# US 12,000,814 B2 · Apparatus and method for producing policosanol having specific chromatographic fingerprint > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 12,000,814 B2 - Document ID: US12000814B2 - Status: Granted - Kind: B2 - Application number: 17/199,832 - Filed: 2021-03-12 - Published: 2021-12-23 - Granted: 2024-06-04 - Earliest claimed: 2021-03-12 - Assignees: Institute of Biological Resources, Jiangxi Academy of Sciences - Applicants: Institute of Biological Resources, Jiangxi Academy of Sciences - Inventors: Lichuang Cai; Jianping Liu; Kexian Ouyang; Xiongchang Guo; Yue Tu - Web page: https://patentgrep.com/patent/US12000814B2 ## CPC - B01D 3/10: Vacuum distillation (B01D3/12 takes precedence) - G01N 30/88: Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 - B01D 3/106: {with the use of a pump for creating vacuum and for removing the distillate} - B01D 3/42: Regulation; Control - C07C 29/80: by distillation - C07C 29/84: by extractive distillation - B01D 2202/00: Details concerning evaporation, distillation or condensation - G01N 2030/025: {Gas chromatography} - G01N 2030/884: {organic compounds} - G01N 2030/8886: {Analysis of industrial production processes} - B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28) - G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q) - C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS ## Abstract The present disclosure provides an apparatus and method for producing a policosanol having a specific chromatographic fingerprint. The apparatus of the present disclosure has a feed tank and receiving tanks which are connected to a vacuum system. The method of the present disclosure is carried out by a high vacuum rectification process and includes: firstly, feeding a saponified crude alkanol into a melting tank in which the material is melted and then flows into the feed tank, and then injecting the material into a rectifying still using a delivery pump, followed by first rectification under vacuum condition and sequential collection of fractions at different phases from the tower top and stillage residue from the tower bottom; and after the completion of the rectification of the first batch crude product, carrying out second feeding on the basis of consistent vacuum in the feed tank and the rectifying tower. ## Claims ### Claim 1 An apparatus for producing a policosanol having a specific chromatographic fingerprint, comprising: a melting tank (1); a feed tank (2), with an inlet of the feed tank (2) being communicated with an outlet of the melting tank (1); a rectifying tower (3) having a rectifying still (4) disposed at a bottom of the rectifying tower, a reflux condenser (5) disposed at a top of the rectifying tower, and a connection section (6) disposed between the top of the rectifying tower and the reflux condenser, with a discharge outlet being formed in the connection section (6), and a feed inlet being formed in the rectifying still (4) and communicated with an outlet of the feed tank (2); wherein an inflation inlet is formed in the connection section (6) to charge an inert gas into a system during a rectifying process; a first receiving tank (7), a second receiving tank (8) and a third receiving tank (9) that are connected in parallel, with inlets of the first receiving tank (7), the second receiving tank (8) and the third receiving tank (9) being communicated with the discharge outlet of the connection section (6); a fourth receiving tank (10) which is communicated with an outlet of the rectifying still (4); a first vacuum unit (11) which is communicated with the reflux condenser (5); and a second vacuum unit (12) which is communicated with the first receiving tank (7), the second receiving tank (8), the third receiving tank (9), the fourth receiving tank (10) and the feed tank (2) separately, to control vacuum degrees in the first receiving tank (7), the second receiving tank (8), the third receiving tank (9), the fourth receiving tank (10), and the feed tank (2). ### Claim 2 (depends on 1) The apparatus according to claim 1, wherein a first valve (I-1) is disposed on a pipe by which the outlet of the melting tank (1) is communicated with the inlet of the feed tank (2), and a second valve (I-2), a third valve (I-3) and a fourth valve (I-4) are disposed on pipes by which the discharge outlet of the connection section (6) is communicated with the inlets of the first receiving tank (7), the second receiving tank (8) and the third receiving tank (9), respectively; a fifth valve (I-5), a sixth valve (I-6), a seventh valve (I-7) and an eighth valve (I-8) are disposed on pipes by which the