CN1073178A - A kind of method of extracting lipositol - Google Patents

A kind of method of extracting lipositol Download PDF

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Publication number
CN1073178A
CN1073178A CN 91111594 CN91111594A CN1073178A CN 1073178 A CN1073178 A CN 1073178A CN 91111594 CN91111594 CN 91111594 CN 91111594 A CN91111594 A CN 91111594A CN 1073178 A CN1073178 A CN 1073178A
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acid
nitric acid
rare nitric
raw material
product
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周武军
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Abstract

The present invention is used for a kind of method of extracting lipositol of plant seed especially for raw material deep processings such as the seeds of rice bran and other farm crop and wheat brans thereof.This method is earlier with the mixing acid of rare nitric acid or rare nitric acid lixiviate raw material at room temperature, filter out luxuriant and rich with fragrance butyrin product through alkali precipitation and acidolysis, neutralization, again behind the cryoconcentration of ion-exchange and decolouring and 60-90 ℃, get the inositol monophosphate fat prod of 75% above concentration, the pH value when wherein acidleach is with precipitation is respectively less than 4 and is controlled at 5-8.The present invention has product extraction yield height, good product quality, and technology is simple, is beneficial to industrialness production, and energy consumption is low and adapt to wide advantage.

Description

A kind of method of extracting lipositol
The present invention relates to from plant, extract the field of fat material, especially for a kind of method of extracting lipositol of crop seeds class and wheat bran deep processing thereof.
Recognize in " under the chemical industry small commodity production method (the 3rd collection) " book by in March, 1991 publication of Hunan science tech publishing house, have and a kind ofly from rice sugar, extract phytic acid (formal name used at school lipositol with dilute hydrochloric acid, referring to 83-84 page or leaf " 30; degreasing rice sugar extracts phytic acid "), phytic acid ca (the luxuriant and rich with fragrance fourth of formal name used at school, be the work in-process of phytic acid, referring to the 85th page " 32; rice sugar extracts medicinal phytic acid ca ") method (under be called for short the salt acid system), according to my practical experience and the relevant knowwhy of being grasped, think that the salt acid system that this book is introduced has following defective: the one, it is more to influence factor of production, such as selecting more auxiliary agent for use and need producing by Various Seasonal, or the like, thereby make complex process and flow process longer, be not easy to industrialness production; The 2nd, the product extraction yield is lower, its mean value is only got by the theoretical mean 12% of the 84th page of numeral that " relatively the yield of rice sugar is 8% " be provided in the book divided by the luxuriant and rich with fragrance fourth content of rice bran for this value of 66.7%(, i.e. 8 ÷ 12=0.66 67=66.7%), thus influenced the use value of product; The 3rd, quality product is relatively poor, and this can draw this conclusion from " being concentrated into the liquid finished product that concentration reaches 48-53% at last ", has more reduced the use value of product thus.In addition, this salt acid system also exists and the conflicting problem of well-known theory adjusting pH value and keeping thickening temperature at aspects such as 110 ℃.
The objective of the invention is at above-mentioned defective, a kind of method of extracting lipositol is provided, this method can be effectively, kind subclass and the wheat bran thereof to farm crop carries out deep processing easily, thereby obtain inositol monophosphate fat prod of many uses, that market is in great demand.
The objective of the invention is to realize: adopt acidleach to put forward the mode of raw material by following scheme, raw material is through rice bran after pulverizing or kind subclass and the wheat bran thereof of other farm crop, at room temperature use rare nitric acid or by the mixing acid lixiviate raw material of rare nitric acid and another diluted acid compatibility, precipitate through alkaline purification, filter back De Feiding crude product, acidolysis again, neutralization filter luxuriant and rich with fragrance butyrin product, then by ion-exchange and decolouring processing, and behind the cryoconcentration, promptly get the liquid inositol monophosphate fat prod of 75% above concentration, in leaching process, some processing parameter is that the acidleach pH value is less than 4, pH value should be controlled at 5-8 during precipitation, and the cryoconcentration temperature should be controlled at 60-90 ℃.
Above-mentioned mixing acid, its percentage concentration can be 0.5-1.5, and its component can have rare nitric acid and dilute hydrochloric acid, and both blended volume percent are (10-90): (90-10), rare nitric acid and thin planting acid also can be arranged, and both blended volume percent are (90-10): (10-90).First liquid before thin planting acid can be taken from cryoconcentration, after the decolouring.
