CN104909979A - Method for preparing high-purity isolongifolene - Google Patents
Method for preparing high-purity isolongifolene Download PDFInfo
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- CN104909979A CN104909979A CN201510286250.0A CN201510286250A CN104909979A CN 104909979 A CN104909979 A CN 104909979A CN 201510286250 A CN201510286250 A CN 201510286250A CN 104909979 A CN104909979 A CN 104909979A
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Abstract
The invention discloses a method for preparing high-purity isolongifolene and belongs to the technical field of preparation of forestry chemical products. The method comprises the steps of putting 100 parts by weight of longifolene into a reactor, heating the reactor to the temperature of 100-105 DEG C, then, adding 15 parts by weight of catalyst into the reactor, stirring for 8 hours at a constant temperature, then, cooling and discharging. According to the method, through adding the catalyst, which is prepared by a specific method, during preparation, the purity of prepared isolongifolene can be effectively improved.
Description
Technical field
The invention belongs to silvichemical preparing technical field, particularly relate to a kind of preparation method of high purity Isolongifolene.
Background technology
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, the purity of the Isolongifolene obtained according to conventional synthetic method is not very high always, and this makes the application of Isolongifolene be subject to certain restrictions.
Summary of the invention
The technical problem that the present invention solves is to provide a kind of preparation method of high purity Isolongifolene, and the Isolongifolene purity that the method obtains is high.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
By weight, 100 parts of longifolenes are put into reactor, be heated to 100 DEG C ~ 105 DEG C, then in this reactor, add 15 parts of catalyzer, constant temperature stirs 8 hours, then cooling discharging;
Wherein, the raw material of described catalyzer is made up of the component of following weight part:
30 parts ~ 45 parts Zeo-karbs, 30 parts ~ 35 parts zirconium whites, 10 parts ~ 15 parts silicon-dioxide and 50 parts ~ 60 part 98% vitriol oils;
The preparation method of this catalyzer comprises the following steps:
A, by above-mentioned parts by weight, zirconium white, silicon-dioxide are put into 98% vitriol oil acidifying 1 hour;
B, at 50 DEG C ~ 55 DEG C, carry out drying by under the zirconium white after step A acidification, silicon-dioxide, and then carry out calcining 4 hours at 550 DEG C ~ 600 DEG C;
C, the zirconium white after step B calcination processing, silicon-dioxide are mixed with Zeo-karb while hot obtained.
In technique scheme, technical scheme is more specifically: 30 parts of Zeo-karbs, 35 parts of zirconium whites, 12 parts of silicon-dioxide and 50 part of 98% vitriol oil;
Further, 45 parts of Zeo-karbs, 32 parts of zirconium whites, 10 parts of silicon-dioxide and 55 part of 98% vitriol oil.
Further, 40 parts of Zeo-karbs, 30 parts of zirconium whites, 15 parts of silicon-dioxide and 60 part of 98% vitriol oil.
Owing to adopting technique scheme, the beneficial effect that the present invention obtains is:
The present invention by adding in preparation process through the obtained catalyzer of ad hoc approach, thus makes the purity of the Isolongifolene obtained be effectively improved.
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
The preparation method of this high purity Isolongifolene is as follows:
1000g longifolene is put into reactor, is heated to 100 DEG C ~ 105 DEG C, then in this reactor, add 150g catalyzer, constant temperature stirs 8 hours, then cooling discharging;
Wherein, the raw material of described catalyzer is composed of the following components:
3000g Zeo-karb, 3500g zirconium white, 1200g silicon-dioxide and the 5000g98% vitriol oil;
The preparation method of this catalyzer comprises the following steps:
A, zirconium white, silicon-dioxide are put into 98% vitriol oil acidifying 1 hour;
B, at 50 DEG C ~ 55 DEG C, carry out drying by under the zirconium white after step A acidification, silicon-dioxide, and then carry out calcining 4 hours at 550 DEG C ~ 600 DEG C;
C, the zirconium white after step B calcination processing, silicon-dioxide are mixed with Zeo-karb while hot obtained.
The high purity 95% of the Isolongifolene that the present embodiment obtains.
