CN104926610A

CN104926610A - Preparation method of dihydromyrcenol

Info

Publication number: CN104926610A
Application number: CN201510276832.0A
Authority: CN
Inventors: 陈伟强; 陈键泉; 苏炳连; 李战; 冯玲; 董俊
Original assignee: GUANGXI WUSONGLIN CHEMICAL GROUP Co Ltd
Current assignee: GUANGXI WUSONGLIN CHEMICAL GROUP Co Ltd
Priority date: 2015-05-27
Filing date: 2015-05-27
Publication date: 2015-09-23
Anticipated expiration: 2035-05-27
Also published as: CN104926610B

Abstract

The invention discloses a preparation method of dihydromyrcenol, belonging to the technical field of forestry chemical product preparation. The method comprises the following steps: according to a certain ratio, putting 36% of acetic acid and water into a reaction kettle, mixing evenly, and then heating to 80 DEG C to 120 DEG C; adding a catalyst into the reaction kettle, and keeping the material temperature in the kettle within the range of 80 DEG C to 120 DEG C; adding 100 parts of dihydromyrcenol preheated to 80 DEG C to 120 DEG C in advance into the reaction kettle, keeping the material temperature in the kettle within the range of 80 DEG C to 120 DEG C, and performing thermostatic reaction for one hour to 3 hours; performing filtering, standing layering and reduced pressure distillation on a product obtained by the reaction, thus obtaining the dihydromyrcenol. According to the preparation method of the dihydromyrcenol, by adopting the home-made catalyst and matching with the corresponding raw material ratio, the production cycle of the product dihydromyrcenol is shortened, and the yield of the dihydromyrcenol is improved.

Description

The preparation method of dihydromyrcenol

Technical field

The invention belongs to silvichemical preparing technical field, particularly relate to a kind of preparation method 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, be mainly used in Harmony and the satisfactory stability of fragrances fragrance, the consumption in essence can reach about 20%, is the kind of large usage quantity in turps synthetic perfume.

The indirect hydration method of current industrial conventional dihydromyrcene and formic acid esterification, saponification is produced.There is the shortcoming of low conversion rate, production cycle length in this technique.

Summary of the invention

The invention provides a kind of preparation method of dihydromyrcenol, the method can solve the problem that the existing reparation technology of dihydroterpineol exists low conversion rate, production cycle length.

In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:

It comprises the following steps:

A, by weight, first 80 parts ~ 90 part 36% acetic acid and 50 parts ~ 60 parts water are put into reactor and mix, be then heated to 80 DEG C ~ 120 DEG C;

B, after step A, in this reactor, add 5 parts ~ 8 parts catalyzer, and to keep in still temperature of charge in the scope of 80 DEG C ~ 120 DEG C;

C, after step B, in this reactor, add the dihydromyrcene that 100 parts are preheated to 80 DEG C ~ 120 DEG C in advance, and to keep in still temperature of charge in the scope of 80 DEG C ~ 120 DEG C, isothermal reaction 1 hour ~ 3 hours;

D, after step C, by be obtained by reacting product filtration, stratification, underpressure distillation, obtained;

Wherein, the preparation method of step B used catalyst is as follows:

20 parts of particle diameters are that 200 order ~ 240 object niobic acids put into 60% nitric acid, normal temperature acidifying 2 hours by A, by weight, and then washing is to neutral;

B, the material obtained after step A process is put into 28% ammoniacal liquor, normal temperature alkalizes 2 hours, and then washing is to neutral;

C, the material obtained after step B process to be mixed with Magnesium Stearate, calcine 3 hours at being then placed in 1200 DEG C, obtained.

In technique scheme, technical scheme is more specifically: 36% acetic acid 85 parts and 60 parts, water, catalyzer 5 parts, dihydromyrcene 100 parts.

Owing to adopting technique scheme, the beneficial effect that the present invention obtains is:

The present invention by adopting homemade catalyzer and coordinating the corresponding proportioning raw materials of the present invention, thus shortens the production cycle of product dihydromyrcenol, improves its yield.

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 dihydromyrcenol comprises the following steps:

A, first 85 part of 36% acetic acid and 60 parts of water are put into reactor and mix, be then heated to 80 DEG C;

B, after step A, in this reactor, add 5 parts of catalyzer, and to keep in still temperature of charge in the scope of 80 DEG C DEG C;

C, after step B, in this reactor, add the dihydromyrcene that 100 parts are preheated to 80 DEG C in advance, and keep temperature of charge in still to be 80 DEG C, isothermal reaction 3 hours;

Wherein, the preparation method of step B used catalyst is as follows:

A, be that 200 object niobic acids put into 60% nitric acid by 20 parts of particle diameters, normal temperature acidifying 2 hours, then washing is to neutral;

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 into reactor and mix, be then heated to 120 DEG C;

B, after step A, in this reactor, add 8 parts of catalyzer, and to keep in still temperature of charge in the scope of 120 DEG C;

C, after step B, in this reactor, add the dihydromyrcene that 100 parts are preheated to 120 DEG C in advance, and keep temperature of charge in still to be 120 DEG C, isothermal reaction 1 hour;

Wherein, the preparation method of step B used catalyst is as follows:

A, be that 240 object niobic acids put into 60% nitric acid by 20 parts of particle diameters, normal temperature acidifying 2 hours, then washing is to neutral;

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 into reactor and mix, be then heated to 100 DEG C;

B, after step A, in this reactor, add 7 parts of catalyzer, and to keep in still temperature of charge in the scope of 100 DEG C;

C, after step B, in this reactor, add the dihydromyrcene that 100 parts are preheated to 100 DEG C in advance, and keep temperature of charge in still to be 100 DEG C, isothermal reaction 2 hours;

Wherein, the preparation method of step B used catalyst is as follows:

A, be that 230 object niobic acids put into 60% nitric acid by 20 parts of particle diameters, normal temperature acidifying 2 hours, then washing is to neutral;

Relative to the preparation technology of existing dihydromyrcenol, the production cycle of the present embodiment dihydroterpineol shortens 50%, and yield is 99.4%.

Claims

1. a preparation method for dihydromyrcenol, is characterized in that:

Wherein, the preparation method of step B used catalyst is as follows:

2. to go the preparation method of the dihydromyrcenol described in 1 according to right, it is characterized in that: 36% acetic acid 85 parts and 60 parts, water, catalyzer 5 parts, dihydromyrcene 100 parts.