CN1634967A - Sterol refining process - Google Patents
Sterol refining process Download PDFInfo
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- CN1634967A CN1634967A CN 200310122952 CN200310122952A CN1634967A CN 1634967 A CN1634967 A CN 1634967A CN 200310122952 CN200310122952 CN 200310122952 CN 200310122952 A CN200310122952 A CN 200310122952A CN 1634967 A CN1634967 A CN 1634967A
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Abstract
This invention relates to a sterol refining method, which comprises the following steps: washing the crude sterol for several times and making the liquid to solid separation; then adding it into the mixture liquid with mass proportion between acetone to ethanol as1 degree 190-210; Heating it to 64-66 degree s for keeping and filtering; the filtered liquid slowly crystallizing in the cooling kettle; after the cold analysis, filtering the liquid and washing the filtered dregs by mixture liquid for several times; drying the dregs to get the sterol.
Description
Technical field
The present invention relates to a kind of fine purification method for sterol technical field.
Background technology
Natural phytosterin is a kind of material with biological value, and it has purposes widely in fields such as medicine, makeup, growth of animal agent and sheet processing thereof, printing, weaving, food.Contain Sitosterol in the plant sterol, campesterol, dish grain sterol, multiple composition such as Stigmasterol, wherein Stigmasterol has very strong anti-inflammatory and antiinflammation and as anti-inflammation drugs, plant sterol has very important physical active function to human body, can suppress the absorption of human body to cholesterol, promotion is to the catabolism of cholesterol, the biochemistry that suppresses cholesterol is synthetic, to coronary heart disease, ulcer, skin carcinoma, atherosclerosis has significant prevention and result of treatment, and plant sterol still is the raw materials for production of steroid drugs and Vitamin D3 500,000 I.U/GM in addition, emulsifying agent as W/O, food antioxidant and nutritional additive thereof or the like.Plant sterol is mainly derived from the refining of vegetables oil and gets a foothold, deodorization distillate particularly, China is grease production big country, full refining throughput has reached 1,200,000 tons at present, has become the problem of the current important solution of China as the reasonable utilization of deodorization procedures byproduct-deodorization distillate in the refining.
The production method that tradition is extracted sterol has: solvent crystallization, and it is that the laboratory study plant sterol separates the main method of purifying, and this method operation steps is many, and quantity of solvent is big, reclaims difficulty, and the sterol rate of recovery is low, therefore also is difficult to industrialization; Complexometry is that DD oil is carried out saponification, and acid is decomposed, extraction, and complex reaction separates complex compound and complexing decomposition and obtains the sterol crude product, and this process solvent reclaims difficulty, and the production cost height still is in the laboratory study stage; The dry type saponification method, be that DD oil is carried out saponification with white lime or unslaked lime under the 60-90 degree, pulverize paste with machine then, through solvent extraction, concentrate and obtain thick sterol, remove impurity through washing again, dehydration obtains smart sterol, the raw material yield of this method, the purity and the yield of product are lower, improve its processing condition and still are in the research that improves yield and purity and carry out; Molecular distillation, present main industrial process, it is at first with the DD greaseization, wash then, decompression removes carbon alcohol, reclaims fatty acid ester by distillation, reclaims vitamin-E through molecular distillation again, residue carries out saponification reaction, acetone extraction has obtained thick sterol, obtains refining sterol through decolouring, recrystallization at last, and this processing method main drawback is a long flow path, operation steps is many, and the purity and the yield of product are lower.
As the patent No. is that 93100259.1 Chinese patent " extracts the novel process of vitamin-E and sterol " from the vegetable oil refining by product, and the technical process of invention comprises steps such as esterification, washing, alcoholysis, cold analysis, distillation.The present invention changes neutral oil into fatty acid methyl ester (or ethyl ester) with alcoholysis reaction, and with simple vacuum distillation plant substituted molecule distillation plant, form a brand-new technical process, extraction and purification have been realized to natural VE, obtain colory plant sterol product simultaneously, defectives such as it no doubt has its progressive one side, but still has long flow path, and operation steps is many.
