CN104945218A - Method for preparing high-purity isolongifolene - Google Patents
Method for preparing high-purity isolongifolene Download PDFInfo
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- CN104945218A CN104945218A CN201510387056.1A CN201510387056A CN104945218A CN 104945218 A CN104945218 A CN 104945218A CN 201510387056 A CN201510387056 A CN 201510387056A CN 104945218 A CN104945218 A CN 104945218A
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- isolongifolene
- catalyzer
- longifolene
- vanadium oxide
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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
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Abstract
The invention discloses a method for preparing high-purity isolongifolene and relates to the technical field of preparing of forestry chemical products. According to the method, alkoxide of vanadium is hydrolyzed and sulfated through sulfuric acid, vanadium oxide which is sulfated is obtained, and then is dried and calcinated, after calcinating, the vanadium oxide is mixed with cation exchange resin after the temperature is reduced to 40 DEG C, and catalyst is obtained; the catalyst is added to longifolene, the reaction is conducted for two or more hours under the temperature of 120-140 DEG C according to the mass ratio of 1-30:100 of the catalyst and the longifolene, and reaction liquid is filtered out after the reaction. The isolongifolene is high in yield and can reach 92% or higher, meanwhile, the catalyst is easily separated and reused, and the production cost is reduced.
Description
Technical field
The present invention relates to silvichemical preparing technical field, especially a kind of preparation method of high purity Isolongifolene.
Background technology
Isolongifolene (Isolongifolene), colourless liquid, boiling range 123-142 & ordm, C/15mmHg, proportion 0.9230-0.9350, refractive index 1.4995-1.5001, specific rotation-17.42 & ordm, purity 86-80% is the raw material of the spices such as synthesis ω-AML, ω-HML, isolongifanone, Isolongifolene alkane ketone.
Isolongifolene is through catalytic isomerization products therefrom by the longifolene in heavy turpentine, the same with longifolene is also a kind of sesquiterpene, be a kind of novel raw material in synthetic perfume industry, the spices such as isolongifanone, Isolongifolenone, Isolongifolene alcohol, isolongifolenyl acetate, amborol can be synthesized; Itself there is banksia rose fragrance, with being widely used in modern synthetic perfume industry.
At present, conventional synthetic method take acetic acid as solvent, and the vitriol oil is the isomerization reaction that catalyzer carries out longifolene, because sulfuric acid has corrodibility and pungency, serious to equipment corrosion, and liquid waste disposal expense is large, and production cost is high.
Summary of the invention
The technical problem that the present invention solves is to provide a kind of preparation method of economical and practical, high purity Isolongifolene that energy consumption is little.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
The preparation of step 1, catalyzer: by the hydrolysis of alkoxide of vanadium, and use sulfate sulfatase, obtains Sulfated vanadium oxide, then this vanadium oxide dry, then calcines, and mixes again, obtain catalyzer after calcining after temperature drops to 40 DEG C with Zeo-karb;
Step 2, by the catalyzer of step 1 gained, be the mass ratio of 1-30:100 by catalyzer and the ratio of longifolene, described catalyzer will be added in longifolene, react more than 2 hours at 120 DEG C ~ 140 DEG C, after reaction, leach reaction solution.
In technique scheme, technical scheme can also be more specifically: the drying temperature of described vanadium oxide is 100 DEG C, and time of drying is 5 hours; Calcining after dry, the temperature of calcining is 550 DEG C ~ 600 DEG C, and calcination time is 4-6 hour.
Further, described longifolene material content is 80%-90%.
Further, described Zeo-karb adopts light-duty ion exchange resin.
Further: in described catalyzer, by weight, described vanadium oxide is 40 parts ~ 60 parts, and Zeo-karb is 40 parts ~ 60 parts.
Owing to adopting technique scheme, the present invention compared with prior art, has following beneficial effect:
The catalyzer adopting Sulfated vanadium oxide and Zeo-karb to be mutually combined into due to the present invention carries out catalyzed reaction to longifolene, and Isolongifolene yield is high, can reach more than 92%; Meanwhile, catalyzer is easy to be separated and recycling, reduces production cost.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, and protection scope of the present invention is not only confined to following examples.
Embodiment 1
By the hydrolysis of alkoxide of vanadium, and use sulfate sulfatase, obtain Sulfated vanadium oxide, then at the temperature of 100 DEG C, carry out drying to this vanadium oxide, time of drying is 5 hours, calcine again, the temperature of calcining is 550 DEG C, calcines 4 hours, after calcining after temperature drops to 40 DEG C, mix with Zeo-karb again, obtain catalyzer; Wherein, the weight part that vanadium oxide accounts for is 40 parts, Zeo-karb 60 parts;
Contain in the longifolene solution of 80% at 100g, add the above-mentioned catalyzer of 1g, stir and temperature is risen to 120 DEG C, react after 2 hours, leach reaction solution, gas chromatographic analysis shows, the transformation efficiency of longifolene is 80%, and isomery yield is 92%.
