CN101289461A - Process for extracting phytic acid from virus-free waste liquid of rapeseed extraction - Google Patents

Process for extracting phytic acid from virus-free waste liquid of rapeseed extraction Download PDF

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Publication number
CN101289461A
CN101289461A CNA2008100697922A CN200810069792A CN101289461A CN 101289461 A CN101289461 A CN 101289461A CN A2008100697922 A CNA2008100697922 A CN A2008100697922A CN 200810069792 A CN200810069792 A CN 200810069792A CN 101289461 A CN101289461 A CN 101289461A
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Prior art keywords
phytic acid
extraction
volume
feature
minutes
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Inventor
周小华
孙峰
蔡怀德
贺爽
苏霞利
廖妙飞
陈林
金挺
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Sichuan Zhongmu Feed Manufacturing Co Ltd
Chongqing University
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Sichuan Zhongmu Feed Manufacturing Co Ltd
Chongqing University
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Priority to CNA2008100697922A priority Critical patent/CN101289461A/en
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Abstract

The invention relates to an art of extracting phytic acid from rapeseed virus-free waste liquid, which relates to the preparation method of the phytic acid. The invention uses the virus-free waste of rapeseed meal as a raw material, and obtains the finished product by extraction, stripping, electrodialysis and vacuum concentration. The invention also prepares the rapeseed polysaccharide and polyphenol with a high purity during the time of extracting the phytic acid, wherein, the phytic acid is concentrate solution with 60 to 70 percent of purity; the rapeseed polysaccharide is freeze-dried powder with 82 to 88 percent of purity; the rapeseed polyphenol is spraying drying powder with 81 to 86.3 of percent. The product yield rate is high; wherein, the extracting yield rate of the phytic acid is high up to 4.22 to 5.36 percent; the yield rate of the polysaccharide is up to 2.83 to 3.44 percent; the yield rate of the polyphenol is up to 1.35 to 3.65 percent. Meanwhile, the art of extracting phytic acid from rapeseed virus-free waste liquid is simple, saves energy and lowers energy consumption, and reduces the production cost sharply, is consistent with the environmental protection requirement, and is a green technology of comprehensive utilization. The products prepared by using the art of the invention can be widely used as the functional additives of feed, foods, health products and cosmetics, etc.

Description

The technology of extraction phytic acid from detoxified waste liquor of rapeseed extraction
One, technical field
The invention belongs to the functional additive preparing technical field, particularly the preparation method of phytic acid.
Two, background technology
Phytic acid mainly is present in cereal seed, beans, rice bran and the vegetable oil material with the form of calcium magnesium salts, and the phytic acid ca magnesium salts is commonly called as luxuriant and rich with fragrance fourth, and general content is lower, and content is all higher in defatted rice bran and the rapeseed meal.Because phytic acid has fresh-keeping foodstuff, delay Oxidation of Fat and Oils and nourishing, reinforcement, promotion human body metabolism etc., is widely used in food, medical treatment, daily-use chemical industry, metallurgy and fields such as metal processing, chemistry, oil and light and textile industries.That the vegetable seed polysaccharide has is anti-oxidant, suppress the function of tumour and lowering blood glucose, and polyphenol from rapeseed also has the Green Tea Extract oxidation, suppress effect such as tumour, is the healthcare products function raw material that market outlook are arranged very much.Therefore, preparation high purity, high-quality phytic acid and polysaccharide and polyphenol have very important significance.
The Semen Brassicae campestris of one of main oil crops of China, annual production account for 38.3% of world's annual production up to 5,000,000 tons.Rape seed oil is one of main edible oil of China, when processing rape seed oil under the modern industry condition, can produce 50～55% rapeseed meal.In rapeseed meal, contain protein up to 35～40%.Rapeseed meal after the detoxification is natural quality plant protein resource, can be widely used as fodder additives, raw materials of soy sauce etc.In the detoxified waste liquor of rapeseed meal, contain the glucosinolate that is equivalent to rapeseed meal mass percent 5.6～9.7%, 4.4～5.6% phytic acid, the polysaccharide of 3.01-3.61% and 1.5～3.5% polyphenol, do not discharge if be not used, not only waste resource, also pollute the environment.Therefore development prepares phytic acid from detoxified waste liquor of rapeseed extraction, also prepares the technology of polysaccharide and polyphenol simultaneously, plays a very important role.
The existing method for preparing phytic acid, as " process study of phytic acid and the application thereof " literary composition in " foodstuffs industry " 2000 the 3rd phase foodstuff additive, the auxiliary material special issue/foodstuff additive, disclosed Preparation of Phytic Acid technology is to be raw material with the defatted rice bran, soak with diluted acid earlier, the back neutralizes with liming and sodium hydroxide, use the dilute sulphuric acid acidifying again, obtain finished product with the resin cation exchange metal ion at last.The main drawback of this method is with precipitating with the generation phytic acid ca in liming and the sodium hydroxide, separate a large amount of alkaline waste waters of back generation, be unfavorable for preparing wherein polyphenol and polysaccharide, discharging the meeting serious environment pollution; The phytic acid ca that precipitation obtains is carried out ion-exchange again with dilute sulphuric acid acidifying dissolving, and the ion exchange resin behind the exchange phytic acid needs to use the acid solution wash-out earlier, uses the remaining acid of deionized water wash again, so produce a large amount of acid wash-out waste liquids; Contain sulfate ion in the product, can influence its quality and purposes.
Three, summary of the invention
The objective of the invention is fault at existing preparation phytic acid method, a kind of technology that extracts phytic acid from detoxified waste liquor of rapeseed extraction is provided, it is simple to have technology, mild condition, can prepare vegetable seed polysaccharide and polyphenol simultaneously, product recovery rate and purity are all high, and waste water produces few, and after treatment can reuse etc. characteristics.