And use the recrystallization method plant sterol of purifying is to utilize plant sterol different with dissolubility difference and the temperature dependence thereof of non-sterol material in organic solvent, and plant sterol is separated from its crude mixture.The key issue of recrystallization separation and purification process is correct selective solvent and Crystallization Separation purified operational condition thereof, if operational condition is undesirable, causes the rate of recovery low or purity is not high enough easily.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of fine purification method for sterol at existing background technology, its rate of recovery and purity can both reach high levels and operational path is short, simple, energy consumption is little, cost is low, provides guarantee for enterprise increases economic benefit.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: a kind of fine purification method for sterol, it is characterized in that steps in sequence is: selecting content for use is the crude product sterol of 50-55% mass percent, join in the acetone solvent, crude product sterol and acetone solvent mass ratio are 1: 1.8-2.2, after stirring, carry out solid-liquid separation through filter, liquid phase is carried out the rectifying first time, obtains the acetone of light phase and grease and two kinds of products of sterol of heavy phase; Add acetone solvent in the solid phase once more, crude product sterol and acetone solvent mass ratio are 1: 1.8-2.2, after stirring, carry out solid-liquid separation through filter, and liquid phase is as the washing first time acetone of next batch; Add entry in the solid phase and stir, after stirring, carry out solid-liquid separation through whizzer; Solid phase is joined acetone and the ethanol mass ratio is 1: in the mixed solvent of 190-210, carry out stirring heating, Heating temperature is incubated 0.5-1.5 hour, then temperature filtration to 64-66 ℃; Filtrate is under agitation carried out slow crystallizing in the cold analysis still, per hour descend when crystallization velocity is 65-40 ℃ 0.4-0.5 ℃, per hour descends 0.8-1.2 ℃ in the time of 40-35 ℃, per hour descends 1.5-2 ℃ in the time of 35-10 ℃; After cold analysis finished, solution carried out temperature filtration, and filter residue is 1 with acetone and ethanol mass ratio: the mixing solutions of 0.9-1.1 washs; Filter residue is dried, and pulverizes to obtain refining sterol.
Add entry in the above-mentioned steps (3) in the solid phase and wash and can adopt twice identical method to wash, the 1.8-2.2 that water consumption is controlled at crude product sterol quality doubly, to improve sterol purity.
Above-mentioned steps (6) filter residue washs with mixing solutions and can adopt twice identical method to wash, to improve sterol purity.
Above-mentioned crude product sterol preferred mass per-cent is 52%, and crude product sterol and acetone solvent mass ratio are 1: 2, and mixed solvent acetone and ethanol mass ratio are 1: 200, makes to optimize to obtain sterol purity among the embodiment and reach more than 97%.
Compared with prior art, the invention has the advantages that: select for use the yield that extraction is extracted sterol than old processing method from DD oil for sterol after the new technology to exceed about 20-25%, also improved the product quality of vitamin-E simultaneously; Extraction for sterol exceeds about 7% than the purity of extracting sterol in the old technology from DD oil, and the quality of product can reach advanced international level, provides guarantee for enterprise exports goods and earns foreign currency and increases economic benefit; Greatly shortened operational path, reduced energy consumption, in the distil process originally, in order to obtain the higher sterol rate of recovery, generally will be through distillation several times, the 2nd, adopt that cryogenic system such as cooling temperature are low to be reached-1 to 5 ℃ and just can reach the high rate of recovery, molecular distillation is the power consumption rich and influential family, and the cooling temperature of this process using is 10 ℃, just can obtain sterol and the vitamin-E product that meets U.S. FCC standard more than 97%, reduce cost and energy consumption, simplified technical process.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment 1:
A kind of fine purification method for sterol is characterized in that steps in sequence is:
(1) is the crude product sterol of 52% mass percent with 200Kg, content, joins in the 400Kg acetone solvent, stirred 30 minutes, evenly, carry out solid-liquid separation through flame filter press, liquid phase is carried out the rectifying first time, obtains the acetone of light phase and grease and two kinds of products of sterol of heavy phase;
(2) add the 400Kg acetone solvent in the solid phase once more, stirred 30 minutes, evenly after, carry out solid-liquid separation through flame filter press, liquid phase is as the washing first time acetone of next batch;
(3) add 400Kg water in the solid phase and stir, stirred 30 minutes, even after, enter whizzer and carry out the high speed solid-liquid separation; And then add 400Kg water and stir, stirred 30 minutes, even after, enter whizzer and separate again once;
(4) solid phase being joined acetone and ethanol mass ratio is in 1: 200 the mixed solvent, to carry out stirring heating lentamente, and Heating temperature to 65 ℃ is incubated 1 hour, then temperature filtration;
(5) filtrate under the 20-30r.p.m agitation condition, is carried out slow crystallizing in the cold analysis still, per hour descends 0.5 ℃ when crystallization velocity is 65-40 ℃, per hour descends 1 ℃ in the time of 40-35 ℃, per hour descends 1.5-2 ℃ in the time of 35-10 ℃;
(6) after cold analysis finished, solution carried out temperature filtration, and filter residue is that 1: 1 mixing solutions washs washed twice with acetone and ethanol mass ratio;
(7) filter residue is dried, and pulverizes to obtain refining sterol, and its content is higher than 97.5%.
