CN101838287B - Method for circularly extracting phytic acid from lactic acid assisted by ultrasonic waves - Google Patents
Method for circularly extracting phytic acid from lactic acid assisted by ultrasonic waves Download PDFInfo
- Publication number
- CN101838287B CN101838287B CN2010101893886A CN201010189388A CN101838287B CN 101838287 B CN101838287 B CN 101838287B CN 2010101893886 A CN2010101893886 A CN 2010101893886A CN 201010189388 A CN201010189388 A CN 201010189388A CN 101838287 B CN101838287 B CN 101838287B
- Authority
- CN
- China
- Prior art keywords
- phytic acid
- acid
- lactic acid
- rice bran
- phytic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Abstract
The invention relates to a method for circularly extracting phytic acid from lactic acid assisted by ultrasonic waves, which is characterized by preparing phytic acid products by directly carrying out the continuous procedures of degreasing, extracting phytic acid, separating films, adsorbing resin, and the like of rice bran, and meanwhile, the method can recover lactic acid, realizes the recycle of the lactic acid, changes wastes into valuables, and is suitable for industrialized production. The purity of the phytic acid produced by using the method is higher than 60 percent. Compared with the prior art, the method not only can greatly shorten the phytic acid extraction time, but also can increase the phytic acid extraction rate by ultrasonic treatment, greatly reduces the production cost by recycling the lactic acid and avoids the pollution of anions, such as Cl-, and the like introduced by using inorganic acid.
Description
Technical field
The invention belongs to deep processing of farm products and changing waste into resources technical field, be specifically related to utilize ultrasonic extraction and membrane separation technique from the processing of farm products by product, to extract the method for phytic acid product.
Background technology
Phytic acid (Phytic Acid), promptly 1,2,3; 4,5,6-dihydrogen phosphoric acid inositol (IUPAC-IUB, 1968); Have another name called myo-Inositol hexaphosphate, have antibiotic, anti-oxidant, remove various biological effect such as metals ion, be used widely at food, medicine and daily use chemicals light industry etc.According to statistics, recent years, whole world phytic acid demand was about 2,000,000 tons, and respective market only can provide 400,000 tons, and present domestic annual requirement is 200,000 tons, but throughput only can provide about 5% about 10,000 tons.Along with the continuous expansion of phytic acid range of application, the consumption consumption of phytic acid will increase year by year, and the phytic acid industry has huge development prospect.
Phytic acid extensively is present in cereal and the oil crops, and its content has very big difference with the difference of plant variety, and particularly content is more in the seed of cereal plants, and is like rice bran, wheat bran, maize germ etc., the highest with the phytic acid content in the rice bran.China produces grain big country, and rice and coarse cereals output occupy first place in the world.The national grain and oil of certificate information center is in formal issue on May 9th, 2007 Chinese mainly grain and oil seeding crops area and the up-to-date predicted data of output in 2007; China's rice yield was 18,257 ten thousand tons in 2006; Wheat yield is 10,384 ten thousand tons, and corn yield is 14,548 ten thousand tons, therefore; The cereal processing byproduct raw material resources that can be used for producing phytic acid are very abundant, and only the YO of rice bran is just more than 1,000 ten thousand tons.But for a long time; These processing of farm products by products are mainly as animal and fowl fodder; Have only the rice bran of 10-15% to be used for extracting oil or further extracting value high product such as phytic acid, inositol, thiaminogen; With developed country their the comprehensive utilization degree of depth and technical difficulty and the economic benefit of bringing are thus compared, also differed greatly, cause the significant wastage of resource.Therefore, seek the phytic acid production technique of a kind of technical feasibility, industrial economy, environment protection standard, to promoting resource rational utilization, solving crisis of resource and environmental pollution has direct realistic meaning.