Mechanism of the present invention is: in rapeseed meal, phytic acid exists with the form of phytic acid ca magnesium salts (luxuriant and rich with fragrance fourth), and luxuriant and rich with fragrance fourth can be used strong acid, and for example therefore dissolving with hydrochloric acid, handles rapeseed meal with diluted hydrochloric acid aqueous solution, can obtain to contain the waste liquid of phytic acid.In addition, polyphenol and polysaccharide also have certain solubility in diluted hydrochloric acid aqueous solution, so contain in the waste liquid of phytic acid a small amount of polyphenol and polysaccharide are arranged also.Polyphenol from rapeseed is the polycondensate of flavonoid compound, is dissolvable in water in methyl alcohol, ethanol or the acetone isopolarity organic solvent, therefore extracts with certain density aqueous ethanolic solution, and polyphenol is dissolved in wherein.Reclaim ethanol then, promptly obtain the polyphenol concentrated solution, obtain the polyphenol from rapeseed powder through spraying drying again.Contain phytic acid, polyphenol, vegetable seed polysaccharide and small molecules inorganic salt in the waste liquid that the diluted hydrochloric acid aqueous solution detoxification produces.Polysaccharide molecular weight is tens thousand of～hundreds thousand of dalton (Da), and the phytic acid molecular weight only is over thousands of dalton, and the polyphenol molecular weight also only has about 2000 dalton.Ultrafilter is based on the separation machinery of molecular weight size separation material, and by ultrafilter, small molecules such as phytic acid, polyphenol, inorganic salt are all through ultra-filtration membrane with detoxified waste liquor, and polysaccharide then is trapped and concentrates.By ultrafiltration repeatedly, can make vegetable seed polysaccharide concentrated solution, pass through spraying drying again, obtain vegetable seed polysaccharide powder; In seeing through the filtered solution of ultra-filtration membrane, the polyphenol neutral can be adsorbed resin absorption, thereby separates with phytic acid; Load has the polymeric adsorbent of polyphenol weakly alkaline aqueous ethanolic solution wash-out, and ethanol is reclaimed in redistillation, obtains the polyphenol concentrated solution, through spraying drying, obtains the polyphenol from rapeseed powder.Phytic acid is electronegative, can generate salt with positively charged ammonium kind of extractants, thereby is extracted the agent extraction, and with other separating substances.Load has the ammonium kind of extractants of phytic acid to strip with dilute alkaline aqueous solution, but promptly obtains the ammonium kind of extractants of the phytate aqueous solution and regenerated reuse.Electrodialyzer is based on ion-exchange membrane and the device of ionophoresis technical point from different charged species undergoes, and under electric field action, charged ion is by the electrode swimming of ion-exchange membrane to opposite charges, thereby acquisition separates.Phytate is made up of the phytic acid of negative charge and the inorganic cation of positive charge, under electric field action, and the swimming of phytic acid anode, inorganic cation separates with phytic acid then to the negative electrode swimming, is discharged at last.Have the inorganic cation and the chlorions such as calcium, magnesium of higher concentration in the raffinate of extraction behind the phytic acid, by electrodialysis unit, positively charged ion moves to negative electrode with this waste water, and the negatively charged ion anode moves, then obtain desalination fresh water, but reuse detoxification once more.The dense hydration of anode and negative electrode and back discharging.
The object of the present invention is achieved like this: a kind of from the detoxified waste liquor of rapeseed meal the technology of extraction phytic acid, be raw material with the detoxification liquid of rapeseed meal, successively through extraction, reextraction, electrodialysis, vacuum concentration and spraying drying and finished product.Concrete processing step is as follows:
(1) extraction
1. prepare extraction liquid
With three sufferings/certain herbaceous plants with big flowers base tertiary amine (N 235) extraction agent adds in the sulfonated kerosene diluent, mixes, and just makes N 235Volumetric molar concentration is the N of 0.1～0.5mol/L 235Extraction liquid.
2. extraction
(1)-1. the step finish after, earlier rapeseed meal detoxification liquid raw material is pumped in the extractor, according to detoxified waste liquor: the volume ratio of the extraction liquid of (1)-1. step preparation is 1: 3～6 ratio, again extraction liquid is pumped in the extractor, under agitation condition, feeding temperature to the extractor interlayer is 20～40 ℃ hot water, after insulation is carried out extracting 10～20 minutes the first time, left standstill 10～25 minutes, and collected extraction liquid that upper strata extraction has phytic acid and the raffinate behind lower floor's extraction phytic acid respectively.Then, pump into the raffinate behind lower floor's extraction phytic acid of collecting in the extractor again, again according to the raffinate behind the extraction phytic acid: the volume ratio of the extraction liquid of (1)-1. step preparation is 1: 3～6 ratio, again extraction liquid is pumped in the extractor, under agitation condition, be 20～40 ℃ hot water again to extractor interlayer feeding temperature, after insulation is carried out extracting 10～20 minutes the second time again, left standstill 10～25 minutes, collect extraction liquid that upper strata extraction has phytic acid and the raffinate behind lower floor's extraction phytic acid more respectively, so repeat 1-3 time.
(2) strip
1. prepare anti-stripping agent
(1) step added sodium hydroxide in the distilled water after finishing, and stirring and dissolving also mixes, and just makes the anti-stripping agent that the sodium hydroxide mass percent is 0.2-0.5%.
2. strip
(2)-1. the step finish after, each time upper strata extraction that (1)-2. step was collected earlier has the extraction liquid of phytic acid to pump in the reextraction still, the extraction liquid that phytic acid is arranged according to extraction: the volume ratio of the anti-stripping agent of (2)-1. step preparation is 1: 1.5～3 ratio, anti-stripping agent is pumped in the reextraction still again, under agitation condition, normal temperature carried out stripping the first time 5～15 minutes, after leaving standstill 20～30 minutes, collecting lower floor's reextraction respectively has the anti-stripping agent of phytic acid and the raffinate behind the upper strata reextraction phytic acid.Once more the raffinate behind the upper strata reextraction phytic acid of collecting is pumped into and send out in the extraction kettle, according to the raffinate behind the reextraction phytic acid: the volume ratio of the anti-stripping agent of (2)-1. step preparation is 1: 1.5～3 ratio, anti-stripping agent is pumped in the reextraction still once more, once more under agitation condition, normal temperature carried out stripping the second time 5～15 minutes, after leaving standstill 20～30 minutes, collecting lower floor's reextraction respectively has the anti-stripping agent of phytic acid and the raffinate behind the upper strata reextraction phytic acid.
(3) electrodialysis anti-stripping agent
(2) step finish after, there is lower floor's anti-stripping agent of phytic acid to merge (2)-2. reextraction that goes on foot twice collection, pump in the electrodialyzer, regulating voltage is 30-60V, and intake pressure is 0.02-0.06MPa, carry out electrodialysis after, collect anode respectively and be enriched with the dense water of phytic acid and dense water and the desalination fresh water that negative electrode is enriched with sodium salt, but the detoxification dilute hydrochloric acid liquid is prepared in the reuse of desalination fresh water, is enriched with the concentrated water discharge of sodium salt.
(4) preparation phytic acid concentrated solution
(3) step finish after, the anode of (3) step collection is enriched with the dense water of phytic acid, pump in the vacuum decker, in vacuum tightness is that 0.05～0.08Mpa, temperature are under 70～90 ℃ of conditions, carry out vacuum concentration, just prepare the phytic acid mass percent and be 60～70% phytic acid concentrated solution, the total recovery rate of phytic acid is 4.22%～5.36% of a rapeseed meal mass percent.
