CN1013438B - Process for preparing phytin, phytic acid and inositol - Google Patents
Process for preparing phytin, phytic acid and inositolInfo
- Publication number
- CN1013438B CN1013438B CN 86102238 CN86102238A CN1013438B CN 1013438 B CN1013438 B CN 1013438B CN 86102238 CN86102238 CN 86102238 CN 86102238 A CN86102238 A CN 86102238A CN 1013438 B CN1013438 B CN 1013438B
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- CN
- China
- Prior art keywords
- phytin
- inositol
- exchange resin
- present
- phytic acid
- 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.)
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Abstract
The present invention relates to a method for industrially producing phytin used as a raw material of inositol, and a method for preparing phytic acid and inositol from phytin. The present invention has the technical scheme that the phytin is absorbed and is separated by anion exchange resin, and the phytin is recovered by alkali elution. The impurities of protein in the phytin is less than that of the existing method, and thus, the burden of the post processes can be lightened, and high recovery rate can be obtained; in addition, the present invention has the advantage that high-purity and high-quality inositol can be economically obtained.
Description
The present invention relates to industrial favourable manufacture method as the phytin of inositol raw material, and the manufacture method of producing phytic acid or inositol by phytin.
Phytin almost is present in potassium, the magnesium double salt of the phosphoric acid ester (phytic acid) that contains a large amount of inositols in all sites of plant materials, particularly seed.
Inositol is except existing with unbound state in the muscle of animal body, heart, liver, and it still as the constituent of phospholipid, is present in the material in mammiferous liver, brain and yolk, soybean, the wheatgerm.
Inositol is important material as a kind of of VITAMIN concerning higher animal, plays an important role in fat, cholesteric metabolism, demonstrates the effect of lipotropism liver, is being effective aspect liver cirrhosis disease, the mistake hypercholesterolemia.Therefore, in recent years, in countries such as the U.S., being used for the nutritive food aspect is just at noticeable useful matter.
In the past, inositol is to adopt the general method manufacturing, promptly use inorganic or organic acid, from rice bran class raw material, extract phytin, then in order to remove protein in the extracting solution, hydrocarbon polymer etc., earlier, pressurize, add water decomposition and make inositol dissociate out with the phytin precipitation and after separating respectively, then through refining, concentrate, operation such as crystallization makes inositol.
In the above method, have and adopt so that phytin precipitates as means, method with an organic solvent, the method for use water-soluble metal salt (iron(ic) chloride, manganous sulfate etc.), the method for use water-soluble alkali etc.
When producing phytin with the method before above-mentioned, it is very difficult that phytin and impurity are fully separated, for example, from rice bran, using hydro-oxidation sodium in the extracting solution of acid extraction, ammoniacal liquor etc., carry out the method for filtering separation after being transferred to pH more than 7.5,, be difficult to its filtering separation because the throw out of phytin is the peptization pasty state.Other method, as with above-mentioned in extracting solution hydro-oxidation potassium, unslaked lime etc., when forming the sylvite of phytic acid and making it sedimentary method,, be difficult to it is removed because a large amount of co-precipitation of impurity of protein are got off.And have since POTASSIUM PHYTATE self also in the pasty state, when with whizzer it being concentrated, its nozzle is easy to stop up, or its is filtered shortcoming such as wait, operating rate is extremely low when cleaning separation.
According to above reason, more than which kind of occasion all can not in manufacturing process, fully remove protein etc., for this reason, the protein that contains in the inositol goods is many, causes quality of item to descend mostly.And in these methods, the amount of the calcium phosphate that produces as byproduct in the operation after phytin adds water decomposition is the several times of inositol, and its thin crystalline substance is very thin.Therefore, when handling respectively, the amount of the inositol that loses with it is very important, causes economically unfavorable thereby inevitable yield reduces.Simultaneously, the purity of byproduct itself is not high yet, sees from this respect to be difficult to economy yet.
Present inventors study repeatedly with regard to the problem of above-mentioned prior art, and the result proposes: contain phytin solution with anion exchange process, phytin is adsorbed on this anionite-exchange resin, put forward the method for phytin then with alkali cleaning.According to this method, from the phytin extracting solution, the operation of phytin precipitate and separate is not all wanted, thereby manufacturing process simplifies, the impurity such as protein of sneaking into during precipitate and separate can be few simultaneously.
