CN1899078A - Method for preparing food grade powder phospholipid - Google Patents
Method for preparing food grade powder phospholipid Download PDFInfo
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- CN1899078A CN1899078A CN 200610085923 CN200610085923A CN1899078A CN 1899078 A CN1899078 A CN 1899078A CN 200610085923 CN200610085923 CN 200610085923 CN 200610085923 A CN200610085923 A CN 200610085923A CN 1899078 A CN1899078 A CN 1899078A
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Abstract
The method of preparing food level powdered phospholipid belongs to the field of fat and oil industrial technology. The mixture liquid compounded with concentrated phospholipid and solvent is treated through filtering with ultrafiltering membrane, acetone extraction of phospholipid from the ultrafiltered reflux liquid, centrifugal separation of the liquid phase, crushing the solid and drying in vacuum fluidized bed to obtain the food level powdered phospholipid. The present invention has the advantages of adoption of ultrafiltering technology, the application of counter micelle principle for the separation of phospholipid from triglyceride, and once acetone extraction of the ultrafiltered reflux liquid to obtain the food level powdered phospholipid.
Description
Technical field
A kind of preparation method of food grade powder phospholipid belongs to the oil prodution industry technical field.
Background technology
Homemade phosphatide is present with the main difference table of high-quality phosphatide in the world: (1) impure amount height (the insoluble object height of ether), and (2) color and luster is dark, and (3) kind is few.
The preparation concentrated phosphatide needs a series of operation, and general technology comprises that Soybean Pretreatment, leaching (solubilizer preparation mixed liquor), desolventizing, hydration degum get hydrated oil foot, centrifugation, concentrate drying.
Membrane separation technique is new and effective, the accurate isolation technics of succeeding in developing in 20th century, and it is that material science combined with intersecting of medium isolation technics, with the separative efficiency height, equipment is simple, easy to operate and advantage such as energy-conservation is applied to every field.Application of membrane starts from the end of the sixties in last century in food industry, at first is applied to Dairy Processing, is applied to the purification and the concentrated aspect of the refining and enzyme preparation of aseptic filtration, the drinks of fruit juice processing, beverage subsequently.And the utilization membrane technology is studied only time decades in grain and oil industry, but development is very fast.
The application of membrane separation technique in oil prodution industry be nearly 30 years inchoate, in initial 20 years, many breadboard researchs are arranged, but seldom industrialization, as: remove mixed liquor solvent, ultrafiltration with counter-infiltration and remove the processing of phosphatide and aliphatic acid in the oil, ultrafiltration oily waste water.Really application of membrane separation technology in oil prodution industry be the appearance of inoranic membrane because advantage such as it is high temperature resistant, organic solvent-resistant, mechanical strength are big, be very suitable for the application of oil prodution industry.
It is not because of the expense of investing that membrane separation technique can not be applied to industrialized reason, but the flux of film, organic film can not make oil loving material pass through owing to make the hydrophily of material, and this has all limited its application in oil prodution industry.
At present, the production of homemade phosphatide generally adopts concentrated phosphatide just can prepare content 95% above phosphatide through extraction process more than three times or three times, and solvent consumption is many and the phosphatide color and luster is darker.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of food grade powder phospholipid utilizes membrane separation technique that sweet three esters are separated from phospholipid prod, prepares the food grade powder phospholipid product.
Technical scheme of the present invention: with concentrated phosphatide solubilizer liquid mixture prepared through ultrafiltration membrance filter, penetrating fluid deals with in addition, phosphatide with acetone extract once in the ultrafiltration phegma, through centrifugation liquid phase part, solid phase is partly pulverized, the vacuum fluidized bed drying obtains acetone insoluble matter greater than 95% food grade powder phospholipid product; Concentrated phosphatide adds solvent preparation mixed liquor No. 6, and the mass volume ratio of concentrated phosphatide and No. 6 solvents is 1: 5, the mixed liquor ultrafiltration: select the inorganic ceramic milipore filter for use, membrane aperture is 0.6 μ m, ultrafiltration pressure reduction is 0.1Mpa, 40～55 ℃ of ultrafiltration temperature, 2～2.5 hours ultrafiltration time.
Used concentrated phosphatide is products such as East Sea grain and oil Industrial Co., Ltd, golden extra large food industry Co., Ltd, and is on sale.No. 6 solvent is commercially available.
