CN104909985B - The preparation method of dihydroterpineol - Google Patents
The preparation method of dihydroterpineol Download PDFInfo
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- CN104909985B CN104909985B CN201510276919.8A CN201510276919A CN104909985B CN 104909985 B CN104909985 B CN 104909985B CN 201510276919 A CN201510276919 A CN 201510276919A CN 104909985 B CN104909985 B CN 104909985B
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- hydrogenation reaction
- hydrogen
- dihydroterpineol
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/17—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrogenation of carbon-to-carbon double or triple bonds
- C07C29/172—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrogenation of carbon-to-carbon double or triple bonds with the obtention of a fully saturated alcohol
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/14—The ring being saturated
Abstract
The present invention discloses the preparation method of a kind of dihydroterpineol, belongs to silvichemical preparing technical field.100 parts of terpineol and 1 part～5 parts of Raney's nickels by a certain percentage, are put in reactor, and are heated to 60 DEG C～65 DEG C by the present invention, then it is passed through hydrogen to this reactor, and carries out hydrogenation reaction, last cooling discharging by certain operation condition, and stratification, filtration, prepare.The present invention coordinates the corresponding proportioning raw materials of the present invention, so that the yield of product dihydroterpineol is improved by the operating condition regulating its hydrogenation process.
Description
Technical field
The invention belongs to silvichemical preparing technical field, particularly relate to the preparation method of a kind of dihydroterpineol.
Background technology
Dihydroterpineol has another name called hydrogenation terpineol, and it has several isomerss, is a kind of colourless oil liquid, there is happy happy Syringa oblata Lindl. fragrance, and lasting fragrance, be a kind of good mediation flavor of raw material and good solvent, can be used for preparing hydrogen peroxide, paint etc., of many uses.
At present, the preparation technology that dihydroterpineol is conventional is generally that Raney's nickel is catalyst with terpineol as raw material, is prepared by catalytic hydrogenation.But this technique is the most perfect, the yield of its dihydroterpineol prepared is not the highest.
Summary of the invention
The present invention provides the preparation method of a kind of dihydroterpineol, and the method can solve dihydroterpineol and commonly use preparation technology and prepare dihydroterpineol and there is the problem that yield is low.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:
It comprises the following steps:
A, by weight, puts into 100 parts of terpineol and 1 part～5 parts of Raney's nickels in reactor, and is heated to 60 DEG C～65 DEG C；
B, after step A, be passed through hydrogen to this reactor, and carry out hydrogenation reaction by following operating condition:
Hydrogen preheating temperature: 60 DEG C～65 DEG C；
Hydrogen purity: ＞ 99.9%；
Hydrogenation reaction temperature: 60 DEG C～65 DEG C；
Hydrogenation reaction pressure: 0.01MPa～0.1
MPa；
Hydrogenation reaction time: 1h～3h；
C, after step B, cooling discharging, and stratification, filtration, prepare.
In technique scheme, more specifically technical scheme is: in described step B:
Hydrogen preheating temperature: 62 DEG C；
Hydrogen purity: 99.99%；
Hydrogenation reaction temperature: 62 DEG C；
Hydrogenation reaction pressure: 0.01MPa；
Hydrogenation reaction time: 3h.
Owing to using technique scheme, the present invention obtains providing the benefit that:
The present invention coordinates the corresponding proportioning raw materials of the present invention, so that the yield of product dihydroterpineol is improved by the operating condition regulating its hydrogenation process.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described, and protection scope of the present invention is not intended to be limited to following example.
Embodiment 1
The preparation method of this dihydroterpineol comprises the following steps:
A, 1000g terpineol and 10g Raney's nickel are put in reactor, and be heated to 62 DEG C；
B, after step A, be passed through hydrogen to this reactor, and carry out hydrogenation reaction by following operating condition:
Hydrogen preheating temperature: 62 DEG C；
Hydrogen purity: 99.99%；
Hydrogenation reaction temperature: 62 DEG C；
Hydrogenation reaction pressure: 0.01MPa；
Hydrogenation reaction time: 3h；
C, after step B, cooling discharging, and stratification, filtration, prepare.
The yield of the dihydroterpineol that the present embodiment prepares is 99.5%.
Embodiment 2
The preparation method of this dihydroterpineol comprises the following steps:
A, 1000g terpineol and 50g Raney's nickel are put in reactor, and be heated to 65 DEG C；
B, after step A, be passed through hydrogen to this reactor, and carry out hydrogenation reaction by following operating condition:
Hydrogen preheating temperature: 65 DEG C；
Hydrogen purity: 99.95%；
Hydrogenation reaction temperature: 65 DEG C；
Hydrogenation reaction pressure: 0.1 MPa；
Hydrogenation reaction time: 1h；
C, after step B, cooling discharging, and stratification, filtration, prepare.
The yield of the dihydroterpineol that the present embodiment prepares is 99.6%.
