阅读说明：本技术 一种生产特定指纹图谱普利醇的装置和方法 (Device and method for producing specific fingerprint polycosanol ) 是由 蔡力创 刘建平 欧阳克氙 郭雄昌 涂越 于 2020-06-23 设计创作，主要内容包括：本发明涉及油脂的提取分离深加工技术领域,提供了一种生产特定指纹图谱普利醇的装置及方法,本发明的装置将进料罐、接收罐连接真空系统,在保证精馏塔真空稳定的条件下,实现了连续批次加料与出料,不用停机操作,提高生产效率；本发明提供的方法采用高真空精馏工艺,首先将皂化粗醇放入化料罐,经化料后放入进料罐,然后用输送泵打入精馏釜中,在真空条件下进行第一批次精馏,塔顶依次收集各段馏分,塔底收集釜残；第一批次粗品精馏完毕,在进料罐真空与精馏塔真空基本一致的条件下,进行下一批次进料。本发明提供的方法分离效率高,普利醇的指纹图谱可控、质量稳定,只需经1次精馏过程就可达到普利醇中二十八烷醇所需纯度的要求。(The invention relates to the technical field of extraction, separation and deep processing of grease, and provides a device and a method for producing specific fingerprint spectrum policosanol, wherein a feeding tank and a receiving tank are connected with a vacuum system, so that continuous batch feeding and discharging are realized under the condition of ensuring the vacuum stability of a rectifying tower, the operation is not required to be stopped, and the production efficiency is improved; the method provided by the invention adopts a high vacuum rectification process, firstly, the saponified crude alcohol is put into a material dissolving tank, then the saponified crude alcohol is put into a material feeding tank after material dissolving, then the saponified crude alcohol is pumped into a rectification kettle by a delivery pump, the first batch of rectification is carried out under the vacuum condition, fractions of all sections are sequentially collected at the top of the tower, and kettle residues are collected at the bottom of the tower; after the crude product of the first batch is rectified, feeding of the next batch is carried out under the condition that the vacuum of the feeding tank is basically consistent with that of the rectifying tower. The method provided by the invention has high separation efficiency, controllable fingerprint spectrum of the policosanol and stable quality, and can meet the requirement of the purity of the octacosanol in the policosanol only by 1 rectification process.)

1. The device for producing the polycosanol with the specific fingerprint spectrum is characterized by comprising a material melting tank (1);

a feed tank (2); the inlet of the feeding tank (2) is communicated with the outlet of the material melting tank (1);

a rectifying column (3); a rectifying still (4) is arranged at the bottom of the rectifying tower, a reflux condenser (5) is arranged at the top of the rectifying tower, a connecting section (6) is arranged between the top of the rectifying tower and the reflux condenser, and a discharge hole is formed in the connecting section (6); a feed inlet is formed in the rectifying kettle (4) and is communicated with an outlet of the feed tank (2);

a first receiving tank (7), a second receiving tank (8) and a third receiving tank (9) which are connected in parallel; inlets of the first receiving tank (7), the second receiving tank (8) and the third receiving tank (9) are communicated with a discharge hole on the connecting section (6);

a fourth receiving tank (10); the fourth receiving tank (10) is communicated with an outlet of the rectifying still (4);

a first vacuum unit (11); the first vacuum unit (11) is communicated with the reflux condenser (5);

a second vacuum assembly (12); and the second vacuum unit (12) is respectively communicated with the first receiving tank (7), the second receiving tank (8), the third receiving tank (9), the fourth receiving tank (10) and the feeding tank (2).

2. The device according to claim 1, characterized in that a first valve (I-1) is arranged on a pipeline communicating the outlet of the material melting tank (1) and the inlet of the material feeding tank (2), and a second valve (I-2), a third valve (I-3) and a fourth valve (I-4) are respectively arranged on a pipeline communicating the outlet of the connecting section (6) and the inlets of the first receiving tank (7), the second receiving tank (8) and the third receiving tank (9);

pipelines for communicating the first receiving tank (7), the second receiving tank (8), the third receiving tank (9), the fourth receiving tank (10) and the second vacuum unit (12) are respectively provided with a fifth valve (I-5), a sixth valve (I-6), a seventh valve (I-7) and an eighth valve (I-8);

a ninth valve (I-9) is arranged on a pipeline for communicating the feeding tank (2) with the second vacuum unit (12);

