborneol by gas phase dehydrogenation - Google Patents
Preparation of camphor with isoborneol by gas phase dehydrogenation Download PDFInfo
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- CN1027755C CN1027755C CN 90107669 CN90107669A CN1027755C CN 1027755 C CN1027755 C CN 1027755C CN 90107669 CN90107669 CN 90107669 CN 90107669 A CN90107669 A CN 90107669A CN 1027755 C CN1027755 C CN 1027755C
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- camphor
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- fixed bed
- gas phase
- isocamphol
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Abstract
The present invention belongs to a method for synthesizing camphor. Zinc and calcium are used a catalyst so that borneolum is depressed and dehydrogenated with gas phase in a fixed bed so as to prepare camphor, a dehydrogenation temperature is from 240 to 320 DEG C, and pressure is from 0 to 60 mmHg; when the material space velocity is from 0.05 to 1.0,-1 is added. The process method provided by the present invention has the advantages of convenient operation, continuous operation, no solvent, high yield, no three waste, etc., the conversion rate of the borneolum is more than or equal to 98 %, and selectivity is more than or equal to 98%.
Description
The invention belongs to the camphor synthesis method.
Camphor is widely used for aspects such as industry and medical and health.Industrial artificial camphor is usually from α-Pai Xi, and four steps such as process isomerization, esterification, hydrolysis and dehydrogenation make.[J.D.Roberts and M.C.Caserio, Basic Principles of Organic Chemistry, W.A.Benjamin, InC., Second Edition 1977, P1467], [chief editor of Nanjing forest product industry institute, chemistry of forest product and manual industry, the first volume, 362-381, China Forest press, Beijing, 1980].Its reaction formula is as follows:
Isocamphol dehydrogenation wherein is to adopt ventilation breather to make catalyzer, and adds dimethylbenzene and make solvent, carries out with intermittent mode.Its main drawback is that catalyzer can not be reused basically, must use solvent, and reaction can not be carried out continuously, and it is relatively low etc. operate cumbersome and recovery rate.
Main points of the present invention are to make catalyzer with zinc-calcium, make isocamphol gas phase decompression dehydrogenation in fixed bed prepare camphor.Need not to add solvent in the reaction, reaction can be carried out continuously.Temperature of reaction is 240-320 ℃, and pressure is 0-60mmHg, when the material air speed is 0.05-1.0
-1The transformation efficiency of this law isocamphol 〉=98%, dehydrogenation generates selectivity 〉=98% of the reaction of camphor.
Dehydrogenation reaction is carried out in the fixed bed flow through reactors.This device mainly is made up of stock bottle, reaction column and susceptor.The reaction column apparatus with catalyst inside has heating system outward, and its lower end links to each other with the stock bottle that has three mouths.All the other two mouths of this bottle connect the hydrogen plenum system respectively and insert thermometer, the outer heating system that is provided with of bottle.The upper end of post links to each other with susceptor, and the latter is joined through condenser and vacuum system.Catalyzer must be used hydrogen reducing before using in reaction column, carried out 2-6 hour under 250-340 ℃ of normal pressure.Catalyzer can be reused, and can regenerate behind active the decline.
Example one
Get purity and be 98.7% isocamphol 40 grams and put into stock bottle.Put 1101 type zinc-calcium catalysts 200 and restrain in reaction column, and 290 ℃ of following logical hydrogen reductions 4 hours.Stop logical hydrogen then, being evacuated to pressure is 20mmHg, keeps column temperature at 290 ℃, heating raw bottle to 135 ℃.After 2 hours, obtain camphor 38.4 grams, purity is 98.8%, receiving and putting forward rate is 97.3%.The transformation efficiency of isocamphol is 99.5%.
