CN101624399B - Method for extracting phytic acid from jatropha curcas seed cake or jatropha curcas seeds - Google Patents
Method for extracting phytic acid from jatropha curcas seed cake or jatropha curcas seeds Download PDFInfo
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- CN101624399B CN101624399B CN2009103054958A CN200910305495A CN101624399B CN 101624399 B CN101624399 B CN 101624399B CN 2009103054958 A CN2009103054958 A CN 2009103054958A CN 200910305495 A CN200910305495 A CN 200910305495A CN 101624399 B CN101624399 B CN 101624399B
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Abstract
The invention discloses a method for extracting phytic acid from jatropha curcas seed cakes or jatropha curcas seeds, and the phytic acid is prepared by using the jatropha curcas seed cakes or the jatropha curcas seeds, the oil which is extracted, as raw materials and adopting the steps as follows: lixiviating with diluted acid, removing impurity, neutralizing with alkali, splitting with acid, ion exchanging, decoloring and concentrating. The invention can also be used for preparing feed protein while prepaing the phytic acid, and has high yield and better purity. The extraction rate of the phytic acid is more than 80 percent, the yield of the phytic acid reaches 8-9 percent, and the prepared phytic acid is concentrated liquid with concentration reaching 50-60 percent. After the phytic acid is extracted, the content of crude protein in the residue is further concentrated and improved to reach 25-30 percent; the in vitro digestibility coefficient of the crude protein reaches 43.57 percent and is improved by about 150 percent, compared with the in vitro digestibility coefficient of the crude protein of the seed cakes the phytic acid of which is not extracted. The invention has simple process, wild condition and low energy consumption, meets the requirement of the environment protection, and is a green process of comprehensively utilizing the jatropha curcas seed cakes or jatropha curcas seeds.
Description
Technical field
The present invention relates to a kind of process for extracting of phytic acid, is a kind of method of from barbadosnut pulp or jatropha curcas seed, extracting phytic acid specifically.
Background technology
Cortex jatrophae; Have another name called the little seeds of a tung oil tree, tar paulownia, tung tree, the living tree of artificial flower etc.; Belong to Euphorbiaceae (Euphorbiaceae) leprosy Pterostyrax; Be a kind of quick growing species of trees of drought-resistant impoverishment tolerant, at the solid soil of water conservation, increase the soil organism, restore vegetation and prevent that aspect such as stony desertification has important value of exploiting and utilizing.The jatropha curcas seed oleaginousness is between 40%-60%, and staple is oleic acid (41.3%), linolic acid (31.4%) and palmitinic acid (19.5%), is the desirable feedstock of preparation biofuel.Study according to the expert; The about 660kg/ mu of wild Cortex jatrophae dry fruit mean yield; Can extract processing biological diesel-oil 180-270kg; This biofuel is applicable to various diesel motors, and key indexs such as its burning-point, zero pour, sulphur content, CO emission, particle all are superior to domestic 0# diesel oil, reach No. two diesel oil standards in present Europe.Many reports also confirmed the biofuel with Cortex jatrophae fruit grease production possess have good burning performance, flash-point is high, pollute advantages such as little, can replace traditional petrifaction diesel, becomes a kind of new clean energy.With Cortex jatrophae fruit production biofuel is to alleviate one of exhausted effective way of oil, has become of researching and producing biofuel at present and has enlivened direction, and relevant project also obtains the National Development and Reform Committee and the each place active support of the government.
Be accompanied by the extensive plantation of Cortex jatrophae and the batch process of biofuel, Cortex jatrophae will produce a large amount of barbadosnut pulps after really carrying oil.Jatropha curcas seed can obtain jatropha curcas seed oil through behind the mechanical expression, and remaining is exactly barbadosnut pulp, and it is the same that its production process is carried oil with vegetable seed.Estimate that according to relevant departments the cultivated area of Chinese future Cortex jatrophae more than 3,000 ten thousand mu, can produce the 650kg dry fruit by every mu of every year at least, the per kilogram dry fruit contains the 0.4kg grease and calculates, and annually can produce 1,170 ten thousand tons of barbadosnut pulps after carrying oil.Many researchs confirm to contain more protein in the grouts, and (crude protein is 18-32%; The seeds content of different sources is different); Be important plant protein material source, grouts also are rich in multiple indispensable amino acids such as Threonine, Xie Ansuan, leucine in addition, have higher nutritive value.Yet barbadosnut pulp contains a spot of toxicant, and protein often combines with materials such as lipids, thereby has limited the utilization of grouts.If grouts are directly discharged, not only can cause the significant wastage of resource, and the environment around a large amount of releases of nitrogen and phosphorus can be polluted in the barbadosnut pulp.Therefore, how making good use of barbadosnut pulp or jatropha curcas seed is a urgent problem.
