CN103435433A - Method for synthesizing isolongifolene by catalytically isomerizing longifolene with solid acid - Google Patents
Method for synthesizing isolongifolene by catalytically isomerizing longifolene with solid acid Download PDFInfo
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- CN103435433A CN103435433A CN2013103779357A CN201310377935A CN103435433A CN 103435433 A CN103435433 A CN 103435433A CN 2013103779357 A CN2013103779357 A CN 2013103779357A CN 201310377935 A CN201310377935 A CN 201310377935A CN 103435433 A CN103435433 A CN 103435433A
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- isolongifolene
- longifolene
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- glacial acetic
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Abstract
The invention discloses a method for synthesizing isolongifolene by catalytically isomerizing longifolene with solid acid. The method comprises the following steps: mixing longifolene and glacial acetic acid; putting the mixture into a reaction container; adding a catalyst to perform an isomerization reaction; filtering after the reaction is finished; recycling the catalyst; distilling to recycle a solvent; rectifying to obtain an isolongifolene finished product. The method is characterized in that the catalyst is solid acid D72 macroporous strong acid ion exchange resin; the weight ratio of the longifolene to the glacial acetic acid to the catalyst is 1:(0.4-1.2):(0.1-0.3); the temperature in the reaction container is 60-110 DEG C, and the reaction time is 4-6 hours. The method can solve the existing problems of high cost and severe pollution for producing isolongifolene or isolongifolenone.
Description
Technical field
The present invention relates to chemical industry rosin deep process technology field, especially a kind of method of using longifolene isoparaffin synthesis Isolongifolene.
Background technology
At present, in longifolene synthesizes the reaction process of Isolongifolene by isomerization reaction, sulfuric acid commonly used is catalyzer.Due to the severe corrosive of sulfuric acid, make the equipment such as the inwall of reactor and inner-walls of duct all be subject to stronger corrosion, reduce service life of equipment; And sulfuric acid belongs to hazardous chemical, human body is had to certain injury, certain danger is arranged in operating process, also need to increase the operation of a washing work post after isomerization reaction, the sulfuric acid left behind with cleaning reaction, expend more solvent and water resources, increased manpower and materials, increase production cost; In addition, the waste liquid that sulfuric acid produces in reaction process and washing waste water out, have larger pollution to water and environment.
Summary of the invention
The invention provides the method for the synthetic Isolongifolene of a kind of solid acid catalysis isomery longifolene, to solve high, the with serious pollution problem of existing Isolongifolene or Isolongifolenone production cost.
In order to address the above problem, technical scheme of the present invention is: the method for the synthetic Isolongifolene of this solid acid catalysis isomery longifolene will be put into reaction vessel after the mixing of longifolene and Glacial acetic acid, add catalyzer, carry out isomerization reaction, reaction is filtered after finishing, catalyst recovery, distillating recovering solvent, rectifying gets final product to obtain the Isolongifolene finished product, it is characterized in that: described catalyzer is solid acid D72 macroporous type strong-acid cation-exchange resin, and the weight ratio of longifolene and Glacial acetic acid and described catalyzer is 1:0.4～1.2:0.1～0.3; Temperature in described reaction vessel is 60 ° of C～110 ° C, and the reaction times is 4～6 hours.
In technique scheme, more specifically scheme can be: the weight ratio of longifolene and Glacial acetic acid and described catalyzer is 1:1:0.2.
Owing to having adopted technique scheme, the present invention compared with prior art has following beneficial effect:
The method of the synthetic Isolongifolene of this solid acid catalysis isomery longifolene, adopt novel solid acid catalyst macroporous type strong-acid cation-exchange resin D72 to replace sulfuric acid as catalyzer, the pollution of the corrosion of minimizing equipment and water, environment, reduce washing step, greatly reduce the loss of solvent, water resources and catalyzer, saved labor force and raw-material cost, the competitive power of product is provided.