Embodiment 2
By the hydrolysis of alkoxide of vanadium, and use sulfate sulfatase, obtain Sulfated vanadium oxide, then at the temperature of 100 DEG C, carry out drying to this vanadium oxide, time of drying is 5 hours, calcine again, the temperature of calcining is 600 DEG C, calcines 6 hours, after calcining after temperature drops to 40 DEG C, mix with Zeo-karb again, obtain catalyzer; Wherein, the weight part that vanadium oxide accounts for is 60 parts, Zeo-karb 40 parts;
Contain in the longifolene solution of 90% at 100g, add the above-mentioned catalyzer of 30g, stir and temperature is risen to 140 DEG C, react after 4 hours, leach reaction solution, gas chromatographic analysis shows, the transformation efficiency of longifolene is 92%, and isomery yield is 95%.
Embodiment 3
By the hydrolysis of alkoxide of vanadium, and use sulfate sulfatase, obtain Sulfated vanadium oxide, then at the temperature of 100 DEG C, carry out drying to this vanadium oxide, time of drying is 5 hours, calcine again, the temperature of calcining is 560 DEG C, calcines 4 hours, after calcining after temperature drops to 40 DEG C, mix with Zeo-karb again, obtain catalyzer; Wherein, the weight part that vanadium oxide accounts for is 50 parts, Zeo-karb 50 parts;
Contain in the longifolene solution of 85% at 100g, add the above-mentioned catalyzer of 10g, stir and temperature is risen to 130 DEG C, react after 3 hours, leach reaction solution, gas chromatographic analysis shows, the transformation efficiency of longifolene is 85%, and isomery yield is 93%.
Claims (5)
1. a preparation method for high purity Isolongifolene, is characterized in that:
The preparation of step 1, catalyzer: by the hydrolysis of alkoxide of vanadium, and use sulfate sulfatase, obtains Sulfated vanadium oxide, then this vanadium oxide dry, then calcines, and mixes again, obtain catalyzer after calcining after temperature drops to 40 DEG C with Zeo-karb;
Step 2, by the catalyzer of step 1 gained, be the mass ratio of 1-30:100 by catalyzer and the ratio of longifolene, described catalyzer will be added in longifolene, react more than 2 hours at 120 DEG C ~ 140 DEG C, after reaction, leach reaction solution.
2. the preparation method of high purity Isolongifolene according to claim 1, is characterized in that: the drying temperature of described vanadium oxide is 100 DEG C, and time of drying is 5 hours; Calcining after dry, the temperature of calcining is 550 DEG C ~ 600 DEG C, and calcination time is 4-6 hour.
3. the preparation method of high purity Isolongifolene according to claim 1, is characterized in that: described longifolene material content is 80%-90%.
4. the preparation method of high purity Isolongifolene according to claim 1, is characterized in that: described Zeo-karb adopts light-duty ion exchange resin.
5. the preparation method of high purity Isolongifolene according to claim 1, is characterized in that: in described catalyzer, by weight, and described vanadium oxide is 40 parts ~ 60 parts, and Zeo-karb is 40 parts ~ 60 parts.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510387056.1A CN104945218A (en) | 2015-07-06 | 2015-07-06 | Method for preparing high-purity isolongifolene |
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| CN201510387056.1A CN104945218A (en) | 2015-07-06 | 2015-07-06 | Method for preparing high-purity isolongifolene |
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| CN104945218A true CN104945218A (en) | 2015-09-30 |
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| CN201510387056.1A Pending CN104945218A (en) | 2015-07-06 | 2015-07-06 | Method for preparing high-purity isolongifolene |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1460668A (en) * | 2003-06-02 | 2003-12-10 | 厦门中坤化学有限公司 | Preparation method of isologifolic olefince |
| CN1849280A (en) * | 2003-05-30 | 2006-10-18 | 科学与工业研究委员会 | Catalytic process for the preparation of isolongifolene |
| CN103435433A (en) * | 2013-08-27 | 2013-12-11 | 梧州市松桦化学品有限公司 | Method for synthesizing isolongifolene by catalytically isomerizing longifolene with solid acid |
| CN104151128A (en) * | 2014-08-21 | 2014-11-19 | 梧州市嘉盈树胶有限公司 | Preparation method of isolongifolene |
-
2015
- 2015-07-06 CN CN201510387056.1A patent/CN104945218A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1849280A (en) * | 2003-05-30 | 2006-10-18 | 科学与工业研究委员会 | Catalytic process for the preparation of isolongifolene |
| CN1460668A (en) * | 2003-06-02 | 2003-12-10 | 厦门中坤化学有限公司 | Preparation method of isologifolic olefince |
| CN103435433A (en) * | 2013-08-27 | 2013-12-11 | 梧州市松桦化学品有限公司 | Method for synthesizing isolongifolene by catalytically isomerizing longifolene with solid acid |
| CN104151128A (en) * | 2014-08-21 | 2014-11-19 | 梧州市嘉盈树胶有限公司 | Preparation method of isolongifolene |
Non-Patent Citations (2)
| Title |
|---|
| 赵振东等: "催化剂对橙花叔醇异构化反应影响的研究", 《林产化学与工业》 * |
| 黄宇平等: "钒化合物催化芳樟醇酯化异构制取香叶醇、橙花醇", 《林产化工通讯》 * |
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Application publication date: 20150930 |
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