(5) preparation vegetable seed polysaccharide
1. ultrafiltration
(4) step finish after, lower floor's raffinate with behind the extraction phytic acid of (1)-2. step collection pumps in the ultrafilter that molecular weight cut-off is 1～50,000 Da, is under the condition of 0.05～0.25Mpa at ultrafiltration pressure, carry out the normal temperature ultrafiltration, small-molecule substance is filtered and macromolecular glycocalix is held back.When the trapped fluid volume be reduced to the lower floor raffinate original volume of extraction behind the phytic acid 1/4～1/10 the time, replenish distilled water to original volume, so repeatedly ultrafiltration to trapped fluid during no phytic acid till, collect trapped fluid and filtered solution more respectively, trapped fluid is vegetable seed polysaccharide ultrafiltration and concentration liquid, and filtered solution is the stock liquid that extracts polyphenol.
2. lyophilize
(5)-1. the step finish after, with (5)-1. step collect contain vegetable seed polysaccharide ultrafiltration and concentration trapped fluid, place freeze drier, in vacuum tightness is that 25～55pa, temperature are under-50～-60 ℃ of conditions, carried out lyophilize 24～30 hours, just prepare the total reducing sugar mass percent and be 82～88% light brown vegetable seed polysaccharide frozen dried powder, the polysaccharide recovery rate is the 2.83-3.44% of rapeseed meal mass percent.
(6) preparation polyphenol from rapeseed
1. absorption
(5) step finish after, according to HZ-803 or HPD-450 polymeric adsorbent volume: the ratio of the filtered solution volume that contains polyphenol from rapeseed that (5)-1. step collected is 1: the ratio of 5-10, filtered solution is pumped into HZ-803 or HPD-450 adsorption resin column, and the control filtered solution cross column flow rate be the polymeric adsorbent volume 3-6 doubly, adsorbing polyphenols.Collected post liquid, so that carry out desalting treatment.
2. prepare elutriant
(6)-1. finish after, in dense ethanol, adding earlier distilled water diluting, to become the ethanol concentration expressed in percentage by volume be the ethanolic soln of 70-85%, add sodium hydroxide solution again, the pH value of regulating mixing solutions is 8.0-9.0, just prepares the polyphenol elutriant that wash-out is adsorbed resin absorption, and is airtight standby.
3. spraying drying
(6)-1. the step finish after, use the distilled water of 1 times of polymeric adsorbent volume earlier, the adsorption resin column of washing (6)-1. step absorption polyphenol from rapeseed, again according to the polymeric adsorbent volume: the effluent volume ratio of (6)-2. step preparation is 1: the ratio of 3-6, and the control elution flow rate be the resin volume 0.5-1.5 doubly, the polyphenol that wash-out is adsorbed.Collecting the post elutriant, and pumped in the vacuum decker, is that 0.05～0.08Mpa, temperature are under 70～90 ℃ of conditions in vacuum tightness, carries out vacuum concentration, just obtains the polyphenol from rapeseed concentrated solution.Again with the polyphenol from rapeseed concentrated solution that obtains, pump into small-sized centrifugal spray dryer, in inlet temperature is 120-135 ℃, air outlet temperature is to carry out spraying drying under 85-95 ℃ the condition, just obtaining the polyphenol mass percent is the polyphenol from rapeseed powder of 81-86.3%, and the polyphenol from rapeseed recovery rate is the 1.35-3.65% of rapeseed meal mass percent.
(7) reclaim desalination fresh water
After (6) step finished, with (6)-1. step collect cross post liquid, pump into electrodialyzer, regulating voltage is that 30-60V, intake pressure are 0.05-0.15MPa, carries out electrodialytic desalting, collects desalination fresh water, can be used to prepare the detoxification dilute hydrochloric acid liquid once more.Abandon dense water of anode and the dense water of negative electrode.
After the present invention adopts technique scheme, mainly contain following effect:
1. can prepare multiple product simultaneously, and the quality product height
Technology of the present invention is in extraction phytic acid from rapeseed meal, can also prepare vegetable seed polysaccharide and polyphenol from rapeseed totally three kinds of products, and three kinds of product purity height, phytic acid is the concentrated solution of 60-70%, the vegetable seed polysaccharide is the 82-88% lyophilized powder, and polyphenol from rapeseed is the spray-drying powder of 81-86.3%.
2. product recovery rate height
The 4.4-5.6% that is equivalent to the rapeseed meal mass percent as the content of phytic acid in detoxified waste liquor of rapeseed extraction, polyphenol is 1.5～3.5%, polysaccharide is 3.06-3.62%, by technology of the present invention, the phytic acid recovery rate is up to 4.22-5.36%, polyphenol recovery rate 1.35-3.65%, the polysaccharide recovery rate is 2.83-3.44%.
3. waste liquid comprehensive utilization, discharge of wastewater is few
Technology of the present invention is to prepare phytic acid from the detoxified waste liquor of rapeseed meal, in the process of preparation phytic acid, making full use of its waste liquid again prepares vegetable seed polysaccharide and polyphenol from rapeseed and reclaims ethanol and desalination fresh water utilizes again, discharged waste water seldom, only for not preparing 1/10 of phytic acid and polysaccharide and polyphenol technology, this not only makes full use of the waste liquid resource, and also compliance with environmental protection requirements is the friendly process of comprehensive utilization.
4. technology is simple, and energy-saving and cost-reducing, production cost is low
Process using solvent extraction of the present invention, ultra-filtration membrane and electrodialytic membranes separate, and simple advanced again production technique such as vacuum concentration has significantly reduced steam consumption quantity, thereby has realized the energy-saving and cost-reducing of production, has improved production environment, has significantly reduced production cost.
Adopt the product of prepared of the present invention, but feed, food, healthcare products, makeup functional additive are made in widespread use, sequestrant etc. is electroplated in industry.
Four, embodiment
Below in conjunction with embodiment, further specify the present invention.
Embodiment 1
A kind of from detoxified waste liquor of rapeseed extraction the concrete grammar step of technology of extraction phytic acid as follows:
(1) extraction
1. prepare extraction liquid
With three sufferings/certain herbaceous plants with big flowers base tertiary amine (N 235) extraction agent joins in the sulfonated kerosene diluent, stirs, and just makes N 235Volumetric molar concentration is the N of 0.1mol/L 235Extraction liquid.
2. extraction
(1)-1. the step finish after, detoxification liquid raw material with rapeseed meal pumps in the extractor earlier, according to detoxified waste liquor: the volume ratio of the extraction liquid of (1)-1. step preparation is 1: 3 a ratio, again extraction liquid is pumped in the extractor, under agitation condition, feeding temperature to the extractor interlayer is 20 ℃ hot water, after insulation is carried out extracting 20 minutes the first time, left standstill 25 minutes, and collected extraction liquid that upper strata extraction has phytic acid and the raffinate behind lower floor's extraction phytic acid respectively.Then, pump into the raffinate behind lower floor's extraction phytic acid of collecting in the extractor again, again according to the raffinate behind the extraction phytic acid: the volume ratio of the extraction liquid of (1)-1. step preparation is 1: 3 a ratio, again extraction liquid is pumped in the extractor, under agitation condition, be 20 ℃ hot water again to extractor interlayer feeding temperature, after insulation is carried out extracting 20 minutes the second time again, left standstill 25 minutes, collect extraction liquid that upper strata extraction has phytic acid and the raffinate behind lower floor's extraction phytic acid more respectively, so repeat 3 times.