Embodiment 2
The preparation method of this high purity Isolongifolene is as follows:
1000g longifolene is put into reactor, is heated to 100 DEG C ~ 105 DEG C, then in this reactor, add 150g catalyzer, constant temperature stirs 8 hours, then cooling discharging;
Wherein, the raw material of described catalyzer is composed of the following components:
4500g Zeo-karb, 3200g zirconium white, 1000g silicon-dioxide and the 5500g98% vitriol oil;
The preparation method of this catalyzer comprises the following steps:
A, zirconium white, silicon-dioxide are put into 98% vitriol oil acidifying 1 hour;
B, at 50 DEG C ~ 55 DEG C, carry out drying by under the zirconium white after step A acidification, silicon-dioxide, and then carry out calcining 4 hours at 550 DEG C ~ 600 DEG C;
C, the zirconium white after step B calcination processing, silicon-dioxide are mixed with Zeo-karb while hot obtained.
The high purity 95.5% of the Isolongifolene that the present embodiment obtains.
Embodiment 3
The preparation method of this high purity Isolongifolene is as follows:
1000g longifolene is put into reactor, is heated to 100 DEG C ~ 105 DEG C, then in this reactor, add 150g catalyzer, constant temperature stirs 8 hours, then cooling discharging;
Wherein, the raw material of described catalyzer is composed of the following components:
4000g Zeo-karb, 3000g zirconium white, 1500g silicon-dioxide and the 6000g98% vitriol oil;
Its preparation method comprises the following steps:
A, zirconium white, silicon-dioxide are put into 98% vitriol oil acidifying 1 hour;
B, at 50 DEG C ~ 55 DEG C, carry out drying by under the zirconium white after step A acidification, silicon-dioxide, and then carry out calcining 4 hours at 550 DEG C ~ 600 DEG C;
C, the zirconium white after step B calcination processing, silicon-dioxide are mixed with Zeo-karb while hot obtained.
The high purity 96% of the Isolongifolene that the present embodiment obtains.
Claims (4)
1. a preparation method for high purity Isolongifolene, is characterized in that:
By weight, 100 parts of longifolenes are put into reactor, be heated to 100 DEG C ~ 105 DEG C, then in this reactor, add 15 parts of catalyzer, constant temperature stirs 8 hours, then cooling discharging;
Wherein, the raw material of described catalyzer is made up of the component of following weight part:
30 parts ~ 45 parts Zeo-karbs, 30 parts ~ 35 parts zirconium whites, 10 parts ~ 15 parts silicon-dioxide and 50 parts ~ 60 part 98% vitriol oils;
The preparation method of this catalyzer comprises the following steps:
A, by above-mentioned parts by weight, zirconium white, silicon-dioxide are put into 98% vitriol oil acidifying 1 hour;
B, at 50 DEG C ~ 55 DEG C, carry out drying by under the zirconium white after step A acidification, silicon-dioxide, and then carry out calcining 4 hours at 550 DEG C ~ 600 DEG C;
C, the zirconium white after step B calcination processing, silicon-dioxide are mixed with Zeo-karb while hot obtained.
2. the preparation method of Isolongifolene production catalyst composition according to claim 1, is characterized in that: 30 parts of Zeo-karbs, 35 parts of zirconium whites, 12 parts of silicon-dioxide and 50 part of 98% vitriol oil.
3. the preparation method of Isolongifolene production catalyst composition according to claim 1, is characterized in that: 45 parts of Zeo-karbs, 32 parts of zirconium whites, 10 parts of silicon-dioxide and 55 part of 98% vitriol oil.
4. the preparation method of Isolongifolene production catalyst composition according to claim 1, is characterized in that: 40 parts of Zeo-karbs, 30 parts of zirconium whites, 15 parts of silicon-dioxide and 60 part of 98% vitriol oil.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510286250.0A CN104909979A (en) | 2015-05-29 | 2015-05-29 | Method for preparing high-purity isolongifolene |
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| CN201510286250.0A CN104909979A (en) | 2015-05-29 | 2015-05-29 | Method for preparing high-purity isolongifolene |
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Citations (2)
| 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 |
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2015
- 2015-05-29 CN CN201510286250.0A patent/CN104909979A/en active Pending
Patent Citations (2)
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 周国斌: "固体超强酸催化萜烯化合物异构化反应的研究", 《中国优秀博硕士学位论文全文数据库(硕士)工程科技I辑》, 15 June 2003 (2003-06-15), pages 014 - 76 * |
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Application publication date: 20150916 |
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