CN104211551A - Preparation method of isolongifolene - Google Patents
Preparation method of isolongifolene Download PDFInfo
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- CN104211551A CN104211551A CN201410399414.6A CN201410399414A CN104211551A CN 104211551 A CN104211551 A CN 104211551A CN 201410399414 A CN201410399414 A CN 201410399414A CN 104211551 A CN104211551 A CN 104211551A
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- isolongifolene
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- longifolene
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Abstract
The invention discloses a preparation method of isolongifolene. The preparation method comprises the following steps: sequentially adding longifolene and a catalyst into a reaction kettle, uniformly stirring, introducing supersonic waves into the reaction kettle, gradually heating to 90-100DEG C, and carrying out an isomerization reaction for 45-60min to obtain isolongifolene, wherein the catalyst is one or two or more of zinc oxide, cobalt acetate and sodium hyposulfite. The method has the advantages of shortening of the reaction time, increase of the raw material conversion rate, and high purity of the above obtained product.
Description
Technical field
The present invention relates to terpene hydrocarbon processing technique field, especially a kind of preparation method of Isolongifolene.
Background technology
Isolongifolene is a kind of sesquiterpene of the longifolene process catalytic isomerization gained in heavy turpentine, Isolongifolene is usually used to the spices such as synthetic isolongifanone, Isolongifolenone, Isolongifolene alcohol, isolongifolenyl acetate, amborol, owing to itself thering is banksia rose fragrance, therefore, being widely used in modern synthetic perfume industry.
At present, it is catalyzer that the synthetic method of Isolongifolene normally be take single organic acid or mineral acid, and the activity of these catalyzer is all undesirable, can not make isomerization reaction efficiently, carry out fast, has affected reaction efficiency.
Summary of the invention
The preparation method who the object of this invention is to provide a kind of Isolongifolene, this method can solve the problem that reaction efficiency is low.
In order to address the above problem, the technical solution used in the present invention is: the preparation method of this Isolongifolene, comprise the following steps: in reactor, add longifolene and catalyzer successively, stir, in reactor, pass into ultrasonic wave, progressively be warming up to 90 ℃～100 ℃, isomerization reaction 45 minutes～60 minutes, can obtain Isolongifolene; Wherein, described catalyzer is zinc oxide, cobaltous acetate, one or more in three kinds of materials of Sulfothiorine.
In technique scheme, scheme can also be more specifically: the addition of described catalyzer is 0.05%～0.1% of longifolene total mass.
Further, hyperacoustic power is 1400 watts～1500 watts.
Further, the massfraction of described longifolene is 60%～65%.
Owing to having adopted technique scheme, the present invention compared with prior art has following beneficial effect:
The present invention is with zinc oxide, cobaltous acetate, one or more in three kinds of materials of Sulfothiorine are as catalyzer, and in reaction process, passed into ultrasonic wave, make on the one hand reaction all to carry out fast and efficiently, compare the preparation method of traditional Isolongifolene, the present invention has shortened the time of reaction greatly; On the other hand, side reaction is few, and the transformation efficiency of raw material is higher higher with product purity.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1
In reactor, adding longifolene and the 1 gram of catalyzer that 1 kilogram-mass mark is 63% successively, stir, is the ultrasonic wave of 1400 watts to passing into power in reactor, is progressively warming up to 100 ℃, and isomerization reaction 45 minutes, obtains Isolongifolene.
Catalyzer in the present embodiment is Sulfothiorine.
Embodiment 2
In reactor, adding longifolene and the 25 grams of catalyzer that 50 kilogram-mass marks are 61% successively, stir, is the ultrasonic wave of 1450 watts to passing into power in reactor, is progressively warming up to 90 ℃, and isomerization reaction 60 minutes, obtains Isolongifolene.
Catalyzer in the present embodiment is Sulfothiorine.
Embodiment 3
To adding double centner massfraction in reactor, being 65% longifolene and 75 grams of catalyzer successively, stirring, is the ultrasonic wave of 1500 watts to passing into power in reactor, is progressively warming up to 95 ℃, and isomerization reaction 50 minutes, obtains Isolongifolene.
Catalyzer in the present embodiment is the mixture of zinc oxide and cobaltous acetate.
Claims (4)
1. a preparation method for Isolongifolene, is characterized in that comprising the following steps: in reactor, add longifolene and catalyzer successively, stir, in reactor, pass into ultrasonic wave, progressively be warming up to 90 ℃～100 ℃, isomerization reaction 45 minutes～60 minutes, can obtain Isolongifolene; Wherein, described catalyzer is zinc oxide, cobaltous acetate, one or more in three kinds of materials of Sulfothiorine.
2. the preparation method of Isolongifolene according to claim 1, is characterized in that: the addition of described catalyzer is 0.05%～0.1% of longifolene total mass.
3. the preparation method of Isolongifolene according to claim 1, is characterized in that: the massfraction of described longifolene is 60%～65%.
4. the preparation method of Isolongifolene according to claim 1, is characterized in that: hyperacoustic power is 1400 watts～1500 watts.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410399414.6A CN104211551B (en) | 2014-08-14 | 2014-08-14 | The preparation method of isolonglifolene |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410399414.6A CN104211551B (en) | 2014-08-14 | 2014-08-14 | The preparation method of isolonglifolene |
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| CN104211551A true CN104211551A (en) | 2014-12-17 |
| CN104211551B CN104211551B (en) | 2016-10-12 |
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Citations (3)
| 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 |
| 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 |
| BRPI0802801A2 (en) * | 2008-06-10 | 2010-03-02 | Univ Minas Gerais | Method of Obtaining Isolongifolene by Isomerizing Longifolene Using an Acid |
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2014
- 2014-08-14 CN CN201410399414.6A patent/CN104211551B/en active Active
Patent Citations (3)
| 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 |
| CN1680225A (en) * | 2005-01-18 | 2005-10-12 | 南京大学 | Method and apparatus for preparing isolongifolene from longifolene |
| BRPI0802801A2 (en) * | 2008-06-10 | 2010-03-02 | Univ Minas Gerais | Method of Obtaining Isolongifolene by Isomerizing Longifolene Using an Acid |
Non-Patent Citations (3)
| Title |
|---|
| 周国斌等: "用S2O82-改性的TiO2固体超强酸催化合成异长叶烯", 《江西师范大学学报（自然科学版）》, vol. 25, no. 3, 31 August 2001 (2001-08-31) * |
| 王石发等: "长叶烯异构化反应的研究", 《林产化学与工业》, vol. 14, no. 4, 31 December 1994 (1994-12-31) * |
| 黄建康等: "L-脯氨甲酰基二茂铁的合成及表征", 《广东化工》, vol. 39, no. 17, 15 December 2012 (2012-12-15) * |
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| CN104211551B (en) | 2016-10-12 |
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