(2) strip
1. prepare anti-stripping agent
(1) step added sodium hydroxide in the distilled water after finishing, and stirring and dissolving also mixes, and just made the sodium hydroxide mass percent and be 0.2% anti-stripping agent.
2. strip
(2)-1. the step finish after, each time upper strata extraction that (1)-2. step was collected earlier has the extraction liquid of phytic acid to pump in the reextraction still, the extraction liquid that phytic acid is arranged according to extraction: the volume ratio of the anti-stripping agent of (2)-1. step preparation is 1: 1.5 a ratio, anti-stripping agent is pumped in the reextraction still again, under agitation condition, normal temperature carried out stripping the first time 5 minutes, leave standstill 20 minutes after, collect lower floor respectively and strip the anti-stripping agent of phytic acid and the raffinate behind the upper strata reextraction phytic acid are arranged.Once more the raffinate behind the upper strata reextraction phytic acid of collecting is pumped into and send out in the extraction kettle, according to the raffinate behind the reextraction phytic acid: the volume ratio of the anti-stripping agent of (2)-1. step preparation is 1: 1.5 a ratio, anti-stripping agent is pumped in the reextraction still once more, once more under agitation condition, normal temperature carried out stripping the second time 5 minutes, after leaving standstill 20 minutes, collecting lower floor's reextraction respectively has the anti-stripping agent of phytic acid and the raffinate behind the upper strata reextraction phytic acid.
(3) electrodialysis anti-stripping agent
(2) step finish after, there is lower floor's anti-stripping agent of phytic acid to merge (2)-2. reextraction that goes on foot twice collection, pump in the electrodialyzer, regulating voltage is 30V, and intake pressure is 0.02MPa, carry out electrodialysis after, collect anode respectively and be enriched with the dense water of phytic acid and dense water and the desalination fresh water that negative electrode is enriched with sodium salt, but the detoxification dilute hydrochloric acid liquid is prepared in the reuse of desalination fresh water, is enriched with the concentrated water discharge of sodium salt.
(4) preparation phytic acid concentrated solution
(3) step finish after, the anode of (3) step collection is enriched with the dense water of phytic acid, pump in the vacuum decker, in vacuum tightness is that 0.05Mpa, temperature are under 70 ℃ of conditions, carry out vacuum concentration, just prepare the phytic acid mass percent and be 60% phytic acid concentrated solution, the total recovery rate of phytic acid is 5.36% of a rapeseed meal quality.
(5) preparation vegetable seed polysaccharide
1. ultrafiltration
(4) step finish after, lower floor's raffinate with behind the extraction phytic acid of (1)-2. step collection pumps in the ultrafilter that molecular weight cut-off is 10,000 Da, is under the condition of 0.05Mpa at ultrafiltration pressure, carry out the normal temperature ultrafiltration, small-molecule substance is filtered and macromolecular glycocalix is held back.When the trapped fluid volume be reduced to the lower floor raffinate original volume of extraction behind the phytic acid 1/4 the time, replenish distilled water to original volume, proceed ultrafiltration to trapped fluid during no phytic acid till, collect trapped fluid and filtered solution respectively, trapped fluid is vegetable seed polysaccharide ultrafiltration and concentration liquid, and filtered solution is the stock liquid that extracts polyphenol.
2. lyophilize
(5)-1. the step finish after, with (5)-1. step collect contain vegetable seed polysaccharide ultrafiltration and concentration trapped fluid, place freeze drier, in vacuum tightness is that 25pa, temperature are under-50 ℃ of conditions, carried out lyophilize 30 hours, just prepare the total reducing sugar mass percent and be 82% light brown vegetable seed polysaccharide frozen dried powder, the total recovery rate of vegetable seed polysaccharide is 2.83% of a rapeseed meal mass percent.
(6) preparation polyphenol from rapeseed
1. absorption
(5) step finish after, according to HZ-803 polymeric adsorbent volume: the ratio of the filtered solution volume that contains polyphenol from rapeseed that (5)-1. step collected is 1: 5 a ratio, filtered solution is pumped into the HZ-803 adsorption resin column, and the column flow rate of crossing of control filtered solution is 3 times of polymeric adsorbent volume, adsorbing polyphenols.Collected post liquid, so that carry out desalting treatment.
2. prepare elutriant
(6)-1. finish after, in dense ethanol, adding earlier distilled water diluting, to become the ethanol concentration expressed in percentage by volume be 70% ethanolic soln, add the sodium hydroxide mass percentage concentration again and be 1% dilute alkaline soln, the pH value of regulating mixing solutions is 8.0, just prepare the polyphenol elutriant that wash-out is adsorbed resin absorption, airtight standby.
3. spraying drying
(6)-1. the step finish after, use the distilled water of 1 times of polymeric adsorbent volume earlier, the adsorption resin column of washing (6)-1. step absorption polyphenol from rapeseed, again according to the polymeric adsorbent volume: the effluent volume ratio of (6)-2. step preparation is 1: 3 a ratio, and the control elution flow rate is 0.5 times of resin volume, the polyphenol that wash-out is adsorbed.Collecting the post elutriant, and pumped in the vacuum decker, is that 0.05Mpa, temperature are under 70 ℃ of conditions in vacuum tightness, carries out vacuum concentration, just obtains the polyphenol from rapeseed concentrated solution.With the polyphenol from rapeseed concentrated solution that obtains, pump into small-sized centrifugal spray dryer, in inlet temperature is 120 ℃, air outlet temperature is to carry out spraying drying under 85 ℃ the condition, just obtain the polyphenol mass percent and be 81% polyphenol from rapeseed powder, the polyphenol from rapeseed recovery rate is 3.65% of a rapeseed meal mass percent.
(7) reclaim desalination fresh water
After (6) step finished, with (6)-1. step collect cross post liquid, pump into electrodialyzer, regulating voltage is that 30V, intake pressure are 0.05MPa, carries out electrodialytic desalting, collects desalination fresh water, can be used to prepare the detoxification dilute hydrochloric acid liquid once more.Abandon dense water of anode and the dense water of negative electrode.
Embodiment 2
A kind of from detoxified waste liquor of rapeseed extraction the concrete grammar step of the technology of extraction phytic acid and polysaccharide and polyphenol as follows:
(1) extraction
1. prepare extraction liquid
With embodiment 1, feature is: make N 235Volumetric molar concentration is the N of 0.25mol/L 235Extraction liquid.
