CN101391940B - Method for separating sclareol - Google Patents

Abstract

The invention relates to the technical field of natural perfume separation, in particular to a separation method of sclareol. The invention overcomes the problems in the prior art that the production efficiency is low, the yield is low, the energy consumption is great and the cost is high. Aiming at overcoming the problems in the prior art, the technical proposal of the invention is as follows: the separation method of the sclareol comprises the following steps sequentially: (1) preliminary treatment: the crude extract of sage clary is heated to be fully melted, and centrifugal extraction is carried out to remove heavy phase substances; (2) primary stage of distillation: the crude extract of the sage clary is sent to a molecular still, after continuous distillation, the extract is divided into heavy phase and light phase, wherein, the light phase is carried out with secondary distillation; and (3) secondary distillation: the light phase obtained in the step (2) is sent to the molecular still again to obtain the sclareol with the concentration of 90 to 98 percent. Compared with the prior art, the method has the advantages of high production efficiency, high yield reaching more than 95 percent, low energy consumption and low cost.

Description

The separation method of sclareol

Technical field:

The present invention relates to the separation technology field of natural perfume, be specifically related to a kind of separation method of sclareol.

Background technology:

Sclareol is that raw material extracts and makes with the inflorescence of Salvia Sclare L. (Salvia Sclare L.), have antibiotic, eliminate many physiologically actives such as acne.The general method that adopts of the industry is at present: with the Salvia Sclare L. crude extract is raw material, adopt underpressure distillation or solvent extration to separate, wherein solvent extration need use a large amount of solvents to carry out periodic crystallisation, the effusion of solvent, seepage are the Hazard Factor of safety in production, can pose a big pressure to environment again, though and underpressure distillation can alleviate the pollution to environment, it also exists following problem: 1, production efficiency is low: be subjected to thermal process to need 12 hours at least in the underpressure distillation; 2, yield is low: the product composition destructible that is heated, so product yield can only reach about 70%; 3, energy consumption is big, cost is high: need consume a large amount of heat energy during underpressure distillation, so energy consumption is big, has also increased production cost.

Summary of the invention:

The present invention will provide a kind of separation method of sclareol, to overcome the problem that production efficiency is low, yield is low, energy consumption is big and cost is high that prior art exists.

For overcoming the problem that prior art exists, technical scheme of the present invention is: a kind of separation method of sclareol comprises the steps: successively

(1) pre-treatment: with the heating of Salvia Sclare L. crude extract, temperature is controlled at 80～250 ℃, until fusion fully, be delivered in the centrifugal extracter of band heat-insulation system, under 135～150 ℃,, remove the heavy phase thing with the Centrifugical extraction that carries out of 500-6000 rev/min rotating speed;

(2) one-level distillation: the Salvia Sclare L. crude extract is delivered to molecular still, control pressure 100 handkerchiefs-150 handkerchief, 190 ℃ to 230 ℃ of temperature, crude extract after continuous still battery, be divided into heavy phase and light mutually, heavy phase directly discards through special pipeline discharge, gently enters secondary distillation mutually;

(3) secondary distillation: the light phase that step (2) obtains is delivered to molecular still once more, pressure 30 handkerchiefs-70 handkerchief, and 260 ℃ to 300 ℃ of temperature can obtain the sclareol that purity is 90%-98%.

In the above-mentioned steps (1): with the heating of Salvia Sclare L. crude extract, temperature is controlled at 80～100 ℃, fully fusion.Energy consumption is lower.

Compared with prior art, advantage of the present invention is as follows:

1, production efficiency height: whole thermal separation process is no more than 10 seconds;

2, yield height: short because of heated time, product composition is kept, and system's total recovery can reach more than 95% like this;

3, energy consumption is low, cost is low: heat-up time is short, thereby energy consumption reduces greatly.

Embodiment:

Below in conjunction with embodiment the present invention is done and to explain.

