CN1485418A - Method for extracting coarse oil from coix seed with hypercritical carbon dioxide - Google Patents
Method for extracting coarse oil from coix seed with hypercritical carbon dioxide Download PDFInfo
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- CN1485418A CN1485418A CNA021373124A CN02137312A CN1485418A CN 1485418 A CN1485418 A CN 1485418A CN A021373124 A CNA021373124 A CN A021373124A CN 02137312 A CN02137312 A CN 02137312A CN 1485418 A CN1485418 A CN 1485418A
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- carbon dioxide
- coix seed
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- 244000077995 Coix lacryma jobi Species 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title claims abstract description 14
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims description 14
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims description 7
- 239000001569 carbon dioxide Substances 0.000 title claims description 7
- 238000000605 extraction Methods 0.000 claims abstract description 27
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 5
- 210000000582 semen Anatomy 0.000 claims description 7
- 238000010298 pulverizing process Methods 0.000 abstract description 4
- 239000010779 crude oil Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
- 239000002253 acid Substances 0.000 description 15
- 235000019198 oils Nutrition 0.000 description 15
- 238000000194 supercritical-fluid extraction Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000002277 temperature effect Effects 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 235000015112 vegetable and seed oil Nutrition 0.000 description 2
- 235000007354 Coix lacryma jobi Nutrition 0.000 description 1
- 235000015459 Lycium barbarum Nutrition 0.000 description 1
- 240000000924 Lycium carolinianum Species 0.000 description 1
- 235000015463 Lycium carolinianum Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000001550 time effect Effects 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
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- Extraction Or Liquid Replacement (AREA)
Abstract
A method or extracting crude oil of coix seed by supercritical carbon dioxide extraction. It comprise:1) drying, the water content of coix seed is below 10%; 2) pulverizing, naturally lowering temperature, after testing, pulverizing into 10-60 meshes; 3) supercritical carbon dioxide extraction, in the extracting vessel, the temperature is 30-60degree C, the pressure is 19-24MPa; in the separating column, the temperature is 30-60degree C, the pressure is 6-15Mpa; in the resolving vessel, the temperature is 30-60degree C, the pressure is2-6Mpa; the flow rate is 10-5000L/Hr; the extraction time is 1-4h.
Description
Technical field
The present invention relates to a kind of method of extracting seed oil from the plant seed, specifically is a kind of method for extracting coarse oil from coix seed with hypercritical carbon dioxide.
Background technology
Chinese patent literature CN1029662C discloses a kind of " Semen Coicis neutral grease and extracting method thereof ", it adopts solvent collection method to extract adlay oil, and the thick oil of every extraction 1kg will consume acetone 15kg, not only the cost height, production operation is also dangerous, and easy contaminate environment.
The supercritical carbon dioxide extraction vegetables oil is brand-new, the efficient separating substances technology that grows up in the last thirty years, and industrial applications has been arranged.Have different compositions and unique working substance owing to be extracted plant, people to carbon dioxide extraction method in the application of each kind of plant always in research and development, a kind of " method of supercritical carbon dioxide extraction Boxthorn Seed Oil " disclosed as Chinese patent literature CN1088745C.Up till now extremely, the report that in Chinese patent literature, does not still have the extracting coarse oil from coix seed with hypercritical carbon dioxide technology.
Summary of the invention
The technical issues that need to address of the present invention are, a kind of method for extracting coarse oil from coix seed with hypercritical carbon dioxide and optimized parameters are provided, and the coarse oil from coix seed that is extracted have with Chinese patent literature CN1029662C in oily same physicochemical property.
Method for extracting coarse oil from coix seed of the present invention comprises;
1) drying: the Semen Coicis moisture drying is arrived≤10%;
2) pulverize: lower the temperature naturally, to be detected qualified after, be crushed to 10～60 orders again;
3) supercritical carbon dioxide extraction: 30～60 ℃ of extraction kettles, pressure 19～24MPa; 30～60 ℃ of separator column temperature, pressure 6～15Mpa; 30～60 ℃ of extraction-container temperature, pressure 2～6Mpa; Flow 10～5000L/h; Extraction time 1～4h.