first receiving tank (7), the second receiving tank (8), the third receiving tank (9) and the fourth receiving tank (10) are communicated with the second vacuum unit (12), respectively; a ninth valve (I-9) is disposed on a pipe by which the feed tank (2) is communicated with the second vacuum unit (12); a tenth valve (I-10) is disposed on a pipe by which the reflux condenser (5) is communicated with the first vacuum unit (11); a first delivery pump (II-1) is disposed on a pipe by which the outlet of the feed tank (2) is communicated with the feed inlet of the rectifying still (4); an eleventh valve (I-11) and a second delivery pump (II-2) are sequentially disposed on a pipe by which the outlet of the rectifying still (4) is communicated with an inlet of the fourth receiving tank (10) in a direction from the outlet of the rectifying still to the inlet of the fourth receiving tank; emptying valves are mounted on the feed 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). ### Claim 3 (depends on 1) The apparatus according to claim 1, wherein the rectifying tower (3) is a packed tower which is 3-5 m high with 15-25 plates. ### Claim 4 (depends on 2) The apparatus according to claim 2, wherein the rectifying tower (3) is a packed tower which is 3-5 m high with 15-25 plates. ### Claim 5 (depends on 1) The apparatus according to claim 1, wherein the first vacuum unit (11) and the second vacuum unit (12) are both four-stage roots vacuum units. ### Claim 6 (depends on 2) The apparatus according to claim 2, wherein the first vacuum unit (11) and the second vacuum unit (12) are both four-stage roots vacuum units. ### Claim 7 (depends on 1) A method for producing a policosanol having a specific chromatographic fingerprint using an apparatus according to claim 1, comprising following steps: step 1, feeding a saponified crude alkanol into the melting tank (1) in which the material is melted by heating and then flows into the feed tank (2), and injecting the material in the feed tank (2) into the rectifying still (4), followed by first rectification under vacuum condition and collection of fractions at different phases from the tower top by means of the first receiving tank (7), the second receiving tank (8) and the third receiving tank (9); step 2, discharging the collected fractions and stillage residue after the completion of the first rectification, carrying out second feeding on the basis of consistent vacuum degree in the feed tank (2) and the rectifying tower (3), and starting receiving the fractions for the second time when the vacuum degree is consistent in the first receiving tank (7), the second receiving tank (8) and the third receiving tank (9) as well the rectifying tower (3); and step 3, repeating step 2 to complete multiple times of rectifications, performing gas chromatographic detection on the collected fractions, and combining the product having similar chromatographic fingerprints in different times to obtain the policosanol having the specific chromatographic fingerprint; wherein the policosanol having the specific chromatographic fingerprint 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. ### Claim 8 (depends on 7) The method for producing a policosanol having a specific chromatographic fingerprint according to claim 7, wherein a first valve (I-1) is disposed on a pipe by which the outlet of the melting tank (1) is communicated with the inlet of the feed tank (2), and a second valve (I-2), a third valve (I-3) and a fourth valve (I-4) are disposed on pipes by which the discharge outlet of the connection section (6) is communicated with the inlets of the first receiving tank (7), the second receiving tank (8) and the third receiving tank (9), respectively; a fifth valve (I-5), a sixth valve (I-6), a seventh valve (I-7) and an eighth valve (I-8) are disposed on pipes by which the first receiving tank (7), the second receiving tank (8), the third receiving tank (9) and the fourth receiving tank (10) are communicated with the second vacuum unit (12), respectively; a ninth valve (I-9) is disposed on a pipe by which the feed tank (2) is communicated with the second vacuum unit (12); a tenth valve (I-10) is disposed on a pipe by which the reflux condenser (5) is communicated with the first vacuum unit (11); a first delivery pump (II-1) is disposed on a pipe by which the outlet of the feed tank (2) is communicated with the feed inlet of the rectifying still (4); an eleventh valve (I-11) and a second delivery pump (II-2) are sequentially disposed on a pipe by which the outlet of the rectifying still (4) is communicated with an inlet of the fourth receiving