And, can phytin be carried out desalting treatment with usual way, just can obtain highly purified phytic acid; Just can obtain highly purified inositol when pressurizeing water decomposition, dephosphorization, means system inositol such as refining with usual way.
The present invention's manufacture method is the solution that contains phytin with anion exchange process, the absorption phytin, produce the method for phytin then with the alkaline solution elution, this phytin is further carried out the method that desalting treatment is produced phytic acid with Zeo-karb etc., and the solution that contains phytin with anion exchange process, the absorption phytin, carry with alkali cleaning then and obtain phytin, with this phytin with usual way pressurize water decomposition, remove phosphoric acid, the refining manufacture method that obtains the inositol of inositol.
Among the present invention, the solution that what is called contains phytin is meant the acid extraction liquid of the phytin made from usual way, or with the corn steep liquor be main in addition suitably refining to it, concentrate and the material of other processing.Corn steep liquor is the sulfurous acid steeping fluid of corn, is a kind of acid extraction liquid, is the raw material commonly used that inositol is made in industry.Wherein contain usually and be equivalent to about 2%(solid) phytic acid or its esters of inositol.In addition, defatted rice bran etc. also are the raw materials that is suitable for making inositol, extract it with 1% aqueous sulfuric acid, and the material behind the residue is removed in use.
The solution that will contain these phytins is by anionite-exchange resin, with phytin absorption thereon.The anionite-exchange resin of usefulness is that CO is arranged herein
3Type, CH
3COO type, Cl type, SO
3Type or OH type exchange group and reproducible anionite-exchange resin are all right, from aspects such as phytin adsorptivity and selectivity, especially with Cl type, SO
3Type is suitable.Except that the anionite-exchange resin these, also can be used for the object of the invention, but therefore the aspects such as removal effect of impurity such as phytin adsorptivity, protein we can say that not as good as above-mentioned resin it is disadvantageous using above-mentioned anionite-exchange resin in addition in practicality.Because the difference of the kind of anionite-exchange resin, aspects such as the phytin rate of recovery are variant, as described later shown in the experimental example.OH type anionite-exchange resin in above-mentioned also has the advantage of simplifying treatment scheme except aforementioned effect is arranged.
The anionite-exchange resin that the present invention uses, be the Amberlite IR-45 that sells on the market, IRA-68, IRA-93, IRA-410, IRA-411(is above be オ Le ガ ノ Co., Ltd. system), Diaion resin SA 20A, SA21A, WA30, WA10, WA11(is above be Japanese experienced Water Co., Ltd system), the above Dowex of Dowex MSA-1, MSA-266(Co., Ltd. system).
The ion exchange resin treatment condition must be led suitable selection according to kind, the character of the quality of the characteristic, the purpose product inositol that contain the solution of phytin or the ion exchange resin that uses, generally, in 5～20 ℃ of temperature, pH1～5, strength of fluid 1～40% is by the speed (SV: the amount of liquid that per hour passes through/ion exchange resin capacity) select in 0.5～20 the scope of liquid.
After using suitable warm water cleaning through the phytin polymeric adsorbent of adsorption treatment like this, from resin, phytin is proposed with alkali cleaning.Used alkali is the aqueous solution such as ordinary hydrogen sodium oxide, potassium hydroxide or ammoniacal liquor, uses other alkali also harmless.The elution process condition, much less, be to change according to the alkali kind of using, concentration of aqueous solution, the kind of ion exchange resin, characteristic and other situation of stock liquid, when for example selecting sodium hydroxide, concentration is about 1～30% the aqueous solution, room temperature～70 ℃, logical liquid speed are (SV) 0.5～10, the pH of eluant are maintained to handle under 9～12 the condition be suitable.Obtain eluant like this and mainly be made up of the phytic acid sodium salt, impurity such as protein that wherein contains and carbohydrate are few, the burden after therefore can alleviating greatly in the operation.
The phytin eluant that obtains like this, subsequently with usual way through adding water decomposition, dephosphorization hydrochlorate, refining, concentrate, operation processing such as crystallization, obtain finished product inositol and byproduct phosphoric acid salt.Can obtain the byproduct Sodium phosphate dibasic when using sodium hydroxide.
If spent ion exchange resin is handled and made the desalination of above-mentioned phytin eluant, can also obtain phytic acid.
Embodiments of the invention below are shown.