Production method of the present invention has characteristics such as cost is low, and production operation is safer; Its process parameter optimizing, yield is higher, and the physical and chemical indexs such as acidity of gained oil meet the requirements, and the injection Semen Coicis oil after making with extra care meets the national drug quality standard.
Embodiment
Below by embodiment, technical scheme originally is described in further detail.
One, 24L scale supercritical extraction
1, significant parameter: charging capacity is about 13.0Kg; Semen Coicis raw material pulverizing granularity is 20 orders, and raw material moisture is 9.58%; The extraction kettle temperature/pressure is 36～38 ℃/21.0～22.5MPa; The separator column temperature/pressure is 47～55 ℃/8.5～13.0Mpa; The extraction-container temperature/pressure is 26～50 ℃/4.5～6.5MPa; CO
2Instantaneous delivery is 65～110L/h; The extraction time is 3h.
24L scale supercritical extraction result:
| Sequence number | Lot number | Yield (%) | Acid number | Peroxide value |
| ????1 | ????01051501 | ????1.80 | ????10.7 | ????3.1 |
| ????2 | ????01051502 | ????3.67 | ????21.9 | ????4.8 |
| ????3 | ????01051503 | ????3.60 | ????23.9 | ????5.3 |
| ????4 | ????01051602 | ????3.32 | ????22.6 | ????3.3 |
| ????5 | ????01051701 | ????2.33 | ????11.2 | ????3.2 |
| ????6 | ????01051702 | ????3.41 | ????12.6 | ????5.1 |
| ????7 | ????01051703 | ????4.49 | ????17.30 | |
| ????8 | ????01051704 | ????4.56 | ????22.12 | |
| ????9 | ????01051705 | ????3.98 | ????19.05 | |
| ????10 | ????01051706 | ????4.44 | ????16.98 | |
| ????11 | ????01052101 | ????3.00 | ????30.50 | |
| ????12 | ????01052102 | ????3.60 | ????11.52 | |
| ????13 | ????01052203 | ????4.60 | ????8.58 | |
| ????14 | ????01052204 | ????3.80 | ????7.80 | |
| ????15 | ????01052301 | ????3.30 | ????7.63 | |
| ????16 | ????01052302 | ????4.10 | ????12.22 | |
| ????17 | ????01052303 | ????4.00 | ????7.47 | |
| ????18 | ????01052304 | ????3.35 | ????11.67 |
2, the relation of parameter and acid number, yield
1) extraction kettle pressure influence result: because extraction is limit by institute batch, pressure influences acid number to be groped according to lab scale, not obvious.
2) separator column pressure influence result:
| Lot number | Separator column pressure (Mpa) | Yield (%) | Acid number |
| ??01051503 | ????8～9 | ????3.60 | ????23.9 |
| ??01051502 | ????9～10 | ????3.67 | ????21.9 |
| ??01052101 | ????10～11 | ????3.00 | ????30.50 |
| ??01051702 | ????11～12 | ????3.41 | ????19.40 |
From last table, along with the increase of separator column pressure, must take the lead in descending raises again, and it is wavy that acid number then is, should be when 9-10Mpa yield the highest relatively, and acid number is lower.
3) extraction-container pressure influence result:
| Lot number | Extraction-container pressure (Mpa) | Yield (%) | Acid number |
| ????01051602 | ????4～5 | ????3.32 | ????22.6 |
| ????01051502 | ????5～6 | ????3.67 | ????21.9 |
| ????01051702 | ????6～7 | ????3.41 | ????19.40 |
As can be seen from the above table, the pressure change of extraction-container is not very big to the influence of yield and acid number.
4) extraction kettle temperature.The temperature condition of extraction kettle is groped according to lab scale, shows that temperature effect is not obvious.
5) separator column temperature effect result:
| Lot number | The separator column temperature (℃) | Yield (%) | Acid number |
| ??01051705 | ????43～44 | ????3.98 | ????19.05 |
| ??01052101 | ????47～48 | ????3.00 | ????30.50 |
| ??01051703 | ????54～55 | ????4.49 | ????17.30 |
By last Biao Kede, the rising of separator column temperature all is beneficial to the raising of yield and the reduction of acid number.