Embodiment
Embodiment mono-:
The method of the synthetic Isolongifolene of this solid acid catalysis isomery longifolene, the lab scale charging is 100 gram longifolenes/pot: the macroporous type strong-acid cation-exchange resin D72 catalyzer of 20 grams is added to the 500ml there-necked flask, then will after the mixing of 100 gram 65% longifolenes and 80 gram Glacial acetic acid, add reaction flask, open to stir and start heating, carry out isomerization reaction in reactor, temperature in reactor is 60 ° of C, sampling analysis Isolongifolene content after 3 hours, every sampling in 0.5-1 hour once, until Isolongifolene content no longer increases or increases to such an extent that even return very slowly after falling to stop adding and start cooling, be cooled to below 40 degree, reaction is total to approximately 4 hours, filtered successively again, catalyst recovery, finally filtrate is carried out to air distillation and reclaim solvent, the analytical results that obtains the Isolongifolene crude product is: Isolongifolene content 61.755%, longifolene content 2.4%.The Isolongifolene crude product is distilled, and rectifying is the finished product according to the Isolongifolene of client's index request intercepting desired content (being greater than 70%, 80% or 85%), and the Isolongifolene product content of this experiment distillation is 80.67%.
The catalyzer filtered out is refunded in the 500ml reaction flask, advance again longifolene and recovered solvent Glacial acetic acid 80 grams of 100 gram 65% content, reclaim solvent and not just add new benefit enough, opening stirring heating is reacted, technological operation is caught up with pot equally, repeat above technological operation, make catalyzer repeat to carry out continuously 1000 pots of lab scales, the Isolongifolene content of the Isolongifolene crude product reflected remains between 58%-63% substantially, longifolene content remains between 2%-4% substantially, and the activity of catalyzer and effect can keep finely.
Embodiment bis-:
The method of the synthetic Isolongifolene of this solid acid catalysis isomery longifolene, extension test 10000 gram longifolenes/pot: the macroporous type strong-acid cation-exchange resin D72 catalyzer of 3000 grams is added in the 30L reactor, then 10000 gram 65% longifolenes and 12000 gram Glacial acetic acid are added respectively to reactor, start to stir, heating, carry out isomerization reaction in reactor, temperature in reactor is 90 ° of C, sampling analysis Isolongifolene content after 3 hours, every sampling in 0.5-1 hour once, until Isolongifolene content no longer increases or increases to such an extent that even return very slowly after falling to stop adding and start cooling, be cooled to below 40 degree, reaction is total to approximately 5 hours, filtered successively again, reclaim catalyzer, finally filtrate is carried out to air distillation and reclaim solvent, the analytical results that obtains the Isolongifolene crude product is: Isolongifolene content 60.632%, longifolene content 2.8%.The Isolongifolene crude product is distilled, and rectifying is the finished product according to the Isolongifolene of client's index request intercepting desired content (being greater than 70%, 80% or 85%), and the Isolongifolene product content of this experiment distillation is 79.57%.
The catalyzer filtered out is refunded in the 30L reactor, advance again longifolene and recovered solvent Glacial acetic acid 12000 grams of 10000 gram 65% content, reclaim solvent and not just add new benefit enough, opening stirring and heating is reacted, technological operation is caught up with pot equally, repeat above technological operation, make catalyzer repeat to carry out continuously 300 pots of extension tests, the Isolongifolene content of the Isolongifolene crude product reflected remains between 58%-63% substantially, longifolene content remains between 2%-4% substantially, and the activity of catalyzer and effect can keep finely.
Embodiment tri-:
The method of the synthetic Isolongifolene of this solid acid catalysis isomery longifolene, pilot scale 100kg longifolene/pot, the macroporous type strong-acid cation-exchange resin D72 catalyzer of 10kg is added in the pilot scale reactor, then 100kg65% longifolene and 60kg Glacial acetic acid are added respectively to reactor, start to stir, heating, carry out isomerization reaction in reactor, temperature in reactor is 110 ° of C, sampling analysis Isolongifolene content after 2 hours, every sampling in 0.5-1 hour once, until Isolongifolene content no longer increases or increases to such an extent that even return very slowly after falling to stop adding and start cooling, be cooled to below 40 degree, reaction is total to approximately 6 hours, filtered successively again, reclaim catalyzer, finally filtrate is carried out to air distillation and reclaim solvent, the analytical results that obtains the Isolongifolene crude product is: Isolongifolene content 59.838%, longifolene content 2.9%.The Isolongifolene crude product is distilled, and rectifying is the finished product according to the Isolongifolene of client's index request intercepting desired content (being greater than 70%, 80% or 85%), and the Isolongifolene product content of this experiment distillation is 78.98%.
