CN108085124B - Method for re-extracting grease from degreased dried euphausia superba residues - Google Patents
Method for re-extracting grease from degreased dried euphausia superba residues Download PDFInfo
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- CN108085124B CN108085124B CN201711397201.XA CN201711397201A CN108085124B CN 108085124 B CN108085124 B CN 108085124B CN 201711397201 A CN201711397201 A CN 201711397201A CN 108085124 B CN108085124 B CN 108085124B
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/108—Production of fats or fatty oils from raw materials by extracting after-treatment, e.g. of miscellae
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- Oil, Petroleum & Natural Gas (AREA)
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Abstract
The invention belongs to the technical field of food, chemistry and medicine, and particularly relates to a method for re-extracting grease from degreased dried shrimp residues of Antarctic krill. Carrying out superfine grinding and screening on degreased dry shrimp residues of Antarctic krill, then homogenizing under high pressure, taking out feed liquid after homogenizing, filtering, carrying out rotary evaporation, and removing a solvent to obtain grease, wherein the grease yield is 6.8-7.1%.
Description
Technical Field
The invention belongs to the technical field of food, chemistry and medicine, and particularly relates to a method for re-extracting grease from degreased dried shrimp residues of Antarctic krill.
Background
Antarctic krill is a huge biomass living in Antarctic oceans (about 5-50 million tons, with differences in different estimation methods). The antarctic krill is rich in oil, and the oil content is different due to factors such as season, age, sex, abundance degree of food, environment and the like. The oil and fat is rich in unsaturated fatty acids (such as EPA, DHA, DPA, etc.), astaxanthin and its lipid, phospholipid, vitamin E, etc. At present, the antarctic krill oil is a high value-added product widely sold in the world, and the antarctic krill oil product is mainly produced in Canada, Japan, Norway and America. After 2009, several manufacturers in China began producing euphausia superba oil that meets international standards.
Chinese patent application (CN 107384585A) discloses a method for preparing antarctic krill oil in a grading manner, which comprises the steps of carrying out first-stage extraction on antarctic krill powder by using acetone to obtain first-stage extracted antarctic krill oil and first-stage extracted antarctic krill powder; performing secondary extraction on the first-stage extracted antarctic krill powder by adopting an alkane solvent to obtain secondary extracted antarctic krill oil and secondary extracted antarctic krill powder; and performing third-stage extraction on the second-stage extracted antarctic krill powder by using an alcohol solvent to obtain third-stage extracted antarctic krill oil. Chinese patent application (CN 104830525A) discloses a multistage countercurrent continuous leaching and refining method of antarctic krill oil, which takes antarctic krill powder as a raw material and comprises the following steps: 1. and (3) taking n-hexane as an extracting agent, extracting the antarctic krill oil by adopting a multi-stage countercurrent continuous leaching method, wherein the extraction stage number is 2-5, filtering and centrifuging the mixed oil, and performing vacuum desolventization on the upper-layer liquid to obtain crude oil. 2. Dissolving crude oil in n-hexane, adding sodium silicate into the mixed oil, stirring, filtering the mixed oil, centrifuging, and collecting the upper layer liquid. 3. Standing at the temperature of-4 ℃, layering, taking the upper layer liquid, centrifuging, and removing the solvent from the upper layer liquid in vacuum to obtain the euphausia superba refined shrimp sauce. Chinese patent application (CN 105154216A) discloses a preparation method of low-residue antarctic krill oil, which comprises the following steps: the method comprises the steps of taking antarctic krill powder as a raw material, taking food-grade n-hexane as an extraction solvent, mixing extraction materials and liquid in a ratio of 1: 5-9 mg/ml, standing, taking supernate, centrifuging, removing precipitate, and removing an organic solvent through twice rotary evaporation under different conditions to obtain the low-solvent-residue antarctic krill oil.