6) extraction-container temperature effect result:
| Lot number | The extraction-container temperature (℃) | Yield (%) | Acid number |
| ????01051502 | ????27～28 | ????3.67 | ????21.9 |
| ????01051702 | ????28～30 | ????3.41 | ????19.40 |
| ????01052301 | ????40～42 | ????3.30 | ????7.63 |
| ????01052203 | ????43～44 | ????4.60 | ????8.58 |
| ????01052302 | ????44～45 | ????4.10 | ????12.22 |
| ????01052102 | ????46～48 | ????3.60 | ????11.52 |
| ????01052204 | ????48～49 | ????3.80 | ????7.80 |
From last table trend, the temperature of extraction-container raises again, yield is improved again, and acid number descends again.
7) flow effect result:
| Lot number | Flow | Yield (%) | Acid number |
| ??01051602 | ????70 | ????3.32 | ????22.6 |
| ??01052102 | ????80 | ????3.60 | ????11.52 |
| ??01051502 | ????90 | ????3.67 | ????21.9 |
| ??01051704 | ????100 | ????4.56 | ????22.12 |
Find out clearly that from last table along with the increase of flow, yield raises up steadily, and also slightly downtrending of acid number.
8) extraction time effects result: fuel-displaced very fast during beginning obviously, after 2 hours, tend towards stability
9) parameters optimization
| Extraction kettle | Separator column | Extraction-container | Flow (L/h) | The extraction time (h) | |||
| Temperature (℃) | Pressure (MPa) | Temperature (℃) | Pressure (MPa) | Temperature (℃) | Pressure (MPa) | ||
| 47～48 | ?21～22.5 | 54～55 | ???9～10 | ??48～49 | ???5～6 | ?100～120 | ?2～3 |
Two, 200L scale supercritical extraction
The extraction parameter: preceding 10 batches of charging capacitys are 130Kg, and back 2 batches of charging capacitys change 148Kg into; Semen Coicis raw material pulverizing granularity is 20 orders, and raw material moisture is 9.58%; The extraction kettle temperature/pressure is 36～38 ℃/21.0～22.5Mpa; The separator column temperature/pressure is 46～50 ℃/10.5～12.0Mpa; The extraction-container temperature/pressure is 28～30 ℃/5.0～6.5Mpa; CO
2Instantaneous delivery is 1000～1200L/h; The extraction time is 3h.
200L scale supercritical extraction result
| Sequence number | Lot number | Yield (%) | Acid number |
| ????1 | ????01051201 | ????3.77 | ????9.44 |
| ????2 | ????01051601 | ????2.00 | |
| ????3 | ????01052201 | ????2.23 | |
| ????4 | ????01052202 | ????5.50 | |
| ????5 | ????01052203 | ????4.97 |
| ????6 | ????01052301 | ????5.10 | ????10.40 |
| ????7 | ????01052302 | ????4.40 | ????7.68 |
| ????8 | ????01052303 | ????4.60 | |
| ????9 | ????01052304 | ????4.90 | |
| ????10 | ????01052401 | ????4.46 | ????17.80 |
| ????11 | ????01052402 | ????4.85 | ????15.30 |
| ????12 | ????01052403 | ????3.70 | ????8.56 |
Three, 600L scale supercritical extraction
1, significant parameter:
| Extraction kettle | Separator column | Extraction-container | Flow (L/h) | The extraction time (h) | |||
| Temperature (℃) | Pressure (MPa) | Temperature (℃) | Pressure (MPa) | Temperature (℃) | Pressure (MPa) | ||
| ??30～45 | ??19～22.5 | ??30～45 | ??8～10 | ?40～50 | ???4～6 | ??1000～ ??3000 | ??2～3 |
2, result of implementation
| Lot number | Charging capacity (Kg) | Get overcritical thick oil mass (Kg) | Oil yield (%) | Get finished product oil mass (Kg) after refining | Yield rate (%) |
| ?20020507 | ????800 | ????50.0 | ????6.25 | ????45.42 | ????5.68 |
| ?20020508 | ????800 | ????46.9 | ????5.86 | ????41.37 | ????5.17 |
| ?20020509 | ????800 | ????45.0 | ????5.62 | ????42.00 | ????5.25 |
The gained finished product all meets injection Semen Coicis oil national drug quality standard through check.