a tenth valve (I-10) is arranged on a pipeline communicated with the reflux condenser (5) and the first vacuum unit (11);

a first delivery pump (II-1) is arranged on a pipeline communicated with the outlet of the feeding tank (2) and the feeding hole of the rectifying still (4);

an eleventh valve (I-11) and a second delivery pump (II-2) are sequentially arranged on a pipeline communicated with the outlet of the rectifying still (4) and the inlet of the fourth receiving tank (10) from the outlet of the rectifying still to the inlet of the fourth receiving tank;

emptying valves are arranged on the feeding tank (2), the reflux condenser (5), the first receiving tank (7), the second receiving tank (8), the third receiving tank (9) and the fourth receiving tank (10); an inflation inlet is arranged on the connecting section (6).

3. The apparatus according to claim 1 or 2, characterized in that the rectification column (3) is a packed column; the height of the packed tower is 3-5 m, and the number of tower plates is 15-25.

4. The device according to claim 1 or 2, characterized in that the first vacuum unit (11) and the second vacuum unit (12) are each a four-stage roots vacuum unit.

5. A method for producing polycosanol with specific fingerprint by using the device of any of claims 1 to 4, comprising the following steps:

(i) putting the saponified crude alcohol into a material dissolving tank (1), putting the heated and dissolved material into a material feeding tank (2), putting the material in the material feeding tank (2) into a rectifying still (4), carrying out first batch rectification under the vacuum condition, and collecting fractions in sections through a first receiving tank (7), a second receiving tank (8) and a third receiving tank (9) at the top of the tower;

(ii) discharging collected fractions and kettle residues after the first batch of rectification is finished, feeding the next batch of rectification under the condition that the vacuum degrees of the feeding tank (2) and the rectifying tower (3) are consistent, and starting to receive the fractions of the second batch when the vacuum degrees of the first receiving tank (7), the second receiving tank (8) and the third receiving tank (9) are consistent with the vacuum degree of the rectifying tower (3);

(iii) (iii) repeating step (ii) to carry out multiple batches of rectification, carrying out gas chromatography detection on the collected fractions, and combining products with similar fingerprints in each batch to obtain specific fingerprint polycosanol;

wherein the specific fingerprint polycosanol comprises the following components in percentage by mass: 0.1-15% of docosanol, 0.1-20% of tetracosanol, 0.5-30% of hexacosanol, 10.0-99.0% of octacosanol, 0.2-15% of triacontanol and 0.1-10% of dotriacontanol.

6. The method as claimed in claim 5, wherein the saponified crude alcohol is a crude fatty alcohol obtained by saponification of rice bran wax or beeswax.

7. The method according to claim 5 or 6, characterized in that the saponified crude alcohol comprises the following components in mass fraction: 0-7% of eicosanol, 0.1-10% of docosanol, 4-20% of tetracosanol, 1-14% of hexacosanol, 10-17% of octacosanol, 17-70% of triacontanol, 4-22% of dotriacontanol, 0.1-20% of tetratriacontanol, 0-14% of hexacosanol and 0-3% of triacontanol.

8. The method as claimed in claim 5, wherein the working vacuum degree of the rectifying tower is 20-50 Pa, the reflux ratio is 1: 5-20, and the temperature of the rectifying kettle is 230-250 ℃.

9. The method according to claim 5, characterized in that said fraction collected in stages is in particular: and in the range of the tower top temperature of 230-250 ℃, one section is arranged at every 0.5-2 ℃, the collected fractions are sequentially marked as a first section fraction to an nth section fraction, n is an integer less than or equal to 40, and the vacuum degree in the receiving tank is consistent with that of the rectifying tower when the fractions are collected.

10. The method according to claim 9, characterized in that said fraction collected in stages is in particular: collecting the first stage fraction into a first receiving tank (7), collecting the second stage fraction into a second receiving tank (8), collecting the third stage fraction by using a third receiving tank (9), closing a second valve (I-2) and a third valve (I-3) while collecting the third stage fraction, discharging the first stage fraction and the second stage fraction after emptying the first receiving tank (7) and the second receiving tank (8), then opening a fifth valve (I-5) and a sixth valve (I-6), closing the fifth valve (I-5) and the sixth valve (I-6) when the vacuum degrees of the first receiving tank (7) and the second receiving tank (8) are consistent with that of the rectifying tower, sequentially opening the second valve (I-2) and the third valve (I-3), receiving the fourth stage fraction and the fifth stage fraction, and receiving the fifth stage fraction, and (3) closing the fourth valve (I-4) and the second valve (I-2), emptying the third receiving tank (9) and the first receiving tank (7), discharging the third section of distillate and the fourth section of distillate, opening the seventh valve (I-7) and the fifth valve (I-5), closing the seventh valve (I-7) and the fifth valve (I-5) when the vacuum degrees of the third receiving tank (9) and the first receiving tank (7) are consistent with that of the rectifying tower, opening the fourth valve (I-4) to receive the sixth section of distillate, and so on until all the distillates are received.