At present, the extraction of the euphausia superba oil is mainly carried out by organic solvent extraction. The extraction of the shrimp oil is a process for breaking mass transfer dynamic balance for multiple times, the antarctic krill contains rich grease, and if the extraction times are few, the residual oil rate in the antarctic krill residues is high; the leaching times are more, the residual oil rate is low, but the dosage of the solvent is increased, and the consumption of the solvent is correspondingly increased. Therefore, the dried shrimp residue of the Antarctic krill after being degreased by the organic solvent also contains a certain amount of grease. How to re-extract grease from the shrimp residues, increase the yield of the shrimp sauce and reduce the extraction cost of the shrimp sauce is an urgent need to solve at present.
Disclosure of Invention
The invention mainly aims to provide a method for re-extracting grease from degreased dried euphausia superba residues.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a method for re-extracting grease from degreased dried shrimp residues of Antarctic krill comprises the following steps: carrying out superfine grinding and sieving on degreased dry shrimp residues of Antarctic krill, then homogenizing under high pressure, taking out feed liquid after homogenizing, filtering, carrying out rotary evaporation, and removing a solvent to obtain the grease.
In the preferred technical scheme of the invention, the superfine grinding step comprises the following steps: 0.6-1kg of degreased dried shrimp residues of Antarctic krill is crushed by a vibration type medicine superfine crusher, a stainless steel vibrating rod phi is 20 multiplied by 174mm, the amplitude is 3-5mm, and superfine crushing is carried out for 0.5-1h, so as to obtain superfine shrimp residue coarse powder.
In the best technical scheme of the invention, the superfine grinding step comprises the following steps: 0.6-1kg of degreased dried shrimp residues of Antarctic krill is pulverized by a vibration type medicine ultrafine pulverizer, a stainless steel vibrating rod phi is 20 multiplied by 174mm, the amplitude is 3mm, and the ultrafine pulverization is carried out for 1h, so as to obtain ultrafine shrimp residue coarse powder.
In the preferred technical scheme of the invention, the ultrafine shrimp residue coarse powder is sieved by a sieve with 100-120 meshes to obtain the ultrafine shrimp residue fine powder.
In a further preferable technical scheme of the invention, the ultrafine shrimp residue coarse powder is sieved by a 110-mesh sieve to obtain ultrafine shrimp residue fine powder.
In the preferred technical scheme of the invention, the ultrafine shrimp residue fine powder and an ethanol solution are mixed according to the mass-volume ratio of 1:10-15, and then are homogenized under high pressure, wherein the conditions are as follows: the pressure is 40-60 MPa, the time is 15-30 minutes, and the flow is 80-120 ml/min; under the condition of high-pressure homogenization, the grease contained in the shrimp residues can be fully extracted, and the grease yield reaches 6.8-7.1%.
In a further preferable technical scheme of the invention, after mixing the ultrafine shrimp residue fine powder and an ethanol solution according to the mass-volume ratio of 1:15, carrying out high-pressure homogenization on the mixture, wherein the conditions are as follows: the pressure was 40MPa, the time was 15 minutes and the flow was 80 ml/min.
In the preferable technical scheme of the invention, the concentration of the ethanol solution is 80-100%.
In a further preferred embodiment of the invention, the ethanol solution is used at a concentration of 100%.
In the preferable technical scheme of the invention, the rotary evaporation temperature is 68-72 ℃.
The degreased dry shrimp residue of the euphausia superba is obtained by degreasing and drying the euphausia superba by using an organic solvent.
Firstly, carrying out superfine grinding on degreased dried shrimp residues of Antarctic krill, screening superfine shrimp residue fine powder with a specific particle size, mixing the superfine shrimp residue fine powder with an ethanol solution according to a certain proportion, and then carrying out high-pressure homogenization, thereby achieving the purpose of more fully extracting grease from the degreased dried shrimp residues of Antarctic krill. The steps of the invention are closely combined, and one parameter can be changed randomly, so that the effect of extracting the grease of the invention can not be obtained.
