CN101791040B - Production method of low-ethylether insoluble food grade soybean concentrated phospholipid - Google Patents

Production method of low-ethylether insoluble food grade soybean concentrated phospholipid Download PDF

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CN101791040B
CN101791040B CN201010122531XA CN201010122531A CN101791040B CN 101791040 B CN101791040 B CN 101791040B CN 201010122531X A CN201010122531X A CN 201010122531XA CN 201010122531 A CN201010122531 A CN 201010122531A CN 101791040 B CN101791040 B CN 101791040B
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phospholipid
food grade
concentrated
solvent
phosphatide
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CN101791040A (en
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郑伟
陈慧
谈黎明
瞿俊勇
张晖
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Shanghai Dongchen Grain and Oil Co.,Ltd.
SHANGHAI GRAIN SCIENCE RESEARCH INSTITUTE
Shanghai Liangyou (Group) Co Ltd
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SHANGHAI INSTITUTE OF FOOD SCIENCE
SHANGHAI LIANGYOU (GROUP) CO Ltd
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Abstract

The invention relates to a production method of low-ethylether insoluble food grade soybean concentrated phospholipid. The food grade soybean concentrated phospholipid prepared by the method contains no more than 0.05% of ethylether insoluble. The production method of the invention comprises the following key steps: dissolving feed grade concentrated soybean phospholipid with solvent to reduce the viscosity, removing ethylether insoluble impurity through centrifugal settling, then adding food grade hydrogen peroxide to decolor phospholipid under the condition of maintaining the solvent, and finally adopting two-stage evaporation to separate and recycle the solvent and obtain the finished product. The method of the invention solves the problems in the original production of the food grade soybean concentrated phospholipid, overcomes the defect that partial fine particles can not be removed in the filtration method for purification and obtains the low-ethylether insoluble food grade soybean concentrated phospholipid.