2. extraction
With embodiment 1, feature is: detoxified waste liquor: the volume ratio of the extraction liquid of (1)-1. step preparation is 1: 4, and feeding temperature to the extractor interlayer is 30 ℃ hot water, after insulation is carried out extracting 15 minutes the first time, leaves standstill 15 minutes; Again by the raffinate behind the extraction phytic acid: the volume ratio of the extraction liquid of (1)-1. step preparation is 1: 4, is 30 ℃ hot water again to extractor interlayer feeding temperature, after insulation is carried out extracting 15 minutes the second time again, leaves standstill 15 minutes; So repeat 2 times.
(2) strip
1. prepare anti-stripping agent
With embodiment 1, feature is: make the sodium hydroxide mass percent and be 0.3% anti-stripping agent.
2. strip
With embodiment 1, feature is: extraction has the extraction liquid of phytic acid: the volume ratio of the anti-stripping agent of (2)-1. step preparation is 1: 2, and normal temperature carried out stripping the first time 10 minutes, left standstill 25 minutes; According to the raffinate behind the reextraction phytic acid: the volume ratio of the anti-stripping agent of (2)-1. step preparation is 1: 2, and normal temperature carried out stripping the second time 10 minutes, left standstill 25 minutes.
(3) electrodialysis anti-stripping agent
With embodiment 1, feature is: regulating voltage is that 40V, intake pressure are 0.04MPa.
(4) preparation phytic acid concentrated solution
With embodiment 1, feature is: vacuum tightness is that 0.06Mpa, temperature are 80 ℃; Prepare the phytic acid mass percent and be 65% phytic acid concentrated solution, the total recovery rate of phytic acid is 4.75% of a rapeseed meal mass percent.
(5) preparation vegetable seed polysaccharide
1. ultrafiltration
With embodiment 1, feature is: pump into the ultrafilter that molecular weight cut-off is 30,000 Da, ultrafiltration pressure is 0.15Mpa; The trapped fluid volume is reduced to 1/6 of the lower floor raffinate original volume of extraction behind the phytic acid;
2. lyophilize
With embodiment 1, feature is: in vacuum tightness is that 35pa, temperature are under-55 ℃ of conditions, carried out lyophilize 26 hours, and just prepared the total reducing sugar mass percent and be 86% light brown vegetable seed polysaccharide frozen dried powder, the polysaccharide recovery rate is 3.18% of a rapeseed meal mass percent.
(6) preparation polyphenol from rapeseed
1. absorption
With embodiment 1, feature is: HZ-803 polymeric adsorbent volume: the filtered solution volume ratio that contains polyphenol that (5)-1. step collected is 1: 8, and the column flow rate excessively of filtered solution is 5 times of polymeric adsorbent volume.
2. prepare elutriant
With embodiment 1, feature is: adding distilled water diluting, to become the ethanol concentration expressed in percentage by volume be 80% ethanolic soln, and adding sodium hydroxide solution again, to regulate the pH value of mixing solutions be 8.5.
3. spraying drying
With embodiment 1, feature is: the polymeric adsorbent volume: the effluent volume ratio of (6)-2. step preparation is 1: 4, and the control elution flow rate is 1.0 times of resin volume; Vacuum tightness is that 0.06Mpa, temperature are to carry out vacuum concentration under 80 ℃, in inlet temperature is 130 ℃, air outlet temperature is to carry out spraying drying under 90 ℃ the condition, obtains the polyphenol mass percent and be 84.5% polyphenol from rapeseed powder, and the polyphenol from rapeseed recovery rate is 2.75% of a rapeseed meal mass percent.
(7) reclaim desalination fresh water
With embodiment 1, feature is: regulating voltage is 40V, and intake pressure is 0.10MPa.
Embodiment 3
A kind of from detoxified waste liquor of rapeseed extraction the concrete grammar step of the technology of extraction phytic acid and polysaccharide and polyphenol as follows:
(1) extraction
1. prepare extraction liquid
With embodiment 1, feature is: make N 235Volumetric molar concentration is the N of 0.5mol/L 235Extraction liquid.
2. extraction
With embodiment 1, feature is: detoxified waste liquor: the volume ratio of the extraction liquid of (1)-1. step preparation is 1: 6, and feeding temperature to the extractor interlayer is 40 ℃ hot water, after insulation is carried out extracting 10 minutes the first time, leaves standstill 10 minutes; Again according to the raffinate behind the extraction phytic acid: the volume ratio of the extraction liquid of (1)-1. step preparation is 1: 6, is 40 ℃ hot water again to extractor interlayer feeding temperature, after insulation is carried out extracting 10 minutes the second time again, leaves standstill 10 minutes; So repeat 1 time.
(2) strip
1. prepare anti-stripping agent
With embodiment 1, feature is: make the sodium hydroxide mass percent and be 0.5% anti-stripping agent.
2. strip
With embodiment 1, feature is: the extraction liquid that phytic acid is arranged according to extraction: the volume ratio of the anti-stripping agent of (2)-1. step preparation is 1: 3, and normal temperature carried out stripping the first time 15 minutes, left standstill 30 minutes; Again according to the raffinate behind the reextraction phytic acid: the volume ratio of the anti-stripping agent of (2)-1. step preparation is 1: 3 a ratio, and normal temperature carried out stripping the second time 15 minutes, left standstill 30 minutes.
(3) electrodialysis anti-stripping agent
With embodiment 1, feature is: regulating voltage is that 60V, intake pressure are 0.06MPa.
(4) preparation phytic acid concentrated solution
With embodiment 1, feature is: vacuum tightness is that 0.08Mpa, temperature are 90 ℃, prepares the phytic acid mass percent and be 70% phytic acid concentrated solution, and the total recovery rate of phytic acid is 4.22% of a rapeseed meal mass percent.
(5) preparation vegetable seed polysaccharide
1. ultrafiltration
With embodiment 1, feature is: pump into the ultrafilter that molecular weight cut-off is 50,000 Da, ultrafiltration pressure is 0.25Mpa; The trapped fluid volume is reduced to 1/10 of the lower floor raffinate original volume of extraction behind the phytic acid;
2. lyophilize
With embodiment 1, feature is: in vacuum tightness is that 55pa, temperature are under-60 ℃ of conditions, carried out lyophilize 24 hours, and just prepared the total reducing sugar mass percent and be 88% light brown vegetable seed polysaccharide frozen dried powder, the polysaccharide recovery rate is 2.83% of a rapeseed meal mass percent.
(6) preparation polyphenol from rapeseed
1. absorption
With embodiment 1, feature is: HPD-450 polymeric adsorbent volume: the filtered solution volume ratio that contains polyphenol that (5)-1. step collected is 1: 10, and the column flow rate excessively of filtered solution is 6 times of polymeric adsorbent volume.
2. prepare elutriant
With embodiment 1, feature is: adding distilled water diluting, to become the ethanol concentration expressed in percentage by volume be 85% ethanolic soln, and adding sodium hydroxide solution again, to regulate the pH value of mixing solutions be 9.0.