Embodiment 2:
A kind of fine purification method for sterol is characterized in that steps in sequence is:
(1) is the crude product sterol of 55% mass percent with 200Kg, content, joins in the 360Kg acetone solvent, stirred 30 minutes, evenly, carry out solid-liquid separation through flame filter press, liquid phase is carried out the rectifying first time, obtains the acetone of light phase and grease and two kinds of products of sterol of heavy phase;
(2) add the 360Kg acetone solvent in the solid phase once more, stirred 30 minutes, evenly after, carry out solid-liquid separation through flame filter press, liquid phase is as the washing first time acetone of next batch;
(3) add 360Kg water in the solid phase and stir, stirred 30 minutes, even after, enter whizzer and carry out the high speed solid-liquid separation; And then add 360Kg water and stir, stirred 30 minutes, even after, enter whizzer and separate again once;
(4) solid phase being joined acetone and ethanol mass ratio is in 1: 210 the mixed solvent, to carry out stirring heating lentamente, and Heating temperature to 66 ℃ is incubated 0.5 hour, then temperature filtration;
(5) filtrate under the 20-30r.p.m agitation condition, is carried out slow crystallizing in the cold analysis still, per hour descends 0.6 ℃ when crystallization velocity is 65-40 ℃, per hour descends 1.2 ℃ in the time of 40-35 ℃, per hour descends 1.5-2 ℃ in the time of 35-10 ℃;
(6) after cold analysis finished, solution carried out temperature filtration, and filter residue is that 1: 1.1 mixing solutions washs washed twice with acetone and ethanol mass ratio;
(7) filter residue is dried, and pulverizes to obtain refining sterol, and its content is higher than 95%.
Embodiment 3:
A kind of fine purification method for sterol is characterized in that steps in sequence is:
(1) is the crude product sterol of 50% mass percent with 200Kg, content, joins in the 440Kg acetone solvent, stirred 30 minutes, evenly, carry out solid-liquid separation through flame filter press, liquid phase is carried out the rectifying first time, obtains the acetone of light phase and grease and two kinds of products of sterol of heavy phase;
(2) add the 440Kg acetone solvent in the solid phase once more, stirred 30 minutes, evenly after, carry out solid-liquid separation through flame filter press, liquid phase is as the washing first time acetone of next batch;
(3) add 440Kg water in the solid phase and stir, stirred 30 minutes, even after, enter whizzer and carry out the high speed solid-liquid separation; And then add 440Kg water and stir, stirred 30 minutes, even after, enter whizzer and separate again once;
(4) solid phase being joined acetone and ethanol mass ratio is in 1: 190 the mixed solvent, to carry out stirring heating lentamente, and Heating temperature to 64 ℃ is incubated 1.5 hours, then temperature filtration;
(5) filtrate under the 20-30r.p.m agitation condition, is carried out slow crystallizing in the cold analysis still, per hour descends 0.4 ℃ when crystallization velocity is 65-40 ℃, per hour descends 0.8 ℃ in the time of 40-35 ℃, per hour descends 1.5-2 ℃ in the time of 35-10 ℃;
(6) after cold analysis finished, solution carried out temperature filtration, and filter residue is that 1: 0.9 mixing solutions washs washed twice with acetone and ethanol mass ratio;
(8) filter residue is dried, and pulverizes to obtain refining sterol, and its content is higher than 95%.
Claims (8)
1, a kind of fine purification method for sterol is characterized in that steps in sequence is:
(1) selecting content for use is the crude product sterol of 50-55% mass percent, join in the acetone solvent, crude product sterol and acetone solvent mass ratio are 1: 1.8-2.2, after stirring, carry out solid-liquid separation through filter, liquid phase is carried out the rectifying first time, obtains the acetone of light phase and grease and two kinds of products of sterol of heavy phase;
(2) add acetone solvent in the solid phase once more, crude product sterol and acetone solvent mass ratio are 1: 1.8-2.2, after stirring, carry out solid-liquid separation through filter, and liquid phase is as the washing first time acetone of next batch;
(3) add entry in the solid phase and stir, after stirring, carry out solid-liquid separation through whizzer;
(4) solid phase being joined acetone and ethanol mass ratio is 1: in the mixed solvent of 190-210, carry out stirring heating, Heating temperature is incubated 0.5-1.5 hour, then temperature filtration to 64-66 ℃;
(5) filtrate is under agitation carried out slow crystallizing in the cold analysis still, per hour descends when crystallization velocity is 65-40 ℃ 0.4-0.6 ℃, per hour descends 0.8-1.2 ℃ in the time of 40-35 ℃, per hour descends 1.5-2 ℃ in the time of 35-10 ℃;
(6) after cold analysis finished, solution carried out temperature filtration, and filter residue is 1 with acetone and ethanol mass ratio: the mixing solutions of 0.9-1.1 washs;
(7) filter residue is dried, and pulverizes to obtain refining sterol.
