CN104194925A - Method for extracting abelmoschus manihot L.Medic. oil with supercritical CO2 - Google Patents

Method for extracting abelmoschus manihot L.Medic. oil with supercritical CO2 Download PDF

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Publication number
CN104194925A
CN104194925A CN201410372245.7A CN201410372245A CN104194925A CN 104194925 A CN104194925 A CN 104194925A CN 201410372245 A CN201410372245 A CN 201410372245A CN 104194925 A CN104194925 A CN 104194925A
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China
Prior art keywords
oil
medic
sunset abelmoschus
abelmoschus root
abelmoschus manihot
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CN201410372245.7A
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Chinese (zh)
Inventor
李少杰
端木国民
马现京
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PUYANG TIANXINGJIAN BIOTECHNOLOGY Co Ltd
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PUYANG TIANXINGJIAN BIOTECHNOLOGY Co Ltd
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Priority to CN201410372245.7A priority Critical patent/CN104194925A/en
Publication of CN104194925A publication Critical patent/CN104194925A/en
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Abstract

The invention belongs to the technical field of edible oil preparation and in particular relates to a method for extracting abelmoschus manihot L.Medic. oil with supercritical CO2. The method comprises the processes of preheating, extraction, primary separation, secondary separation and molecular distillation. The prepared abelmoschus manihot L.Medic. oil has bright orange-yellow color and has the special smell of abelmoschus manihot L.Medic. The total unsaturated fatty acids in the abelmoschus manihot L.Medic. oil are not less than 87%, the content of linoleic acid in the abelmoschus manihot L.Medic. oil is not less than 28.2%, the content of palmitic acid in the abelmoschus manihot L.Medic. oil is not less than 26%, and the aroma of the abelmoschus manihot L.Medic. oil is four times that of sesame oil, so that the abelmoschus manihot L.Medic. oil is vegetable oil rich in nutrients. The method provided by the invention has the beneficial effects that in the extraction process, the technology is mature and is easy to operate; the method has the advantages of high yield, high purity, good quality of prepared abelmoschus manihot L.Medic. oil and the like; through further physiochemical index detection of the prepared abelmoschus manihot L.Medic. oil, the unsaturated fatty acid ingredients in the abelmoschus manihot L.Medic. oil are better retained, so that the abelmoschus manihot L.Medic. oil has better economic values.