Phytic acid has another name called myo-Inositol hexaphosphate, nucite six phosphides, is the mixture of myo-inositol phosphates.Phytic acid mainly extensively is present in cereal, beans and the oil grain 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.Because phytic acid has protective foods, delays Oxidation of Fat and Oils, promote the effects such as generation of human body metabolism, reduce fat, inhibition SUV, be widely used in fields such as food, medical treatment, daily-use chemical industry, metallurgy and metal processing, chemical, oil and light and textile industries.
At present, the working method of phytic acid has chemosynthesis, biosynthesizing, solvent extration, the precipitator method and ion exchange method.Chemical synthesis is with inositol and P
2O
5Be the feedstock production phytic acid, but do not have industrial significance.Biological synthesis process is by modern biotechnology, prepares phytic acid through microbe fermentation method.Solvent extration, the precipitator method and ion exchange method are raw material with cereal, beans and oil grain mainly, through various separating and purifying technologies, the phytic acid in the plant seed are extracted.Because phytic acid content exists than big-difference, so the extraction yield of phytic acid also has very big-difference in the various plant seeds.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method from barbadosnut pulp or jatropha curcas seed extraction phytic acid; Technology of the present invention is simple, mild condition, and energy consumption requires low; Compliance with environmental protection requirements is barbadosnut pulp or the friendly process of carrying behind the oil of jatropha curcas seed comprehensive utilization.
In order to address the above problem, the invention provides following method:
This method is that raw material extracts phytic acid with barbadosnut pulp or the jatropha curcas seed of carrying behind the oil.
Concrete steps are following: barbadosnut pulp or the jatropha curcas seed that 1) will carry behind the oil grind with kibbler, and particle is the 10-100 order;
2) with concentration of volume percent be dilute acid soln and barbadosnut pulp or the jatropha curcas seed 5-25 by volume of 1-10%: 1 mixed, stir or oscillating condition under lixiviate 0.5-2h;
3) mixed solution of above-mentioned diluted acid and barbadosnut pulp or jatropha curcas seed is filtered or centrifugal, collect filtrating;
4) filtrating that collection in the step 3) is obtained is added mass percent concentration under agitation condition be the alkaline solution of 10-30%, regulates pH 6-8, and neutralization reaction 20-60min stops to stir then, leaves standstill the 1-5h after-filtration, collects the sodium phytate deposition;
5) in the above-mentioned sodium phytate deposition of collecting, add dilute acid soln again, transfer pH 1-3 to carry out the acid dissolving, make the sodium phytate deposition form plant acid solution;
6) plant acid solution in the step 5) is used resin anion(R.A) and each IX 5-10min of resin cation(R.C.) successively, remove remaining negatively charged ion and positively charged ion, assorted negatively charged ion is mainly Cl
-, SO
4 2-Deng, assorted positively charged ion is mainly K
+, Ca
2+, Mg
2+, Na
+Deng;
7) discoloring agent is joined in the above-mentioned solution decolour then; Solution centrifugal with after the decolouring obtains plant acid solution;
8) the solution direct heating after will decolouring concentrates, and obtaining mass percent concentration is the phytic acid liquid concentrator of 50-60%.
Said diluted acid is Hydrogen chloride, dilute sulphuric acid, dilute phosphoric acid or dilute acetic acid etc.; Wherein strong acid such as Hydrogen chloride and dilute sulphuric acid effect is better, and effects such as dilute phosphoric acid or dilute acetic acid are general;
Said alkaline solution is sodium hydroxide solution or potassium hydroxide solution etc.;
Described resin anion(R.A) is a strongly basic anionic resin, like 717 resin anion(R.A)s etc., with the sodium chloride solution wash-out of 0.5-1.0mol/L, phytic acid is replaced during anionresin;
Described resin cation(R.C.) is a strong acidic ion resin, like 732 resin cation(R.C.)s etc.; During cationic exchange without eluent because in the ion exchange process mainly with K
+, Ca
2+, Mg
2+, Na
+Be adsorbed on the resin Deng hetero-ion, phytic acid can not be adsorbed, thereby reaches the removal of impurities purpose;
Said discoloring agent is gac, Poly aluminum Chloride (PAC) or other organic high molecular polymer with strong positive charge.