2, fine purification method for sterol according to claim 1 is characterized in that adding in step (3) solid phase entry and washs and can adopt twice identical method to wash, and the 1.8-2.2 that water consumption is controlled at crude product sterol quality doubly.
3, fine purification method for sterol according to claim 1 is characterized in that step (6) filter residue washs with mixing solutions can adopt twice identical method to wash.
4, fine purification method for sterol according to claim 1 is characterized in that step (5) stirs its speed control in the 20-30r.p.m condition.
5, fine purification method for sterol according to claim 1 is characterized in that crude product sterol mass percent is 52%.
6, fine purification method for sterol according to claim 1 is characterized in that crude product sterol and acetone solvent mass ratio are 1: 2.
7, fine purification method for sterol according to claim 1 is characterized in that mixed solvent acetone and ethanol mass ratio are 1: 200.
8, fine purification method for sterol according to claim 2 is characterized in that adding in step (3) solid phase entry and washs and can adopt twice identical method to wash, and water consumption is controlled at 2 times of crude product sterol quality.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310122952 CN1634967A (en) | 2003-12-30 | 2003-12-30 | Sterol refining process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310122952 CN1634967A (en) | 2003-12-30 | 2003-12-30 | Sterol refining process |
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| CN1634967A true CN1634967A (en) | 2005-07-06 |
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| CN 200310122952 Pending CN1634967A (en) | 2003-12-30 | 2003-12-30 | Sterol refining process |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100358989C (en) * | 2005-11-02 | 2008-01-02 | 尤新 | Method for extracting lipid containing plant sterol |
| CN101942002A (en) * | 2010-09-24 | 2011-01-12 | 岳阳环宇药业有限公司 | Refining technology for steroid 21-position ester |
| CN101607977B (en) * | 2009-06-12 | 2011-06-29 | 天津工业大学 | Method for extracting and purifying natural phytosterol from oil deodorization distillate residual oil and technique thereof |
| CN101701029B (en) * | 2009-01-09 | 2012-05-23 | 天津工业大学 | Method for extracting natural phytosterin from residual oil of vegetable fat deodorizing distillate |
| CN109705182A (en) * | 2019-01-24 | 2019-05-03 | 上海新华联制药有限公司 | A kind of preparation method of Nilestriol |
| CN110818762A (en) * | 2019-11-19 | 2020-02-21 | 福建省格兰尼生物工程股份有限公司 | Residual oil treatment method for recovering sterol and refining sylvite |
| CN111875659A (en) * | 2020-08-21 | 2020-11-03 | 宜春大海龟生命科学有限公司 | Method for purifying phytosterol |
-
2003
- 2003-12-30 CN CN 200310122952 patent/CN1634967A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100358989C (en) * | 2005-11-02 | 2008-01-02 | 尤新 | Method for extracting lipid containing plant sterol |
| CN101701029B (en) * | 2009-01-09 | 2012-05-23 | 天津工业大学 | Method for extracting natural phytosterin from residual oil of vegetable fat deodorizing distillate |
| CN101607977B (en) * | 2009-06-12 | 2011-06-29 | 天津工业大学 | Method for extracting and purifying natural phytosterol from oil deodorization distillate residual oil and technique thereof |
| CN101942002A (en) * | 2010-09-24 | 2011-01-12 | 岳阳环宇药业有限公司 | Refining technology for steroid 21-position ester |
| CN109705182A (en) * | 2019-01-24 | 2019-05-03 | 上海新华联制药有限公司 | A kind of preparation method of Nilestriol |
| CN109705182B (en) * | 2019-01-24 | 2021-08-31 | 上海新华联制药有限公司 | Preparation method of nilestriol |
| CN110818762A (en) * | 2019-11-19 | 2020-02-21 | 福建省格兰尼生物工程股份有限公司 | Residual oil treatment method for recovering sterol and refining sylvite |
| CN110818762B (en) * | 2019-11-19 | 2022-08-05 | 福建省格兰尼生物工程股份有限公司 | Residual oil treatment method for recovering sterol and refining sylvite |
| CN111875659A (en) * | 2020-08-21 | 2020-11-03 | 宜春大海龟生命科学有限公司 | Method for purifying phytosterol |
| CN111875659B (en) * | 2020-08-21 | 2021-10-08 | 宜春大海龟生命科学有限公司 | Method for purifying phytosterol |
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