CN105130735A - Preparation method for camphene - Google Patents

Abstract

The invention discloses a preparation method for camphene, and belongs to the camphene preparation technology field. The preparation method comprises steps: firstly, turpentine is placed in a distillation still, heating distillation is carried out at 0MPa-0.01MPa, and an alpha-pinene fraction is collected; then, by weight, 100 parts of the alpha-pinene fraction and 10-30 parts of water are mixed uniformly, the mixture is heated to 120 DEG C-145 DEG C, 5-8 parts of a catalyst prepared through a special method is added, a constant temperature reaction is carried out for 2-4h, and the product is prepared. During the preparation process, the catalyst prepared through a special method is employed, therefore the raw material amount is reduced effectively, the preparation time is shortened, and the camphene product yield is raised greatly.

Description

The preparation method of amphene

Technical field

The invention belongs to amphene preparing technical field, particularly relate to a kind of preparation method of amphene.

Background technology

Amphene is a kind of bicyclic diterpene vinyl compound, is the composition of the multiple natural volatile oil of turpentine wet goods, main as organic synthesis raw material, can be used for artificial camphor, spices, agricultural chemicals, thiocyanic acid acetic acid different thatch ester, the different thatch ester of acetic acid, toxaphene etc.

But mostly there is the problem that productive rate is low, cost is high in existing amphene preparation method.

Summary of the invention

The technical problem that the present invention solves is to provide a kind of preparation method of amphene, and this preparation method can solve existing amphene preparation method and mostly there is the problem that productive rate is low, cost is high.

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:

First turps is put into still kettle, under 0MPa ~ 0.01MPa, carry out adding thermal distillation, and collect α-pinene cut; Then by weight, 100 parts of described α-pinene cuts are mixed with 10 parts ~ 30 parts water, and is heated to 120 DEG C ~ 145 DEG C, add 5 parts ~ 8 parts catalyzer, isothermal reaction 2 hours ~ 4 hours, obtained;

Wherein, described catalyzer is obtained by following steps:

A, by weight, under agitation, by 0.5 part of metatitanic acid, 0.3 part of metasilicic acid and 2.4 parts of concentration be 40% sodium hydroxide solution put into reactor, first stir 1 hour at normal temperatures, be then warming up to 120 DEG C and continue stirrings 11 hours, filter, collect and obtain the first throw out;

B, the first precipitate washed with water that step A is obtained to the pH value of described first sedimentary rinsing solution in 7.3 ~ 8.0 scopes;

C, in the first throw out after step B process, add 1 part of concentration be the acetum of 30%, carries out acidification reaction 8 hours, filters, and collects and obtain the second precipitation;

D, the second throw out water washing that step C is obtained to the pH value of described second throw out rinsing solution in 2.5 ~ 3.5 scopes;

E, 0.3 part of aluminum oxide, 0.08 part of zirconium white and 0.3 part of Zinic stearas are joined D step process after the second throw out solution in stir, then use Bag filter, by the filtrate centrifugation obtained, the lower floor's sediment obtained;

F, in the obtained lower floor's sediment of E step, add 0.04 part of aqueous solution of titanyle sulfate, stir, then first at the temperature of 50 DEG C ~ 60 DEG C, be dried to its water content in the scope of 15% ~ 18%, then at the temperature lower calcination 4 hours of 1200 DEG C, obtained.

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

The present invention by preparation process, by using through the obtained catalyzer of special methods, thus effective reduce raw material consumption, shorten the preparation time used and greatly improve the productive rate of amphene product.

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 amphene comprises the following steps:

First turps is put into still kettle, under 0MPa, carry out adding thermal distillation, and collect α-pinene cut; Then α-pinene cut described in 1000g is mixed with 100g water, and be heated to 120 DEG C, add 50g catalyzer, isothermal reaction 4 hours, obtained;

Wherein, described catalyzer is obtained by following steps:

A, under agitation, by 5g metatitanic acid, 3g metasilicic acid and 24g concentration be 40% sodium hydroxide solution put into reactor, first stir 1 hour at normal temperatures, be then warming up to 120 DEG C and continue stirrings 11 hours, filter, collect and obtain the first throw out;

B, the first precipitate washed with water that step A is obtained to the pH value of described first sedimentary rinsing solution in 7.3 ~ 8.0 scopes;

C, in the first throw out after step B process, add the acetum that 10g concentration is 30%, carry out acidification reaction 8 hours, filter, collect and obtain the second precipitation;

D, the second throw out water washing that step C is obtained to the pH value of described second throw out rinsing solution in 2.5 ~ 3.5 scopes;

E, 3g aluminum oxide, 0.8g zirconium white and 3g Zinic stearas are joined D step process after the second throw out solution in stir, then use Bag filter, by the filtrate centrifugation obtained, the lower floor's sediment obtained;

F, in the obtained lower floor's sediment of E step, add 0.4g aqueous solution of titanyle sulfate, stir, then first at the temperature of 50 DEG C ~ 60 DEG C, being dried to its water content is 15%, then at the temperature lower calcination 4 hours of 1200 DEG C, obtained.

Compare existing amphene preparation method, the production cost of the present embodiment reduces 30%, and the yield of product amphene reaches 90%.