Technical Field

The invention relates to the technical field of extraction, separation and deep processing of grease, in particular to a device and a method for producing specific fingerprint polycosanol.

Background

Polycosanol mainly comes from rice bran wax and beeswax, the main components comprise higher fatty alkanol such as docosanol, tetracosanol, hexacosanol, octacosanol, triacontanol and dotriacontanol, and when the mass ratio of the components reaches a similar traditional Chinese medicine fingerprint spectrum, the components have the best synergistic effect and the best physiological activity. Policosanol is mainly used for blood lipid regulating drugs, health products, high-grade cosmetics, feed additives and the like.

Currently, policosanol is generally prepared from rice bran wax or beeswax as a raw material by saponification, extraction (purification), filtration and other processes. Wherein, the purification process is a key factor influencing the policosanol fingerprint, and the recrystallization method, the molecular distillation method and the rectification method are adopted at present.

The purity of the octacosanol can reach as high as 60 percent after repeated recrystallization is needed in the recrystallization process; a large amount of solvent is needed in the purification process, heavy metal is brought in, the solvent and the heavy metal are left in the product, the solvent volatilization and discharge cause adverse effects on the environment, and the loss rate of the crude product and the solvent reaches 10% in every recrystallization.

Molecular distillation is a distillation process operating under high vacuum, which utilizes the difference in the evaporation rates of the components in the feed solution to separate liquid mixtures. The molecular distillation is generally carried out for multiple times, and the octacosanol with the purity of 60-90% can be obtained through multiple times of distillation. The molecular distillation process is simpler than a heavy crystallization process, the utilization rate of raw materials is higher, and the process has no pollution to the environment. But the molecular distillation does not use the packing, namely the number of the tower plates is 1, and the separation efficiency is low; moreover, the most important point is that the proportion of each component of the product is uncontrollable, the policosanol of a specific fingerprint spectrum can not be produced, and the stability of the physiological activity and the efficacy can not be ensured.

The existing rectification method is generally a high vacuum rectification process, and octacosanol with the purity of 40-95% can be obtained through 2-3 times of rectification processes. Compared with the molecular distillation process, the method has the advantages of high separation efficiency and relatively controllable octacosanol content of each segmented product. However, the method needs to be carried out under normal pressure every time feeding and discharging, not only needs to rebalance the vacuum degree and the temperature at the top of the tower to collect the products in sections, but also cannot realize continuous batch feeding and discharging, prolongs the rectification time of each batch, and causes large difference of the content of octacosanol in the products collected in sections of each batch and cannot ensure stable product quality during each normal pressure-negative pressure switching operation; 2-3 times of rectification process is needed, and the production efficiency is not high enough; finally, the process can only produce octacosanol with a specific content, and cannot produce polycosanol with a specific fingerprint.

Disclosure of Invention

In view of the above, the present invention provides an apparatus and method for producing polycosanol with specific fingerprint. The device for producing policosanol does not need to carry out normal pressure-negative pressure switching operation during feeding and discharging, can realize continuous batch feeding and discharging under the condition of ensuring the vacuum stability of the rectifying tower, does not need to stop the operation, has high production efficiency and stable product quality, and can obtain policosanol with a specific fingerprint.

In order to achieve the above object, the present invention provides the following technical solutions:

a device for producing specific fingerprint spectrum policosanol comprises a material dissolving tank 1;

a feed tank 2; the inlet of the feeding tank 2 is communicated with the outlet of the material melting tank 1;

a rectifying column 3; a rectifying still 4 is arranged at the bottom of the rectifying tower, a reflux condenser 5 is arranged at the top of the rectifying tower, a connecting section 6 is arranged between the top of the rectifying tower and the reflux condenser, and a discharge hole is formed in the connecting section 6; a feed inlet is formed in the rectifying still 4 and is communicated with an outlet of the feed tank 2;

a first receiving tank 7, a second receiving tank 8 and a third receiving tank 9 which are connected in parallel; inlets of the first receiving tank 7, the second receiving tank 8 and the third receiving tank 9 are communicated with a discharge hole on the connecting section 6;

a fourth receiving tank 10; the fourth receiving tank 10 is communicated with an outlet of the rectifying still 4;

a first vacuum unit 11; the first vacuum unit 11 is communicated with the reflux condenser 5;

a second vacuum aggregate 12; the second vacuum unit 12 is respectively communicated with the first receiving tank 7, the second receiving tank 8, the third receiving tank 9, the fourth receiving tank 10 and the feeding tank 2.

