CN101570718A - Method for extracting and decoloring rapeseed phosphatide - Google Patents

Abstract

The invention discloses a method for extracting and decoloring rapeseed phosphatide, belonging to the technical field of refining side product extraction. The method comprises the following steps: (1) heating bottom oil to obtain softening oil; (2) placing the softening oil in a vessel, and dissolving the softening oil with acetone according to the ratio of mass/volume of 12mL/g to obtain deoiled raw phosphatide; (3) adding aether in the raw phsophatide to be refined and sufficiently dissolving the raw phsophatide, filtering the mixture after standing for 10 minutes to obtain filtrate; (4) decompressing and concentrating the filtrate, and removing solvent to obtain concentrated phosphatide; (5) decoloring the concentrated phosphatide by H2O2 with concentration of 5.85 percent at a temperature of 30 DEG C for 14.5 minutes to obtain concentrated and decolored phosphatide; and (6) centrifugating the concentrated and decolored phosphatide for 10 minutes according to 8,000r/min, and drying the concentrated and decolored phosphatide in vacuum at a temperature of 50 DEG C to be stored for standby. The method is simple and convenient, has low production cost, high extraction rate of phosphatide reaching 28.1 percent; the product has good property and light color, and is light yellow paste; and the method is applicable to comprehensively extracting vegetable bottom oil phosphatide.

Description

The method that a kind of vegetable seed phosphatide extracts and decolours

Technical field

The invention belongs to oil refining by product extractive technique field, relate in particular to that a kind of vegetable seed phosphatide extracts and the method for decolouring, specifically, be to be the method for raw material separation and Extraction and refined phosphatide, and comprise method the phosphatide decolouring with the rapeseed oil residue.

Technical background

There is abundant oil resource in China, and oil prodution industry development in recent years is swift and violent, and a year refining working ability surpasses 1,460 ten thousand t, but processes roughly, and technology is backward relatively, many high-grade grease chemical article dependence on import.Oil crops are main soybean, rape, peanut and corn etc.Oil foot is to be processed into the tankage that produce the essential oil process from crude oil, accounts for 20% of essential oil quality; Rapeseed oil residue is the by product of hydration degum in the vegetable seed oil and fat refining process, accounts for 5%～10% of quality of crude oil.The main component of rapeseed oil residue is phosphatide, neutral oil, moisture and other lipoid, also has a spot of protein, carbohydrate, wax and pigment, and organic impurity and inorganic impurity.Rapeseed oil residue very easily becomes sour, smelly and cause environmental pollution.In the refining course of processing, produce nearly 3,000,000 t of vegetable oil residue per year.Before soy industry is risen, egg is one of main source of commodity phosphatide, and owing to the fast development of oil prodution industry, the main source of commodity phosphatide has turned to soybean gradually afterwards, especially soybean oil residue is subjected to the extensive utilization of phosphatide industry because of its phospholipids content height.

Phosphatide is one of main component of rapeseed oil residue, is a kind of high nutrition-fortifying agent of pure natural, is again a kind of natural tensio-active agent simultaneously, is widely used in fields such as leather, feed, weaving and makeup, has higher scientific research value and economic worth.Therefore, utilize the dissimilar vegetable seed phosphatide of rapeseed oil residue processing, become the oils industry new growth engines.But present most rapeseed oil residue is not utilized, and rapeseed oil phospholipid wherein is along with the prolongation of storage period, the aggravation of becoming sour, and color burn directly influences the quality of phospholipid prod, so the decolouring of phosphatide is with regard to referred important position.

The extraction process of phosphatide has a lot, and at present organic solvent lixiviation process that adopt utilize the solvability of phosphatide in different solvents that it is separated from oil foot more.Along with the development of isolation technique, many new extracting method have appearred, and most representative is supercritical CO ₂Extraction process.This technology utilize fluid (solvent) near stagnation point with vegetables oil in phosphatide the behavior that balances each other is unusually arranged and transmits performance, thereby and it to the dissolving power of phosphatide with the change of pressure and temperature in quite wide scope change reach the isolating a kind of technology of phosphatide.The advantage of this technology is good product quality, purity height; Shortcoming is exactly that production cost is too high.

Summary of the invention

Purpose of the present invention just is exploitation, utilizes this high value added product of phosphatide, and the method that provides a kind of vegetable seed phosphatide to extract and decolour is carried out deep processing research for the comprehensive utilization of oil foot and offered help.