Embodiment 3
The preparation method of this dihydroterpineol comprises the following steps:
A, 1000g terpineol and 30g Raney's nickel are put in reactor, and be heated to 60 DEG C；
B, after step A, be passed through hydrogen to this reactor, and carry out hydrogenation reaction by following operating condition:
Hydrogen preheating temperature: 60 DEG C；
Hydrogen purity: 99.98%；
Hydrogenation reaction temperature: 60 DEG C；
Hydrogenation reaction pressure: 0.05MPa；
Hydrogenation reaction time: 2h；
C, after step B, cooling discharging, and stratification, filtration, prepare.
The yield of the dihydroterpineol that the present embodiment prepares is 99.7%.
Claims (3)
1. the preparation method of a dihydroterpineol, it is characterised in that comprise the following steps:
100 parts of terpineol and 1 part of Raney's nickel are put in reactor, and are heated to 62 DEG C by A, by weight；
B, after step A, be passed through hydrogen to this reactor, and carry out hydrogenation reaction by following operating condition:
Hydrogen preheating temperature: 62 DEG C；
Hydrogen purity: 99.99%；
Hydrogenation reaction temperature: 62 DEG C；
Hydrogenation reaction pressure: 0.01MPa；
Hydrogenation reaction time: 3h；
C, after step B, cooling discharging, and stratification, filtration, prepare.
2. the preparation method of a dihydroterpineol, it is characterised in that comprise the following steps:
100 parts of terpineol and 5 parts of Raney's nickels are put in reactor, and are heated to 65 DEG C by A, by weight；
B, after step A, be passed through hydrogen to this reactor, and carry out hydrogenation reaction by following operating condition:
Hydrogen preheating temperature: 65 DEG C；
Hydrogen purity: 99.95%；
Hydrogenation reaction temperature: 65 DEG C；
Hydrogenation reaction pressure: 0.1 MPa；
Hydrogenation reaction time: 1h；
C, after step B, cooling discharging, and stratification, filtration, prepare.
3. the preparation method of a dihydroterpineol, it is characterised in that comprise the following steps:
100 parts of terpineol and 3 parts of Raney's nickels are put in reactor, and are heated to 60 DEG C by A, by weight；
B, after step A, be passed through hydrogen to this reactor, and carry out hydrogenation reaction by following operating condition:
Hydrogen preheating temperature: 60 DEG C；
Hydrogen purity: 99.98%；
Hydrogenation reaction temperature: 60 DEG C；
Hydrogenation reaction pressure: 0.05MPa；
Hydrogenation reaction time: 2h；
C, after step B, cooling discharging, and stratification, filtration, prepare.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510276919.8A CN104909985B (en) | 2015-05-27 | 2015-05-27 | The preparation method of dihydroterpineol |
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| CN201510276919.8A CN104909985B (en) | 2015-05-27 | 2015-05-27 | The preparation method of dihydroterpineol |
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| CN104909985A CN104909985A (en) | 2015-09-16 |
| CN104909985B true CN104909985B (en) | 2016-08-24 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2600934C1 (en) * | 2015-10-06 | 2016-10-27 | Акционерное общество "Управляющая компания "Биохимического холдинга "Оргхим" | Method of producing dihydroterpineol |
| CN112707792A (en) * | 2020-12-25 | 2021-04-27 | 厦门中坤化学有限公司 | Method for increasing cis-dihydroterpineol content in terpineol hydrogenation reaction |
| CN114045103A (en) * | 2021-11-23 | 2022-02-15 | 合众（佛山）化工有限公司 | Modified polyurethane resin water-based paint with lasting fragrance |
| CN114045096A (en) * | 2021-11-23 | 2022-02-15 | 合众（佛山）化工有限公司 | Modified water-based alkyd resin functional coating |
| CN113999380A (en) * | 2021-11-23 | 2022-02-01 | 合众（佛山）化工有限公司 | Hydrogenated terpineol modified waterborne alkyd resin and preparation method thereof |
| CN114149557A (en) * | 2021-11-23 | 2022-03-08 | 合众（佛山）化工有限公司 | Hydrogenated terpineol end-capped aqueous polyurethane resin and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104607207A (en) * | 2015-01-21 | 2015-05-13 | 江西创赢香精香料科技协同创新有限公司 | Titanium-salt-modified Raney nickel catalyst and method for synthesizing dihydroterpineol |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0952854A (en) * | 1995-08-09 | 1997-02-25 | Kao Corp | Production of alpha-dihydroterpineol |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104607207A (en) * | 2015-01-21 | 2015-05-13 | 江西创赢香精香料科技协同创新有限公司 | Titanium-salt-modified Raney nickel catalyst and method for synthesizing dihydroterpineol |
Non-Patent Citations (2)
| Title |
|---|
| 二氢松油醇生产工艺的改进;陈正桂;《林产化工通讯》;20021231;第36卷(第3期);第32-33页 * |
| 催化加氢合成二氢松油醇的研究;黄宗凉等;《精细石油化工》;20020730(第4期);第23-26页 * |
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