Description

A kind of production method of low-ethylether insoluble food grade soybean concentrated phospholipid
Technical field
The present invention relates to grease processed side product comprehensive utilization---soybean lecithin processing technique field, be specifically related to a kind of production method of low-ethylether insoluble food grade soybean concentrated phospholipid.
Background technology
China is the cradle of soybean.Soybean is one of maximum oil crops in the whole world, also is the maximum oil crops of China's consumption figure, and consumption figure is extremely huge.Soybean oil certainly leads to a certain amount of oil foot---phosphatide in process, its main component is lecithin (PC), cephalin (PE), phosphatidylinositols (PI) etc.Because lecithin has a series of health care physiological functions such as softening blood vessel, protection liver; Become a kind of nutraceutical of popularizing very much already in developed country; Also become widely known day by day in China, development phosphatide industry has proposed quite harsh requirement to the raw material of phosphatide.Because homemade concentrated phosphatide raw material can not satisfy its requirement mostly, therefore high-grade phospholipid prod manufacturing enterprise has to spend a large amount of foreign exchanges from external imported raw material, causes production cost high for a long time, and the performance of enterprises is difficult to significantly improve.
In addition; High-quality concentrated phosphatide product all has very wide range of application in industries such as food service industrys such as candy, cake and light industry, medicine, weaving, rubber, chemical industry; And the concentrating soya lecithin that domestic grease processing enterprise produces, because impurity content high (the ether insolubles content is high), color and luster is dark; Can only be used for feedstuff industry, range of application is very limited.Therefore,,, prepare the high-quality concentrated phosphatide product that satisfies food service industry to high-quality concentrated phosphatide product demand, will have higher added value and good market prospects with less input as if being raw material with homemade concentrating soya lecithin.If can the quality control of raw material phosphatide is proper, then might process and satisfy the required raw material of pharmacy corporation production high-quality high purity phosphorus fat prod.Domestic have many researchs and patent utilization membrane technology to produce high-quality concentrated soybean phospholipid (invention such as Wang Xingguo is produced high-quality concentrated soybean phospholipid through the method for " dicyandiamide solution decolouring-membrane filtration-vacuum evaporation ", Chinese patent publication number CN101006824A, Wang Yong etc. " the inorganic ceramic membrane microfiltration prepares the research of food-level concentrated soybean phospholipid "; Chinese oil; 2007,22 (3), 50-54); The investment of membrane separation plant and operating cost are all very high but at present.
Summary of the invention
The production method that the purpose of this invention is to provide a kind of low-ethylether insoluble food grade soybean concentrated phospholipid, this method is easy to accomplish scale production.
The invention provides a kind of production method of food grade concentrated soybean phospholipid, comprise the following steps:
1) dissolving and sedimentation removal of impurities: with the feed grade concentrated soybean phospholipid is raw material, obtains phospholipid solution with non-polar solven dissolving, and separation of supernatant behind the ether insoluble matter impurity in the phosphatide is removed in centrifugal sedimentation;
2) decolouring: add the food grade hydrogen peroxide solution in the supernatant and carry out the phosphatide decolouring;
3) evaporation precipitation: adopt dual evaporation Separation and Recovery solvent, obtain low-ethylether insoluble food grade soybean concentrated phospholipid.
After above-mentioned steps, also can further dry and obtain dry finished product.
Step 1) adopts the abundant dissolved dilution feed grade of non-polar solven concentrated soybean phospholipid to reduce its viscosity.Preferable, concentrated soybean phospholipid and non-polar solven are 4-1.5 according to mass ratio: 1 mixed dissolution, centrifugal sedimentation is 15 ~ 30 minutes under separating factor 950 ~ 6200 conditions, separates and removes the ether insoluble matter impurity in the phosphatide.
Step 2) in, under the situation that keeps solvent, adds the food-grade hydrogen peroxide solution phosphatide is decoloured.Preferable; The quality of the hydrogen peroxide solution that adds is the 0.6-1.5% of concentrated phosphatide quality; Can adopt the mode of 2 ~ 5% the 30wt% hydrogen peroxide solution that adds the concentrated phosphatide quality to control the addition of hydrogen peroxide solution, under 30 ~ 70 ℃, react and decoloured in 40 ~ 80 minutes.
In the step 3), adopt the dual evaporation technology Separation and Recovery solvent of different condition, wherein, the one-level evaporation conditions is 64-80 ℃, and normal pressure preferably is higher than boiling temperature 4-10 ℃ under the solvent normal pressure; Dual evaporation is a negative pressure evaporation, and condition is 85-95 ℃, residual voltage 0.15-0.2kPa.