Description

A kind of supercritical CO of Sunset Abelmoschus Root oil 2extracting process
Technical field
The invention belongs to edible oil preparing technical field, be specifically related to a kind of supercritical CO of Sunset Abelmoschus Root oil 2extracting process.
Background technology
Sunset Abelmoschus Root ( abelmoschus manihot L.Medic.), have another name called gumbo, leopard eyes flower, despot's day umbrella, cotton wormwood artemisia, be the annual or perennial sturdy upright herbaceous plant of Malvaceae Abelmoschus.Being used as medicine with root, leaf, flower and seed, can be used for clearing heat and detoxicatingly, moisturize laxation, is a kind of Chinese medicinal materials that the field of Chinese medicines is comparatively conventional.Now there are some researches show, high with fat fat content in yellow hollyhock seed, oil quality is good, has good economic worth and edible, pharmaceutical use, but in prior art, there is not yet the comparatively suitable method of squeezing Sunset Abelmoschus Root oil.
About grease what produce general employing is mainly milling process and solvent extraction method.Generally speaking, it is interior compared with the nutrition of horn of plenty that milling process has retained oil plant, and pollute without chemical solvents, thereby be considered to the safest preparation method, but because milling process exists the defect that oil yield is low, thereby in actual production, be subject to restriction largely.Solvent extraction method is generally to adopt solvent oil (No. six petroleum naphthas) glyceride stock to be carried out after abundant immersion to high temperature extraction, then pass through " six de-" technique (degreasing, come unstuck, dehydration, decolouring, deodorization, depickling) and process, its maximum feature is that oil yield is high, production cost is low.But solvent extraction method exists the defect of dissolvent residual, and production technique is comparatively complicated, thereby is subject to restriction to a certain extent in reality is promoted.
In grease extractive technique, also has a kind of noteworthy aqueous enzymatic method.It is in Mechanical Crushing ground foundation that aqueous enzymatic method is carried oil tech, adopt enzyme (comprising cellulase, polygalacturonase, amylase, proteolytic enzyme etc.) to act on oil plant, make grease be easy to discharge from oil plant solid, then utilize non-oil component (albumen and carbohydrate) to oil and the avidity difference of water, utilize profit proportion difference simultaneously and oil is separated with non-oil component.Compared with traditional technology, it has significant advantage at aspects such as energy consumption, environment and safety and sanitation, is considered to the oil tech of carrying of a kind of " green, environmental protection ".But because this technique is still in the experiment stage of fumbling, the actual utilization and extention of distance still has one section of larger distance.
Supercritical CO in recent years 2abstraction technique has been because its extraction efficiency is high, obtained promoting comparatively widely without advantages such as organic contamination, security height, but in prior art, there is not yet about supercritical CO 2be used for the correlative study report of the comparatively detailed industrial applications that extracts Sunset Abelmoschus Root oil.
Summary of the invention
The object of the invention is to provide a kind of supercritical CO of the Sunset Abelmoschus Root oil that is suitable for industrial applications 2extracting process.
The technical solution used in the present invention is as follows.
A kind of supercritical CO of Sunset Abelmoschus Root oil 2extracting process, comprises that preheating, extraction, the first separation, second separate, molecular distillation process, specifically comprises the following steps:
(1) choose the clean yellow hollyhock seed without the impurity such as limb, stone, pulverization process, preferably 40 ~ 60 orders are pulverized;
(2) yellow hollyhock seed after pulverizing in step (1) is placed in to extraction kettle and carries out supercritical CO 2extraction, concrete extraction process is:
The first, first extraction kettle is preheated to 40 ~ 45 DEG C, then material in step (1) is placed in to extraction kettle, regulate and enter extraction kettle mesohigh CO 2hydrodynamicpressure to 26 ~ 30MPa, stablizes 2 hours;
The second, high pressure CO 2fluid carries dissolved substance in extraction kettle and enters the first separating still through the first preheater, and the temperature of the first preheater is 50 DEG C, regulates first separating still internal pressure to 8.5 ~ 9MPa, and part Sunset Abelmoschus Root oil is separated out;
The 3rd, after the first separating still carry extract high pressure CO 2fluid is depressurized to 6MPa, then through the second preheater, enters the second separating still, and the temperature of the second preheater is 35 ~ 40 DEG C, again isolates Sunset Abelmoschus Root oil, through dividing the CO after isolating 2gas returns to refrigeration system and again participates in extraction cycle;