Preferably, a first valve I-1 is arranged on a pipeline communicated with the outlet of the material melting tank 1 and the inlet of the material feeding tank 2, and a second valve I-2, a third valve I-3 and a fourth valve I-4 are respectively arranged on pipelines communicated with the outlet of the connecting section 6 and the inlets of the first receiving tank 7, the second receiving tank 8 and the third receiving tank 9;

the pipelines of the first receiving tank 7, the second receiving tank 8, the third receiving tank 9 and the fourth receiving tank 10 which are communicated with the second vacuum unit 12 are respectively provided with a fifth valve I-5, a sixth valve I-6, a seventh valve I-7 and an eighth valve I-8;

a ninth valve I-9 is arranged on a pipeline for communicating the feeding tank 2 with the second vacuum unit 12;

a tenth valve I-10 is arranged on a pipeline communicated with the reflux condenser 5 and the first vacuum unit 11;

a first delivery pump II-1 is arranged on a pipeline for communicating the outlet of the feeding tank 2 with the feeding hole of the rectifying still 4;

an eleventh valve I-11 and a second delivery pump II-2 are sequentially arranged on a pipeline communicated with the outlet of the rectifying still 4 and the inlet of the fourth receiving tank 10 from the outlet of the rectifying still to the inlet of the fourth receiving tank;

emptying valves are arranged on the feeding tank 2, the reflux condenser 5, the first receiving tank 7, the second receiving tank 8, the third receiving tank 9 and the fourth receiving tank 10; an inflation inlet is arranged on the connecting section (6).

Preferably, the rectifying tower 3 is a packed tower; the height of the packed tower is 3-5 m, and the number of tower plates is 15-25.

Preferably, the first vacuum unit 11 and the second vacuum unit 12 are both four-stage roots vacuum units.

The invention also provides a method for producing the polycosanol with the specific fingerprint spectrum by using the device in the scheme, which comprises the following steps:

(i) adding the saponified crude alcohol into a material dissolving tank 1, feeding the heated and dissolved material into a material feeding tank 2, feeding the material in the material feeding tank 2 into a rectifying still 4, carrying out first batch rectification under the vacuum condition, and collecting fractions in sections through a first receiving tank 7, a second receiving tank 8 and a third receiving tank 9 at the top of the tower;

(ii) discharging collected fractions and kettle residues after the first batch of rectification is finished, feeding the next batch of rectification under the condition that the vacuum degrees of the feeding tank 2 and the rectifying tower 3 are consistent, and starting to receive the fractions of the second batch when the vacuum degrees of the first receiving tank 7, the second receiving tank 8 and the third receiving tank 9 are consistent with the vacuum degree of the rectifying tower 3;

(iii) (iii) repeating step (ii) to carry out multiple batches of rectification, carrying out gas chromatography detection on the collected fractions, and combining products with similar fingerprints in each batch to obtain specific fingerprint polycosanol;

wherein the specific fingerprint polycosanol comprises the following components in percentage by mass: 0.1-15% of docosanol, 0.1-20% of tetracosanol, 0.5-30% of hexacosanol, 10.0-99.0% of octacosanol, 0.2-15% of triacontanol and 0.1-10% of dotriacontanol.

Preferably, the saponified crude alcohol is a crude fatty alcohol product prepared by saponification of rice bran wax or beeswax as a raw material.

Preferably, the saponified crude alcohol comprises the following components in parts by mass: 0-7% of eicosanol, 0.1-10% of docosanol, 4-20% of tetracosanol, 1-14% of hexacosanol, 10-17% of octacosanol, 17-70% of triacontanol, 4-22% of dotriacontanol, 0.1-20% of tetratriacontanol, 0-14% of hexacosanol and 0-3% of triacontanol.

