CN105218292A - The preparation method of amphene - Google Patents

Abstract

The present invention discloses a kind of preparation method of amphene, belongs to amphene preparing technical field.The present invention includes and first turps is put into still kettle, carry out adding thermal distillation under 0MPa ~ 0.01MPa, 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 obtained through special methods, isothermal reaction 2 hours ~ 4 hours, obtained.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.

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, by 0.7 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 130 DEG C and continue stirrings 10 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, 0.1 part of zirconium white, 0.08 part of rare earth chloride and 0.3 part of Magnesium Stearate 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 be placed in hydrogen atmosphere, and reduce 3 hours at 200 DEG C, to obtain final product.

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, by 7g 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 130 DEG C and continue stirrings 10 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, 1g zirconium white, 0.8g rare earth chloride and 3g Magnesium Stearate 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 is placed in hydrogen atmosphere, and reduces 3 hours at 200 DEG C, to obtain final product.

Compare existing amphene preparation method, the production cost of the present embodiment reduces 31%, 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, by 7g 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 130 DEG C and continue stirrings 10 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, 1g zirconium white, 0.8g rare earth chloride and 3g Magnesium Stearate 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 is placed in hydrogen atmosphere, and reduces 3 hours at 200 DEG C, to obtain final product.

Compare existing amphene preparation method, the production cost of the present embodiment reduces 30%, and the yield of product amphene reaches 92%.

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, by 7g 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 130 DEG C and continue stirrings 10 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, 1g zirconium white, 0.8g rare earth chloride and 3g Magnesium Stearate 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 is placed in hydrogen atmosphere, and reduces 3 hours at 200 DEG C, to obtain final product.

Compare existing amphene preparation method, the production cost of the present embodiment reduces 30%, and the yield of product amphene reaches 91%.

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, by 0.7 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 130 DEG C and continue stirrings 10 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, 0.1 part of zirconium white, 0.08 part of rare earth chloride and 0.3 part of Magnesium Stearate 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 be placed in hydrogen atmosphere, and reduce 3 hours at 200 DEG C, to obtain final product.