The 4th, carry out molecular distillation through the Sunset Abelmoschus Root oil of twice separation and obtain Sunset Abelmoschus Root oil finished product.
Described molecular distillation is divided into 5 grades:
First step molecular distillation adopts thin-film evaporator, with except the small molecular weight material such as anhydrating;
Second stage molecular distillation heating thermal oil to 180 DEG C by light, heavy constituent receiving tank, removes residual glycerine, free fatty acids under 3Pa state after secondary molecular distillation;
Third stage molecular distillation heating thermal oil to 200 DEG C by weight component receiving tank, removes C under 4Pa state after three grades of molecular distillations 12-C 14small molecules lipid acid;
Fourth stage molecular distillation heating thermal oil to 200 DEG C by weight component receiving tank, extracts most of linolenic acid (C under 5Pa state after level Four molecular distillation 18-C 20);
Level V molecular distillation heating thermal oil to 200 DEG C by weight component receiving tank, extracts the linolenic acid in raffinate under 5Pa state after Pyatyi molecular distillation, and raffinate is C 22-C 24the macromolecular substance that color is darker;
After 5 grades of molecular distillations, Sunset Abelmoschus Root oil is final Sunset Abelmoschus Root oil finished product.
The described supercritical CO that utilizes 2sunset Abelmoschus Root oil prepared by extracting process, it is bright-coloured orange-yellow that color is, there is the special odor of Sunset Abelmoschus Root, in Sunset Abelmoschus Root oil, unsaturated fatty acids total amount is not less than 87%, linoleic acid content is not less than 28.2%, and palmitic acid content is not less than 26%, and its fragrance perfume degree is 4 times of sesame oil, being rich in the mineral substance such as vitamin b6 usp, mineral substance, vitamin-E, Yelkin TTS, calcium, phosphorus, iron, potassium, magnesium, is a kind of nutritious vegetables oil.
The supercritical CO of Sunset Abelmoschus Root oil provided by the present invention 2extracting process, in extraction process, technical maturity, easy handling, non-pollutant discharge process in whole production process, environmental protection has the advantages such as productive rate is high, purity is high, prepared Sunset Abelmoschus Root oil quality is good simultaneously.Further physical and chemical index by the Sunset Abelmoschus Root oil to preparation detects, and the unsaturated fatty acids composition in Sunset Abelmoschus Root oil has obtained good reservation, thereby has good economic worth.
Brief description of the drawings
Fig. 1 is the supercritical CO of Sunset Abelmoschus Root oil provided by the present invention 2extraction process flow figure;
Fig. 2 is through supercritical CO 2the further molecular distillation process flow sheet of the Sunset Abelmoschus Root oil after extraction.
Embodiment
Below in conjunction with embodiment the present invention will be further explained explanation.
embodiment 1
As shown in Figure 1 and Figure 2, the supercritical CO of Sunset Abelmoschus Root oil provided by the present invention 2extracting process, comprises that preheating, extraction, the first separation, second separate, molecular distillation process, specifically comprises the following steps:
(1) choose the clean yellow hollyhock seed without the impurity such as limb, stone, pulverization process, preferably 40 ~ 60 orders are pulverized;
(2) yellow hollyhock seed after pulverizing in step (1) is placed in to extraction kettle and carries out supercritical CO 2extraction, concrete extraction process is:
The first, first extraction kettle is preheated to 40 ~ 45 DEG C, then material in step (1) is placed in to extraction kettle, regulate and enter extraction kettle mesohigh CO 2hydrodynamicpressure to 26 ~ 30MPa, stablizes 2 hours;
The second, high pressure CO 2fluid carries dissolved substance in extraction kettle and enters the first separating still through the first preheater, and the temperature of the first preheater is 50 DEG C, regulates first separating still internal pressure to 8.5 ~ 9MPa, and part Sunset Abelmoschus Root oil is separated out;
The 3rd, after the first separating still carry extract high pressure CO 2fluid is depressurized to 6MPa, then through the second preheater, enters the second separating still, and the temperature of the second preheater is 35 ~ 40 DEG C, again isolates Sunset Abelmoschus Root oil, through dividing the CO after isolating 2gas returns to refrigeration system and again participates in extraction cycle;
The 4th, carry out molecular distillation through the Sunset Abelmoschus Root oil of twice separation and obtain Sunset Abelmoschus Root oil finished product.
Described molecular distillation is divided into 5 grades:
First step molecular distillation adopts thin-film evaporator, with except the small molecular weight material such as anhydrating;
Second stage molecular distillation heating thermal oil to 180 DEG C by light, heavy constituent receiving tank, removes residual glycerine, free fatty acids under 3Pa state after secondary molecular distillation;
Third stage molecular distillation heating thermal oil to 200 DEG C by weight component receiving tank, removes C under 4Pa state after three grades of molecular distillations 12-C 14small molecules lipid acid;
Fourth stage molecular distillation heating thermal oil to 200 DEG C by weight component receiving tank, extracts most of linolenic acid (C under 5Pa state after level Four molecular distillation 18-C 20);
Level V molecular distillation heating thermal oil to 200 DEG C by weight component receiving tank, extracts the linolenic acid in raffinate under 5Pa state after Pyatyi molecular distillation, and raffinate is C 22-C 24the macromolecular substance that color is darker;
After 5 grades of molecular distillations, Sunset Abelmoschus Root oil is final Sunset Abelmoschus Root oil finished product.
Concrete the present embodiment, taking the overcritical Chinese style equipment of 5L as example, has carried out preliminary productive experiment, to drop into Sunset Abelmoschus Root 2Kg raw material as example, and after removing impurity, surplus stock 1.85Kg, 60 order pulverization process.
In extraction process, preheating temperature to 40 DEG C in extraction kettle, extraction kettle inner high voltage CO 2hydrodynamicpressure is 26MPa, stablizes 2 hours; In the first separating still, carry the high pressure CO of extract 2hydrodynamicpressure is 9MPa, and the first preheater temperature is 50 DEG C; In the second separating still, carry the high pressure CO of extract 2hydrodynamicpressure is 6MPa, and the second preheater temperature is 35 DEG C.
Supercritical CO 2after extraction, further after 5 grades of molecular distillations, obtain Sunset Abelmoschus Root oil finished product.
The final Sunset Abelmoschus Root oil finished product 0.28Kg that obtains in the present embodiment, percentage extraction is 15.5%, the Sunset Abelmoschus Root oil extracting, it is bright-coloured orange-yellow that color is, and has the special odor of Sunset Abelmoschus Root, and in Sunset Abelmoschus Root oil, unsaturated fatty acids total amount can reach 88%, linoleic acid content 28.6%, palmitic acid content 29%.
embodiment 2
The present embodiment is produced the step of Sunset Abelmoschus Root oil with embodiment 1, and only adjusting clean Sunset Abelmoschus Root oil raw material is 1.85Kg, 40 order pulverization process.
In extraction process, preheating temperature to 45 DEG C in extraction kettle, extraction kettle inner high voltage CO 2hydrodynamicpressure is 30MPa, stablizes 2 hours; In the first separating still, carry the high pressure CO of extract 2hydrodynamicpressure is 8.5MPa, and the first preheater temperature is 50 DEG C; In the second separating still, carry the high pressure CO of extract 2hydrodynamicpressure is 6MPa, and the second preheater temperature is 40 DEG C.
Supercritical CO 2after extraction, further after 5 grades of molecular distillations, obtain Sunset Abelmoschus Root oil finished product.
The present embodiment finally obtains Sunset Abelmoschus Root oil finished product 0.3Kg, and percentage extraction is 16.2%, the Sunset Abelmoschus Root oil extracting, it is bright-coloured orange-yellow that color is, and has the special odor of Sunset Abelmoschus Root, and in Sunset Abelmoschus Root oil, unsaturated fatty acids total amount can reach 87%, linoleic acid content 30.6%, palmitic acid content 26%.
embodiment 3
The present embodiment is produced the step of Sunset Abelmoschus Root oil with embodiment 1, and only adjusting clean Sunset Abelmoschus Root oil raw material is 1.85Kg, 60 order pulverization process.
In extraction process, preheating temperature to 42 DEG C in extraction kettle, extraction kettle inner high voltage CO 2hydrodynamicpressure is 28MPa, stablizes 2 hours; In the first separating still, carry the high pressure CO of extract 2hydrodynamicpressure is 9MPa, and the first preheater temperature is 50 DEG C; In the second separating still, carry the high pressure CO of extract 2hydrodynamicpressure is 6MPa, and the second preheater temperature is 40 DEG C.
Supercritical CO 2after extraction, further after 5 grades of molecular distillations, obtain Sunset Abelmoschus Root oil finished product.
The present embodiment finally obtains Sunset Abelmoschus Root oil finished product 0.26Kg, and percentage extraction is 14%, the Sunset Abelmoschus Root oil extracting, it is bright-coloured orange-yellow that color is, and has the special odor of Sunset Abelmoschus Root, and in Sunset Abelmoschus Root oil, unsaturated fatty acids total amount can reach 89%, linoleic acid content 28.2%, palmitic acid content 28%.
The prepared Sunset Abelmoschus Root oil of above-described embodiment is carried out to fragrant degree Comprehensive Assessment, its fragrance perfume degree is 4 times of sesame oil, further detect and prove, the mineral substance such as rich in vitamin E, Yelkin TTS, calcium, phosphorus, iron, potassium, magnesium in prepared Sunset Abelmoschus Root oil finished product, because of but a kind of nutritious vegetables oil.

Claims (3)

1. the supercritical CO of a Sunset Abelmoschus Root oil 2extracting process, is characterized in that, the method comprises that preheating, extraction, the first separation, second separate, molecular distillation process, and concrete extraction process is:
(1) choose clean yellow hollyhock seed, pulverization process;
(2) yellow hollyhock seed after pulverizing in step (1) is placed in to extraction kettle and carries out supercritical CO 2extraction, process is as follows:
The first, first extraction kettle is preheated to 40 ~ 45 DEG C, then material in step (1) is placed in to extraction kettle, regulate and enter extraction kettle mesohigh CO 2hydrodynamicpressure to 26 ~ 30MPa, stablizes 2 hours;
The second, high pressure CO 2fluid carries dissolved substance in extraction kettle and enters the first separating still through the first preheater, and the temperature of the first preheater is 50 DEG C, regulates first separating still internal pressure to 8.5 ~ 9MPa;
The 3rd, after the first separating still carry extract high pressure CO 2fluid is depressurized to 6MPa, then enters the second separating still through the second preheater, and the temperature of the second preheater is 35 ~ 40 DEG C;
The 4th, carry out molecular distillation through the Sunset Abelmoschus Root oil of twice separation and obtain Sunset Abelmoschus Root oil finished product.
2. the supercritical CO of Sunset Abelmoschus Root oil as claimed in claim 1 2extracting process, is characterized in that, described molecular distillation is divided into 5 grades:
First step molecular distillation adopts thin-film evaporator;
Second stage molecular distillation heating thermal oil to 180 DEG C passes through weight component receiving tank under 3Pa state;
Third stage molecular distillation heating thermal oil to 200 DEG C passes through weight component receiving tank under 4Pa state;
Fourth stage molecular distillation heating thermal oil to 200 DEG C passes through weight component receiving tank under 5Pa state;
Level V molecular distillation heating thermal oil to 200 DEG C passes through weight component receiving tank under 5Pa state.
3. utilize the supercritical CO of the arbitrary described Sunset Abelmoschus Root oil of claim 1-2 2the Sunset Abelmoschus Root oil that extracting process is prepared, it is characterized in that, Sunset Abelmoschus Root oil color is bright-coloured orange-yellow, there is the special odor of Sunset Abelmoschus Root, in Sunset Abelmoschus Root oil, unsaturated fatty acids total amount is not less than 87%, linoleic acid content is not less than 28.2%, and palmitic acid content is not less than 26%, and fragrance perfume degree is 4 times of sesame oil.
CN201410372245.7A 2014-07-31 2014-07-31 Method for extracting abelmoschus manihot L.Medic. oil with supercritical CO2 Pending CN104194925A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106074693A (en) * 2016-07-29 2016-11-09 许备占 Wild Hibisci Mutabilis mouth sprays

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Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1397632A (en) * 2001-07-19 2003-02-19 刘玉 Process for extracting from flax seeds by supercritical CO2
CN1490066A (en) * 2003-08-27 2004-04-21 李绍光 Method for extracting effective components from natural materials
CN101317611A (en) * 2007-11-23 2008-12-10 尹英遂 Multi-stage molecular distillation continuous depickling technique for oil and fat with high acidity number

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Publication number Priority date Publication date Assignee Title
CN106074693A (en) * 2016-07-29 2016-11-09 许备占 Wild Hibisci Mutabilis mouth sprays

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