Embodiment 1
(3.5 Baumes (baume), pH4.1, conversion inositol content are 2.0kg/m with the corn steep liquor of 150l
3), the intermediate base anion exchange resin regeneration is being become in the 75l resin of Cl type with hydrochloric acid, with the logical liquid of the speed of SV4, and the absorption phytin.After the resin back washing that will adsorb phytin with warm water is cleaned, be that 1 speed feeds 15% aqueous sodium hydroxide solution wherein with SV, obtain being approximately the sodium phytate extracting solution of 12l.Concentrate this extracting solution then, making the content of sodium phytate reach the content that 43～48%(is converted into inositol is 8.5～9.5%), the pressurization of carrying out in autoclave again 180 ℃, 3 hours adds water decomposition, and the decomposed solution that obtains is filtered, and removes water-insoluble salts such as calcium phosphate contained in the decomposed solution, magnesium.Because phosphoric acid disodium hydrogen in the filtrate, after utilizing crystallization operation that it is separated, removes, spent ion exchange resin decolours, desalting treatment, inositol content are concentrated to about 25%, carrying out powder activated carbon again handles, crystallization goes out to have the inositol salt of 2 parts of water then, and vacuum-drying obtains the anhydrous inositol (moisture is below 0.5%) of about 250g.Product is impure hardly.The Sodium phosphate dibasic crystallization that obtains in the operation is about 6kg, and it can be used as by-product utilization.
Embodiment 2
In the extracting solution of 1% aqueous sulfuric acid of 10kg defatted rice bran, add the liquid that obtains with the clean once more aforementioned extraction residue of 0.3% aqueous sulfuric acid and be total to 100l, be that 2 speed is by the Cl type anionite-exchange resin identical with embodiment with SV, the absorption phytin, after with warm water it being cleaned, with SV be 1 speed by 10% sodium hydroxide solution, obtain the eluant of about 15l sodium phytate.Obtain about 206 grams of refining anhydrous inositol with embodiment 1 same operation.
Embodiment 3
In the 13l corn steep liquor, add 35% hydrochloric acid 100ml, with the solution of gained with SV be 2 speed by 1lOH type anionite-exchange resin (Amberlite IRA-93), the absorption phytin.Below processing is identical with embodiment 1, obtains purified inositol 22g.
Embodiment 4
The eluant of the sodium phytate that embodiment 1 or embodiment 2 are made is 2 the speed OH type ion exchange resin (Amberlite IR-120B, DiaioN resin SK1B, Dowex 88 etc.) by 4l with SV, and desalting treatment is concentrated to about 55% with it.Make its decolouring with Powdered Activated Carbon, obtain 50% phytic acid 1340g.The phytic acid that obtains has high purity.
Among the present invention, need be with the very complicated phytin precipitate and separate operation of pre-treatment, as long as simple adsorption operations can directly be isolated phytin from the phytin extracting solution.In this absorption process owing to used CO
3Type, CO
3COO type, Cl type, SO
3Type, OH type anionite-exchange resin, can be selectively fractionation by adsorption phytin efficiently.Therefore fully can method be the sort of will free the filtering complex process of colloidal sol pasty state throw out from existing, and impurity major part such as protein remains in the extracting solution, and sneak into few in the phytin, thereby alleviated the burden of back operation, can make high-purity high-quality inositol goods economically simultaneously.
Below example illustrates effect of the present invention by experiment.
Experimental example
Use each 20l of corn steep liquor, separate phytin, the inositol rate of recovery more separately, the protein content in the regenerant with following the whole bag of tricks.Corn steep liquor is that pH4.1, concentration are 7.7%, contain the material of 2% inositol approximately as used herein.
With the organophosphorus in the phytin as phytic acid (C
6H
18O
24P
6, molecular weight 660) calculate as phytic acid, again it is converted into inositol (C
6H
12O
6, molecular weight 180) just can obtain inositol.
(1) existing method
Add potassium hydroxide (15%) in corn steep liquor, be adjusted to pH6.0, make the calcium precipitation of phytin, the warm water 1.5l with 50 ℃ after it is separated cleans, and promptly obtaining phytin (regarding phytic acid ca as) 249g(is inositol 34.1g).
(2) method of the present invention 1.