At present the industrialized method of the easiest realization is to be raw material, to extract and the alkali neutralization precipitation is the working method of basic technology with mineral acid with processing of farm products by products such as rice brans.Though at present China has built up tens tame phytic acid factories, because technology falls behind, throughput capacity is big in the production process; The production floor space is bigger, and time consumption and energy consumption is more, and production cost is higher; Because working method is different, the skill level difference causes product quality variance, and is off quality in addition; Range of application is restricted, and it is fully up to expectations that the economic benefit that should reach is failed.Domestic phytic acid extraction and purification process is general to adopt traditional hydrochloric acid separation and Extraction method to extract phytic acid, and also some producer utilizes the oxalic acid acidifying to extract phytic acid.The former exceeds standard because of chloride ion content, and corrodibility is big, and environmental pollution is serious; Latter's oxalic acid acidifying pH value not only is difficult to control, and can in phytic acid, form residually, influences HUMAN HEALTH, can only manufacture level phytic acid, all can not adapt to the requirement that current phytic acid industry develops to luxury food additive direction.
Summary of the invention
Deficiency to the problems referred to above and prior art; The present invention provides the method for the use circularly extracting phytic acid from lactic acid assisted by ultrasonic waves that a kind of technology is simple, easy to operate, added value is high; The appreciation that realizes agricultural byproducts such as rice bran transforms, and increases economic efficiency, and reduces contaminate environment.
The method of circularly extracting phytic acid from lactic acid assisted by ultrasonic waves of the present invention is operated according to the following steps:
(1) skimming treatment: by weight/volume be 1: 2 (w/v) ratio with rice bran respectively successively through chloroform, methyl alcohol soak, air-dry, removing its surperficial lipid material, defatted rice bran;
(2) phytic acid extracts: be 40% lactic acid solution to defatted rice bran or middle adding concentration; Earlier in the ultrasonic extraction device, carry out supersound extraction, must extract mixed liquor A, will extract mixed liquor A and in the presence of non-UW, extract; Must extract mixed liquid B; To extract mixed liquid B and carry out centrifugally, collect supernatant, the phytic acid extracting solution;
(3) ultrafiltration: with above-mentioned phytic acid extracting solution under 15-50 ℃, 0.2-1.0Mpa working pressure earlier through the one-level ultrafiltration membrane system, remove impurity, ultrafiltration membrane permeate liquid C; With ultrafiltration membrane permeate liquid C under 15-50 ℃, 0.2-1.0Mpa working pressure through two-stage ultrafiltering film system, realize effectively separating of phytic acid and lactic acid, obtain purity and be phytic acid liquid concentrator D and lactic acid concn more than 50% greater than 37% ultrafiltration membrane permeate liquid E.
(4) phytic acid is refining: through negatively charged ion macroporous resin adsorption post, phytic acid is by resin absorption with rice bran phytic acid liquid concentrator D; After absorption is accomplished, use concentration to be adsorbed the phytic acid that post adsorbs, obtain elutriant F as sodium hydroxide (NaOH) eluant solution of 1.5mg/mL; Elutriant F collects effluent G directly through cation exchange resin column, and effluent G is plant acid solution, and phytic acid content reaches more than 60% in the plant acid solution.
Skimming treatment described in the said step (1) comprises: (1) by weight/volume is that the ratio of 1: 2 (w/v) adds chloroform in rice bran, soaks 2 hours, filter, natural air drying, rice bran A; (2) by weight/volume is that the ratio of 1: 2 (w/v) adds methyl alcohol in rice bran A, soaks 2 hours, filter, natural air drying, defatted rice bran.
Phytic acid described in the said step (2) extract be the mixed solution of defatted rice bran and lactic acid first be that 400W and temperature are to carry out supersound extraction 10min under 70 ℃ the condition at ultrasonic power; Must extract mixed liquor A; To extract mixed liquor A again and place 70 ℃ of water-baths to continue to extract 1.0 hours, must extract mixed liquid B, will extract mixed liquid B centrifugal 10min under 12000r/min; Collect supernatant, get the phytic acid extracting solution.