Said non-polar solven is selected from n-hexane, food-grade industrial hexane, benzinum or (GB) soybean and leaches solvent (6# solvent), preferred n-hexane.
The food grade concentrated soybean phospholipid that adopts technology of the present invention to obtain, its ether insolubles content are at 0.05 (wt) below the %.
Preferred technology is:
1) dissolving and sedimentation removal of impurities: with the feed grade concentrated soybean phospholipid is raw material; Obtain phospholipid solution with n-hexane dissolution; The ratio of feed grade concentrated soybean phospholipid and n-hexane is about 3: 2; The centrifugal sedimentation process is 980 times centrifugal treating of separating factor 30 minutes, and separation of supernatant behind the ether insoluble matter impurity in the phosphatide is removed in centrifugal sedimentation;
2) decolouring: add the food grade hydrogen peroxide solution in the supernatant and carry out the phosphatide decolouring, the amount of 30% hydrogen peroxide solution (percentage by weight) is 4% of a concentrated phosphatide quality, reacts down at about 60 ℃ and decolours in 60 minutes;
3) evaporation precipitation: adopt dual evaporation Separation and Recovery solvent, obtain low-ethylether insoluble food grade soybean concentrated phospholipid, the one-level evaporation conditions is 80 ℃ (looking the solvent difference possibly change to some extent); Normal pressure reclaims about 90% solvent, and dual evaporation is a negative pressure evaporation; Condition is 90 ℃; Residual voltage 0.18kPa dries by the fire to moisture up to standardly at last in 90 ~ 100 ℃ of vacuum drying ovens, obtains finished product.
Core of the present invention is after the concentrating soya lecithin of feed grade is reduced its viscosity with the dissolution with solvents dilution; Adopt the method for centrifugal sedimentation to remove the ether insoluble matter impurity in the phosphatide; Then under the situation that keeps solvent; Add the food-grade hydrogen peroxide solution phosphatide is decoloured, adopt dual evaporation Separation and Recovery solvent wherein at last, obtain finished product.
Method of the present invention has solved the problem that exists in original food-level concentrated soybean phospholipid production; Overcome the shortcoming that still has the parts of fine granule to leak that exists in the filter method removal of impurities; Help phospholipid prod the promoting the use of of fields such as food, medicine, cosmetics, chemical industry, the import that helps China to break away from high-end phospholipid prod relies on.
The specific embodiment
The production of embodiment 1 low-ethylether insoluble food grade soybean concentrated phospholipid
The high-quality feed grade soybean concentrated phospholipid is dissolved in the n-hexane; The mass ratio of high-quality feed grade soybean concentrated phospholipid and n-hexane is about 3: 2; The centrifugal sedimentation process is 980 times centrifugal treating of separating factor 30 minutes, is equivalent under the 2500rpm rotating speed, stop 30 minutes, then under the situation that keeps solvent; Adding the food-grade hydrogen peroxide solution decolours to phosphatide; According to the actual conditions of homemade phosphatide with to requirement of products, the amount that adds 30% hydrogen peroxide solution is 4% of a concentrated phosphatide quality, reacts down at ~ 60 ℃ and decolours in 60 minutes.The phospholipid solution of accomplishing decolouring adopts dual evaporation Separation and Recovery solvent wherein, and the one-level evaporation conditions is 80 ℃, normal pressure; Reclaim about 90% solvent, the dual evaporation condition is 90 ℃, residual voltage 0.18kPa; In 90 ~ 100 ℃ of vacuum drying ovens, dried by the fire about 2 hours at last, up to standard to moisture, obtain finished product; Use the LS/T3219-1994 method to detect the ether insolubles content for being lower than 0.01 (wt) %; Detect fine particle content with centrifugal method and be lower than 0.05 (wt) %, detecting Gardner (Gartner) with the SN/T0802.1.2 method is 7, reaches the food-grade requirement.
The production of embodiment 2 low-ethylether insoluble food grade soybean concentrated phospholipids
The feed grade concentrated soybean phospholipid is dissolved in the n-hexane; The mass ratio of feed grade concentrated soybean phospholipid and n-hexane is about 4: 1; The centrifugal sedimentation process is 950 times centrifugal treating of separating factor 30 minutes, under the situation that keeps solvent, adds the food-grade hydrogen peroxide solution phosphatide is decoloured then; The amount that adds 30% hydrogen peroxide solution is 5% of a concentrated phosphatide quality, reacts down at ~ 30 ℃ and decolours in 40 minutes.The phospholipid solution of accomplishing decolouring adopts dual evaporation Separation and Recovery solvent wherein, and the one-level evaporation conditions is 74 ℃, normal pressure; Reclaim about 90% solvent, the dual evaporation condition is 85 ℃, residual voltage 0.15kPa; In 90 ~ 100 ℃ of vacuum drying ovens, dried by the fire about 2 hours at last, up to standard to moisture, obtain finished product; The LS/T3219-1994 method detects the ether insolubles content for being lower than 0.01wt%; Detect fine particle content with centrifugal method and be lower than 0.05wt%, it is 7 that the SN/T0802.1.2 method detects Gardner (Gartner), reaches the food-grade requirement.