3. spraying drying
With embodiment 1, feature is: according to the polymeric adsorbent volume: the effluent volume ratio of (6)-2. step preparation is 1: 6 a ratio, and the control elution flow rate is 1.5 times of resin volume; Vacuum tightness is that 0.08Mpa, temperature are 90 ℃; In inlet temperature is 135 ℃, and air outlet temperature is to carry out spraying drying under 95 ℃ the condition, obtains the polyphenol mass percent and be 86.3% polyphenol from rapeseed powder, and the polyphenol from rapeseed recovery rate is 1.35% of a rapeseed meal mass percent.
(7) reclaim desalination fresh water
With embodiment 1, feature is: regulating voltage is that 60V, intake pressure are 0.15MPa.

Claims (4)

  1. One kind from detoxified waste liquor of rapeseed extraction the extraction phytic acid technology, it is characterized in that concrete processing step is as follows:
    (1) extraction
    1. prepare extraction liquid
    With three sufferings/certain herbaceous plants with big flowers base tertiary amine is N 235Add in the sulfonated kerosene, mix, just make N 235Volumetric molar concentration is the N of 0.1～0.5mol/L 235Extraction liquid;
    2. extraction
    (1)-1. the step finish after, earlier rapeseed meal detoxification liquid raw material is pumped in the extractor, according to detoxified waste liquor: the volume ratio of the extraction liquid of (1)-1. step preparation is 1: 3～6 ratio, again extraction liquid is pumped in the extractor, under agitation condition, feeding temperature to the extractor interlayer is 20～40 ℃ hot water, the insulation extraction is after 10～20 minutes, left standstill 10～25 minutes, collect extraction liquid that upper strata extraction has phytic acid and the raffinate behind lower floor's extraction phytic acid respectively, pump into the raffinate behind lower floor's extraction phytic acid of collecting in the extractor more then, again according to the raffinate behind the extraction phytic acid: the volume ratio of the extraction liquid of (1)-1. step preparation is 1: 3～6 ratio, extraction liquid being pumped in the extractor, under agitation condition, is 20～40 ℃ hot water to extractor interlayer feeding temperature more again, the insulation extraction is after 10～20 minutes again, left standstill 10～25 minutes, and collected extraction liquid that upper strata extraction has phytic acid and the raffinate behind lower floor's extraction phytic acid more respectively, so repeat 1-3 time;
    (2) strip
    1. prepare anti-stripping agent
    (1) step added sodium hydroxide in the distilled water after finishing, and stirring and dissolving also mixes, and just makes the anti-stripping agent that the sodium hydroxide mass percent is 0.2-0.5%;
    2. strip
    (2)-1. the step finish after, each time upper strata extraction that (1)-2. step was collected earlier has the extraction liquid of phytic acid to pump in the reextraction still, the extraction liquid that phytic acid is arranged according to extraction: the volume ratio of the anti-stripping agent of (2)-1. step preparation is 1: 1.5～3 ratio, anti-stripping agent is pumped in the reextraction still again, normal temperature stirs down and stripped 5～15 minutes, after leaving standstill 20～30 minutes, collect lower floor's reextraction respectively the anti-stripping agent of phytic acid and the raffinate behind the upper strata reextraction phytic acid are arranged, once more the raffinate behind the upper strata reextraction phytic acid of collecting is pumped in the reextraction still, according to the raffinate behind the reextraction phytic acid: the volume ratio of the anti-stripping agent of (2)-1. step preparation is 1: 1.5～3 ratio, anti-stripping agent is pumped in the reextraction still once more, stir at normal temperatures once more and stripped 5～15 minutes, after leaving standstill 20～30 minutes, collecting lower floor's reextraction respectively has the anti-stripping agent of phytic acid and the raffinate behind the upper strata reextraction phytic acid;
    (3) electrodialysis anti-stripping agent
    (2) step finish after, there is lower floor's anti-stripping agent of phytic acid to merge (2)-2. reextraction that goes on foot twice collection, pump in the electrodialyzer, regulating voltage is 30-60V, intake pressure is 0.02-0.06MPa, collects anode respectively and is enriched with the dense water of phytic acid and dense water and the desalination fresh water that negative electrode is enriched with sodium salt;
    (4) preparation phytic acid concentrated solution
    (3) step finish after, the anode of (3) step collection is enriched with the dense water of phytic acid, pumping in the vacuum decker, is that 0.05～0.08Mpa, temperature are under 70～90 ℃ of conditions in vacuum tightness, just prepares the phytic acid mass percent and be 60～70% phytic acid concentrated solution;
    (5) preparation vegetable seed polysaccharide
    1. ultrafiltration
    (4) step finish after, with the lower floor's raffinate behind the extraction phytic acid of (1)-2. step collection, pump in the ultrafilter that molecular weight cut-off is 1～50,000 Da, at ultrafiltration pressure is to carry out ultrafiltration under 0.05～0.25Mpa, when the trapped fluid volume be reduced to the lower floor raffinate original volume of extraction behind the phytic acid 1/4～1/10 the time, replenish distilled water to original volume, so repeatedly to trapped fluid during no phytic acid till, collect trapped fluid and filtered solution more respectively;
    2. lyophilize
    (5)-1. the step finish after, with (5)-1. step collect contain vegetable seed polysaccharide ultrafiltration and concentration trapped fluid, place freeze drier, in vacuum tightness is that 25～55pa, temperature are under-50～-60 ℃ of conditions and carried out lyophilize 24～30 hours, just prepares the total reducing sugar mass percent and be 82～88% light brown vegetable seed polysaccharide frozen dried powder;
    (6) preparation polyphenol from rapeseed
    1. absorption
    (5) step finish after, according to HZ-803 or HPD-450 polymeric adsorbent volume: the ratio of the filtered solution volume that contains polyphenol from rapeseed that (5)-1. step collected is 1: the ratio of 5-10, filtered solution is pumped into HZ-803 or HPD-450 adsorption resin column, and the control filtered solution cross column flow rate be the polymeric adsorbent volume 3-6 doubly, collected post liquid;
    2. prepare elutriant
    (6)-1. finish after, in dense ethanol, adding earlier distilled water diluting, to become the ethanol concentration expressed in percentage by volume be the ethanolic soln of 70-85%, adds sodium hydroxide solution again, the pH value of regulating mixing solutions is 8.0-9.0;
    3. spraying drying
    (6)-1. the step finish after, use the distilled water of 1 times of polymeric adsorbent volume earlier, the adsorption resin column of washing (6)-1. step absorption polyphenol from rapeseed, again according to the polymeric adsorbent volume: the effluent volume ratio of (6)-2. step preparation is 1: the ratio of 3-6, and the control elution flow rate is that the 0.5-1.5 of resin volume doubly crosses post, collected the post elutriant, pump in the vacuum decker, in vacuum tightness is 0.05～0.08Mpa, temperature is under 70～90 ℃ of conditions, carrying out vacuum concentration is the concentrated solution that contains polyphenol from rapeseed, again with the polyphenol from rapeseed concentrated solution, pump into small-sized centrifugal spray dryer, in inlet temperature is 120～135 ℃, and air outlet temperature is that spraying drying is the polyphenol from rapeseed powder of 81-86.3% for the polyphenol mass percent under 85-95 ℃ the condition;
    (7) reclaim desalination fresh water
    After (6) step finished, with (6)-1. step collect cross post liquid, pump into electrodialyzer and carry out electrodialytic desalting, regulating voltage is that 30-60V, intake pressure are 0.05-0.15MPa, collects fresh water.