By mass percentage, the amount of said adding discoloring agent is the 0.1%-0.5% of plant acid solution amount;
Marking the phytic acid solution temperature controlled at 50-80 ° C, bleaching time was 30-60min.
Compared with prior art, the present invention has following advantage:
1) phytic acid extraction yield of the present invention is greater than 80%, and the phytic acid yield is up to 8-9%, and phytic acid impurity is less, and the gained phytic acid is the liquid concentrator up to 50-60%.
2) technology of the present invention is simple, and is low for equipment requirements, mild condition, and energy consumption requires low, is easy to go into operation; Compliance with environmental protection requirements is the friendly process of barbadosnut pulp or jatropha curcas seed comprehensive utilization.
3) after the acid extraction, the crude protein content in the residue further concentrates and improves, and reaches 25-30%; Crude protein external digestion rate has improved about 150% than the crude protein external digestion rate of not extracting the phytic acid grouts up to 43.57%.
Description of drawings
Fig. 1 is a method flow diagram of the present invention.
Embodiment
Embodiment 1: the present invention extracts the method for phytic acid from barbadosnut pulp or jatropha curcas seed, is that raw material extracts phytic acid with barbadosnut pulp or the jatropha curcas seed of carrying behind the oil.Barbadosnut pulp or the jatropha curcas seed wherein carried behind the oil mainly are that the southwest of Guizhou Province, Xingyi, Guizhou Condar Bio-energy Technology Ltd. (GB) Suite 1, Bristol House, 80A Southampton Row Loud provides.
Shown in Fig. 1 schema, the method for from barbadosnut pulp or jatropha curcas seed, extracting phytic acid comprises the steps:
1) barbadosnut pulp or jatropha curcas seed pre-treatment: barbadosnut pulp or the jatropha curcas seed that will carry behind the oil grind with kibbler, and particle reaches the 30-50 order;
2) Hydrogen chloride soaks: first dose volume percentage concentration is the dilute hydrochloric acid solution of 1-2%, then with Hydrogen chloride and barbadosnut pulp or by volume 10: 1 mixed of jatropha curcas seed, and lixiviate 2h under stirring or oscillating condition;
3) Hydrogen chloride solid-liquid separation: with step 2) and barbadosnut pulp mixed solution are removed filter residue and are collected filtrating with 120 order filtered through gauze.
4) acid-base neutralisation: with step 3) collect the filtrating obtain under agitation condition and mass percent concentration be 20% sodium hydroxide solution thorough mixing; Carry out neutralization reaction 30min at pH about 7; Stop then stirring; Mixed solution filters after leaving standstill 2h again, discards filtrating, collects the sodium phytate deposition;
5) acidifying: add and step 2 in the sodium phytate deposition of collecting toward step 4)) identical dilute hydrochloric acid solution is transferred and is carried out acid dissolving about pH1.5, makes sodium phytate precipitate the formation phytic acid aqueous solution;
6) IX removes hetero-ion: the phytic acid aqueous solution in the step 5) earlier with 717 resin anion(R.A) IXs 5 minutes, with the sodium chloride solution wash-out of 0.5-1.0mol/L, is replaced phytic acid get off, mainly remove Cl wherein
-, SO
4 2-Etc. assorted negatively charged ion; And then with 732 resin cation(R.C.) IXs 5 minutes, during cationic exchange without eluent because in the ion exchange process mainly with K
+, Ca
2+, Mg
2+, Na
+Be adsorbed on the resin Deng hetero-ion, phytic acid can not be adsorbed, thereby reaches the removal of impurities purpose;
7) decolouring: by mass percentage, the gac that in plant acid solution, adds its quality 0.2% decolours; Solution temperature preferably is controlled at 70-80 ℃ during decolouring, under stirring condition, and decolouring 30min, the solution centrifugal after will decolouring then obtains the transparent liquid of phytic acid;
8) concentrate: the solution direct heating after will decolouring concentrates, and can get concentration is the phytic acid liquid concentrator of 50-60%.Because the high density plant acid solution has certain viscosity, also be unfavorable for further concentrating, and industriallization phytic acid product concentration generally is about 60% on the market, gets final product so the present invention only need be concentrated into 50-60%.