Embodiment 2

The preparation method of this amphene comprises the following steps:

First turps is put into still kettle, under 0.01MPa, carry out adding thermal distillation, and collect α-pinene cut; Then α-pinene cut described in 1000g is mixed with 300g water, and be heated to 145 DEG C, add 80g catalyzer, isothermal reaction 2 hours, obtained;

Wherein, described catalyzer is obtained by following steps:

A, under agitation, by 5g metatitanic acid, 3g metasilicic acid and 24g concentration be 40% sodium hydroxide solution put into reactor, first stir 1 hour at normal temperatures, be then warming up to 120 DEG C and continue stirrings 11 hours, filter, collect and obtain the first throw out;

B, the first precipitate washed with water that step A is obtained to the pH value of described first sedimentary rinsing solution in 7.3 ~ 8.0 scopes;

C, in the first throw out after step B process, add the acetum that 10g concentration is 30%, carry out acidification reaction 8 hours, filter, collect and obtain the second precipitation;

D, the second throw out water washing that step C is obtained to the pH value of described second throw out rinsing solution in 2.5 ~ 3.5 scopes;

E, 3g aluminum oxide, 0.8g zirconium white and 3g Zinic stearas are joined D step process after the second throw out solution in stir, then use Bag filter, by the filtrate centrifugation obtained, the lower floor's sediment obtained;

F, in the obtained lower floor's sediment of E step, add 0.4g aqueous solution of titanyle sulfate, stir, then first at the temperature of 50 DEG C ~ 60 DEG C, being dried to its water content is 17%, then at the temperature lower calcination 4 hours of 1200 DEG C, obtained.

Compare existing amphene preparation method, the production cost of the present embodiment reduces 30%, and the yield of product amphene reaches 90%.

Embodiment 3

The preparation method of this amphene comprises the following steps:

First turps is put into still kettle, under 0MPa, carry out adding thermal distillation, and collect α-pinene cut; Then α-pinene cut described in 1000g is mixed with 200g water, and be heated to 135 DEG C, add 70g catalyzer, isothermal reaction 3 hours, obtained;

Wherein, described catalyzer is obtained by following steps:

A, under agitation, by 5g metatitanic acid, 3g metasilicic acid and 24g concentration be 40% sodium hydroxide solution put into reactor, first stir 1 hour at normal temperatures, be then warming up to 120 DEG C and continue stirrings 11 hours, filter, collect and obtain the first throw out;

B, the first precipitate washed with water that step A is obtained to the pH value of described first sedimentary rinsing solution in 7.3 ~ 8.0 scopes;

C, in the first throw out after step B process, add the acetum that 10g concentration is 30%, carry out acidification reaction 8 hours, filter, collect and obtain the second precipitation;

D, the second throw out water washing that step C is obtained to the pH value of described second throw out rinsing solution in 2.5 ~ 3.5 scopes;

E, 3g aluminum oxide, 0.8g zirconium white and 3g Zinic stearas are joined D step process after the second throw out solution in stir, then use Bag filter, by the filtrate centrifugation obtained, the lower floor's sediment obtained;

F, in the obtained lower floor's sediment of E step, add 0.4g aqueous solution of titanyle sulfate, stir, then first at the temperature of 50 DEG C ~ 60 DEG C, being dried to its water content is 18%, then at the temperature lower calcination 4 hours of 1200 DEG C, obtained.

Compare existing amphene preparation method, the production cost of the present embodiment reduces 30%, and the yield of product amphene reaches 90%.

Claims (1)

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

First turps is put into still kettle, under 0MPa ~ 0.01MPa, carry out adding thermal distillation, and collect α-pinene cut; Then by weight, 100 parts of described α-pinene cuts are mixed with 10 parts ~ 30 parts water, and is heated to 120 DEG C ~ 145 DEG C, add 5 parts ~ 8 parts catalyzer, isothermal reaction 2 hours ~ 4 hours, obtained;

Wherein, described catalyzer is obtained by following steps:

A, by weight, under agitation, by 0.5 part of metatitanic acid, 0.3 part of metasilicic acid and 2.4 parts of concentration be 40% sodium hydroxide solution put into reactor, first stir 1 hour at normal temperatures, be then warming up to 120 DEG C and continue stirrings 11 hours, filter, collect and obtain the first throw out;

B, the first precipitate washed with water that step A is obtained to the pH value of described first sedimentary rinsing solution in 7.3 ~ 8.0 scopes;

C, in the first throw out after step B process, add 1 part of concentration be the acetum of 30%, carries out acidification reaction 8 hours, filters, and collects and obtain the second precipitation;

D, the second throw out water washing that step C is obtained to the pH value of described second throw out rinsing solution in 2.5 ~ 3.5 scopes;

E, 0.3 part of aluminum oxide, 0.08 part of zirconium white and 0.3 part of Zinic stearas are joined D step process after the second throw out solution in stir, then use Bag filter, by the filtrate centrifugation obtained, the lower floor's sediment obtained;

F, in the obtained lower floor's sediment of E step, add 0.04 part of aqueous solution of titanyle sulfate, stir, then first at the temperature of 50 DEG C ~ 60 DEG C, be dried to its water content in the scope of 15% ~ 18%, then at the temperature lower calcination 4 hours of 1200 DEG C, obtained.