In the superfine pulverizing equipment, the efficiency of the vibration mill is 10-20 times higher than that of the common mill, the milling speed is faster than that of the conventional ball mill, and the energy consumption is lower than that of the common ball mill. The technical personnel of the invention find through experiments that the vibration type drug ultrafine pulverizer with the parameters of the stainless steel vibrating rod phi 20 multiplied by 174mm and the amplitude of 3-5mm can play a good crushing effect on the degreased dried shrimp residues of the antarctic krill; when the shrimp residue powder is crushed for 0.5 to 1 hour, not only can the grease component in the shrimp residue powder be fully dissolved out, but also wall sticking and overhigh material temperature caused by over-grinding can be effectively avoided.
The technical personnel of the invention find that the mesh number of the shrimp residue powder obtained by screening has great influence on the subsequent homogenization treatment and the final oil yield, if the granularity of the shrimp residue powder obtained by screening is too large, the dissolution of oil in the shrimp residue is not facilitated, and the final oil yield is low; if the granularity of the shrimp residue powder obtained by screening is too small, wall sticking is easy to happen, incomplete separation of feed liquid can be caused, and residual oil is contained in the filtered feed residue. The ultrafine shrimp residue fine powder obtained by screening can well overcome the problems.
The choice of the solvent for extracting the oil directly influences the yield of the oil. The technical personnel of the invention find that the ethanol solution (with the concentration of 80-100%) and the ultrafine shrimp residue fine powder obtained by sieving with the 100-fold 120-mesh sieve can obtain excellent effect after being mixed and homogenized under high pressure.
The invention realizes the purpose of effectively re-extracting the grease from the degreased dried shrimp residues of the Antarctic krill, and the grease yield reaches 6.8-7.1%; the method disclosed by the invention can be used in the extraction process of the antarctic krill grease, so that the grease yield can be improved, the production cost of the functional grease can be reduced, and the large-scale production of the antarctic krill grease is facilitated.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of the stated features, steps, operations, elements, and/or combinations thereof, unless the context clearly indicates otherwise.
In order to make the technical solutions of the present invention more clearly understood by those skilled in the art, the technical solutions of the present invention will be described in detail below with reference to specific embodiments.
Example 1 method for re-extracting oil from degreased dried euphausia superba residue
The extraction method comprises the following steps: putting 1Kg of degreased dried shrimp residues of Antarctic krill into an ultrafine pulverizer for pulverizing, wherein a stainless steel vibrating rod has the diameter of 20 x 174mm and the amplitude of 3mm, performing ultrafine pulverization for 45 minutes, sieving the obtained ultrafine shrimp residue coarse powder with a 110-mesh sieve, taking 10g of the sieved ultrafine shrimp residue fine powder, adding 100ml of 95% ethanol solution, homogenizing under 60MPa for 20 minutes at a high pressure, wherein the flow is 100ml/min, and discharging the feed liquid after homogenization. Filtering the feed liquid, rotatably evaporating the filtrate at 70 deg.C, and removing solvent to obtain oil.
Example 2 method for re-extracting oil from degreased dried euphausia superba residue
The extraction method comprises the following steps: putting 1Kg of degreased dried shrimp residues of Antarctic krill into an ultrafine pulverizer for pulverizing, carrying out ultrafine pulverization on the degreased dried shrimp residues for 30 minutes with a stainless steel vibrating rod phi of 20X 174mm and an amplitude of 4mm, sieving the obtained ultrafine shrimp residue coarse powder for 120 meshes, taking 10g of sieved ultrafine shrimp residue fine powder, adding 120ml of 80% ethanol solution, carrying out high-pressure homogenization for 30 minutes at 50MPa, and discharging feed liquid after the homogenization is finished. Filtering the feed liquid, rotatably evaporating the filtrate at 68 deg.C, and removing solvent to obtain oil.