Preferably, the working vacuum degree of the rectifying tower is 20-50 Pa, the reflux ratio is 1: 5-20, and the temperature of the rectifying kettle is 230-250 ℃.

Preferably, the fraction collected by stages is specifically: and in the range of the tower top temperature of 230-250 ℃, one section is arranged at every 0.5-2 ℃, the collected fractions are sequentially marked as a first section fraction to an nth section fraction, n is an integer less than or equal to 40, and the vacuum degree in the receiving tank is consistent with that of the rectifying tower when the fractions are collected.

Preferably, the fraction collected by stages is specifically: collecting the first stage fraction in a first receiving tank 7, collecting the second stage fraction in a second receiving tank 8, collecting the third stage fraction in a third receiving tank 9, closing a second valve I-2 and a third valve I-3 while collecting the third stage fraction, discharging the first stage fraction and the second stage fraction after emptying the first receiving tank 7 and the second receiving tank 8, then opening a fifth valve I-5 and a sixth valve I-6, closing the fifth valve I-5 and the sixth valve I-6 when the vacuum degrees of the first receiving tank 7 and the second receiving tank 8 are consistent with that of the rectifying tower, opening the second valve I-2 and the third valve I-3 in sequence, receiving the fourth stage fraction and the fifth stage fraction, closing the fourth valve I-4 and the second valve I-2 when receiving the fifth stage fraction, discharging the third stage fraction and the fourth stage fraction after emptying the third receiving tank 9 and the first receiving tank 7, and then opening a seventh valve I-7 and a fifth valve I-5, closing the seventh valve I-7 and the fifth valve I-5 when the vacuum degrees of the third receiving tank 9 and the first receiving tank 7 are consistent with the vacuum degree of the rectifying tower, opening a fourth valve I-4 to receive the fraction of the sixth section, and the like until all the fractions are received.

The invention provides a device for producing polycosanol with a specific fingerprint spectrum, which is provided with a first vacuum unit and a second vacuum unit, wherein the first vacuum unit is used for controlling the vacuum degree of a rectifying tower, the second vacuum unit is used for controlling the vacuum degree of a receiving tank and a feeding tank, the vacuum degree in the whole device for feeding and discharging can be conveniently controlled by utilizing the two vacuum units, normal pressure-negative pressure switching is not needed during feeding and discharging, continuous batch feeding and discharging can be realized under the condition of ensuring the vacuum stability of the rectifying tower, the shutdown operation is not needed, and the production efficiency is greatly improved; in addition, in the traditional rectification operation, the top fraction is directly extracted from the reflux condenser when the top fraction is extracted, but the invention arranges a connecting section between the top of the rectification tower and the reflux condenser, and the fraction is extracted from the connecting section, thereby avoiding the phenomenon of pipeline blockage (liquid-solid mixture after condensation) when the condensed liquid is directly extracted from the reflux condenser; in addition, the device is provided with 3 fraction receiving tanks connected in parallel, and the three receiving tanks are used for receiving fractions in different time periods, so that the efficiency can be obviously improved.

The invention provides a method for producing specific fingerprint spectrum policosanol by using the device in the scheme, which adopts a high vacuum rectification process, firstly, saponified crude alcohol is put into a material melting tank, enters a material feeding tank after material melting, then is put into a rectification kettle, is rectified for the first time under the vacuum condition, all sections of fractions are sequentially collected at the top of the tower, kettle residues are collected at the bottom of the tower, and the vacuum degrees of a receiving tank and the rectification tower are kept consistent in the process of collecting the fractions; after the first batch of distillation is finished, feeding the next batch of material under the condition that the vacuum of the material feeding tank is basically consistent with that of the distillation tower. The method provided by the invention can meet the requirement of the purity of octacosanol in policosanol only by 1 rectification process, the separation efficiency is more than 15 times of that of a molecular distillation method, the process is simple, the separation efficiency is high, the fingerprint spectrum of the policosanol is controllable, the quality is stable, and the activity effect is ensured; the method provided by the invention does not need any solvent in the production process, does not bring heavy metals, does not waste raw materials, has low production cost and high product purity, and is safe and environment-friendly; furthermore, the invention can produce various policosanol which accords with the fingerprint spectrum of the invention by controlling the temperature of the tower bottom and the reflux ratio.