The present invention includes following steps:

1. heat oil foot, press the centrifugal 10min of 4000r/min, dry under 40～50 ℃ vacuum condition, must soften oil foot;

2. will soften oil foot and place container, be that 12mL/g adds acetone solution by the ratio of mass/volume, suction filtration behind 46～48 ℃ of dissolving 40min, during stirred once the raw phospholipid after obtaining deoiling every 10 minutes; And with the raw phospholipid quality divided by raw materials used quality, obtain extraction yield;

3. it is refining to add ether in raw phospholipid, makes it abundant dissolving, leaves standstill suction filtration behind the 10min, filtrate;

4. filtrate decompression is concentrated, remove and desolvate, get concentrated phosphatide;

5. with concentrated phosphatide at 30 ℃, be 5.85% H with concentration ₂O ₂Decolouring 14.5min must concentrate decolouring phosphatide;

6. will concentrate the decolouring phosphatide by the centrifugal 10min of 8000r/min after, store for future use through 50 ℃ of vacuum-dryings again.

The present invention has following advantage and positively effect

1, method is easy, and production cost is low;

2, extraction yield height, the extraction yield of phosphatide can reach 28.1%;

3, the product proterties is good, and paler colour is a kind of faint yellow paste;

4, be applicable to comprehensive extraction vegetable oil residue phosphatide.

Description of drawings

Fig. 1 is the UV scanning figure of concentrated phosphatide of the present invention;

Fig. 2 is the UV scanning figure of concentrated decolouring phosphatide of the present invention;

Fig. 3 is the UV scanning figure of sigma Yelkin TTS (PC) standard substance;

Fig. 4 is the infrared scan comparison diagram of concentrated decolouring phosphatide of the present invention and sigma Yelkin TTS (PC) standard substance.

Embodiment

Describe in detail below in conjunction with drawings and Examples:

One, relevant step

1,2. about step

Described acetone consumption refers to the ratio of the used acetone volume total amount and the raw materials quality of getting, and the adding method is that insolubles is added acetone repeatedly, stirs, leaves standstill the back suction filtration.The acetone of Jia Ruing is more first, reduces one by one then, adds up to the ratio according to 1: 1.

2,3. about step

Described ether adding method is with to add acetone similar, up to filtrate be substantially colourless till.

3,4. about step

Utilize the Rotary Evaporators concentrating under reduced pressure.

Two, embodiment

Embodiment 1

Get the 5.6g oil foot 45 ℃ of thermoplastics, choose large particulate matter wherein; The centrifugal 10min of 4000r/min removes upper water and neutral oil while hot, and residual moisture in the oil foot is removed in 45 ℃ vacuum-drying.Add its neutral oil of acetone solution again, 48 ℃ of following suction filtrations behind the dissolving 40min, during stir once every 10min, again the upper strata insolubles is placed beaker, continue to add acetone, stir, leave standstill the back suction filtration, repeatedly several times, the insolubles that obtains is the raw phospholipid that deoils.The acetone of Jia Ruing is more first, reduces one by one then, adds up to the ratio according to 1: 1, and total additional proportion is 12mL/g.Obtain the 1.58g raw phospholipid and add ether again, raw phospholipid is fully dissolved, leave standstill suction filtration behind the 10min.Again the upper strata insolubles is placed beaker, the similar acetone of adding method, up to the ether that suction filtration gets off be colourless till.Merge filtrate several times, use the Rotary Evaporators vacuum concentration, obtain concentrated phosphatide.Add concentration again and be 5.85% H ₂O ₂Decolouring, add-on is 0.25mL/0.1g, at 30 ℃ of 14.5min that decolour down.

Extract the result: the concentrated phosphatide extraction yield is 28.1%

Embodiment 2

Get the 5.7g oil foot 45 ℃ of thermoplastics, choose large particulate matter wherein; The centrifugal 10min of 4000r/min removes upper water and neutral oil while hot, and residual moisture in the oil foot is removed in 45 ℃ vacuum-drying.Add its neutral oil of acetone solution again, 30 ℃ of following suction filtrations behind the dissolving 30min, during stir once every 10min, again the upper strata insolubles is placed beaker, continue to add acetone, stir, leave standstill the back suction filtration, repeatedly several times, the insolubles that obtains is the raw phospholipid that deoils.The acetone of Jia Ruing is more first, reduces one by one then, adds up to the ratio according to 1: 1, and total additional proportion is 14mL/g.Obtain the 1.43g raw phospholipid.Add ether again, raw phospholipid is fully dissolved, leave standstill suction filtration behind the 10min.Again the upper strata insolubles is placed beaker, the similar acetone of adding method, up to the ether that suction filtration gets off be colourless till.Merge filtrate several times, use the Rotary Evaporators vacuum concentration, obtain concentrated phosphatide.Add concentration again and be 6% H ₂O ₂Decolouring, add-on is 0.25mL/0.1g, at 20 ℃ of 15min that decolour down.