Example 3 method for re-extracting oil from degreased dried euphausia superba residue
The extraction method comprises the following steps: putting 1Kg of degreased dried shrimp residues of Antarctic krill into an ultrafine pulverizer for pulverizing, wherein a stainless steel vibrating rod has the diameter of 20X 174mm and the amplitude of 5mm, performing ultrafine pulverization for 60 minutes, sieving the obtained ultrafine shrimp residue coarse powder with a 100-mesh sieve, taking 10g of the sieved ultrafine shrimp residue fine powder, adding 150ml of absolute ethyl alcohol, homogenizing under 40MPa for 15 minutes at high pressure and the flow rate of 80ml/min, and discharging the feed liquid after homogenization. Filtering the feed liquid, rotatably evaporating the filtrate at 72 ℃, and removing the solvent to obtain the grease.
Comparative example 1 method for re-extracting grease from degreased dried shrimp residues of Antarctic krill
The difference from example 3 is that the obtained ultra-fine shrimp residue meal is sieved by a 90-mesh sieve, and the rest is similar to example 3.
Comparative example 2 method for re-extracting grease from degreased dried euphausia superba residue
The difference from example 3 is that the obtained ultra-fine shrimp residue meal is sieved by a 130-mesh sieve, and the rest is similar to example 3.
Comparative example 3 method for re-extracting grease from degreased dried shrimp residues of Antarctic krill
The difference from example 3 is that n-hexane was used in place of absolute ethanol, and the rest is similar to example 3.
Comparative example 4 method for re-extracting grease from degreased dried shrimp residues of Antarctic krill
The difference from example 3 is that acetone is used instead of absolute ethanol, and the rest is similar to example 3.
Test examples measurement of oils and fats obtained by different extraction methods
The fats and oils extracted by the extraction methods of examples 1 to 3 and comparative examples 1 to 4 were weighed, and the experimental results are shown in table 1.
TABLE 1 weight and yield of oils obtained by different extraction methods
Group of | Weight of oil (g) | Oil yield (%) |
Example 1 | 0.7 | 7.0 |
Example 2 | 0.68 | 6.8 |
Example 3 | 0.71 | 7.1 |
Comparative example 1 | 0.52 | 5.2 |
Comparative example 2 | 0.47 | 4.7 |
Comparative example 3 | 0.43 | 4.3 |
Comparative example 4 | 0.45 | 4.5 |
As is clear from Table 1, in the extraction methods of examples 1 to 3, the weight of the fat and oil obtained in example 3 was 0.71g, and the oil yield was 7.1%, which are the most preferable examples of the present invention. The oil extracted in the embodiment 3 of the invention is higher than that extracted in the comparative examples 1 and 2, so that the oil yield can be greatly influenced by the granularity of the ultrafine shrimp residue fine powder obtained by crushing, and the effect of combining the ultrafine shrimp residue fine powder obtained by sieving with a 100-mesh sieve in the embodiment 3 with other process conditions is optimal; the grease obtained by extraction in example 3 is higher than that obtained in comparative examples 3 and 4, which shows that the effect of extraction by adding absolute ethyl alcohol is best when homogenizing.
Claims (7)
1. A method for extracting grease from dry degreased shrimp residues of Antarctic krill is characterized in that the dry degreased shrimp residues of Antarctic krill are subjected to superfine grinding and sieving, then are subjected to high-pressure homogenization, and after homogenization, feed liquid is taken out, filtered and subjected to rotary evaporation to remove a solvent, so that grease is obtained;
the superfine grinding step comprises: pulverizing defatted dried residue of Euphausia superba 0.6-1kg with vibration type medicinal ultrafine pulverizer to obtain ultrafine residue coarse powder, wherein the diameter of stainless steel vibrating rod is 20 × 174mm, the amplitude is 3-5mm, and the ultrafine powder is pulverized for 0.5-1 h; sieving the ultrafine shrimp residue coarse powder with a sieve of 100-plus 120 meshes to obtain ultrafine shrimp residue fine powder;
mixing the ultrafine shrimp residue fine powder with an ethanol solution according to the mass volume ratio of 1:10-15, and then homogenizing under high pressure, wherein the conditions are as follows: the pressure is 40-60 MPa, the time is 15-30 minutes, and the flow is 80-120 ml/min.