Ultrafiltration described in the said step (3) is that the phytic acid extracting solution is 10000 daltonian one-level ultrafiltration membrane system through molecular weight cut-off earlier, obtains ultrafiltration membrane permeate liquid C; Be 3000 daltonian two-stage ultrafiltering film systems with ultrafiltration membrane permeate liquid C through molecular weight cut-off again, realize separating of lactic acid and phytic acid, the liquid concentrator D that obtains is the rice bran phytic acid, obtains ultrafiltration membrane permeate liquid E simultaneously and is lactic acid solution.
The lactic acid solution that obtains in the said step (3) can be used as the repeated use of phytic acid extraction agent after adjusting concentration to 40%.
The used phytic acid process for refining of said step (4) is the series connection chromatogram arrangement of being made up of anion-exchange resin column and cation exchange resin column with a group; Wherein anionite-exchange resin is D-201 macroporous strong basic styrene series anionite-exchange resin, and Zeo-karb is 732 strongly acidic styrene type cation exchange resins.
Compare with traditional technology, technology of the present invention has following advantage: use organic acid to avoid mineral acid and the C1 that introduces in (1) technology
-Etc. anionic pollution; (2) use ultrasonication to shorten extraction time of phytic acid greatly in the technology, than without the shortening of ultrasonication 2.5h; (3) use ultrasonication to improve the extraction yield of phytic acid greatly in the technology, than without the raising of ultrasonication 84.4%; (4) adopt membrane separation technique can realize that phytic acid and the effective of lactic acid separate, the lactic acid recovery reaches more than 90%, thereby has realized recycling of lactic acid, greatly reduces production cost; (5) discharging of no bronsted lowry acids and bases bronsted lowry in the technology has reduced the pollution of production process to environment.
Description of drawings
Fig. 1 is the extraction process flow process of circularly extracting phytic acid from lactic acid assisted by ultrasonic waves of the present invention.
Embodiment
Below in conjunction with embodiment the present invention is done to describe further.
Embodiment:
Referring to Fig. 1, the method for circularly extracting phytic acid from lactic acid assisted by ultrasonic waves is operated according to the following steps:
Step 1: rice bran degreasing: take by weighing the 1000g rice bran, by weight/volume is that the ratio of 1: 2 (w/v) adds chloroform in rice bran, soaks 2 hours, filter, natural air drying, 975g rice bran A; By weight/volume is that the ratio of 1: 2 (w/v) adds methyl alcohol in rice bran A, soaks 2 hours, filter, natural air drying, the 950g defatted rice bran.
Step 2: phytic acid extracts: get the defatted rice bran in the 500g step 1, adding concentration is 40% lactic acid (v/v) 5L in defatted rice bran, in the ultrasonic extraction device, carries out earlier supersound extraction 10min; Ultrasonic power is made as 400W, and extracting temperature is 70 ℃, must extract mixed liquor A; To extract mixed liquor A and place 70 ℃ of water-baths to extract 1.0 hours, must extract mixed liquid B, will extract mixed liquid B centrifugal 10min under 12000r/min; Collect supernatant, get the phytic acid extracting solution, the phytic acid yield reaches 7.82%.
Step 3: ultrafiltration: is 10000 daltonian one-level ultrafiltration membrane system through molecular weight cut-off with above-mentioned phytic acid extracting solution earlier under 15-50 ℃, 0.2-1.0Mpa working pressure, obtains ultrafiltration membrane permeate liquid C; Be 3000 daltonian two-stage ultrafiltering film systems with ultrafiltration membrane permeate liquid C through molecular weight cut-off again; Realization lactic acid separates with phytic acid; Obtaining purity is the rice bran phytic acid liquid concentrator D more than 50%; Liquid concentrator D is the rice bran phytic acid, and obtains ultrafiltration membrane permeate liquid E, and seeing through liquid E is that concentration is greater than 37% lactic acid solution.The lactic acid solution that obtains is through adding the extraction that can directly be used for the rice bran phytic acid to 40% concentration.