Claims (4)
1, a kind of extracting coarse oil from coix seed with hypercritical carbon dioxide is characterized in that:
1) drying: the Semen Coicis moisture drying is arrived≤10%;
2) pulverize: lower the temperature naturally, to be detected qualified after, be crushed to 10～60 orders again;
3) supercritical carbon dioxide extraction: 30～60 ℃ of extraction kettle temperature, pressure 19～24MPa; 30～60 ℃ of separator column temperature, pressure 6～15Mpa; 30～60 ℃ of extraction-container temperature, pressure 2～6Mpa; Flow 10～5000L/Hr; Extraction time 1～4h.
2, method for extracting coarse oil from coix seed according to claim 1 is characterized in that: 24L scale supercritical carbon dioxide extraction: 47～48 ℃ of extraction kettle temperature, pressure 21～22.5MPa; 54～55 ℃ of separator column temperature, pressure 9～10Mpa; 48～49 ℃ of extraction-container temperature, pressure 5～6Mpa; Flow 100～120L/h; Extraction time 2～3h.
3, method for extracting coarse oil from coix seed according to claim 1 is characterized in that: 200L scale supercritical carbon dioxide extraction: 36～38 ℃ of extraction kettle temperature, pressure 21～22.5MPa; 46～50 ℃ of separator column temperature, pressure 10.5～12.0Mpa; 28～30 ℃ of extraction-container temperature, pressure 5.0～6.5Mpa; Flow 1000～1200L/h; Extraction time 2～3h.
4, method for extracting coarse oil from coix seed according to claim 1 is characterized in that: 600L scale supercritical carbon dioxide extraction: 30～45 ℃ of extraction kettles, pressure 19～22.5MPa; 30～45 ℃ of separator column temperature, pressure 8～10Mpa; 40～50 ℃ of extraction-container temperature, pressure 4～6Mpa; Flow 1000～3000L/h; Extraction time 2～3h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02137312 CN1200995C (en) | 2002-09-28 | 2002-09-28 | Method for extracting coarse oil from coix seed with hypercritical carbon dioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02137312 CN1200995C (en) | 2002-09-28 | 2002-09-28 | Method for extracting coarse oil from coix seed with hypercritical carbon dioxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1485418A true CN1485418A (en) | 2004-03-31 |
| CN1200995C CN1200995C (en) | 2005-05-11 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02137312 Expired - Lifetime CN1200995C (en) | 2002-09-28 | 2002-09-28 | Method for extracting coarse oil from coix seed with hypercritical carbon dioxide |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101036761B (en) * | 2007-04-23 | 2010-05-19 | 肖志勇 | Process for preparing coix seed oil |
| CN101863764A (en) * | 2010-06-18 | 2010-10-20 | 福建仙芝楼生物科技有限公司 | Method for extracting and separating coixenolide and coix seed oil step-by-step by using supercritical CO2 |
| CN102177978A (en) * | 2011-04-14 | 2011-09-14 | 西南大学 | Coix seed bran and use thereof |
| CN102229856A (en) * | 2011-06-10 | 2011-11-02 | 四川省自然资源科学研究院 | Kiwi fruit seed oil and preparation method |
| CN102229855A (en) * | 2011-06-05 | 2011-11-02 | 江苏江大源生态生物科技有限公司 | Method for extracting coix seed oil by supercritical CO2 extraction and rectification |
| CN102618382A (en) * | 2012-03-21 | 2012-08-01 | 上海交通大学 | Method for extracting coix seed rice bran oil by utilizing supercritical CO2 technology |
| CN104560379A (en) * | 2014-11-26 | 2015-04-29 | 浙江康莱特药业有限公司 | Coix seed oil and extraction process thereof |
| CN104834777A (en) * | 2015-05-01 | 2015-08-12 | 长春工业大学 | CO2 supercritical extraction process set value parameter optimizing method |