2. The method for re-extracting the oil from the defatted dried krill meal of Antarctic krill according to claim 1, wherein the micronizing step comprises: 0.6-1kg of degreased dried shrimp residues of Antarctic krill is pulverized by a vibration type medicine ultrafine pulverizer, a stainless steel vibrating rod phi is 20 multiplied by 174mm, the amplitude is 3mm, and the ultrafine pulverization is carried out for 1h, so as to obtain ultrafine shrimp residue coarse powder.
3. The method for re-extracting oil from the degreased and dried euphausia superba residue as claimed in claim 1, wherein the ultra-fine powder of the euphausia superba residue is sieved with a 110-mesh sieve to obtain the ultra-fine powder of the euphausia superba residue.
4. The method for re-extracting the grease from the degreased and dried euphausia superba residue as claimed in claim 1, wherein the superfine fine powder of the euphausia superba residue is mixed with the ethanol solution according to the mass-to-volume ratio of 1:15, and then the mixture is homogenized under high pressure, wherein the specific conditions are as follows: the pressure was 40MPa, the time was 15 minutes and the flow was 80 ml/min.
5. The method for re-extracting the grease from the degreased dry shrimp residues of the Antarctic krill according to claim 1, wherein the concentration of the ethanol solution is 80-100%.
6. The method for re-extracting oil from the defatted dried krill meal of Antarctic krill according to claim 1, wherein the ethanol solution is used at a concentration of 100%.
7. The method for re-extracting the grease from the degreased dry shrimp residues of the Antarctic krill according to claim 1, wherein the rotary evaporation temperature is 68-72 ℃.
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CN102492545A (en) * | 2011-12-28 | 2012-06-13 | 中国水产科学研究院黄海水产研究所 | Methods for extracting high-quality shrimp oil from Antarctic krill and for preparing defatted krill protein powder |
CN102492537A (en) * | 2011-11-14 | 2012-06-13 | 辽宁省大连海洋渔业集团公司 | Method for extracting krill oil from antarctic krill |
CN102766530A (en) * | 2012-08-08 | 2012-11-07 | 辽宁省大连海洋渔业集团公司 | Method for extracting phospholipid-rich krill oil from Antarctic krill |
CN102899163A (en) * | 2012-10-25 | 2013-01-30 | 山东师范大学 | Process for extracting fluoride-free shrimp oil from dried antarctic krill |
CN104152263A (en) * | 2014-08-18 | 2014-11-19 | 安徽中盛食用油科技有限公司 | Tea-seed oil extraction method with high oil yield |
CN106010784A (en) * | 2016-07-19 | 2016-10-12 | 广西驰胜农业科技有限公司 | Method for leaching camellia oleifera seed oil by using high pressure homogenization technology |
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Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102492537A (en) * | 2011-11-14 | 2012-06-13 | 辽宁省大连海洋渔业集团公司 | Method for extracting krill oil from antarctic krill |
CN102492545A (en) * | 2011-12-28 | 2012-06-13 | 中国水产科学研究院黄海水产研究所 | Methods for extracting high-quality shrimp oil from Antarctic krill and for preparing defatted krill protein powder |
CN102766530A (en) * | 2012-08-08 | 2012-11-07 | 辽宁省大连海洋渔业集团公司 | Method for extracting phospholipid-rich krill oil from Antarctic krill |
CN102899163A (en) * | 2012-10-25 | 2013-01-30 | 山东师范大学 | Process for extracting fluoride-free shrimp oil from dried antarctic krill |
CN104152263A (en) * | 2014-08-18 | 2014-11-19 | 安徽中盛食用油科技有限公司 | Tea-seed oil extraction method with high oil yield |
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