The catalyzer filtered out is refunded in the pilot scale reactor, advance again longifolene and the recovered solvent Glacial acetic acid 60kg of 100kg65% content, reclaim solvent and not just add new benefit enough, opening stirring and heating is reacted, technological operation is caught up with pot equally, repeat above technological operation, make catalyzer repeat to carry out continuously 40 pots of pilot plant tests, the Isolongifolene content of the Isolongifolene crude product reflected remains between 58%-63% substantially, longifolene content remains between 2%-4% substantially, and the activity of catalyzer and effect can keep finely.
The detection index of the Isolongifolene of so producing is as following table:
According to the data of upper table, can show that the Isolongifolene indices synthetic by present method is up to state standards, and reduce corrosion and the pollution of equipment, greatly reduce the loss of solvent, water resources and catalyzer.
Claims (2)
1. the method for the synthetic Isolongifolene of a solid acid catalysis isomery longifolene, comprise the following steps: will after the mixing of longifolene and Glacial acetic acid, put into reaction vessel, add catalyzer, carry out isomerization reaction, reaction is filtered after finishing, catalyst recovery, distillating recovering solvent, rectifying gets final product to obtain the Isolongifolene finished product, it is characterized in that: described catalyzer is solid acid D72 macroporous type strong-acid cation-exchange resin, and the weight ratio of longifolene and Glacial acetic acid and described catalyzer is 1:0.4～1.2:0.1～0.3;
Temperature in described reaction vessel is 60 ° of C～110 ° C, and the reaction times is 4～6 hours.
2. solid acid catalysis isomery longifolene according to claim 1 synthesizes the method for Isolongifolene, and it is characterized in that: the weight ratio of longifolene and Glacial acetic acid and described catalyzer is 1:1:0.2.
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| CN2013103779357A CN103435433A (en) | 2013-08-27 | 2013-08-27 | Method for synthesizing isolongifolene by catalytically isomerizing longifolene with solid acid |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104151128A (en) * | 2014-08-21 | 2014-11-19 | 梧州市嘉盈树胶有限公司 | Preparation method of isolongifolene |
| CN104945218A (en) * | 2015-07-06 | 2015-09-30 | 梧州市嘉盈树胶有限公司 | Method for preparing high-purity isolongifolene |
| CN106117005A (en) * | 2016-06-27 | 2016-11-16 | 广西梧松林化集团有限公司 | The preparation method of high-purity isolonglifolene |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1680225A (en) * | 2005-01-18 | 2005-10-12 | 南京大学 | Method and apparatus for preparing isolongifolene from longifolene |
-
2013
- 2013-08-27 CN CN2013103779357A patent/CN103435433A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1680225A (en) * | 2005-01-18 | 2005-10-12 | 南京大学 | Method and apparatus for preparing isolongifolene from longifolene |
Non-Patent Citations (1)
| Title |
|---|
| 蒋凤池，李希成: "异长叶烯的Prins反应", 《林产化学与工业》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104151128A (en) * | 2014-08-21 | 2014-11-19 | 梧州市嘉盈树胶有限公司 | Preparation method of isolongifolene |
| CN104945218A (en) * | 2015-07-06 | 2015-09-30 | 梧州市嘉盈树胶有限公司 | Method for preparing high-purity isolongifolene |
| CN106117005A (en) * | 2016-06-27 | 2016-11-16 | 广西梧松林化集团有限公司 | The preparation method of high-purity isolonglifolene |
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Application publication date: 20131211 |