The impurity in the concentrated phosphatide is held back in filtration, but phosphatide has also effectively been held back in filter process.Phosphatide and impurity all are retained in the phegma, and sweet three esters are retained in the penetrating fluid.If use the less concentrated phosphatide of impurity content to make raw material, with the film pipe filtration of certain pore size, the saturating filmed passing tube of sweet three esters, and phosphatide is effectively held back, and so just phosphatide effectively can be separated with sweet three esters.
The index determining of concentrated phosphatide is as shown in table 1.
Table 1
| Index | Acetone insoluble matter (%) | Hexane undissolved substance (%) | Moisture (%) |
| Measurement result | 63.42 | 0.07424 | 0.38 |
Because the content of hexane undissolved substance, moisture is all very low in the concentrated phosphatide, concentrated phosphatide is considered as anhydrous system substantially, in the index determining afterwards, mainly investigates the content of acetone insoluble matter.
Theoretically, the molecular mass (being approximately 900D) of sweet three esters and phosphatide differs very little.Therefore be difficult to they be separated with film.But phosphatide is a kind of natural surfactant, and it has hydrophilic end and hydrophobic end simultaneously, forms the reverse micelle of spherical structure under water-less environment.After forming this reverse micelle, its molecular weight can reach 20000D even bigger.And the molecular weight of sweet three esters is about 900D, and so just making ultrafiltration take off sweet three esters becomes possibility.Therefore, after forming reverse micelle, phosphatide can select suitable film that phosphatide is separated from sweet three esters.Two parts of phegma and penetrating fluid have been produced in the separation process based on membrane technology.Though all contain sweet three esters and the phosphatide of different content in these two parts separately, but content of phospholipid constantly increases in the phegma, sweet three ester contents constantly reduce, on the contrary sweet three esters constantly been separated in the penetrating fluid, the acetone insoluble matter content that is embodied in phegma constantly increases.
According to experimental result, we have selected operating condition: select the inorganic ceramic ultrafiltration membrane pipe for use, membrane aperture is 0.6 μ m, and ultrafiltration pressure reduction is 0.1Mpa, and the ultrafiltration temperature is 40～55 ℃, 2～2.5 hours ultrafiltration time.
With phosphatide acetone extract in the above-mentioned ultrafiltration gained phegma, (ultrafiltration system is no water system to adopt phosphatide, the key component of phegma is a phosphatide): the mass volume ratio of acetone is that (w: ratio v) extracted once in 1: 15,25～35 ℃ of extraction temperature, 20-50 minute extraction time, back centrifugation liquid phase part, solid phase are partly pulverized the back at 45～75 ℃ of following vacuum fluidized bed dryings through the particle pulverizer.Gained powder phospholipid acetone insoluble matter is greater than 95%, and it is faint yellow that color and luster is, and is the product food grade powder phospholipid.
Beneficial effect of the present invention: the present invention has adopted the ultrafiltration membrance filter technology to remove impurity on the one hand, uses the reverse micelle principle on the other hand and realizes separating of phosphatide and sweet three esters.Phosphatide in the ultrafiltration gained phegma is carried out that acetone extract is purified as long as just can obtain acetone insoluble matter content greater than 95% food grade powder phospholipid product through primary purification.And if without ultrafiltration membrance filter, only must be through just reaching acetone insoluble matter content behind three to four acetone extracts greater than 95% phospholipid prod with the phospholipid prod of gained behind the general filtering and impurity removing, and the present invention has reduced the consumption of acetone solvent, and the phospholipid prod color and luster is more shallow.
Description of drawings
The variation of acetone insoluble matter content in the different ultrafiltration time period gained penetrating fluids of Fig. 1
The variation of acetone insoluble matter content in the different ultrafiltration time period gained phegmas of Fig. 2
The specific embodiment
The selection of embodiment 1 ultrafiltration membrane pipe and ultrafiltration condition
Install the film pipe, with concentrated phosphatide: the 20L mixed liquor that No. 6 solvents (W/V)=1: 5 ratio prepares is poured in the feed liquid bucket (feed liquid bucket position should a little higher than membrane separation plant), opens valve and is full of circulation line voluntarily by feed liquid.Open motor, control required pressure reduction and flow velocity by regulating control valve and return valve.
The permeate samples of obtaining in the experimentation is passed through rotary evaporation in vacuo, remove No. 6 solvents in the solution, distinguish the content of acetone insoluble matter in the analytic sample then.