Step 4: phytic acid is refining: through the adsorption column of D-201 macroporous strong basic styrene series anionite-exchange resin is housed, phytic acid is adsorbed with resulting rice bran phytic acid liquid concentrator D in the step 3; The loadings of adsorption column intermediate ion exchange resin is by 10% of the liquid concentrator A weight of each processing; Adsorption operations uses in NaOH eluant solution adsorption column to the effluent of concentration as 1.5mg/mL and can not detect sodium phytate (spectrophotometric analysis) after accomplishing, and gets elutriant D; Directly through the resin column of 732 strongly acidic styrene type cation exchange resins is housed, effluent is the purified plant acid solution to elutriant D, and phytic acid purity reaches more than 60%.
Claims (6)
1. the method for circularly extracting phytic acid from lactic acid assisted by ultrasonic waves is characterized in that operating according to the following steps:
(1) skimming treatment: by weight/volume be 1: 2 ratio with rice bran respectively successively through chloroform, methyl alcohol soak, air-dry, removing its surperficial lipid material, defatted rice bran;
(2) phytic acid extracts: be 40% lactic acid solution to defatted rice bran or middle adding concentration; Earlier in the ultrasonic extraction device, carry out supersound extraction, must extract mixed liquor A, will extract mixed liquor A and in the presence of non-UW, extract; Must extract mixed liquid B; To extract mixed liquid B and carry out centrifugally, collect supernatant, the phytic acid extracting solution;
(3) ultrafiltration: is 10000 daltonian one-level ultrafiltration membrane system through molecular weight cut-off with above-mentioned phytic acid extracting solution earlier under 15-50 ℃, 0.2-1.0Mpa working pressure, removes impurity, ultrafiltration membrane permeate liquid C; Is 3000 daltonian two-stage ultrafiltering film systems through molecular weight cut-off with ultrafiltration membrane permeate liquid C under 15-50 ℃, 0.2-1.0Mpa working pressure; Realize effectively separating of phytic acid and lactic acid, obtain purity and be phytic acid liquid concentrator D and lactic acid concn more than 50% greater than 37% ultrafiltration membrane permeate liquid E;
(4) phytic acid is refining: through negatively charged ion macroporous resin adsorption post, phytic acid is by resin absorption with rice bran phytic acid liquid concentrator D; After absorption is accomplished, use concentration to be adsorbed the phytic acid that post adsorbs, obtain elutriant F as the sodium hydroxide solution wash-out of 1.5mg/mL; Elutriant F collects effluent G directly through cation exchange resin column, and effluent G is plant acid solution, and phytic acid content reaches more than 60% in the plant acid solution.
2. the method for circularly extracting phytic acid from lactic acid assisted by ultrasonic waves according to claim 1, it is characterized in that: the skimming treatment described in the said step (1) comprises: (1) by weight/volume is that 1: 2 ratio adds chloroform in rice bran; Soaked 2 hours; Filter, natural air drying gets rice bran A; (2) by weight/volume is that 1: 2 ratio adds methyl alcohol in rice bran A, soaks 2 hours, filter, natural air drying, defatted rice bran.
3. the method for circularly extracting phytic acid from lactic acid assisted by ultrasonic waves according to claim 1; It is characterized in that: phytic acid described in the said step (2) extract be the mixed solution of defatted rice bran and lactic acid first be that 400W and temperature are to carry out supersound extraction 10min under 70 ℃ the condition at ultrasonic power; Must extract mixed liquor A; To extract mixed liquor A again and place 70 ℃ of water-baths to continue to extract 1.0 hours, must extract mixed liquid B, will extract mixed liquid B centrifugal 10min under 12000r/min; Collect supernatant, get the phytic acid extracting solution.