| CN105254498A (en) * | 2014-07-18 | 2016-01-20 | 浙江康莱特集团有限公司 | 1,3-oleic acid-2-linoleic acid glyceride, preparation, preparation method and applications thereof |
| WO2016008442A1 (en) * | 2014-07-18 | 2016-01-21 | 浙江康莱特集团有限公司 | Coix seed oil comprising 11 triglycerides, formulation and application thereof |
| WO2016008439A1 (en) * | 2014-07-18 | 2016-01-21 | 浙江康莱特集团有限公司 | Coix seed oil comprising 8 triglycerides, formulation and application thereof |
| WO2016008440A1 (en) * | 2014-07-18 | 2016-01-21 | 浙江康莱特集团有限公司 | Coix seed oil comprising 13 glycerides, formulation and application thereof |
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2002
- 2002-09-28 CN CN 02137312 patent/CN1200995C/en not_active Expired - Lifetime
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| CN101863764A (en) * | 2010-06-18 | 2010-10-20 | 福建仙芝楼生物科技有限公司 | Method for extracting and separating coixenolide and coix seed oil step-by-step by using supercritical CO2 |
| CN101863764B (en) * | 2010-06-18 | 2013-03-27 | 福建仙芝楼生物科技有限公司 | Method for extracting and separating coixenolide and coix seed oil step-by-step by using supercritical CO2 |
| CN102177978A (en) * | 2011-04-14 | 2011-09-14 | 西南大学 | Coix seed bran and use thereof |
| CN102177978B (en) * | 2011-04-14 | 2013-01-30 | 西南大学 | Coix seed bran and use thereof |
| CN102229855A (en) * | 2011-06-05 | 2011-11-02 | 江苏江大源生态生物科技有限公司 | Method for extracting coix seed oil by supercritical CO2 extraction and rectification |
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| CN106470680B (en) * | 2014-07-18 | 2017-09-12 | 浙江康莱特集团有限公司 | Coix seed oil, preparation and its application containing 16 kinds of glyceride |
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| EA033688B1 (en) * | 2014-07-18 | 2019-11-15 | Zhejiang Kanglaite Group Co Ltd | Coix seed oil containing 16 glycerides, and pharmaceutical preparation and use thereof |
| AU2015291531B2 (en) * | 2014-07-18 | 2018-03-29 | Zhejiang Kanglaite Group Co., Ltd. | Coix seed oil containing 11 triglycerides, and pharmaceutical preparation and use thereof |
| AU2015291529B2 (en) * | 2014-07-18 | 2018-04-19 | Zhejiang Kanglaite Group Co., Ltd. | Coix seed oil containing 13 glycerides, and pharmaceutical preparation and use thereof |
| CN107320469B (en) * | 2014-07-18 | 2018-12-18 | 浙江康莱特药业有限公司 | A kind of coix seed oil containing 16 kinds of glyceride, preparation and its application |
| EA033647B1 (en) * | 2014-07-18 | 2019-11-13 | Zhejiang Kanglaite Group Co Ltd | Coix seed oil containing 11 triglycerides, and pharmaceutical preparation and use thereof |
| US10314878B2 (en) | 2014-07-18 | 2019-06-11 | Zhejiang Kanglaite Group Co., Ltd. | Coix seed oil containing 11 triglycerides, and pharmaceutical preparation and use thereof |
| CN104560379A (en) * | 2014-11-26 | 2015-04-29 | 浙江康莱特药业有限公司 | Coix seed oil and extraction process thereof |
| CN104834777B (en) * | 2015-05-01 | 2018-02-23 | 长春工业大学 | Carbon dioxide supercritical extraction process settings parameter optimization method |
| CN104834777A (en) * | 2015-05-01 | 2015-08-12 | 长春工业大学 | CO2 supercritical extraction process set value parameter optimizing method |
| CN109576051A (en) * | 2018-12-06 | 2019-04-05 | 江西省药明扬海医药科技有限公司 | The extracting method of coix seed oil in a kind of oxidation waste slag of aluminum |
| CN110029015A (en) * | 2019-04-12 | 2019-07-19 | 福州帅宝生物科技有限公司 | A kind of extracting method of coix seed oil |
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| CN1200995C (en) | 2005-05-11 |
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