Drawings

FIG. 1 is a schematic diagram of an apparatus for producing polycosanol having a specific fingerprint pattern;

in fig. 1: 1-material melting tank, 2-material feeding tank, 3-rectifying tower, 4-rectifying still, 5-reflux condenser, 6-connecting section, 7-first receiving tank, 8-second receiving tank, 9-third receiving tank, 10-fourth receiving tank, 11-first vacuum unit, 12-second vacuum unit, I-1-first valve, I-2-second valve, I-3-third valve, I-4-fourth valve, I-5-fifth valve, I-6-sixth valve, I-7-first seven valve, I-8-eighth valve, I-9-ninth valve, I-10-tenth valve, I-11-eleventh valve, II-1-first delivery pump, II-2-second delivery pump.

Detailed Description

The invention provides a device for producing polycosanol with a specific fingerprint spectrum, which has a structure shown in figure 1 and is specifically explained by combining figure 1.

The device provided by the invention comprises a material melting tank 1. The invention has no special requirements on the material dissolving tank, and the material dissolving tank well known to the technical personnel in the field can be used.

The device provided by the invention comprises a feeding tank 2; the inlet of the feeding tank is communicated with the outlet of the material melting tank, and a first valve I-1 is preferably arranged on a communicated pipeline.

The apparatus provided by the present invention comprises a rectification column 3. In the present invention, the rectification column 3 is preferably a packed column; the height of the packed tower is preferably 3-5 m, more preferably 4m, and the number of tower plates is preferably 15-25, more preferably 18-20. In the invention, a rectifying still 4 is arranged at the bottom of a rectifying tower 3, and a reflux condenser 5 is arranged at the top of the rectifying tower; a connecting section 6 is arranged between the top of the rectifying tower and the reflux condenser; the length of the connecting section 6 is preferably 0.1-0.3 m; a discharge hole is formed in the connecting section; the connecting section 6 is preferably provided with an inflation inlet; in specific application, inert gas is filled into the system from the inflation inlet to prevent explosion caused by material combustion. In the invention, the condensed fraction is a liquid-solid mixture, and the condensed fraction is directly extracted from the reflux condenser and is easy to block a pipeline. In the present invention, the reflux ratio can be controlled by controlling the volume ratio of the produced fraction and the reflux liquid. In the embodiment of the invention, the reflux ratio can be controlled by controlling the collection time, for example, reflux liquid is refluxed for 10s, and fraction of 1s is collected, wherein the reflux ratio is 10: 1.

In the invention, a feed inlet is arranged on the rectifying still 4, the feed inlet is communicated with an outlet of the feed tank 2, and a first delivery pump II-1 is preferably arranged on a communicated pipeline.

The device provided by the invention comprises a first receiving tank 7, a second receiving tank 8 and a third receiving tank 9 which are connected in parallel; inlets of the first receiving tank 7, the second receiving tank 8 and the third receiving tank 9 are communicated with a discharge hole on the connecting section 6; and the pipelines of the first receiving tank 7, the second receiving tank 8 and the third receiving tank 9 which are communicated with the discharge hole of the connecting section 6 are respectively provided with a second valve I-2, a third valve I-3 and a fourth valve I-4.

The apparatus provided by the present invention comprises a fourth receiving tank 10. In the present invention, the fourth receiving tank 10 is used for receiving the still residue; the fourth receiving tank 10 is communicated with an outlet of the rectifying still 4, and an eleventh valve I-11 and a second delivery pump II-2 are preferably sequentially arranged on a communicated pipeline from the outlet of the rectifying still to the inlet of the fourth receiving tank.

The apparatus provided by the present invention comprises a first vacuum unit 11. In the invention, the first vacuum unit 11 is communicated with the reflux condenser 5, and a tenth valve I-10 is preferably arranged on a communicated pipeline; the first vacuum unit 11 is preferably a four-stage roots vacuum unit; and the first vacuum unit is used for controlling the vacuum degree of the rectifying tower during rectification.

The apparatus provided by the present invention includes a second vacuum assembly 12. In the present invention, the second vacuum unit 12 is preferably a four-stage roots vacuum unit; the second vacuum unit 12 is respectively communicated with the first receiving tank 7, the second receiving tank 8, the third receiving tank 9, the fourth receiving tank 10 and the feeding tank 2, and pipelines for communicating the first receiving tank 7, the second receiving tank 8, the third receiving tank 9 and the fourth receiving tank 10 with the second vacuum unit 12 are preferably respectively provided with a fifth valve I-5, a sixth valve I-6, a seventh valve I-7 and an eighth valve I-8; a ninth valve I-9 is preferably arranged on a pipeline for communicating the feeding tank 2 with the second vacuum unit 12; the second unit is used for controlling the vacuum degrees of the receiving tank and the feeding tank so as to realize continuous batch feeding under the condition of ensuring the stable vacuum of the rectifying tower; in the invention, the first receiving tank 7, the second receiving tank 8 and the third receiving tank 9 are used for receiving fractions, and can be alternately used through the control of valves to realize continuous and non-stop discharge; and the fourth receiving tank is used for receiving the kettle residue.