Extract the result: the concentrated phosphatide extraction yield is 25.08%

Embodiment 3

Get the 4.5g oil foot 45 ℃ of thermoplastics, choose large particulate matter wherein; The centrifugal 10min of 4000r/min removes upper water and neutral oil while hot, and residual moisture in the oil foot is removed in 45 ℃ vacuum-drying.Add its neutral oil of acetone solution again, 45 ℃ of following suction filtrations behind the dissolving 20min, during stir once every 10min, again the upper strata insolubles is placed beaker, continue to add acetone, stir, leave standstill the back suction filtration, repeatedly several times, the insolubles that obtains is the raw phospholipid that deoils.The acetone of Jia Ruing is more first, reduces one by one then, adds up to the ratio according to 1: 1, and total additional proportion is 10mL/g, obtains the 1.03g raw phospholipid.Add ether again, raw phospholipid is fully dissolved, leave standstill suction filtration behind the 10min.Again the upper strata insolubles is placed beaker, the similar acetone of adding method, up to the ether that suction filtration gets off be colourless till.Merge filtrate several times, use the Rotary Evaporators vacuum concentration, obtain concentrated phosphatide.Add concentration again and be 8% H ₂O ₂Decolouring, add-on is 0.25mL/0.1g, at 10 ℃ of 30min that decolour down.

Extract the result: the concentrated phosphatide extraction yield is 22.89%

Three, test result analysis

1, uv-spectrogram analysis

As Fig. 1, the assorted peak of the ultraviolet absorpting spectrum of the concentrated phosphatide that obtains a lot (200～240nm), and can know also that from the color and luster (tawny) of concentrated phosphatide foreign matter content wherein is very high, especially there is tangible absorption peak at 280～300nm place, be likely the inhalation effects phosphatide color and luster of this wavelength region, and reach maximum in wavelength 288nm place absorbancy, need further decolouring to handle.

As Fig. 2, after decolouring, tangible absorption peak vanishes in the preceding 280～300nm scope of the decolouring of phosphatide, and the many assorted peak in 200～250nm scope has also lacked many.Before and after decolouring, can know decolorizing effect clearly the contrast of twice UV scanning collection of illustrative plates.

As Fig. 3, the maximum absorption wavelength of Yelkin TTS is 200～210nm, can find out obviously also that from Fig. 2 decolouring phosphatide also has maximum absorption in this wavelength region, illustrate and contain a certain amount of Yelkin TTS in the vegetable seed phosphatide.

2, infared spectrum analysis

As Fig. 4, the absorption peak wave number is 3410cm ^-1About the strong peak located be the stretching vibration of OH, and decolouring phosphatide does not have, and may be because standard substance purity is quite high, suction easily, and the sample proterties is oiliness, is not easy suction is not so the absorption peak under this wave number has Yelkin TTS mark product obviously.Wave number is 2921cm ^-1About the strong peak located be the absorption peak of methyl and methylene radical, 3009cm ^-1And 2853cm ^-1About absorption peak occur simultaneously, show that containing saturated CH contains undersaturated CH, 1740cm again ^-1About the spike located be C=O absorption peak in the aliphatic saturated monocarboxylic acid ester, wave number 1241cm ^-1About the spike located be the stretching vibration of P=O group, wave number is 1090cm ^-1About the flexural vibration located be the absorption peak of P-O-C.Because used just Yelkin TTS standard substance, and the phosphatide after the decolouring not only contains the phosphatide that Yelkin TTS also contains other types such as kephalin, lipositol, so some places of misfitting on collection of illustrative plates, just occurred, but feature is received the peak basically identical, can infer that thus both structures are identical substantially.

Claims (1)

1, the method for a kind of vegetable seed phosphatide extraction and decolouring is characterized in that may further comprise the steps:

1. heat oil foot, press the centrifugal 10min of 4000r/min, dry under 40～50 ℃ vacuum condition, get softening oil;

2. softening oil being placed container, is that 12mL/g adds acetone solution by the ratio of mass/volume, suction filtration behind 46～48 ℃ of dissolving 40min, during stirred once the raw phospholipid after obtaining deoiling every 10 minutes; And with the raw phospholipid quality divided by raw materials used quality, obtain extraction yield;

3. it is refining to add ether in raw phospholipid, makes it abundant dissolving, leaves standstill suction filtration behind the 10min, filtrate;

4. filtrate decompression is concentrated, remove and desolvate, get concentrated phosphatide;

5. with concentrated phosphatide under 30 ℃, be 5.85% H with concentration ₂O ₂Decolouring 14.5min must concentrate decolouring phosphatide;

6. will concentrate the decolouring phosphatide by the centrifugal 10min of 8000r/min after, store for future use through 50 ℃ of vacuum-dryings again.

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