CN104926610B - The preparation method of dihydromyrcenol - Google Patents
The preparation method of dihydromyrcenol Download PDFInfo
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- CN104926610B CN104926610B CN201510276832.0A CN201510276832A CN104926610B CN 104926610 B CN104926610 B CN 104926610B CN 201510276832 A CN201510276832 A CN 201510276832A CN 104926610 B CN104926610 B CN 104926610B
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- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/03—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by addition of hydroxy groups to unsaturated carbon-to-carbon bonds, e.g. with the aid of H2O2
- C07C29/04—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by addition of hydroxy groups to unsaturated carbon-to-carbon bonds, e.g. with the aid of H2O2 by hydration of carbon-to-carbon double bonds
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Abstract
The present invention discloses the preparation method of a kind of dihydromyrcenol, belongs to silvichemical preparing technical field.36% acetic acid and water by a certain percentage, are first put in reactor and are mixed, be then heated to 80 DEG C～120 DEG C by the present invention；In this reactor, add catalyst, and in keeping still temperature of charge in the range of 80 DEG C～120 DEG C；In this reactor, add 100 parts be preheated to 80 DEG C～the dihydromyrcene of 120 DEG C in advance, and in keeping still temperature of charge in the range of 80 DEG C～120 DEG C, isothermal reaction 1 hour～3 hours；The product filtration that reaction obtained, stratification, decompression distillation, prepare.The present invention is by using homemade catalyst and coordinating the present invention corresponding raw material proportioning, thus shortens the production cycle of product dihydromyrcenol, improves its yield.
Description
Technical field
The invention belongs to silvichemical preparing technical field, particularly relate to the preparation method of a kind of dihydromyrcenol.
Background technology
Dihydromyrcenol, chemical name 2,6-dimethyl-7-octen-2-ol, there is the fresh fragrance of a flower, limette sample fruital, being mainly used in the harmony of fragrances fragrance and good stability, the consumption in essence, up to about 20%, is the kind of large usage quantity in turpentine oil synthetic perfume.
The indirect hydration method of current industrial conventional dihydromyrcene and formic acid esterification, saponification is produced.This technique exists that conversion ratio is low, the shortcoming of production cycle length.
Summary of the invention
The present invention provides the preparation method of a kind of dihydromyrcenol, and the method can solve the existing reparation technology of dihydroterpineol and have that conversion ratio is low, the problem of production cycle length.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:
It comprises the following steps:
80 parts～90 part of 36% acetic acid and 50 parts～60 parts of water are first put in reactor and are mixed, are then heated to 80 DEG C～120 DEG C by A, by weight；
B, after step A, in this reactor, add 5 parts～8 parts of catalyst, and in keeping still temperature of charge in the range of 80 DEG C～120 DEG C；
C, after step B, in this reactor, add 100 parts be preheated to 80 DEG C～the dihydromyrcene of 120 DEG C in advance, and in keeping still temperature of charge in the range of 80 DEG C～120 DEG C, isothermal reaction 1 hour～3 hours；
D, after step C, product filtration that reaction is obtained, stratification, decompression distillation, prepare；
Wherein, the preparation method of step B used catalyst is as follows:
A, by weight, puts in 60% nitric acid by the niobic acid that 20 parts of particle diameters are 200 mesh～240 mesh, and normal temperature is acidified 2 hours, is washed out to neutrality；
B, step A is processed after the material that obtains put in 28% ammoniacal liquor, normal temperature alkalizes 2 hours, is washed out to neutrality；
C, step B is processed after the material that obtains mix with magnesium stearate, be subsequently placed at 1200 DEG C calcining 3 hours, prepared.
In technique scheme, more specifically technical scheme is: 36% acetic acid 85 parts and 60 parts of water, catalyst 5 parts, dihydromyrcene 100 parts.
Owing to using technique scheme, the present invention obtains providing the benefit that:
The present invention is by using homemade catalyst and coordinating the present invention corresponding raw material proportioning, thus shortens the production cycle of product dihydromyrcenol, improves its yield.
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 dihydromyrcenol comprises the following steps:
A, first 85 part of 36% acetic acid and 60 parts of water are put in reactor and mixed, be then heated to 80 DEG C；
B, after step A, in this reactor, add 5 parts of catalyst, and in keeping still temperature of charge in the range of 80 DEG C DEG C；
C, after step B, in this reactor, add 100 parts be preheated to the dihydromyrcene of 80 DEG C in advance, and to keep temperature of charge in still be 80 DEG C, isothermal reaction 3 hours；
D, after step C, product filtration that reaction is obtained, stratification, decompression distillation, prepare；
Wherein, the preparation method of step B used catalyst is as follows:
A, being that the niobic acid of 200 mesh is put in 60% nitric acid by 20 parts of particle diameters, normal temperature is acidified 2 hours, is washed out to neutrality；
B, step A is processed after the material that obtains put in 28% ammoniacal liquor, normal temperature alkalizes 2 hours, is washed out to neutrality；
C, step B is processed after the material that obtains mix with magnesium stearate, be subsequently placed at 1200 DEG C calcining 3 hours, prepared.
Relative to the preparation technology of existing dihydromyrcenol, the production cycle of the present embodiment dihydroterpineol shortens 50%, and yield is 99%.