The production of embodiment 3 low-ethylether insoluble food grade soybean concentrated phospholipids
The feed grade concentrated soybean phospholipid is dissolved in the n-hexane; The mass ratio of feed grade concentrated soybean phospholipid and n-hexane is about 3: 1; The centrifugal sedimentation process is 6200 times centrifugal treating of separating factor 15 minutes, under the situation that keeps solvent, adds the food-grade hydrogen peroxide solution phosphatide is decoloured then; The amount that adds 30% hydrogen peroxide solution is 2% of a concentrated phosphatide quality, reacts down at ~ 40 ℃ and decolours in 80 minutes.The phospholipid solution of accomplishing decolouring adopts dual evaporation Separation and Recovery solvent wherein, and the one-level evaporation conditions is 78 ℃, normal pressure; Reclaim about 90% solvent, the dual evaporation condition is 95 ℃, residual voltage 0.2kPa; In 90 ~ 100 ℃ of vacuum drying ovens, dried by the fire about 2 hours at last, up to standard to moisture, obtain finished product; Use the LS/T3219-1994 method to detect the ether insolubles content and be 0.01wt%; Detect fine particle content with centrifugal method and be lower than 0.05wt%, detecting Gardner (Gartner) with the SN/T0802.1.2 method is 7, reaches the food-grade requirement.
The production of embodiment 4 low-ethylether insoluble food grade soybean concentrated phospholipids
The feed grade concentrated soybean phospholipid is dissolved in the food-grade industrial hexane; The mass ratio of feed grade concentrated soybean phospholipid and industrial hexane is about 2: 1; The centrifugal sedimentation process is 6000 times centrifugal treating of separating factor 15 minutes, under the situation that keeps solvent, adds the food-grade hydrogen peroxide solution phosphatide is decoloured then; The amount that adds 30% hydrogen peroxide solution is 3% of a concentrated phosphatide quality, reacts down at ~ 50 ℃ and decolours in 60 minutes.The phospholipid solution of accomplishing decolouring adopts dual evaporation Separation and Recovery solvent wherein, and the one-level evaporation conditions is 78 ℃, normal pressure; Reclaim about 90% solvent, the dual evaporation condition is 90 ℃, residual voltage 0.18KPa; In 90 ~ 100 ℃ of vacuum drying ovens, dried by the fire about 2 hours at last, up to standard to moisture, obtain finished product; Use the LS/T3219-1994 method to detect the ether insolubles content and be 0.01wt%; Be lower than 0.05wt% with centrifugal method fine particle content, detecting Gardner (Gartner) with the SN/T0802.1.2 method is 7, reaches the food-grade requirement.
The production of embodiment 5 low-ethylether insoluble food grade soybean concentrated phospholipids
The feed grade concentrated soybean phospholipid is dissolved in the benzinum; The mass ratio of feed grade concentrated soybean phospholipid and benzinum is about 7: 3; The centrifugal sedimentation process is 4200 times centrifugal treating of separating factor 18 minutes, under the situation that keeps solvent, adds the food-grade hydrogen peroxide solution phosphatide is decoloured then; The amount that adds 30% hydrogen peroxide solution is 3.5% of a concentrated phosphatide quality, reacts down at ~ 55 ℃ and decolours in 65 minutes.The phospholipid solution of accomplishing decolouring adopts dual evaporation Separation and Recovery solvent wherein, and the one-level evaporation conditions is 64 ℃, normal pressure; Reclaim about 90% solvent, the dual evaporation condition is 90 ℃, residual voltage 0.18kPa; In 90 ~ 100 ℃ of vacuum drying ovens, dried by the fire about 2 hours at last, up to standard to moisture, obtain finished product; Use the LS/T3219-1994 method to detect the ether insolubles content for being lower than 0.01wt%; Detect fine particle content with centrifugal method and be lower than 0.05wt%, detecting Gardner (Gartner) with the SN/T0802.1.2 method is 7, reaches the food-grade requirement.
The production of embodiment 6 low-ethylether insoluble food grade soybean concentrated phospholipids
The feed grade concentrated soybean phospholipid is dissolved in soybean to be leached in the solvent (6# solvent); The mass ratio that feed grade concentrated soybean phospholipid and soybean are leached solvent is about 3: 2; The centrifugal sedimentation process is 2500 times centrifugal treating of separating factor 25 minutes, under the situation that keeps solvent, adds the food-grade hydrogen peroxide solution phosphatide is decoloured then; The amount that adds 30% hydrogen peroxide solution is 4.5% of a concentrated phosphatide quality, reacts down at ~ 60 ℃ and decolours in 60 minutes.The phospholipid solution of accomplishing decolouring adopts dual evaporation Separation and Recovery solvent wherein, and the one-level evaporation conditions is 75 ℃, normal pressure; Reclaim about 90% solvent, the dual evaporation condition is 90 ℃, residual voltage 0.18k Pa; In 90 ~ 100 ℃ of vacuum drying ovens, dried by the fire about 2 hours at last, up to standard to moisture, obtain finished product; Use the LS/T3219-1994 method to detect the ether insolubles content for being lower than 0.01wt%; Detect fine particle content with centrifugal method and be lower than 0.05wt%, detecting Gardner (Gartner) with the SN/T0802.1.2 method is 7, reaches the food-grade requirement.