In the present invention, the feed tank 2, the connecting section 6, the first receiving tank 7, the second receiving tank 8, the third receiving tank 9 and the fourth receiving tank 10 are all provided with evacuation valves, and the specific installation method of the evacuation valves is not particularly limited in the present invention, and methods well known to those skilled in the art can be used.

The invention provides a method for producing polycosanol with a specific fingerprint spectrum by using the device in the scheme, which comprises the following steps:

(i) adding the saponified crude alcohol into a material dissolving tank 1, feeding the heated and dissolved material into a material feeding tank 2, feeding the material in the material feeding tank 2 into a rectifying still 4, carrying out first batch rectification under the vacuum condition, and collecting fractions in sections through a first receiving tank 7, a second receiving tank 8 and a third receiving tank 9 at the top of the tower;

(ii) discharging collected fractions and kettle residues after the first batch of rectification is finished, feeding the next batch of rectification under the condition that the vacuum degrees of the feeding tank 2 and the rectifying tower 3 are consistent, and starting to receive the fractions of the second batch when the vacuum degrees of the first receiving tank 7, the second receiving tank 8 and the third receiving tank 9 are consistent with the vacuum degree of the rectifying tower 3;

(iii) and (3) repeating the step (ii) to carry out rectification of a plurality of batches, carrying out gas chromatography detection on the collected fractions, and combining products with similar fingerprints of each batch to obtain the specific fingerprint polycosanol.

The method comprises the steps of putting saponified crude alcohol into a material dissolving tank 1, feeding the heated and dissolved material into a material feeding tank 2, feeding the material in the material feeding tank 2 into a rectifying still 4, carrying out first batch rectification under the vacuum condition, and collecting fractions in sections through a first receiving tank 7, a second receiving tank 8 and a third receiving tank 9 at the top of the tower. In the invention, the saponified crude alcohol is preferably a crude fatty alcohol product prepared by taking rice bran wax or beeswax as a raw material and performing saponification reaction; the saponified crude alcohol comprises the following components in parts by mass: 0-7% of eicosanol, 0.1-10% of docosanol, 4-20% of tetracosanol, 1-14% of hexacosanol, 10-17% of octacosanol, 17-70% of triacontanol, 4-22% of dotriacontanol, 0.1-20% of tetratriacontanol, 0-14% of hexacosanol and 0-3% of triacontanol; preferably, the composition comprises 0-3% of eicosanol, 1-8% of docosanol, 5-15% of tetracosanol, 2-13% of hexacosanol, 13-15% of octacosanol, 25-50% of triacontanol, 5-20% of dotriacontanol, 0.5-18% of tetradecanol and 1-4% of hexadecanol.

In the invention, the temperature of the heating material is preferably 80-90 ℃; the heated and melted materials enter a feeding tank 2, and the materials in the feeding tank 2 are preferably pumped into a rectifying still 4 through a first conveying pump I-1; after entering a rectifying still 4, a rectifying system consisting of a rectifying tower 3, the rectifying still 4 and a reflux condenser 5 starts first batch rectification under the vacuum condition, the vacuum degree of the rectifying tower 3 in the rectifying process is preferably 20-50 Pa, the reflux ratio is preferably 1: 5-20, more preferably 1: 10-15, and the temperature of the rectifying still is preferably 230-250 ℃; during the rectification, inert gas (particularly nitrogen gas) is preferably filled into the system through the gas inlet of the connecting section 6 to prevent explosion caused by material combustion. The polycosanol with different fingerprint spectra is preferably produced by controlling the temperature of the tower bottom and the reflux ratio, and in the invention, the higher the temperature of the tower bottom is, the higher the content of heavy components in the product collected from the tower top is.