  2. 2. according to the described technology that from detoxified waste liquor of rapeseed extraction, extracts phytic acid of claim 1, it is characterized in that concrete step is as follows:
    (1) extraction
    1. prepare extraction liquid
    With claim 1, feature is: make N 235Volumetric molar concentration is the N of 0.1mol/L 235Extraction liquid;
    2. extraction
    With claim 1, feature is: detoxified waste liquor: the volume ratio of the extraction liquid of (1)-1. step preparation is 1: 3, feeding temperature to the extractor interlayer is 20 ℃ hot water, the insulation extraction was left standstill 25 minutes after 20 minutes, and again according to the raffinate behind the extraction phytic acid: the volume ratio of the extraction liquid of (1)-1. step preparation is 1: 3, be 20 ℃ hot water again to extractor interlayer feeding temperature, the insulation extraction was left standstill 25 minutes after 20 minutes again, so repeated 3 times;
    (2) strip
    1. prepare anti-stripping agent
    With claim 1, feature is: make the sodium hydroxide mass percent and be 0.2% anti-stripping agent;
    2. strip
    With claim 1, feature is: extraction has the extraction liquid of phytic acid: the volume ratio of the anti-stripping agent of (2)-1. step preparation is 1: 1.5, normal temperature stirs down and stripped 5 minutes, left standstill 20 minutes, raffinate behind the reextraction phytic acid: the volume ratio of the anti-stripping agent of (2)-1. step preparation is 1: 1.5, stir at normal temperatures once more and stripped 5 minutes, left standstill 20 minutes;
    (3) electrodialysis anti-stripping agent
    With claim 1, feature is: regulating voltage is that 30V, intake pressure are 0.02MPa;
    (4) preparation phytic acid concentrated solution
    With claim 1, feature is: in vacuum tightness is that 0.05Mpa, temperature are under 70 ℃ of conditions, just prepares the phytic acid mass percent and be 60% phytic acid concentrated solution;
    (5) preparation vegetable seed polysaccharide
    1. ultrafiltration
    With claim 1, feature is: pump in the ultrafilter that molecular weight cut-off is 10,000 Da, ultrafiltration pressure is 0.05Mpa, 1/4 of the lower floor's raffinate original volume after the trapped fluid volume is reduced to the extraction phytic acid;
    2. lyophilize
    With claim 1, feature is: vacuum tightness is 25pa, temperature for-50 ℃ of conditions under, carried out lyophilize 30 hours, just prepare the total reducing sugar mass percent and be 82% light brown vegetable seed polysaccharide frozen dried powder;
    (6) preparation polyphenol from rapeseed
    1. absorption
    With claim 1, feature is: HZ-803 polymeric adsorbent volume: the ratio of the filtered solution volume that contains polyphenol from rapeseed that (5)-1. step collected is 1: 5, and the column flow rate excessively of filtered solution is 3 times of polymeric adsorbent volume;
    2. prepare elutriant
    With claim 1, feature is: adding distilled water diluting, to become the ethanol concentration expressed in percentage by volume be 70% ethanolic soln, adds sodium hydroxide solution again, and the pH value of regulating mixing solutions is 8.0;
    3. spraying drying
    With claim 1, feature is: the polymeric adsorbent volume: the effluent volume ratio of (6)-2. step preparation is 1: 3, the control elution flow rate is that 0.5 times of resin volume is crossed post, in vacuum tightness is that 0.05Mpa, temperature are under 70 ℃ of conditions, carry out vacuum concentration, in inlet temperature is that 120 ℃, air outlet temperature are that spraying drying is 81% polyphenol from rapeseed powder for the polyphenol mass percent under 85 ℃ the condition;
    (7) reclaim desalination fresh water
    With claim 1, feature is: regulating voltage is that 30V, intake pressure are 0.05MPa.
  3. 3. according to the described technology that from detoxified waste liquor of rapeseed extraction, extracts phytic acid of claim 1, it is characterized in that concrete step is as follows:
    (1) extraction
    1. prepare extraction liquid
    With claim 1, feature is: make N 235Volumetric molar concentration is the N of 0.25mol/L 235Extraction liquid;
    2. extraction
    With claim 1, feature is: detoxified waste liquor: the volume ratio of the extraction liquid of (1)-1. step preparation is 1: 4, feeding temperature to the extractor interlayer is 30 ℃ hot water, the insulation extraction was left standstill 15 minutes after 15 minutes, and again according to the raffinate behind the extraction phytic acid: the volume ratio of the extraction liquid of (1)-1. step preparation is 1: 4, be 30 ℃ hot water again to extractor interlayer feeding temperature, the insulation extraction was left standstill 15 minutes after 15 minutes again, so repeated 2 times;
    (2) strip
    1. prepare anti-stripping agent
    With claim 1, feature is: just make the sodium hydroxide mass percent and be 0.3% anti-stripping agent;
    2. strip
    With claim 1, feature is: extraction has the extraction liquid of phytic acid: the volume ratio of the anti-stripping agent of (2)-1. step preparation is 1: 2, normal temperature stirs down and stripped 10 minutes, left standstill 25 minutes, according to the raffinate behind the reextraction phytic acid: the volume ratio of the anti-stripping agent of (2)-1. step preparation is 1: 2, stir at normal temperatures once more and stripped 10 minutes, left standstill 25 minutes;
    (3) electrodialysis anti-stripping agent
    With claim 1, feature is: regulating voltage is that 40V, intake pressure are 0.04MPa;
    (4) preparation phytic acid concentrated solution
    With claim 1, feature is: in vacuum tightness is that 0.06Mpa, temperature are to carry out vacuum concentration under 80 ℃ of conditions, just prepares the phytic acid mass percent and be 65% phytic acid concentrated solution;
    (5) preparation vegetable seed polysaccharide
    1. ultrafiltration
    With claim 1, feature is: pump in the ultrafilter that molecular weight cut-off is 30,000 Da, ultrafiltration pressure is 0.15Mpa, and the trapped fluid volume is reduced to 1/6 of the lower floor raffinate original volume of extraction behind the phytic acid;
    2. lyophilize
    With claim 1, feature is: vacuum tightness is 35pa, temperature for-55 ℃ of conditions under, carried out lyophilize 26 hours, just prepare the total reducing sugar mass percent and be 86% light brown vegetable seed polysaccharide frozen dried powder;
    (6) preparation polyphenol from rapeseed
    1. absorption
    With claim 1, feature is: according to HZ-803 polymeric adsorbent volume: the ratio of the filtered solution volume that contains polyphenol from rapeseed that (5)-1. step collected is 1: 8, and the column flow rate of crossing of control filtered solution is 5 times of polymeric adsorbent volume;
    2. prepare elutriant
    With claim 1, feature is: adding distilled water diluting, to become the ethanol concentration expressed in percentage by volume be 80% ethanolic soln, adds sodium hydroxide solution again, and the pH value of regulating mixing solutions is 8.5;
    3. spraying drying
    With claim 1, feature is: the polymeric adsorbent volume: the effluent volume ratio of (6)-2. step preparation is 1: 4, the control elution flow rate is that 1.0 times of resin volume are crossed post, in vacuum tightness is that 0.06Mpa, temperature are to carry out vacuum concentration under 80 ℃ of conditions, is that 130 ℃, air outlet temperature are that to carry out spraying drying be 84.5% polyphenol from rapeseed powder for the polyphenol mass percent for 90 ℃ condition in inlet temperature;
    (7) reclaim desalination fresh water
    With claim 1, feature is: regulating voltage is that 40V, intake pressure are 0.10MPa.
