CN102952005A - Method for synthesizing isolongifolenone - Google Patents
Method for synthesizing isolongifolenone Download PDFInfo
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- CN102952005A CN102952005A CN2012104598161A CN201210459816A CN102952005A CN 102952005 A CN102952005 A CN 102952005A CN 2012104598161 A CN2012104598161 A CN 2012104598161A CN 201210459816 A CN201210459816 A CN 201210459816A CN 102952005 A CN102952005 A CN 102952005A
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- isolongifolenone
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- isolongifolene
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- oxidizing reaction
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Abstract
The invention discloses a method for synthesizing isolongifolenone. The method comprises the following steps of: adding isolongifolene and a catalyst into a reaction kettle in sequence for performing an oxidation reaction; and filtering, distilling, crystalizing and performing suction filtering in sequence to obtain finished isolongifolenone, wherein cobaltous acetate is taken as the catalyst; the weight part ratio of the catalyst to the isolongifolene is (1-3):100; the oxidizingation reaction comprises stirring a mixture, and jetting mist compressed air into the reaction kettle by using an air compressor for oxidizing the mixture and the air; and the temperature in the reaction kettle is 60-90 DEG C in the oxidizingation reaction, and the oxidizingation reaction is performed for 28-48 hours. Compared with the prior art, the method has the advantage that: the problem of high production cost existing in the conventional isolongifolenone can be solved.
Description
Technical field
The present invention relates to chemical industry rosin deep process technology field, especially a kind of method of using the synthetic Isolongifolenone of Isolongifolene.
Background technology
At present, use in the process of the synthetic Isolongifolenone of Isolongifolene, have a procedure need Isolongifolene in reactor with the abundant oxidation of oxygen, filter again afterwards, the operations such as distillation, crystallization are synthesized Isolongifolenone.Existing Isolongifolene oxidizing reaction, generally be to use oxygen enricher output oxygen enrichment in reactor, make the interior reactant of reactor touch oxygen and obtain oxidation, owing to oxygen enrichment form bubbling with liquid from the take-off equipment of oxygen enricher goes out, oxygen enrichment distributes even not in reactor, contact not comprehensively with reaction mixture, make the oxidation of reaction mixture abundant not; And, equipment-oxygen enricher that the oxygen enrichment of the need of production special use of oxygen enrichment is collected, its price comparison is expensive, and cost of use is also higher, causes the production cost of Isolongifolenone also higher.
Summary of the invention
The invention provides a kind of synthetic method of Isolongifolenone, to solve the high problem of existing Isolongifolenone production cost.
In order to address the above problem, technical scheme of the present invention is: may further comprise the steps: may further comprise the steps: add successively Isolongifolene and catalyzer carries out oxidizing reaction in reactor, filter successively again, distillation, crystallization, suction filtration gets final product to get the Isolongifolenone finished product, and described catalyzer is cobaltous acetate, and the weight part ratio of described catalyzer and Isolongifolene is 1～3:100; Described oxidizing reaction comprises described mixture stirred, and uses simultaneously air compressor machine to spray vaporific pressurized air in the described reactor and makes described mixture and air carry out oxidation; Temperature in the reactor of described oxidizing reaction is 60 ° of C～90 ° C, and the time is 28～48 hours.
In the technique scheme, more specifically scheme can be: the pressure of described distillation is 0.1kpa～5kpa.
Further: the weight part ratio of described catalyzer and Isolongifolene is 2:100; Temperature in the reactor of described oxidizing reaction is 75 ° of C～85 ° C, and the time is 28～32 hours.
Owing to adopted technique scheme, the present invention compared with prior art has following beneficial effect:
The synthetic method of this Isolongifolenone adopts provides oxygen with the vaporific compressed-air actuated mode of the direct injection of pressurized air to the Isolongifolene in the reactor, accessing the mode that allows the oxygen rich gas bubbling in the reactor and go out with the oxygen enricher of prior art compares, spouting vaporific pressurized air increases the air capacity of time per unit reaction mixture contact to some extent, make the more quick and reaction mixture comprehensive engagement of airborne oxygen, make the abundant oxidation of reaction mixture, use to spray the Isolongifolene content of the whole oxidizing reaction of vaporific pressurized air in the reaction mixture less than time of 3%, close with the oxidation time that uses the oxygen supply of oxygen enrichment synthesis device 24～50 hours, and use compressed air unit to replace the oxygen enrichment synthesis device, reaction cost has reduced by 31%～35%.
Embodiment
Embodiment one:
The synthetic method of this Isolongifolenone, process 650 kilograms of Isolongifolenones: with the mixture of the cobaltous acetate of 1000 kilogram of 80% Isolongifolene and 20 kilograms, in reactor, carry out oxidizing reaction, described oxidizing reaction comprises described mixture is stirred, using simultaneously air compressor machine to spray vaporific pressurized air in the described reactor makes described mixture carry out oxidation, temperature in the reactor of oxidizing reaction is controlled at 75 ° of C～85 ° C, after 24 hours, carry out sampling analysis, until Isolongifolene content is less than 3% rear stopped reaction, about 30 hours of the process of whole oxidizing reaction, filter successively again, distillation, crystallization, suction filtration get final product to get the Isolongifolenone finished product, and wherein the pressure of distillation is 0.5kpa.