Get OH type anionite-exchange resin IRA-411(オ Le ガ ノ Co., Ltd. system) regeneration CO
3The resin 1l of type passes through above-mentioned resin with the speed of SV4 with corn steep liquor solution, with phytin absorption thereon.After with 50 ℃ of warm water 1.5l it being cleaned then, being that 1 speed goes out phytin by aqueous sodium hydroxide solution (7%) and elution with SV, is 18.8g thereby obtain the inositol that the every 1l resin of phytin (can regard sodium phytate as) 115g(makes).
(3) method of the present invention 2.
1. identical with the present invention, get the exchange group regeneration CH of anionite-exchange resin
3The resin 1l of COO type handles equally, and elution goes out phytin, obtains phytin (inositol that every 1l resin makes is 16.5g) 92g.
(4) the inventive method 3.
Get OH type anionite-exchange resin IRA-68(オ Le ガ ノ Co., Ltd. system) the resin 1l of regeneration Cl type, treatment process is identical with the present invention 1, and elution goes out phytin, obtaining the inositol that phytin 212g(makes is every 1l34.8g).
(5) method of the present invention 4.
3. identical with the present invention, use regeneration SO
3The anionite-exchange resin of type carries out same processing, and obtaining the inositol that the every 1l resin of phytin 219g(makes is 35.9g)
(6) method of the present invention 5.
Use OH type anionite-exchange resin IRA-411, handling equally and obtaining the inositol that the every 1l resin of phytin 106g(makes is 17.3g).
The result is as follows.
The thick inositol rate of recovery of method * * * protein containing ratio
Existing method 94.2% 73.5%
Method of the present invention 1. 51.9% 1.7%
Method of the present invention 2. 45.6% 1.4%
Method of the present invention 3. 96.1% 0.8%
Method of the present invention 4. 99.2% 1.2%
Method of the present invention 5. 47.8% 2.1%
* the phytin that reclaims is converted into inositol, uses with respect to the percentage of the inositol in the corn steep liquor and represent it.
* uses with respect to the percentage of the inositol conversion amount that reclaims phytin and represents to reclaim protein content in the phytin.
Can know according to above result and to find out,, use anionite-exchange resin according to the present invention, the fractionation by adsorption phytin, the phytin that uses alkali to reclaim with the elution method, more much lower as the protein content of impurity than existing methods.And, with exchange group regeneration Cl, the SO of anionite-exchange resin
3Resin etc. type can obtain the extra high rate of recovery.
Claims (2)
1, the manufacture method of phytin is characterized in that, contains the solution of phytin with anion exchange process, and the absorption phytin puts forward with alkali cleaning then.
2, the manufacture method of phytic acid is characterized in that, contains the solution of phytin with anion exchange process, carries the phytin that obtains with alkali cleaning then, makes phytic acid through common desalting treatment, method such as refining.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 86102238 CN1013438B (en) | 1984-08-24 | 1986-03-01 | Process for preparing phytin, phytic acid and inositol |
| CN 90110253 CN1026693C (en) | 1986-03-01 | 1986-03-01 | Process for preparing inositol |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59177303A JPS6156142A (en) | 1984-08-24 | 1984-08-24 | Production of phytin, phytic acid and inositol |
| CN 86102238 CN1013438B (en) | 1984-08-24 | 1986-03-01 | Process for preparing phytin, phytic acid and inositol |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 90110253 Division CN1026693C (en) | 1986-03-01 | 1986-03-01 | Process for preparing inositol |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN86102238A CN86102238A (en) | 1988-04-20 |
| CN1013438B true CN1013438B (en) | 1991-08-07 |
Family
ID=25742190
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 86102238 Expired CN1013438B (en) | 1984-08-24 | 1986-03-01 | Process for preparing phytin, phytic acid and inositol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1013438B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105001257A (en) * | 2015-06-03 | 2015-10-28 | 山东大宗生物开发股份有限公司 | Method for extracting calcium-magnesium phytate from corn soaked liquid |
| CN106629790B (en) * | 2016-09-27 | 2018-07-17 | 中南大学 | A method of separation is containing magnesium lithium in magnesium, lithium solution |
| CN113980047B (en) * | 2021-10-15 | 2023-08-18 | 山东寿光巨能金玉米开发有限公司 | Preparation method of phytic acid |
-
1986
- 1986-03-01 CN CN 86102238 patent/CN1013438B/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| CN86102238A (en) | 1988-04-20 |
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