Example two
Get isocamphol 20 grams and put into stock bottle.1101 type zinc-calcium catalysts 100 are restrained in the reaction column of packing into, and 305 ℃ of following logical hydrogen reductions 4 hours.Stop logical hydrogen then, being evacuated to pressure is 25mmHg, keeps column temperature at 295 ℃, heating raw bottle to 150 ℃.After 0.4 hour, obtain camphor 19 grams, recovery rate is 96.3%, the isocamphol transformation efficiency is 99.2%
Claims (3)
1, a kind ofly prepare the method for camphor by isocamphol, this method is carried out dehydrogenation reaction with isocamphol, it is characterized by dehydrogenation reaction and carries out under the gas phase decompression, must not add any solvent, temperature of reaction is 240-320 ℃, and pressure is 0-60mmHg, when the material air speed is 0.05-1.0
-1, whole process is finished in the fixed bed flow through reactors, and fixed bed catalyst is zinc-calcium type solid catalyst.
2, according to the method described in the claim 1, it is characterized in that described fixed bed flow through reactors, by stock bottle, reaction column and susceptor are formed, and catalyzer is housed in the reaction column, heating system is arranged outward, one end links to each other with stock bottle, and the other end is through susceptor, and condenser is connected with vacuum system, stock bottle links to each other with hydrogen gas system, and heating system is arranged.
3, according to claim 1,2 described methods, it is characterized in that described catalyzer must be through hydrogen reducing before using, reduction temperature is 250-340 ℃, time 2-6 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90107669 CN1027755C (en) | 1990-09-10 | 1990-09-10 | Preparation of camphor with isoborneol by gas phase dehydrogenation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90107669 CN1027755C (en) | 1990-09-10 | 1990-09-10 | Preparation of camphor with isoborneol by gas phase dehydrogenation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1059710A CN1059710A (en) | 1992-03-25 |
| CN1027755C true CN1027755C (en) | 1995-03-01 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 90107669 Expired - Fee Related CN1027755C (en) | 1990-09-10 | 1990-09-10 | Preparation of camphor with isoborneol by gas phase dehydrogenation |
Country Status (1)
| Country | Link |
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| CN (1) | CN1027755C (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102004011543A1 (en) | 2004-03-08 | 2005-10-06 | Basf Ag | Process for the preparation of optically active carbonyl compounds |
| CN103012097A (en) * | 2012-11-08 | 2013-04-03 | 南宁辰康生物科技有限公司 | Method for preparing fenchone |
| CN105152883A (en) * | 2015-09-07 | 2015-12-16 | 广西梧州通轩林产化学有限公司 | Method for preparing camphor by using camphene as raw material |
| CN105126891A (en) * | 2015-09-07 | 2015-12-09 | 广西梧州通轩林产化学有限公司 | Preparation method for copper-based catalyst for camphor production |
| CN105126890A (en) * | 2015-09-07 | 2015-12-09 | 广西梧州通轩林产化学有限公司 | Preparation method for copper-based catalyst for camphor production |
| CN105669411B (en) * | 2016-03-07 | 2018-06-26 | 华北电力大学 | A kind of method that yellow cinnamon leaf catalysis pyrolysis prepares camphor |
| CN108314611B (en) * | 2017-12-27 | 2021-04-27 | 福建南平青松化工有限公司 | Equipment and production process for preparing camphor by continuous gas phase dehydrogenation of isoborneol |
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1990
- 1990-09-10 CN CN 90107669 patent/CN1027755C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1059710A (en) | 1992-03-25 |
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| Date | Code | Title | Description |
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| C10 | Entry into substantive examination | ||
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| C06 | Publication | ||
| PB01 | Publication | ||
| CI01 | Correction of invention patent gazette |
Correction item: First inventor Correct: Li Yunlong False: Ji Yunlong Number: 13 Volume: 8 |
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| ERR | Gazette correction |
Free format text: CORRECT: THE FIRST INVENTOR; FROM: JI YUNLONG TO: LI YUNLONG |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C15 | Extension of patent right duration from 15 to 20 years for appl. with date before 31.12.1992 and still valid on 11.12.2001 (patent law change 1993) | ||
| OR01 | Other related matters | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |