CN100566581C - A kind of method of samara efficiently being developed extraction - Google Patents
A kind of method of samara efficiently being developed extraction Download PDFInfo
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- CN100566581C CN100566581C CNB2007100620199A CN200710062019A CN100566581C CN 100566581 C CN100566581 C CN 100566581C CN B2007100620199 A CNB2007100620199 A CN B2007100620199A CN 200710062019 A CN200710062019 A CN 200710062019A CN 100566581 C CN100566581 C CN 100566581C
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Abstract
The present invention relates to the extracting method of a vegetable oil and high concentration VE, be specially and a kind of samara efficiently developed the method for extraction, abandon the full-scale development utilization that causes the wasting of resources and can not realize samara for solution utilizes the oil cake after will squeezing in traditional cold pressing method; And utilize the supercritical carbon dioxide extracting method to have that cost is higher, oil extracting rate is lower and fail to isolate defectives such as VE, the present invention combines the supercritical carbon dioxide extraction process of cold pressing technology with the advanced person, at first extract the samara oil of 6-8% through cold pressing technology, then remaining oil cake is extracted the samara oil of 20-25% through the supercritical carbon dioxide extraction process, isolate vitamin E and unsaponifiable matter simultaneously from samara oil, wherein the concentration of vitamin E is greater than 12%.The present invention comprehensively develops samara under the prerequisite that guarantees product efficacy and composition, realize the product utilization maximization, and production cost is lower, easy and simple to handle, has certain popularization value.
Description
Technical field
The present invention relates to the extracting method of a vegetable oil and high concentration VE, be specially and a kind ofly utilize traditional cold pressing method and CO 2 supercritical abstracting method to combine samara efficiently to be developed the method for extraction.
Background technology
Elaeagnus mollis is the woody oleiferous plants plant of the distinctive national second class protection of China, samara is a kind of nut, shell is hard, and to become maturation appearance at it be velvet-like very thin undercoat, samara kind benevolence oil content reaches more than 45%, and samara oil contains the unrighted acid more than 95%, and oleic acid and linoleic acid content are very abundant in the samara oil that correct method extracts, reach more than 88%, the abundant grease of oleic acid and linoleic acid content hardens to prevention of arterial and has important function to resisting free-radical oxidation; Samara oil also contains the alpha-linolenic acid of 4-6% simultaneously, and alpha-linolenic acid has reducing blood lipid, norcholesterol and promotion fat metabolism, and liver cell regeneration promotes effects such as brain nervous cell growth; Also contain abundant vitamin E in the samara oil, be the hat of various oil plants, than 10 times of wheat embryo innages, vitamin E has good anti-oxidant and physiological regulatory action, thereby to anti-aging in advance, cardiovascular and cerebrovascular disease, cancer and the nervous system disease etc. all has good effect.
Existing extracting method to samara oil mainly is physical low-temperature milling process and CO
2Overcritical extraction method, wherein the physical low-temperature milling process is simple to operate, but its oil extracting rate is lower, it is higher to extract temperature, can make that effective active composition such as leukotrienes is subjected to heavy damage in the samara oil, and with remaining and still contain the oil cake that enriches grease and vitamin E and abandon, cause the waste of resource, failed to realize the maximum using of product.
Continuous development along with art technology, people begin to utilize the supercritical carbon dioxide extracting method to extract samara oil from samara, the defective of its existence is: 1, just merely utilize the supercritical carbon dioxide extracting method to extract samara oil, way is to extract fully directly putting into extraction equipment after samara or the fragmentation of samara benevolence, oil extracting rate is lower, cost is higher, serious waste of resources, and can not realize the full-scale development utilization of samara; 2, extraction temperature is higher, pressure is lower, and 3, lower as the carbon dioxide purity of extractant, be generally 95%, be not easy liquefaction, thereby be difficult for reaching critical condition.
Summary of the invention
The present invention utilizes traditional cold pressing method samara to be developed oil cake after will squeezing in the process of extraction to abandon and cause the wasting of resources and can not realize the full-scale development utilization of samara in order to solve; And utilize the supercritical carbon dioxide extracting method to have that cost is higher, oil extracting rate is lower and fail to isolate defectives such as VE, a kind of method of samara efficiently being developed extraction is provided, this method comprehensively develops samara, realizes the product utilization maximization.
The present invention adopts following technical scheme to realize: a kind of samara is efficiently developed the method for extraction, may further comprise the steps: (1) with the samara of maturation select seed, clear up, roll embryo, the low-temperature cold pressing operation obtains samara crude oil and oil cake; Innovative point of the present invention is that the oil cake that will obtain adopts supercritical carbon dioxide abstraction process extracting grease wherein, concrete steps are as follows: pack remaining oil cake in the extractor (2), with the carbon dioxide is extractant, under supercriticality, extract, extracting pressure is controlled at 35-45Mpa, extraction temperature is controlled at 35-45 ℃, and the carbon dioxide that contains grease flows out from the extractor top; (3) after the extraction, be decompressed to 100-150Kpa, temperature is reduced to 20-30 ℃, and carbon dioxide is thoroughly separated with samara oil; (4) collecting the samara oil that extracts gained, drop into extractor once more, is extractant with the carbon dioxide, under supercriticality, extract, extracting pressure is controlled at 15-30Mpa, and extraction temperature is controlled at 40-60 ℃, and effective ingredient vitamin E in the samara oil and unsaponifiable matter are carried out further extracting and enriching; (5) after the extraction, be decompressed to 100-150Kpa, temperature is reduced to 20-30 ℃, and carbon dioxide and samara oil and vitamin E, unsaponifiable matter are thoroughly separated.
The above-mentioned samara crude oil that obtains is filtered at normal temperatures, obtain samara oil, then samara oil is carried out multiple filter at low temperature in 9-10 ℃ low temperature environment.
Above-mentioned samara oil behind cold pressing operation and filter at low temperature carries out adsorption bleaching craft again, concrete steps are as follows: be 90-96KPa with samara oil in vacuum earlier, temperature is under 55-65 ℃ the condition, be to stir dehydration in the mixer of 50-60r/min with the adjustment rotating speed, to the dehydration pot till the no water smoke; Adding then by weight of oil conversion is filler-atlapulgite of 2%, again the mixer rotating speed being adjusted into 50-60r/min stirs fast, decolouring 0.5h, samara oil after the decolouring is 90-100kPa in vacuum, temperature is to carry out steam distillation 5h under the 90-100 ℃ of condition, be cooled to vacuum breaker below 70 ℃ then, get finished product samara oil after filtration.The finished product samara oil colours pool, the quality that obtain through adsorption bleaching craft of the present invention all reach desirable index.
Carbon dioxide abstraction agent after separating in the above-mentioned supercritical carbon dioxide abstraction process recycles after heating, pressurizeing, and reduces production costs.
The purity of described carbon dioxide abstraction agent makes its easier liquefaction, to reach critical condition greater than 99%.
Compared with prior art, the present invention combines the supercritical carbon dioxide extraction process of traditional cold pressing technology with the advanced person, at first extract the samara oil of 6-8% through cold pressing technology, then remaining oil cake is extracted the samara oil of 20-25% through the supercritical carbon dioxide extraction process, isolate vitamin E and unsaponifiable matter simultaneously from samara oil, wherein the concentration of vitamin E is greater than 12%.Utilize technology of the present invention, under the prerequisite that guarantees product efficacy and composition, samara is comprehensively developed, realize the product utilization maximization, and production cost is lower, easy and simple to handle, has certain popularization value.
The specific embodiment
Embodiment 1:
A kind of samara is efficiently developed the method for extraction, may further comprise the steps: (1) with the samara of maturation select seed, clear up, roll embryo, the low-temperature cold pressing operation obtains 6% samara crude oil and oil cake; (2) at normal temperatures the samara crude oil that obtains is filtered to obtain samara oil, can adopt the filter of two or more different filter opening specifications that above-mentioned samara crude oil is carried out multi-filtering and obtain samara oil; (3) samara oil is carried out multiple filter at low temperature in 9 ℃ low temperature environment; Above-mentioned samara oil behind cold pressing operation and filter at low temperature carries out adsorption bleaching craft again, concrete steps are as follows: be 90KPa with samara oil in vacuum earlier, temperature is under 55 ℃ the condition, with the adjustment rotating speed is to stir dehydration in the mixer of 50r/min, to the dehydration pot till the no water smoke; Adding then by weight of oil conversion is filler-atlapulgite of 2%, again the mixer rotating speed being adjusted into 50r/min stirs fast, decolouring 0.5h, samara oil after the decolouring is 90kPa in vacuum, temperature is to carry out steam distillation 5h under 90 ℃ of conditions, be cooled to vacuum breaker below 70 ℃ then, get finished product samara oil after filtration.The oil cake that obtains is adopted supercritical carbon dioxide abstraction process extracting grease wherein, concrete steps are as follows: pack remaining oil cake in the extractor (4), with the carbon dioxide is extractant, under supercriticality, extract, extracting pressure is controlled at 35Mpa, extraction temperature is controlled at 35 ℃, and the carbon dioxide that contains grease flows out from the extractor top; (5) after the extraction, be decompressed to 100Kpa, temperature is reduced to 20 ℃, and carbon dioxide is thoroughly separated with samara oil, and the carbon dioxide abstraction agent after the separation recycles after heating, pressurizeing; (6) collecting the samara oil that extracts gained, drop into extractor once more, is extractant with the carbon dioxide, under supercriticality, extract, extracting pressure is controlled at 15Mpa, and extraction temperature is controlled at 40 ℃, and effective ingredient vitamin E in the samara oil and unsaponifiable matter are carried out further extracting and enriching; (7) after the extraction, be decompressed to 100Kpa, temperature is reduced to 20 ℃, and carbon dioxide and samara oil and vitamin E, unsaponifiable matter are thoroughly separated, and the carbon dioxide abstraction agent after the separation recycles after heating, pressurizeing.
Embodiment 2:
A kind of samara is efficiently developed the method for extraction, may further comprise the steps: (1) with the samara of maturation select seed, clear up, roll embryo, the low-temperature cold pressing operation obtains 8% samara crude oil and oil cake; (2) at normal temperatures the samara crude oil that obtains is filtered to obtain samara oil, can adopt the filter of two or more different filter opening specifications that above-mentioned samara crude oil is carried out multi-filtering and obtain samara oil; (3) samara oil is carried out multiple filter at low temperature in 10 ℃ low temperature environment; Above-mentioned samara oil behind cold pressing operation and filter at low temperature carries out adsorption bleaching craft again, concrete steps are as follows: be 96KPa with samara oil in vacuum earlier, temperature is under 65 ℃ the condition, with the adjustment rotating speed is to stir dehydration in the mixer of 60r/min, to the dehydration pot till the no water smoke; Adding then by weight of oil conversion is filler-atlapulgite of 2%, again the mixer rotating speed being adjusted into 60r/min stirs fast, decolouring 0.5h, samara oil after the decolouring is 100kPa in vacuum, temperature is to carry out steam distillation 5h under 100 ℃ of conditions, be cooled to vacuum breaker below 70 ℃ then, get finished product samara oil after filtration.Innovative point of the present invention is that the oil cake that will obtain adopts supercritical carbon dioxide abstraction process extracting grease wherein, concrete steps are as follows: pack remaining oil cake in the extractor (4), with the carbon dioxide is extractant, under supercriticality, extract, extracting pressure is controlled at 45Mpa, extraction temperature is controlled at 45 ℃, and the carbon dioxide that contains grease flows out from the extractor top; (5) after the extraction, be decompressed to 150Kpa, temperature is reduced to 30 ℃, and carbon dioxide is thoroughly separated with samara oil, and the carbon dioxide abstraction agent after the separation recycles after heating, pressurizeing; (6) collecting the samara oil that extracts gained, drop into extractor once more, is extractant with the carbon dioxide, under supercriticality, extract, extracting pressure is controlled at 30Mpa, and extraction temperature is controlled at 60 ℃, and effective ingredient vitamin E in the samara oil and unsaponifiable matter are carried out further extracting and enriching; (7) after the extraction, be decompressed to 150Kpa, temperature is reduced to 30 ℃, and carbon dioxide and samara oil and vitamin E, unsaponifiable matter are thoroughly separated, and the carbon dioxide abstraction agent after the separation recycles after heating, pressurizeing.
Embodiment 3:
A kind of samara is efficiently developed the method for extraction, may further comprise the steps: (1) with the samara of maturation select seed, clear up, roll embryo, the low-temperature cold pressing operation obtains 7% samara crude oil and oil cake; (2) at normal temperatures the samara crude oil that obtains is filtered to obtain samara oil, can adopt the filter of two or more different filter opening specifications that above-mentioned samara crude oil is carried out multi-filtering and obtain samara oil; (3) samara oil is carried out multiple filter at low temperature in 9 ℃ low temperature environment; Above-mentioned samara oil behind cold pressing operation and filter at low temperature carries out adsorption bleaching craft again, concrete steps are as follows: be 95KPa with samara oil in vacuum earlier, temperature is under 60 ℃ the condition, with the adjustment rotating speed is to stir dehydration in the mixer of 55r/min, to the dehydration pot till the no water smoke; Adding then by weight of oil conversion is filler-atlapulgite of 2%, again the mixer rotating speed being adjusted into 55r/min stirs fast, decolouring 0.5h, samara oil after the decolouring is 95kPa in vacuum, temperature is to carry out steam distillation 5h under 95 ℃ of conditions, be cooled to vacuum breaker below 70 ℃ then, get finished product samara oil after filtration.Innovative point of the present invention is that the oil cake that will obtain adopts supercritical carbon dioxide abstraction process extracting grease wherein, concrete steps are as follows: pack remaining oil cake in the extractor (4), with the carbon dioxide is extractant, under supercriticality, extract, extracting pressure is controlled at 40Mpa, extraction temperature is controlled at 40 ℃, and the carbon dioxide that contains grease flows out from the extractor top; (5) after the extraction, be decompressed to 125Kpa, temperature is reduced to 25 ℃, and carbon dioxide is thoroughly separated with samara oil, and the carbon dioxide abstraction agent after the separation recycles after heating, pressurizeing; (6) collecting the samara oil that extracts gained, drop into extractor once more, is extractant with the carbon dioxide, under supercriticality, extract, extracting pressure is controlled at 25Mpa, and extraction temperature is controlled at 50 ℃, and effective ingredient vitamin E in the samara oil and unsaponifiable matter are carried out further extracting and enriching; (7) after the extraction, be decompressed to 125Kpa, temperature is reduced to 25 ℃, and carbon dioxide and samara oil and vitamin E, unsaponifiable matter are thoroughly separated, and the carbon dioxide abstraction agent after the separation recycles after heating, pressurizeing.
Embodiment 4:
A kind of samara is efficiently developed the method for extraction, may further comprise the steps: (1) with the samara of maturation select seed, clear up, roll embryo, the low-temperature cold pressing operation obtains 8% samara crude oil and oil cake; (2) at normal temperatures the samara crude oil that obtains is filtered to obtain samara oil, can adopt the filter of two or more different filter opening specifications that above-mentioned samara crude oil is carried out multi-filtering and obtain samara oil; (3) samara oil is carried out multiple filter at low temperature in 9-10 ℃ low temperature environment; Above-mentioned samara oil behind cold pressing operation and filter at low temperature carries out adsorption bleaching craft again, concrete steps are as follows: be 92KPa with samara oil in vacuum earlier, temperature is under 58 ℃ the condition, with the adjustment rotating speed is to stir dehydration in the mixer of 58r/min, to the dehydration pot till the no water smoke; Adding then by weight of oil conversion is filler-atlapulgite of 2%, again the mixer rotating speed being adjusted into 60r/min stirs fast, decolouring 0.5h, samara oil after the decolouring is 98kPa in vacuum, temperature is to carry out steam distillation 5h under 92 ℃ of conditions, be cooled to vacuum breaker below 70 ℃ then, get finished product samara oil after filtration.Innovative point of the present invention is that the oil cake that will obtain adopts supercritical carbon dioxide abstraction process extracting grease wherein, concrete steps are as follows: pack remaining oil cake in the extractor (4), with the carbon dioxide is extractant, under supercriticality, extract, extracting pressure is controlled at 36Mpa, extraction temperature is controlled at 38 ℃, and the carbon dioxide that contains grease flows out from the extractor top; (5) after the extraction, be decompressed to 140Kpa, temperature is reduced to 23 ℃, and carbon dioxide is thoroughly separated with samara oil, and the carbon dioxide abstraction agent after the separation recycles after heating, pressurizeing; (6) collecting the samara oil that extracts gained, drop into extractor once more, is extractant with the carbon dioxide, under supercriticality, extract, extracting pressure is controlled at 20Mpa, and extraction temperature is controlled at 45 ℃, and effective ingredient vitamin E in the samara oil and unsaponifiable matter are carried out further extracting and enriching; (7) after the extraction, be decompressed to 130Kpa, temperature is reduced to 22 ℃, and carbon dioxide and samara oil and vitamin E, unsaponifiable matter are thoroughly separated, and the carbon dioxide abstraction agent after the separation recycles after heating, pressurizeing.
Embodiment 5:
A kind of samara is efficiently developed the method for extraction, may further comprise the steps: (1) with the samara of maturation select seed, clear up, roll embryo, the low-temperature cold pressing operation obtains 6% samara crude oil and oil cake; (2) at normal temperatures the samara crude oil that obtains is filtered to obtain samara oil, can adopt the filter of two or more different filter opening specifications that above-mentioned samara crude oil is carried out multi-filtering and obtain samara oil; (3) samara oil is carried out multiple filter at low temperature in 9 ℃ low temperature environment; Above-mentioned samara oil behind cold pressing operation and filter at low temperature carries out adsorption bleaching craft again, concrete steps are as follows: be 94KPa with samara oil in vacuum earlier, temperature is under 62 ℃ the condition, with the adjustment rotating speed is to stir dehydration in the mixer of 53r/min, to the dehydration pot till the no water smoke; Adding then by weight of oil conversion is filler-atlapulgite of 2%, again the mixer rotating speed being adjusted into 60r/min stirs fast, decolouring 0.5h, samara oil after the decolouring is 92kPa in vacuum, temperature is to carry out steam distillation 5h under 97 ℃ of conditions, be cooled to vacuum breaker below 70 ℃ then, get finished product samara oil after filtration.Innovative point of the present invention is that the oil cake that will obtain adopts supercritical carbon dioxide abstraction process extracting grease wherein, concrete steps are as follows: pack remaining oil cake in the extractor (4), with the carbon dioxide is extractant, under supercriticality, extract, extracting pressure is controlled at 42Mpa, extraction temperature is controlled at 43 ℃, and the carbon dioxide that contains grease flows out from the extractor top; (5) after the extraction, be decompressed to 135Kpa, temperature is reduced to 28 ℃, and carbon dioxide is thoroughly separated with samara oil, and the carbon dioxide abstraction agent after the separation recycles after heating, pressurizeing; (6) collecting the samara oil that extracts gained, drop into extractor once more, is extractant with the carbon dioxide, under supercriticality, extract, extracting pressure is controlled at 27Mpa, and extraction temperature is controlled at 55 ℃, and effective ingredient vitamin E in the samara oil and unsaponifiable matter are carried out further extracting and enriching; (7) after the extraction, be decompressed to 142Kpa, temperature is reduced to 28 ℃, and carbon dioxide and samara oil and vitamin E, unsaponifiable matter are thoroughly separated, and the carbon dioxide abstraction agent after the separation recycles after heating, pressurizeing.