In the invention, the fraction collected by stages is specifically: and in the range of the tower top temperature of 230-250 ℃, one section is arranged at every 0.5-2 ℃, collected fractions are sequentially marked as a first section fraction to an nth section fraction, n is an integer less than or equal to 40, preferably 18-30, and further preferably 18-25, and the vacuum degree in the receiving tank is consistent with that of the rectifying tower when the fractions are collected.

In the present invention, the fraction collected by stages is more specifically: collecting the first stage fraction in a first receiving tank 7, collecting the second stage fraction in a second receiving tank 8, collecting the third stage fraction in a third receiving tank 9, closing a second valve I-2 and a third valve I-3 while collecting the third stage fraction, discharging the first stage fraction and the second stage fraction after emptying the first receiving tank 7 and the second receiving tank 8, then opening a fifth valve I-5 and a sixth valve I-6, closing the fifth valve I-5 and the sixth valve I-6 when the vacuum degrees of the first receiving tank 7 and the second receiving tank 8 are consistent with that of the rectifying tower, opening the second valve I-2 and the third valve I-3 in sequence, receiving the fourth stage fraction and the fifth stage fraction, closing the fourth valve I-4 and the second valve I-2 when receiving the fifth stage fraction, discharging the third stage fraction and the fourth stage fraction after emptying the third receiving tank 9 and the first receiving tank 7, and then opening a seventh valve I-7 and a fifth valve I-5, closing the seventh valve I-7 and the fifth valve I-5 when the vacuum degrees of the third receiving tank 9 and the first receiving tank 7 are consistent with the vacuum degree of the rectifying tower, opening a fourth valve I-4 to receive the fraction of the sixth section, and the like until all the fractions are received.

After the first batch of rectification is finished, discharging collected fractions and kettle residues, wherein the kettle residues are preferably discharged into a fourth receiving tank 10 through an eleventh valve I-11 and a second delivery pump II-2, and the method specifically comprises the following steps: the method comprises the steps of firstly opening an eighth valve I-8, closing the eighth valve I-8 when the vacuum degree in a fourth receiving tank is consistent with the vacuum degree of a rectifying tower, opening an eleventh valve I-11, putting kettle residues into a fourth receiving tank 10 through a second conveying pump II-2, then closing the eleventh valve I-11, and discharging the kettle residues after the fourth receiving tank 10 is emptied. In the present invention, the method of discharging the fractions is the same as the above scheme, and is not described herein; the invention finishes the rectification when no more distillate flows out from the tower top.

After the distillate and the kettle residue are discharged, the invention feeds the next batch under the condition that the vacuum degrees of the feeding tank 2 and the rectifying tower 3 are consistent, and starts to receive the distillate of the second batch when the vacuum degrees of the first receiving tank 7, the second receiving tank 8 and the third receiving tank 9 are consistent with the vacuum degree of the rectifying tower 3. The vacuum degree of the feeding tank is preferably controlled by a ninth valve I-9; the method of receiving the second batch fraction is identical to the method of receiving the first batch fraction and will not be described in detail here.

The invention repeats the step (ii) to carry out rectification of a plurality of batches, carries out gas chromatography detection on collected fractions, and combines products with similar fingerprints of each batch to obtain the specific fingerprint polycosanol. In the present invention, the gas chromatography detection method is not particularly required in the present invention, and a method well known to those skilled in the art may be used. In the specific embodiment of the invention, the composition of fractions at each stage is preferably obtained through gas chromatography detection, fractions with similar fingerprint spectra at each stage in each batch are combined, and then the combined fractions are mixed according to the target fingerprint spectrum of policosanol to obtain the policosanol of the target fingerprint spectrum, wherein the specific mixing ratio of the mixing is determined according to the components of the combined fractions and the components of the target fingerprint spectrum policosanol; in the specific embodiment of the present invention, each of the combined fractions may be further rectified for 2 times to separate and obtain various high-purity higher fatty alkanols, and the rectification method is consistent with the above scheme, and is not described herein again.

In the invention, the specific fingerprint polycosanol comprises the following components in percentage by mass: 0.1-15% of docosanol, 0.1-20% of tetracosanol, 0.5-30% of hexacosanol, 10.0-99.0% of octacosanol, 0.2-15% of triacontanol and 0.1-10% of dotriacontanol; the components with the following mass fractions are preferably included: 0.5-12% of docosanol, 0.5-18% of tetracosanol, 1-28% of hexacosanol, 15-95% of octacosanol, 0.5-12% of triacontanol and 0.5-9% of dotriacontanol.

The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention.