CN106146606A - In a kind of natural Vitamin E production process, evaporative crystallization reclaims plant sterol method - Google Patents
In a kind of natural Vitamin E production process, evaporative crystallization reclaims plant sterol method Download PDFInfo
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- CN106146606A CN106146606A CN201510169922.XA CN201510169922A CN106146606A CN 106146606 A CN106146606 A CN 106146606A CN 201510169922 A CN201510169922 A CN 201510169922A CN 106146606 A CN106146606 A CN 106146606A
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Abstract
The present invention provides the evaporative crystallization in a kind of natural Vitamin E production process to reclaim plant sterol method, comprise the steps: that A: the distillation after the leftover bits and pieces deodorize separated in production process of vegetable oil adds methanol ester and swaps after completion of the reaction, after the most neutralized washing, become esterised oil；B: esterised oil passes through two-stage molecular distillation；The esterised oil after two-stage molecular distillation of C: step B is placed in crystallization kettle, crystallization initiation temperature 40 DEG C-60 DEG C, lowers the temperature with the speed of 2 DEG C/h-3 DEG C/h, and final crystallization temperature is at 8 DEG C-20 DEG C, after reaching final crystallization temperature, is incubated 8 hours；D: filter the crystal plant sterol of separating step C.The key feature of the present invention is to use evaporative crystallization to reclaim plant sterol, and crystallization time is short, the plant sterol product moisture-free obtained, and purity is high.
Description
Technical field
The present invention relates to the process of the extraction of a plant sterols.
Background technology
Plant sterol is distributed widely in biosphere, has a structure that
Plant sterol has a following physiological function: 1: antiinflammatory action；2: prophylactic treatment coronary atherosclerosis；3: protection skin, antioxidation；4: for carrier medicament and the production of vitamin D3.
Industrial often first will extract vitamin E after plant oil leftover deodorize after, remaining residue carries out the Hydrolysis kinetics of sterol again.
Summary of the invention
The present invention provides the evaporative crystallization in a kind of natural Vitamin E production process to reclaim plant sterol method, its objective is to provide a kind of crystallization time short, and product moisture-free, purity is high, and evaporative crystallization reclaims the method for plant sterol.
The technical solution adopted for the present invention to solve the technical problems is:
Evaporative crystallization in a kind of natural Vitamin E production process reclaims plant sterol method, it is characterised in that: comprise the steps:
A: the distillation after the leftover bits and pieces deodorize separated in production process of vegetable oil adds methanol ester and swaps after completion of the reaction, then after neutralized washing, becomes esterised oil；
B: esterised oil passes through two-stage molecular distillation, and first order molecular distillation is moisture and the methanol of residual in evaporation removing esterised oil, and secondary molecules distillation is the fatty acid methyl ester of 5%-25% for volume ratio in evaporation removing esterised oil；
The esterised oil after two-stage molecular distillation of C: step B is placed in crystallization kettle, crystallization initiation temperature 40 DEG C-60 DEG C, lowers the temperature with the speed of 2 DEG C/h-3 DEG C/h, and final crystallization temperature is at 8 DEG C-20 DEG C, after reaching final crystallization temperature, is incubated 8 hours；
D: filter the crystal plant sterol of separating step C.
In step B, the condition of first order molecular distillation is vacuum-0.09Pa to 0.099Pa, temperature 110 DEG C to 130 DEG C；The condition of secondary molecules distillation is vacuum 3Pa to 10Pa, temperature 130 DEG C to 170 DEG C.
The invention have benefit that:
The key feature of the present invention is to use evaporative crystallization to reclaim plant sterol, and crystallization time is short, the plant sterol product moisture-free obtained, and purity is high.
Detailed description of the invention
Embodiment 1:
Evaporative crystallization in a kind of natural Vitamin E production process reclaims plant sterol method, comprises the steps:
A: the distillation (namely DD oil) after the leftover bits and pieces deodorize separated in production process of vegetable oil adds methanol ester and swaps after completion of the reaction, then after neutralized washing, becomes the esterised oil of separating plant sterol to be crystallized；
B: esterised oil passes through two-stage molecular distillation, at vacuum-0.09PaPa, first order molecular distillation is carried out under the conditions of temperature 110 DEG C, first order molecular distillation is moisture and the methanol of residual in evaporation removing esterised oil, in vacuum 3Pa, carrying out secondary molecules distillation under the conditions of temperature 130 DEG C, secondary molecules distillation is the fatty acid methyl ester of 5%-25% for volume ratio in evaporation removing esterised oil；
The esterised oil after two-stage molecular distillation of C: step B is placed in crystallization kettle, crystallization initiation temperature 40 DEG C, begins with plant sterol crystallization, lowers the temperature with the speed of 2 DEG C, and final crystallization temperature is at 8 DEG C, after reaching final crystallization temperature, is incubated 8 hours；
D: filter the crystal plant sterol of separating step C.
Embodiment 2:
Evaporative crystallization in a kind of natural Vitamin E production process reclaims plant sterol method, comprises the steps:
A: the distillation (namely DD oil) after the leftover bits and pieces deodorize separated in production process of vegetable oil adds methanol ester and swaps after completion of the reaction, then after neutralized washing, becomes the esterised oil of separating plant sterol to be crystallized；
B: esterised oil passes through two-stage molecular distillation, in vacuum 0.099Pa, first order molecular distillation is carried out under the conditions of temperature 130 DEG C, first order molecular distillation is moisture and the methanol of residual in evaporation removing esterised oil, in vacuum 10Pa, carrying out secondary molecules distillation under the conditions of temperature 170 DEG C, secondary molecules distillation is the fatty acid methyl ester of 5%-25% for volume ratio in evaporation removing esterised oil；
The esterised oil after two-stage molecular distillation of C: step B is placed in crystallization kettle, crystallization initiation temperature 60 DEG C, begins with plant sterol crystallization, lowers the temperature with the speed of 3 DEG C/h, and final crystallization temperature is at 20 DEG C, after reaching final crystallization temperature, is incubated 8 hours；
D: filter the crystal plant sterol of separating step C.
Embodiment 3:
Evaporative crystallization in a kind of natural Vitamin E production process reclaims plant sterol method, comprises the steps:
A: the distillation (namely DD oil) after the leftover bits and pieces deodorize separated in production process of vegetable oil adds methanol ester and swaps after completion of the reaction, then after neutralized washing, becomes the esterised oil of separating plant sterol to be crystallized；
B: esterised oil passes through two-stage molecular distillation, in vacuum 0.01Pa, first order molecular distillation is carried out under the conditions of temperature 120 DEG C, first order molecular distillation is moisture and the methanol of residual in evaporation removing esterised oil, in vacuum 5Pa, carrying out secondary molecules distillation under the conditions of temperature 150 DEG C, secondary molecules distillation is the fatty acid methyl ester of 5%-25% for volume ratio in evaporation removing esterised oil；
The esterised oil after two-stage molecular distillation of C: step B is placed in crystallization kettle, crystallization initiation temperature 50 DEG C, begins with plant sterol crystallization, lowers the temperature with the speed of 2.5 DEG C/h, and final crystallization temperature is at 15 DEG C, after reaching final crystallization temperature, is incubated 8 hours；
D: filter the crystal plant sterol of separating step C.
Embodiment 4:
Evaporative crystallization in a kind of natural Vitamin E production process reclaims plant sterol method, comprises the steps:
A: the distillation (namely DD oil) after the leftover bits and pieces deodorize separated in production process of vegetable oil adds methanol ester and swaps after completion of the reaction, then after neutralized washing, becomes the esterised oil of separating plant sterol to be crystallized；
B: esterised oil passes through two-stage molecular distillation, in vacuum 0.02Pa, first order molecular distillation is carried out under the conditions of temperature 100 DEG C, first order molecular distillation is moisture and the methanol of residual in evaporation removing esterised oil, in vacuum 3Pa, carrying out secondary molecules distillation under the conditions of temperature 170 DEG C, secondary molecules distillation is the fatty acid methyl ester of 5%-25% for volume ratio in evaporation removing esterised oil；
The esterised oil after two-stage molecular distillation of C: step B is placed in crystallization kettle, crystallization initiation temperature 60 DEG C, begins with plant sterol crystallization, lowers the temperature with the speed of 2 DEG C/h, and final crystallization temperature is at 20 DEG C, after reaching final crystallization temperature, is incubated 8 hours；
D: filter the crystal plant sterol of separating step C.
Embodiment 5:
Evaporative crystallization in a kind of natural Vitamin E production process reclaims plant sterol method, comprises the steps:
A: the distillation (namely DD oil) after the leftover bits and pieces deodorize separated in production process of vegetable oil adds methanol ester and swaps after completion of the reaction, then after neutralized washing, becomes the esterised oil of separating plant sterol to be crystallized；
B: esterised oil passes through two-stage molecular distillation, at vacuum-0.05Pa, first order molecular distillation is carried out under the conditions of temperature 110 DEG C, first order molecular distillation is moisture and the methanol of residual in evaporation removing esterised oil, in vacuum 10Pa, carrying out secondary molecules distillation under the conditions of temperature 130 DEG C, secondary molecules distillation is the fatty acid methyl ester of 5%-25% for volume ratio in evaporation removing esterised oil；
The esterised oil after two-stage molecular distillation of C: step B is placed in crystallization kettle, crystallization initiation temperature 40 DEG C, begins with plant sterol crystallization, lowers the temperature with the speed of 3 DEG C/h, and final crystallization temperature is at 8 DEG C, after reaching final crystallization temperature, is incubated 8 hours；
D: filter the crystal plant sterol of separating step C.