Embodiment 2: the present invention extracts the method for phytic acid from barbadosnut pulp or jatropha curcas seed, is that raw material extracts phytic acid with barbadosnut pulp or the jatropha curcas seed of carrying behind the oil.Barbadosnut pulp or the jatropha curcas seed wherein carried behind the oil mainly are that the southwest of Guizhou Province, Xingyi, Guizhou Condar Bio-energy Technology Ltd. (GB) Suite 1, Bristol House, 80A Southampton Row Loud provides.
Shown in Fig. 1 schema, the method for from barbadosnut pulp or jatropha curcas seed, extracting phytic acid comprises the steps:
1) barbadosnut pulp or jatropha curcas seed pre-treatment: barbadosnut pulp or the jatropha curcas seed that will carry behind the oil grind with kibbler, and particle reaches the 30-50 order;
2) dilute sulphuric acid soaks: first dose volume percentage concentration is the dilution heat of sulfuric acid of 1-2%, then with dilute sulphuric acid and barbadosnut pulp or by volume 8: 1 mixed of jatropha curcas seed, and lixiviate 1h under stirring or oscillating condition;
3) dilute sulphuric acid solid-liquid separation: with step 2) and barbadosnut pulp mixed solution are removed filter residue and are collected filtrating with 120 order filtered through gauze.
4) acid-base neutralisation: with step 3) collect the filtrating obtain under agitation condition and mass percent concentration be 25% potassium hydroxide solution thorough mixing; Carry out neutralization reaction 30min at pH about 7; Stop then stirring; Mixed solution filters after leaving standstill 2h again, discards filtrating, collects the sodium phytate deposition;
5) acidifying: add and step 2 in the sodium phytate deposition of collecting toward step 4)) identical dilution heat of sulfuric acid is transferred and is carried out acid dissolving about pH1.5, makes sodium phytate precipitate the formation phytic acid aqueous solution;
6) IX removes hetero-ion: the phytic acid aqueous solution in the step 5) earlier with 717 resin anion(R.A) IXs 5 minutes, with the sodium chloride solution wash-out of 0.5-1.0mol/L, is replaced phytic acid get off, mainly remove Cl wherein
-, SO
4 2-Etc. assorted negatively charged ion; And then with 732 resin cation(R.C.) IXs 5 minutes, during cationic exchange without eluent because in the ion exchange process mainly with Ca
2+, Mg
2+, Na
+, K
+Be adsorbed on the resin Deng hetero-ion, phytic acid can not be adsorbed, thereby reaches the removal of impurities purpose;
7) decolouring: by mass percentage 3, the gac that in plant acid solution, adds its quality 0.2% decolours; Solution temperature preferably is controlled at 70-80 ℃ during decolouring, under stirring condition, and decolouring 60min, the solution centrifugal after will decolouring then obtains the transparent liquid of phytic acid;
8) concentrate: the solution direct heating after will decolouring concentrates, and can get concentration is the phytic acid liquid concentrator of 50-60%.Because the high density plant acid solution has certain viscosity, also be unfavorable for further concentrating, and industriallization phytic acid product concentration generally is about 60% on the market, gets final product so the present invention only need be concentrated into 50-60%.
Implement through the present invention, the phytic acid extraction yield is greater than 80% in barbadosnut pulp or the jatropha curcas seed, and the phytic acid yield is up to 8-9%, and the gained phytic acid is the liquid concentrator up to 50-60%.After phytic acid extracted, the crude protein content in the residue further concentrated and improves, and reaches 25-30%; Crude protein external digestion rate has improved about 150% than the crude protein external digestion rate of not extracting the phytic acid grouts up to 43.57%.