Embodiment two:
The synthetic method of this Isolongifolenone, process 650 kilograms Isolongifolenone: with the mixture of the cobaltous acetate of 990 kilograms Isolongifolenes and 10 kilograms, in reactor, carry out oxidizing reaction, described oxidizing reaction comprises described mixture is stirred, using simultaneously air compressor machine to spray vaporific pressurized air in the described reactor makes described mixture carry out oxidation, temperature in the reactor of oxidizing reaction is controlled at 90 ° of C, after 24 hours, carry out sampling analysis, until Isolongifolene content is less than 3% rear stopped reaction, about 48 hours of the process of whole oxidizing reaction, filter successively again, distillation, crystallization, suction filtration get final product to get the Isolongifolenone finished product, and wherein the pressure of distillation is 0.25kpa.
Embodiment three:
The synthetic method of this Isolongifolenone, process 650 kilograms Isolongifolenone: with the mixture of the cobaltous acetate of 970 kilograms Isolongifolenes and 30 kilograms, in reactor, carry out oxidizing reaction, described oxidizing reaction comprises described mixture is stirred, using simultaneously air compressor machine to spray vaporific pressurized air in the described reactor makes described mixture carry out oxidation, temperature in the reactor of oxidizing reaction is controlled at 60 ° of C, after 24 hours, carry out sampling analysis, until Isolongifolene content is less than 3% rear stopped reaction, about 28 hours of the process of whole oxidizing reaction, filter successively again, distillation, crystallization, suction filtration get final product to get the Isolongifolenone finished product, and wherein the pressure of distillation is 0.1kpa.
Claims (3)
1. the synthetic method of an Isolongifolenone, may further comprise the steps: in reactor, add successively Isolongifolene and catalyzer carries out oxidizing reaction, filter successively again, distillation, crystallization, suction filtration gets final product to get the Isolongifolenone finished product, it is characterized in that: described catalyzer is cobaltous acetate, and the weight part ratio of described catalyzer and Isolongifolene is 1～3:100;
Described oxidizing reaction comprises described mixture stirred, and uses simultaneously air compressor machine to spray vaporific pressurized air in the described reactor and makes described mixture and air carry out oxidation;
Temperature in the reactor of described oxidizing reaction is 60 ° of C～90 ° C, and the time is 28～48 hours.
2. the synthetic method of Isolongifolenone according to claim 1, it is characterized in that: the pressure of described distillation is 0.1kpa～1.1kpa.
3. the synthetic method of Isolongifolenone according to claim 1 and 2, it is characterized in that: the weight part ratio of described catalyzer and Isolongifolene is 2:100; Temperature in the reactor of described oxidizing reaction is 75 ° of C～85 ° C, and the time is 28～32 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210459816.1A CN102952005B (en) | 2012-11-15 | 2012-11-15 | Method for synthesizing isolongifolenone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210459816.1A CN102952005B (en) | 2012-11-15 | 2012-11-15 | Method for synthesizing isolongifolenone |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102952005A true CN102952005A (en) | 2013-03-06 |
| CN102952005B CN102952005B (en) | 2015-05-06 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201210459816.1A Expired - Fee Related CN102952005B (en) | 2012-11-15 | 2012-11-15 | Method for synthesizing isolongifolenone |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106187722A (en) * | 2016-06-27 | 2016-12-07 | 广西梧松林化集团有限公司 | The production method of Isolongifolenone |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3718698A (en) * | 1969-11-24 | 1973-02-27 | Int Flavors & Fragrances Inc | Isolongifolene processes and product |
| CN1460668A (en) * | 2003-06-02 | 2003-12-10 | 厦门中坤化学有限公司 | Preparation method of isologifolic olefince |
| CN101801901A (en) * | 2007-07-13 | 2010-08-11 | 美国农业部 | Use Isolongifolene ketone and/or the arthropodan method of Isolongifolene keto analog repellent |
-
2012
- 2012-11-15 CN CN201210459816.1A patent/CN102952005B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3718698A (en) * | 1969-11-24 | 1973-02-27 | Int Flavors & Fragrances Inc | Isolongifolene processes and product |
| CN1460668A (en) * | 2003-06-02 | 2003-12-10 | 厦门中坤化学有限公司 | Preparation method of isologifolic olefince |
| CN101801901A (en) * | 2007-07-13 | 2010-08-11 | 美国农业部 | Use Isolongifolene ketone and/or the arthropodan method of Isolongifolene keto analog repellent |
Non-Patent Citations (4)
| Title |
|---|
| 刘震等: "异长叶烯的空气催化氧化反应", 《林产化学与工业》, vol. 17, no. 2, 30 June 1997 (1997-06-30), pages 1 - 6 * |
| 武法文等: "Membrane-based air separation for catalytic oxidation of isolongifolene", 《CHEMICAL ENGINEERING JOURNAL》, vol. 158, 31 December 2010 (2010-12-31), pages 426 - 430 * |
| 武法文等: "异长叶烯酮的绿色合成", 《精细化工》, vol. 26, no. 1, 30 November 2009 (2009-11-30), pages 1116 - 1119 * |
| 武法文等: "膜法富氧空气用于异长叶烯烃催化氧化研究", 《南京大学学报》, vol. 42, no. 2, 31 March 2006 (2006-03-31), pages 163 - 169 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106187722A (en) * | 2016-06-27 | 2016-12-07 | 广西梧松林化集团有限公司 | The production method of Isolongifolenone |
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| CN102952005B (en) | 2015-05-06 |
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