Use the ceramic-film tube in 0.2,0.6,1.2,2.0 μ m apertures to measure the relation that the penetrating fluid flux changed with pressure reduction, time respectively.In the incipient stage, flux increases with the increase of pressure reduction, and flux slightly increases with the increase of pressure reduction subsequently.In ultra-filtration process, there is a critical pressure, for about 0.1Mpa.Below critical pressure, pressure reduction and membrane flux are proportional, and on critical pressure, because the influence of factors such as concentration polarization, no longer there are linear relationship in pressure reduction and membrane flux, and pressure reduction is little to the influence of flux.Under uniform pressure, the membrane flux minimum in 1.2 μ m apertures, reason may be that the size of the diameter of impurity particle and membrane aperture is very approaching, have seriously stopped up the film endoporus, so its flux minimum.
Therefore to adopt membrane aperture be 0.6 μ m in the present invention, the ceramic membrane that adopts Hunan Ever-Shine Environmental Protection Industry Co., Ltd. to produce, size: internal diameter 3mm, external diameter 26mm, length 250mm.Its film pore footpath 0.6 μ m, effective film area 0.05m
2, 10～80 ℃ of temperature applicable ranges, molecular weight＞1000KDa dams.Operating pressure is 0.1Mpa.
Embodiment 2 phosphatide separate the selection of ultrafiltration time with sweet three esters
Install the film pipe, with concentrated phosphatide: the 20L mixed liquor that No. 6 solvents (W/V)=1: 5 ratio prepares is poured in the feed liquid bucket (feed liquid bucket position should a little higher than membrane separation plant), opens valve and is full of circulation line voluntarily by feed liquid.Open motor, control required pressure reduction and flow velocity by regulating control valve and return valve.Adjustment pressure reduction is 0.1Mpa, and the ultrafiltration temperature is 40 ℃-55 ℃, about the penetrating fluid 2L that each run was obtained in 30 minutes and the phegma sample by rotary evaporation in vacuo, remove No. 6 solvents in the solution, then the content of acetone insoluble matter in the analytic sample respectively.(attention must be used for detecting only getting sub-fraction behind the sample precipitation in the phegma, and remaining part is still refunded in the phegma), 7 minutes flux after the measurement each run is normal.
The variation of acetone insoluble matter content as shown in Figure 1 in the different ultrafiltration time period gained penetrating fluids.
The variation of acetone insoluble matter content as shown in Figure 2 in the different ultrafiltration time period gained phegmas.
Experimental result shows that acetone insoluble matter content is the highest in 2～2.5 hours phegmas of ultrafiltration, is 2～2.5 hours so the present invention selects the ultrafiltration time.
With phosphatide acetone extract in the above-mentioned ultrafiltration gained phegma, (ultrafiltration system is no water system to adopt phosphatide, the key component of phegma is a phosphatide): the mass volume ratio of acetone is that (w: ratio v) extracted once in 1: 15,25～35 ℃ of extraction temperature, 20-50 minute extraction time, back centrifugation liquid phase part, solid phase are partly pulverized the back at 45～75 ℃ of following vacuum fluidized bed dryings through the particle pulverizer.Gained powder phospholipid acetone insoluble matter is greater than 95%, and it is faint yellow that color and luster is, and is the product food grade powder phospholipid.
Claims (1)
1. the preparation method of a food grade powder phospholipid, it is characterized in that concentrated phosphatide solubilizer liquid mixture prepared through ultrafiltration membrance filter, penetrating fluid deals with in addition, phosphatide with acetone extract once in the ultrafiltration phegma, through centrifugation liquid phase part, solid phase is partly pulverized, and the vacuum fluidized bed drying obtains the food grade powder phospholipid product; Concentrated phosphatide adds solvent preparation mixed liquor No. 6, and the mass volume ratio of concentrated phosphatide and No. 6 solvents is 1: 5, the mixed liquor ultrafiltration: select the inorganic ceramic milipore filter for use, membrane aperture is 0.6 μ m, ultrafiltration pressure reduction is 0.1Mpa, 40～55 ℃ of ultrafiltration temperature, 2～2.5 hours ultrafiltration time.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200610085923 CN1899078A (en) | 2006-05-26 | 2006-05-26 | Method for preparing food grade powder phospholipid |
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| CN 200610085923 CN1899078A (en) | 2006-05-26 | 2006-05-26 | Method for preparing food grade powder phospholipid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111548862A (en) * | 2020-05-26 | 2020-08-18 | 内蒙古铂贝曼科技有限公司 | Self-aggregating aqueous phospholipid |
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- 2006-05-26 CN CN 200610085923 patent/CN1899078A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111548862A (en) * | 2020-05-26 | 2020-08-18 | 内蒙古铂贝曼科技有限公司 | Self-aggregating aqueous phospholipid |
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