Claims (8)
1. one kind is extracted the method for phytic acid from barbadosnut pulp or jatropha curcas seed, it is characterized in that: this method is that raw material extracts phytic acid with barbadosnut pulp or the jatropha curcas seed of carrying behind the oil, comprises the steps:
1) barbadosnut pulp or the jatropha curcas seed that will carry behind the oil grind, and particle is the 10-100 order;
2) with concentration of volume percent be 1-10% dilute acid soln with pulverize after barbadosnut pulp or jatropha curcas seed 5-25 by volume: 1 mixed, stir or oscillating condition under lixiviate 0.5-2h;
3) mixed solution of above-mentioned diluted acid and barbadosnut pulp or jatropha curcas seed is filtered or centrifugal, collect filtrating;
4) filtrating that collection in the step (3) is obtained is added mass percent concentration under agitation condition be the alkaline solution of 10-30%, regulates pH 6-8, and neutralization reaction 20-60min stops to stir then, leaves standstill the 1-5h after-filtration, collects the sodium phytate deposition;
5) in the above-mentioned sodium phytate deposition of collecting, add dilute acid soln again, transfer pH 1-3 to carry out the acid dissolving, make the sodium phytate deposition form plant acid solution;
6) plant acid solution in the step 5) is used resin anion(R.A) and each IX 5-10min of resin cation(R.C.) successively;
7) discoloring agent is joined in the plant acid solution after the above-mentioned IX decolour then; Solution centrifugal with after the decolouring obtains transparent plant acid solution;
8) the solution direct heating after will decolouring concentrates, and obtaining mass percent concentration is the phytic acid liquid concentrator of 50-60%.
2. the method from barbadosnut pulp or jatropha curcas seed extraction phytic acid according to claim 1, it is characterized in that: said diluted acid is Hydrogen chloride, dilute sulphuric acid, dilute phosphoric acid or dilute acetic acid.
3. the method from barbadosnut pulp or jatropha curcas seed extraction phytic acid according to claim 1, it is characterized in that: said alkaline solution is sodium hydroxide solution or potassium hydroxide solution.
4. the method from barbadosnut pulp or jatropha curcas seed extraction phytic acid according to claim 1, it is characterized in that: described resin anion(R.A) is a strongly basic anionic resin.
5. the method from barbadosnut pulp or jatropha curcas seed extraction phytic acid according to claim 1, it is characterized in that: described resin cation(R.C.) is a strong acidic ion resin.
6. the method from barbadosnut pulp or jatropha curcas seed extraction phytic acid according to claim 1, it is characterized in that: said discoloring agent is gac, Poly aluminum Chloride (PAC) or other organic high molecular polymer with strong positive charge.
7. according to claim 1 or 6 described methods from barbadosnut pulp or jatropha curcas seed extraction phytic acid, it is characterized in that: by mass percentage, the amount of said adding discoloring agent is the 0.1%-0.5% of plant acid solution amount.
8. according to claim 1 or 6 described methods from barbadosnut pulp or jatropha curcas seed extraction phytic acid, it is characterized in that: the plant acid solution temperature is controlled at 50-80 ℃ during decolouring, and bleaching time is 30-60min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| AP3548A (en) * | 2010-12-21 | 2016-01-15 | Gea Mechanical Equipment Gmbh | Method for fractionating jatropha seeds |
| CN102702251B (en) * | 2012-06-25 | 2015-06-17 | 华东理工大学 | Method for extracting phytic acid from rubber seeds |
| CN102793063A (en) * | 2012-09-13 | 2012-11-28 | 重庆油桐产业研究中心 | Processing method comprehensively utilizing plant oil cake |
| CN102928581B (en) * | 2012-11-12 | 2014-08-06 | 孙哲 | External measurement method for transgenic plant material digestibility |
| DE102014104986A1 (en) * | 2014-04-08 | 2015-10-08 | Gea Mechanical Equipment Gmbh | Process for the recovery of one or more valuable substances from seeds |
| CN105886127A (en) * | 2014-11-06 | 2016-08-24 | 童必炎 | Method for recycling tung seed press cakes to convert into biodiesel |
Citations (2)
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|---|---|---|---|---|
| CN1294128A (en) * | 2000-10-30 | 2001-05-09 | 李国荣 | Process for preparing phytic acid |
| CN1724545A (en) * | 2005-07-08 | 2006-01-25 | 刘秀丽 | Improved method for extracting phytic acid |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1294128A (en) * | 2000-10-30 | 2001-05-09 | 李国荣 | Process for preparing phytic acid |
| CN1724545A (en) * | 2005-07-08 | 2006-01-25 | 刘秀丽 | Improved method for extracting phytic acid |
Non-Patent Citations (2)
| Title |
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| 佘珠花等.溶剂萃取脱酸前后麻疯树籽油脂肪酸组成分析.《粮食与油脂》.2005,(第7期),30-31. * |
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