4. the method for circularly extracting phytic acid from lactic acid assisted by ultrasonic waves according to claim 1; It is characterized in that: the ultrafiltration described in the said step (3) is that the phytic acid extracting solution is 10000 daltonian one-level ultrafiltration membrane system through molecular weight cut-off earlier, obtains ultrafiltration membrane permeate liquid C; Be 3000 daltonian two-stage ultrafiltering film systems with ultrafiltration membrane permeate liquid C through molecular weight cut-off again, realize separating of lactic acid and phytic acid, the liquid concentrator D that obtains is the rice bran phytic acid, obtains ultrafiltration membrane permeate liquid E simultaneously and is lactic acid solution.
5. the method for circularly extracting phytic acid from lactic acid assisted by ultrasonic waves according to claim 1 is characterized in that: the lactic acid solution that obtains in the said step (3) can be used as the phytic acid extraction agent after through adjustment concentration to 40% and reuses.
6. the method for circularly extracting phytic acid from lactic acid assisted by ultrasonic waves according to claim 1; It is characterized in that: the used phytic acid process for refining of said step (4) is the series connection chromatogram arrangement of being made up of anion-exchange resin column and cation exchange resin column with a group; Wherein anionite-exchange resin is D-201 macroporous strong basic styrene series anionite-exchange resin, and Zeo-karb is 732 strongly acidic styrene type cation exchange resins.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101893886A CN101838287B (en) | 2010-05-27 | 2010-05-27 | Method for circularly extracting phytic acid from lactic acid assisted by ultrasonic waves |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101893886A CN101838287B (en) | 2010-05-27 | 2010-05-27 | Method for circularly extracting phytic acid from lactic acid assisted by ultrasonic waves |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101838287A CN101838287A (en) | 2010-09-22 |
| CN101838287B true CN101838287B (en) | 2012-07-04 |
Family
ID=42741988
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010101893886A Expired - Fee Related CN101838287B (en) | 2010-05-27 | 2010-05-27 | Method for circularly extracting phytic acid from lactic acid assisted by ultrasonic waves |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101838287B (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102127108A (en) * | 2010-12-08 | 2011-07-20 | 东北电力大学 | Method for extracting phytic acid from rice bran |
| CN102702251B (en) * | 2012-06-25 | 2015-06-17 | 华东理工大学 | Method for extracting phytic acid from rubber seeds |
| CN103214512A (en) * | 2013-04-22 | 2013-07-24 | 江南大学 | Technology for preparing high-purity phytic acid with membrane technology by taking defatted rice bran as raw material |
| CN103980305A (en) * | 2014-04-04 | 2014-08-13 | 浙江恒乐粮食有限公司 | Ultrafiltration membrane treating method for degreased rice bran phytic acid extract |
| CN104193780A (en) * | 2014-08-01 | 2014-12-10 | 刘秀丽 | Extraction method of solid phytic acid |
| CN108329345A (en) * | 2018-04-17 | 2018-07-27 | 叶盛权 | The extracting method of phospho phytate in a kind of seawater rice |
| CN109158096A (en) * | 2018-10-29 | 2019-01-08 | 江苏九九久科技有限公司 | Accelerate the method for macroporous resin adsorption and desorption rate |
| CN110437060A (en) * | 2019-07-26 | 2019-11-12 | 刘秀丽 | The method of lactic acid is recycled in a kind of production of phytic acid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1992016534A1 (en) * | 1991-03-14 | 1992-10-01 | Reilly Industries, Inc. | Recovery of phytic and/or lactic acid and direct retrieval of inositol |
| WO1997035489A1 (en) * | 1996-03-27 | 1997-10-02 | A. E. Staley Manufacturing Company | A process for obtaining phytic acid and lactic acid |
| CN101289461A (en) * | 2008-06-03 | 2008-10-22 | 重庆大学 | Process for extracting phytic acid from virus-free waste liquid of rapeseed extraction |
-
2010