Claims (5)

1. the production method of a food grade concentrated soybean phospholipid comprises the following steps:
1) dissolving and sedimentation removal of impurities: with the feed grade concentrated soybean phospholipid is raw material; Obtain phospholipid solution with the non-polar solven dissolving; Separation of supernatant behind the ether insoluble matter impurity in the phosphatide is removed in centrifugal sedimentation, and wherein, concentrated soybean phospholipid and non-polar solven are 4-1.5 according to mass ratio: 1 mixed dissolution; Under separating factor 950-6200 condition centrifugal sedimentation 15-30 minute, separate and remove the ether insoluble matter impurity in the phosphatide;
2) decolouring: add the food grade hydrogen peroxide solution in the supernatant and carry out the phosphatide decolouring;
3) evaporation precipitation: adopt dual evaporation Separation and Recovery solvent, obtain low-ethylether insoluble food grade soybean concentrated phospholipid, in the said dual evaporation technology Separation and Recovery solvent, the one-level evaporation conditions is 64-80 ℃, normal pressure; Dual evaporation is a negative pressure evaporation, and condition is 85-95 ℃, residual voltage 0.15-0.20kPa.
2. the production method of food grade concentrated soybean phospholipid according to claim 1 is characterized in that step 2) in, the quality of the hydrogen peroxide solution of adding is the 0.6-1.5% of concentrated phosphatide quality.
3. the production method of food grade concentrated soybean phospholipid according to claim 1 is characterized in that, said one-level evaporating temperature is for being higher than under the solvent for use normal pressure boiling temperature 4-10 ℃.
4. like the production method of the said food grade concentrated soybean phospholipid of arbitrary claim among the claim 1-3, it is characterized in that said non-polar solven is selected from n-hexane, food-grade industrial hexane, benzinum or soybean and leaches solvent.
5. like the production method of the said food grade concentrated soybean phospholipid of arbitrary claim among the claim 1-3, it is characterized in that, after the said step 3), obtain dry finished product through oven dry.
CN201010122531XA 2010-03-11 2010-03-11 Production method of low-ethylether insoluble food grade soybean concentrated phospholipid Active CN101791040B (en)

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CN105010721A (en) * 2015-07-21 2015-11-04 江南大学 Multi-step coupling method to prepare concentrated phospholipids with a high transparency
CN108003187A (en) * 2016-11-01 2018-05-08 中粮集团有限公司 A kind of method for preparing transparent concentrating soya lecithin
CN108299495A (en) * 2018-02-11 2018-07-20 山东渤海油脂工业有限公司 The edible phospholipid that a kind of production method of edible phospholipid and production obtain
CN112851707A (en) * 2021-01-22 2021-05-28 浙江省粮食科学研究所有限责任公司 Method for preparing high-quality soybean concentrated phospholipid by combined progressive filtration

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Address after: 200122 No. 88 Zhang Yang Road, Shanghai, Pudong New Area

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Patentee after: Shanghai Grain Science Research Institute

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