Embodiment 1:

A kind of separation method of sclareol comprises the steps: successively

(1) pre-treatment: with 200kg content is that 45.2% clary sage concrete adds and is heated to 85～90 degree fusions in the still kettle to liquid, use has the centrifugal extracter of heat-insulation system with 150 ℃ of temperature, 2000 rev/mins rotating speed carries out Centrifugical extraction, remove heavy phase thing (be mainly impurity such as foreign matter, high polarity high-density high-melting-point extract, wherein partial impurities has very big harm to the normal operation of molecular still);

(2) one-level distillation: after pre-treatment finishes primary extract is added molecular still, 130 handkerchiefs keep-up pressure, temperature 200 degree, crude extract is divided into heavy phase (waste impurity) and light (the Salvia Sclare L. crude extract of high level) mutually after distillation, heavy phase is directly discharged through special pipeline and is discarded, and gently enters secondary distillation mutually;

(3) secondary distillation: the molecular still that gently is added to normal operation that step (2) obtains, molecular still 50 handkerchiefs that keep-up pressure, temperature 290 degree can obtain the sclareol 91.5KG of content 94.0%, and yield is 95.14%.

Embodiment 2:

A kind of separation method of sclareol comprises the steps: successively

(1) pre-treatment: with 260kg content is that 48.6% clary sage concrete adds and is heated to 90～95 degree fusions in the still kettle to liquid, use has the centrifugal extracter of heat-insulation system with 135 ℃ of temperature, 5000 rev/mins rotating speed carries out Centrifugical extraction, removes the heavy phase thing;

(2) one-level distillation: after pre-treatment finishes primary extract is added molecular still, 140 handkerchiefs that keep-up pressure, temperature 205 degree, crude extract after distillation, be divided into heavy phase and light mutually, heavy phase directly discards through special pipeline discharge, gently enters secondary distillation mutually;

(3) secondary distillation: the molecular still that gently is added to normal operation that step (2) obtains, molecular still 60 handkerchiefs that keep-up pressure, temperature 295 degree can obtain the sclareol 134KG of content 90.5%, and yield is 95.97%.

Embodiment 3:

A kind of separation method of sclareol comprises the steps: successively

(1) pre-treatment: with 150kg content is that 50.2% clary sage concrete adds and is heated to 150～155 degree fusions in the still kettle to liquid, use has the centrifugal extracter of heat-insulation system with 150 ℃ of temperature, 1000 rev/mins rotating speed carries out Centrifugical extraction, removes the heavy phase thing;

(2) one-level distillation: after pre-treatment finishes primary extract is added molecular still, 110 handkerchiefs that keep-up pressure, temperature 195 degree, crude extract after distillation, be divided into heavy phase and light mutually, heavy phase directly discards through special pipeline discharge, gently enters secondary distillation mutually;

(3) secondary distillation: the molecular still that gently is added to normal operation that step (2) obtains, molecular still 40 handkerchiefs that keep-up pressure, temperature 270 degree can obtain the sclareol 76KG of content 94.8%, and yield is 95.68%.

Claims (2)

1. the separation method of a sclareol comprises the steps: successively

(1) pre-treatment: with the heating of Salvia Sclare L. crude extract, temperature is controlled at 80～250 ℃, until fusion fully, be delivered in the centrifugal extracter of band heat-insulation system, under 135～150 ℃,, remove the heavy phase thing with the Centrifugical extraction that carries out of 500-6000 rev/min rotating speed;

(2) one-level distillation: the Salvia Sclare L. crude extract is delivered to molecular still, control pressure 100 handkerchiefs-150 handkerchief, 190 ℃ to 230 ℃ of temperature, crude extract after continuous still battery, be divided into heavy phase and light mutually, heavy phase directly discards through special pipeline discharge, gently enters secondary distillation mutually;

(3) secondary distillation: the light phase that step (2) obtains is delivered to molecular still once more, pressure 30 handkerchiefs-70 handkerchief, and 260 ℃ to 300 ℃ of temperature can obtain the sclareol that purity is 90%-98%.

2. the separation method of sclareol as claimed in claim 1 is characterized in that: in the described step (1): with the heating of Salvia Sclare L. crude extract, temperature is controlled at 80～100 ℃, fully fusion.