- 2010-05-27 CN CN2010101893886A patent/CN101838287B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1992016534A1 (en) * | 1991-03-14 | 1992-10-01 | Reilly Industries, Inc. | Recovery of phytic and/or lactic acid and direct retrieval of inositol |
| WO1997035489A1 (en) * | 1996-03-27 | 1997-10-02 | A. E. Staley Manufacturing Company | A process for obtaining phytic acid and lactic acid |
| CN101289461A (en) * | 2008-06-03 | 2008-10-22 | 重庆大学 | Process for extracting phytic acid from virus-free waste liquid of rapeseed extraction |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101838287A (en) | 2010-09-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101838287B (en) | Method for circularly extracting phytic acid from lactic acid assisted by ultrasonic waves | |
| CN103044570B (en) | A kind of extraction process of high efficiency extraction sea grass polysaccharide | |
| CN102690372B (en) | Method for co-production of de-boned raw chicken, chicken bone soup-stock and chondroitin sulfate using chicken skeleton | |
| CN102219866B (en) | Method for extracting and separating ganoderma lucidum polysaccharide from ganoderma lucidum sporocarp | |
| CN104688801B (en) | A kind of complex enzyme combination ultrasound extracts the production technology of eucommia bark flavone from folium cortex eucommiae | |
| CN104187456A (en) | Technical method for extracting dietary fiber from pear residue | |
| CN102250195A (en) | Method for producing xanthoceraside | |
| CN103755822A (en) | Brasenia schreberi polysaccharide preparation method | |
| CN104480168A (en) | Method for preparing chondroitin sulfate and co-producing collagen peptide and biological calcium by using fishbone | |
| CN102174121A (en) | Process for extracting pectin from citrus peel and producing organic fertilizer by using waste residues | |
| CN101863758A (en) | Technology for preparing ferulic acid and phytic acid from rice bran | |
| CN103113422B (en) | Method for separating and refining high-purity L-arabinose and D-xylose with simulated moving bed | |
| CN102816633A (en) | Method for synchronously extracting corn germ oil and separation protein by using alcohol-assisted enzyme method | |
| CN105647978A (en) | Method for degrading aflatoxin in corn raw material | |
| CN102070681B (en) | Konjak ceramide and extraction method thereof | |
| CN103435682B (en) | Wheat germ protein source antioxidative peptide, and preparation method and application thereof | |
| CN103588892B (en) | A kind of solvent extraction process of wheat bran active polysaccharide | |
| CN101366829B (en) | Method for synchronously extracting flavone and alkaloid from folium nelumbinis | |
| CN104093485B (en) | The method that pentose is extracted from lignocellulosic matrix | |
| CN104264262A (en) | Method for extracting araboxylan and protein fiber from wheat bran | |
| CN101095454B (en) | Method of separating protein from cereal kernel by adopting membrane separation technique | |
| CN105255965A (en) | Method for preparing high-purity xylo-oligosaccarides by taking cottonseed hulls as raw materials | |
| CN104928341A (en) | Preparation method for ferulic acid combining ultrasonic-assisted enzymolysis and microbial-fermented bran | |
| Wang et al. | Valorization of spent shiitake substrate for recovery of antitumor fungal sterols by ultrasound‐assisted extraction | |
| CN104404094A (en) | Method for extracting taurine by use of enzymatic conversion method on the basis of clams |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C53 | Correction of patent for invention or patent application | ||
| CB03 | Change of inventor or designer information |
Inventor after: Cha Xueqiang Inventor after: Luo Jianping Inventor after: Wang Lin Inventor after: Zhang Hailin Inventor before: Luo Jianping Inventor before: Cha Xueqiang Inventor before: Wang Lin Inventor before: Zhang Hailin |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: INVENTOR; FROM: LUO JIANPING CHA XUEQIANG WANG LIN ZHANG HAILIN TO: CHA XUEQIANG LUO JIANPING WANG LIN ZHANG HAILIN |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120704 Termination date: 20150527 |
|
| EXPY | Termination of patent right or utility model |