Embodiment 6:
Evaporative crystallization in a kind of natural Vitamin E production process reclaims plant sterol method, comprises the steps:
A: the distillation (namely DD oil) after the leftover bits and pieces deodorize separated in production process of vegetable oil adds methanol ester and swaps after completion of the reaction, then after neutralized washing, becomes the esterised oil of separating plant sterol to be crystallized；
B: esterised oil passes through two-stage molecular distillation, in vacuum 0.099Pa, first order molecular distillation is carried out under the conditions of temperature 130 DEG C, first order molecular distillation is moisture and the methanol of residual in evaporation removing esterised oil, in vacuum 8Pa, carrying out secondary molecules distillation under the conditions of temperature 160 DEG C, secondary molecules distillation is the fatty acid methyl ester of 5%-25% for volume ratio in evaporation removing esterised oil；
The esterised oil after two-stage molecular distillation of C: step B is placed in crystallization kettle, crystallization initiation temperature 60 DEG C, begins with plant sterol crystallization, lowers the temperature with the speed of 3 DEG C/h, and final crystallization temperature is at 10 DEG C, after reaching final crystallization temperature, is incubated 8 hours；
D: filter the crystal plant sterol of separating step C.
Claims (2)
1. the evaporative crystallization in a natural Vitamin E production process reclaims plant sterol method, it is characterised in that: comprise the steps:
A: the distillation after the leftover bits and pieces deodorize separated in production process of vegetable oil adds methanol ester and swaps after completion of the reaction, then after neutralized washing, becomes esterised oil；
B: esterised oil passes through two-stage molecular distillation, and first order molecular distillation is moisture and the methanol of residual in evaporation removing esterised oil, and secondary molecules distillation is the fatty acid methyl ester of 5%-25% for volume ratio in evaporation removing esterised oil；
The esterised oil after two-stage molecular distillation of C: step B is placed in crystallization kettle, crystallization initiation temperature 40 DEG C-60 DEG C, lowers the temperature with the speed of 2 DEG C/h-3 DEG C/h, and final crystallization temperature is at 8 DEG C-20 DEG C, after reaching final crystallization temperature, is incubated 8 hours；
D: filter the crystal plant sterol of separating step C.
Evaporative crystallization in a kind of natural Vitamin E production process the most as claimed in claim 1 reclaims plant sterol method, it is characterised in that: in step B, the condition of first order molecular distillation is vacuum-0.09Pa to 0.099Pa, temperature 110 DEG C to 130 DEG C；The condition of secondary molecules distillation is vacuum 3Pa to 10Pa, temperature 130 DEG C to 170 DEG C.
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| CN201510169922.XA CN106146606A (en) | 2015-04-13 | 2015-04-13 | In a kind of natural Vitamin E production process, evaporative crystallization reclaims plant sterol method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106978252A (en) * | 2017-05-24 | 2017-07-25 | 中国农业大学 | A kind of method that pumpkin sterol is extracted based on subcritical fluids and molecular distillation |
| CN107129865A (en) * | 2017-05-24 | 2017-09-05 | 中国农业大学 | A kind of method that pumpkin phylloquinone is extracted based on subcritical fluids and molecular distillation |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101225414A (en) * | 2008-01-09 | 2008-07-23 | 河南工业大学 | Novel method for extracting natural vitamin E, phytosterol, fatty acid methyl ester by enzyme catalysis and molecular distillation |
| CN103319446A (en) * | 2013-07-05 | 2013-09-25 | 河南懿丰油脂有限公司 | Method for extracting natural vitamin E from vegetable oil deodorization distillate |
-
2015
- 2015-04-13 CN CN201510169922.XA patent/CN106146606A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101225414A (en) * | 2008-01-09 | 2008-07-23 | 河南工业大学 | Novel method for extracting natural vitamin E, phytosterol, fatty acid methyl ester by enzyme catalysis and molecular distillation |
| CN103319446A (en) * | 2013-07-05 | 2013-09-25 | 河南懿丰油脂有限公司 | Method for extracting natural vitamin E from vegetable oil deodorization distillate |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106978252A (en) * | 2017-05-24 | 2017-07-25 | 中国农业大学 | A kind of method that pumpkin sterol is extracted based on subcritical fluids and molecular distillation |
| CN107129865A (en) * | 2017-05-24 | 2017-09-05 | 中国农业大学 | A kind of method that pumpkin phylloquinone is extracted based on subcritical fluids and molecular distillation |
| CN107129865B (en) * | 2017-05-24 | 2020-11-20 | 中国农业大学 | Method for extracting cucurbitacin based on subcritical fluid and molecular distillation |
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Application publication date: 20161123 |