  4. 4. according to the described technology that from detoxified waste liquor of rapeseed extraction, extracts phytic acid of claim 1, it is characterized in that concrete step is as follows:
    (1) extraction
    1. prepare extraction liquid
    With claim 1, feature is: make N 235Volumetric molar concentration is the N of 0.5mol/L 235Extraction liquid;
    2. extraction
    With claim 1, feature is: detoxified waste liquor: the volume ratio of the extraction liquid of (1)-1. step preparation is 1: 6, feeding temperature to the extractor interlayer is 40 ℃ hot water, the insulation extraction was left standstill 10 minutes after 10 minutes, and again according to the raffinate behind the extraction phytic acid: the volume ratio of the extraction liquid of (1)-1. step preparation is 1: 6, be 40 ℃ hot water again to extractor interlayer feeding temperature, the insulation extraction was left standstill 10 minutes after 10 minutes again, so repeated 1 time;
    (2) strip
    1. prepare anti-stripping agent
    With claim 1, feature is: make the sodium hydroxide mass percent and be 0.5% anti-stripping agent;
    2. strip
    With claim 1, feature is: the extraction liquid that phytic acid is arranged according to extraction: the volume ratio of the anti-stripping agent of (2)-1. step preparation is 1: 3, normal temperature stirs down and stripped 15 minutes, after leaving standstill 30 minutes, again according to the raffinate behind the reextraction phytic acid: the volume ratio of the anti-stripping agent of (2)-1. step preparation is 1: 3, stir at normal temperatures once more and stripped 15 minutes, left standstill 30 minutes;
    (3) electrodialysis anti-stripping agent
    With claim 1, feature is: regulating voltage is that 60V, intake pressure are 0.06MPa;
    (4) preparation phytic acid concentrated solution
    With claim 1, feature is: in vacuum tightness is that 0.08Mpa, temperature are to carry out vacuum concentration under 90 ℃ of conditions, prepares the phytic acid mass percent and be 70% phytic acid concentrated solution;
    (5) preparation vegetable seed polysaccharide
    1. ultrafiltration
    With claim 1, feature is: pump in the ultrafilter that molecular weight cut-off is 50,000 Da, ultrafiltration pressure is 0.25Mpa, and the trapped fluid volume is reduced to 1/10 of the lower floor raffinate original volume of extraction behind the phytic acid;
    2. lyophilize
    With claim 1, feature is: vacuum tightness is 55pa, temperature for-60 ℃ of conditions under, carried out lyophilize 24 hours, prepare total reducing sugar quality percentage composition and be 88% light brown vegetable seed polysaccharide frozen dried powder;
    (6) preparation polyphenol from rapeseed
    1. absorption
    With claim 1, feature is: HPD-450 polymeric adsorbent volume: the ratio of the filtered solution volume that contains polyphenol from rapeseed that (5)-1. step collected is 1: 10, and the column flow rate excessively of control filtered solution is 6 times of polymeric adsorbent volume;
    2. prepare elutriant
    With claim 1, feature is: adding distilled water diluting, to become the ethanol concentration expressed in percentage by volume be 85% ethanolic soln, adds sodium hydroxide solution again, and the pH value of regulating mixing solutions is 9.0;
    3. spraying drying
    With claim 1, feature is: the polymeric adsorbent volume: the effluent volume ratio of (6)-2. step preparation is 1: 6, the control elution flow rate is that 1.5 times of resin volume are crossed post, in vacuum tightness is that 0.08Mpa, temperature are to carry out vacuum concentration under 90 ℃ of conditions, in inlet temperature is that 135 ℃, air outlet temperature are that spraying drying is 86.3% polyphenol from rapeseed powder for the polyphenol mass percent under 95 ℃ the condition;
    (7) reclaim desalination fresh water
    Regulating voltage is that 60V, intake pressure are 0.15MPa.
CNA2008100697922A 2008-06-03 2008-06-03 Process for extracting phytic acid from virus-free waste liquid of rapeseed extraction Pending CN101289461A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101838287A (en) * 2010-05-27 2010-09-22 合肥工业大学 Method for circularly extracting phytic acid from lactic acid assisted by ultrasonic waves
CN102515394A (en) * 2011-12-23 2012-06-27 东华大学 Method for pre-extracting and recovering polyphenol compounds in olive oil treatment wastewater
CN103820219A (en) * 2014-03-07 2014-05-28 张家界金绿油脂有限责任公司 Method for extracting various active substances from rapeseed hull
CN110256487A (en) * 2019-07-11 2019-09-20 刘秀丽 A kind of preparation method of high-purity liquid phytic acid

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101838287A (en) * 2010-05-27 2010-09-22 合肥工业大学 Method for circularly extracting phytic acid from lactic acid assisted by ultrasonic waves
CN101838287B (en) * 2010-05-27 2012-07-04 合肥工业大学 Method for circularly extracting phytic acid from lactic acid assisted by ultrasonic waves
CN102515394A (en) * 2011-12-23 2012-06-27 东华大学 Method for pre-extracting and recovering polyphenol compounds in olive oil treatment wastewater
CN102515394B (en) * 2011-12-23 2013-06-05 东华大学 Method for pre-extracting and recovering polyphenol compounds in olive oil treatment wastewater
CN103820219A (en) * 2014-03-07 2014-05-28 张家界金绿油脂有限责任公司 Method for extracting various active substances from rapeseed hull
CN103820219B (en) * 2014-03-07 2015-03-11 张家界金绿油脂有限责任公司 Method for extracting various active substances from rapeseed hull
CN110256487A (en) * 2019-07-11 2019-09-20 刘秀丽 A kind of preparation method of high-purity liquid phytic acid

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