Embodiment 2
The preparation method of this dihydromyrcenol comprises the following steps:
A, first 80 part of 36% acetic acid and 50 parts of water are put in reactor and mixed, be then heated to 120 DEG C；
B, after step A, in this reactor, add 8 parts of catalyst, and in keeping still temperature of charge in the range of 120 DEG C；
C, after step B, in this reactor, add 100 parts be preheated to the dihydromyrcene of 120 DEG C in advance, and to keep temperature of charge in still be 120 DEG C, isothermal reaction 1 hour；
D, after step C, product filtration that reaction is obtained, stratification, decompression distillation, prepare；
Wherein, the preparation method of step B used catalyst is as follows:
A, being that the niobic acid of 240 mesh is put in 60% nitric acid by 20 parts of particle diameters, normal temperature is acidified 2 hours, is washed out to neutrality；
B, step A is processed after the material that obtains put in 28% ammoniacal liquor, normal temperature alkalizes 2 hours, is washed out to neutrality；
C, step B is processed after the material that obtains mix with magnesium stearate, be subsequently placed at 1200 DEG C calcining 3 hours, prepared.
Relative to the preparation technology of existing dihydromyrcenol, the production cycle of the present embodiment dihydroterpineol shortens 50%, and yield is 99.5%.
Embodiment 3
The preparation method of this dihydromyrcenol comprises the following steps:
A, first 90 part of 36% acetic acid and 55 parts of water are put in reactor and mixed, be then heated to 100 DEG C；
B, after step A, in this reactor, add 7 parts of catalyst, and in keeping still temperature of charge in the range of 100 DEG C；
C, after step B, in this reactor, add 100 parts be preheated to the dihydromyrcene of 100 DEG C in advance, and to keep temperature of charge in still be 100 DEG C, isothermal reaction 2 hours；
D, after step C, product filtration that reaction is obtained, stratification, decompression distillation, prepare；
Wherein, the preparation method of step B used catalyst is as follows:
A, being that the niobic acid of 230 mesh is put in 60% nitric acid by 20 parts of particle diameters, normal temperature is acidified 2 hours, is washed out to neutrality；
B, step A is processed after the material that obtains put in 28% ammoniacal liquor, normal temperature alkalizes 2 hours, is washed out to neutrality；
C, step B is processed after the material that obtains mix with magnesium stearate, be subsequently placed at 1200 DEG C calcining 3 hours, prepared.
Relative to the preparation technology of existing dihydromyrcenol, the production cycle of the present embodiment dihydroterpineol shortens 50%, and yield is 99.4%.
Claims (2)
1. the preparation method of a dihydromyrcenol, it is characterised in that:
80 parts～90 part of 36% acetic acid and 50 parts～60 parts of water are first put in reactor and are mixed, are then heated to 80 DEG C～120 DEG C by A, by weight；
B, after step A, in this reactor, add 5 parts～8 parts of catalyst, and in keeping still temperature of charge in the range of 80 DEG C～120 DEG C；
C, after step B, in this reactor, add 100 parts be preheated to 80 DEG C～the dihydromyrcene of 120 DEG C in advance, and in keeping still temperature of charge in the range of 80 DEG C～120 DEG C, isothermal reaction 1 hour～3 hours；
D, after step C, product filtration that reaction is obtained, stratification, decompression distillation, prepare；
Wherein, the preparation method of step B used catalyst is as follows:
A, by weight, puts in 60% nitric acid by the niobic acid that 20 parts of particle diameters are 200 mesh～240 mesh, and normal temperature is acidified 2 hours, is washed out to neutrality；
B, step A is processed after the material that obtains put in 28% ammoniacal liquor, normal temperature alkalizes 2 hours, is washed out to neutrality；
C, step B is processed after the material that obtains mix with magnesium stearate, be subsequently placed at 1200 DEG C calcining 3 hours, prepared.
2. the preparation method of dihydromyrcenol described in 1 is gone according to right, it is characterised in that: 36% acetic acid 85 parts and 60 parts of water, catalyst 5 parts, dihydromyrcene 100 parts.
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| WO2018049252A1 (en) | 2016-09-08 | 2018-03-15 | P2 Science, Inc. | Methods for the continuous alkoxylation and derivatization of terpenes |
| CN106924224A (en) * | 2017-03-09 | 2017-07-07 | 新乡医学院 | A kind of pharmaceutical composition for treating craniocerebral injury caused by mental disorder and its application |
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| JPS5013910A (en) * | 1973-06-08 | 1975-02-13 | ||
| JPS6154241A (en) * | 1984-08-21 | 1986-03-18 | シ−ビ−エムエム・インタ−ナシヨナル・リミタ−ダ | Water containing niobium oxide solid acid catalyst |
| CN1204103C (en) * | 2002-06-12 | 2005-06-01 | 中国石油化工股份有限公司 | Process for preparing ethandiol by catalyzing epoxyethane hydration |
| WO2012017447A2 (en) * | 2010-08-04 | 2012-02-09 | Vijay Kumar Doppalapudi | Method for selective hydration of aroma olefins to alcohols in continuous solid catalyst column reactor |
| CN101921176B (en) * | 2010-08-10 | 2013-01-23 | 福州大学 | Novel method for producing dihydromyrcenol |
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