tank (10) in a direction from the outlet of the rectifying still to the inlet of the fourth receiving tank; emptying valves are mounted on the feed 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). ### Claim 9 (depends on 7) The method for producing a policosanol having a specific chromatographic fingerprint according to claim 7, wherein the rectifying tower (3) is a packed tower which is 3-5 m high with 15-25 plates. ### Claim 10 (depends on 8) The method for producing a policosanol having a specific chromatographic fingerprint according to claim 8, wherein the rectifying tower (3) is a packed tower which is 3-5 m high with 15-25 plates. ### Claim 11 (depends on 7) The method for producing a policosanol having a specific chromatographic fingerprint according to claim 7, wherein the first vacuum unit (11) and the second vacuum unit (12) are both four-stage roots vacuum units. ### Claim 12 (depends on 8) The method for producing a policosanol having a specific chromatographic fingerprint according to claim 8, wherein the first vacuum unit (11) and the second vacuum unit (12) are both four-stage roots vacuum units. ### Claim 13 (depends on 7) The method according to claim 7, wherein the saponified crude alkanol is a crude aliphatic alkanol prepared from rice bran wax or beeswax through a saponification reaction. ### Claim 14 (depends on 8) The method according to claim 8, wherein the saponified crude alkanol is a crude aliphatic alkanol prepared from rice bran wax or beeswax through a saponification reaction. ### Claim 15 (depends on 7) The method according to claim 7, wherein the saponified crude alkanol comprises the following components in percentage 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 tetratriacontano1, 0-14% of hexatriacontanol and 0-3% of octatriacontanol. ### Claim 16 (depends on 13) The method according to claim 13, wherein the saponified crude alkanol comprises the following components in percentage 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 hexatriacontanol and 0-3% of octatriacontanol. ### Claim 17 (depends on 14) The method according to claim 14, wherein the saponified crude alkanol comprises the following components in percentage 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 hexatriacontanol and 0-3% of octatriacontanol. ### Claim 18 (depends on 7) The method according to claim 7, wherein the rectifying tower operates at a vacuum degree of 20-50 Pa and a reflux ratio of 1:(5-20), and the rectifying still is at a temperature of 230-250° C. ### Claim 19 (depends on 7) The method according to claim 7, wherein collecting fractions at different phases is specifically as follows: the range of a tower top temperature of 230-250° C. is divided into phases, each phase being 0.5-2° C., and the collected fractions are sequentially marked as first to nth fractions, n being an integer of less than or equal to 40; and the vacuum degree is consistent in the receiving tanks and the rectifying tower when the fractions are collected. ### Claim 20 (depends on 19) The method according to claim 19, wherein collecting fractions at different phases is specifically as follows: the first fraction is collected in the first receiving tank (7), while a second fraction is collected in the second receiving tank (8) and a third fraction is collected in the third receiving tank (9); when the third fraction is collected, the second valve (I-2) and the third valve (I-3) are closed to empty the first receiving tank (7) and the second receiving tank (8), followed by discharging the first fraction and the second fraction; the fifth valve (I-5) and the sixth valve (I-6) are opened; when the vacuum degree is consistent in the first receiving tank (7) and the second receiving tank (8) as well as the rectifying tower, the fifth valve (I-5) and the sixth valve (I-6) are closed, and the second valve (I-2) and the third valve (I-3) are orderly opened to receive a fourth fraction and a fifth fraction; when the fifth fraction is received, the fourth valve (I-4) and the second valve (I-2) are closed to empty the third receiving tank (9) and the first receiving tank (7), followed by discharging the third fraction and the fourth fraction; the seventh valve (I-7) and the fifth valve (I-5) are opened; when the vacuum degree is consistent in the third receiving tank (9) and the first receiving tank (7) as well as the rectifying tower, the seventh valve (I-7) and the fifth valve (I-5) are closed, and the fourth valve (I-4) is opened to receive a sixth fraction; and remaining fractions are received similarly until all the fractions are completely received.