Claims (5)
1, a kind of samara is efficiently developed the method for extraction, may further comprise the steps:
(1) samara with maturation selects seed, clears up, rolls embryo, the low-temperature cold pressing operation obtains samara crude oil and oil cake;
It is characterized in that the oil cake that will obtain adopts supercritical carbon dioxide abstraction process extracting grease wherein, concrete steps are as follows:
(2) remaining oil cake being packed in the extractor, is extractant with the carbon dioxide, extracts under supercriticality, and extracting pressure is controlled at 35-45Mpa, and extraction temperature is controlled at 35-45 ℃, and the carbon dioxide that contains grease flows out from the extractor top;
(3) after the extraction, be decompressed to 100-150Kpa, temperature is reduced to 20-30 ℃, and carbon dioxide is thoroughly separated with samara oil;
(4) collecting the samara oil that extracts gained, drop into extractor once more, is extractant with the carbon dioxide, under supercriticality, extract, extracting pressure is controlled at 15-30Mpa, and extraction temperature is controlled at 40-60 ℃, and effective ingredient vitamin E in the samara oil and unsaponifiable matter are carried out further extracting and enriching;
(5) after the extraction, be decompressed to 100-150Kpa, temperature is reduced to 20-30 ℃, and carbon dioxide and samara oil and vitamin E, unsaponifiable matter are thoroughly separated.
2, according to claim 1ly a kind of samara is efficiently developed the method for extraction, it is characterized in that the above-mentioned samara crude oil that obtains is filtered at normal temperatures, obtain samara oil, then samara oil is carried out multiple filter at low temperature in 9-10 ℃ low temperature environment.
3, a kind of method of samara efficiently being developed extraction according to claim 2, it is characterized in that above-mentioned samara oil behind cold pressing operation and filter at low temperature carries out adsorption bleaching craft again, concrete steps are as follows: be 90-96KPa with samara oil in vacuum earlier, temperature is under 55-65 ℃ the condition, be to stir dehydration in the mixer of 50-60r/min with the adjustment rotating speed, to the dehydration pot till the no water smoke; Adding then by weight of oil conversion is filler-atlapulgite of 2%, again the mixer rotating speed being adjusted into 50-60r/min stirs fast, decolouring 0.5h, samara oil after the decolouring is 90-100kPa in vacuum, temperature is to carry out steam distillation 5h under the 90-100 ℃ of condition, be cooled to vacuum breaker below 70 ℃ then, get finished product samara oil after filtration.
4, describedly a kind of samara is efficiently developed the method for extraction according to claim 1 or 2 or 3, the carbon dioxide abstraction agent after it is characterized in that separating in the above-mentioned supercritical carbon dioxide abstraction process recycles after heating, pressurizeing.
5, according to claim 4ly a kind of samara is efficiently developed the method for extraction, the purity that it is characterized in that the carbon dioxide abstraction agent is greater than 99%.
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| CN103393104B (en) * | 2013-07-22 | 2014-07-23 | 山西琪尔康翅果生物制品有限公司 | Preparation method of samara oil pulverized tablet |
| CN103860613B (en) * | 2014-03-23 | 2016-04-13 | 山西隆水生物技术有限公司 | A kind of samara oil compound preparation with high-efficiency antioxidant function and preparation method thereof |
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Non-Patent Citations (4)
| Title |
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| 翅果油树的开发与应用. 陈晓蓉.山西食品工业，第2004年02期. 2004 |
| 翅果油树的开发与应用. 陈晓蓉.山西食品工业，第2004年02期. 2004 * |
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