When the above-mentioned rare nitric acid lixiviate of independent employing raw material, the percentage concentration of rare nitric acid can be 0.5-1, with 0.7 for well.
The present invention has adopted the mixing acid of rare nitric acid or rare nitric acid owing to find a new way, at room temperature, and the technology of the raw material after lixiviate is pulverized, so advantage is obvious: one, product extraction yield height can reach more than 88%; Its two, good product quality, the product concentration after concentrating can reach more than 75%, is higher than the practical concentration 65% of commercially available prod; Its three, technology is simple, flow process shortens, and can be regardless of conventional production in season, thereby has reduced the factor that influence is produced, and helps the big production of industrialness; Its four, energy consumption is low, need not heat and carry out diluted acid lixiviate raw material, and cost is reduced; Its five, adapt to wide, can be to the rice bran deep processing after pulverizing, also can be to the kind subclass of other farm crop after pulverizing, as wheat, another name for Sichuan Province (being corn) grain (being millet, jowar), beans etc. and their wheat bran carry out deep processing.In addition, adopt the mixing acid of rare nitric acid and thin planting acid, also have some advantages, do not need to add other bronsted lowry acids and bases bronsted lowry in addition, do not have the discharging of alkali acid waste liquid, flow process can further shorten, and makes quality product guaranteed.
Accompanying drawing is a process flow diagram of the present invention.
The invention will be further described below in conjunction with embodiment and accompanying drawing thereof:
The present invention is provided with the mixed acid process of rare nitrate method (I method) and rare nitric acid, and the latter can divide rare nitric acid to add the watery hydrochloric acid method (II method) and rare nitric acid add rare phytic acid method (III method). These three kinds of methods can also can confuse separately carries out deep processing to the raw material after pulverizing. Their concentration and mixed volume percentage see Table one, table two.
Technological process is as shown in drawings: above-mentioned " I ", " II " method can be walked by the solid line flow process, and " III " method can be walked by the dotted line flow process. Rare phytic acid source of " III " method, the first liquid of part of taking from bleaching process in front two methods (flow to enrichment process under the first liquid of residue, form product), this first liquid is made into earlier the working solution of " III " method with the rare nitric acid that increases, together return again into diluted acid lixiviate operation, the sedimentation and filtration, acidolysis of then walking around later on " I ", " II " method filter and in and filter progress, and directly enter ion-exchange and bleaching process, form just liquid. This first liquid divided again for two steps flowed to, and a part becomes the additional source of rare phytic acid of " III " method as previously mentioned, and another part residue just liquid flows to enrichment process under then continuing, the formation product. Go round and begin again, rare phytic acid and the final product of output lipositol constantly are provided.
Embodiment:
The present invention divides extraction, purifying and the lipositol three big steps of luxuriant and rich with fragrance fourth:
One, the extraction of luxuriant and rich with fragrance fourth
Comprise raw material, pulverizing, diluted acid lixiviate and sedimentation and filtration four operations.
1, raw material: can select rice bran (present embodiment selects for use rice bran to make raw material) for use, perhaps select the class of having planted of other farm crop for use, as wheat, another name for Sichuan Province, grain, beans etc. and wheat bran thereof.
2, pulverize: after raw material pulverizing, cross 20 mesh sieves.
3, diluted acid lixiviate: raw material after will pulverizing drops into pH value less than in 4 the diluted acid, in stirring at room 2 hours, and suction filtration De Feiding extracting solution.Used diluted acid concentration fourth extraction yield luxuriant and rich with fragrance with it relation sees Table one, table two.
4, sedimentation and filtration: with luxuriant and rich with fragrance fourth extracting solution alkali precipitation, after filtering white luxuriant and rich with fragrance fourth crude product.Used bases, concentration and luxuriant and rich with fragrance fourth extraction yield see Table three, wherein with method two for well, best pH value is 6.5, deposition rate is 96.3%.
Two, luxuriant and rich with fragrance fourth purifying
Comprise that acidolysis is filtered, two-step is filtered in neutralization.
5, acidolysis is filtered: with the luxuriant and rich with fragrance fourth crude product of vitriolization, behind the stirring and dissolving suction filtration, get faint yellow luxuriant and rich with fragrance fourth solution.
6, neutralization is filtered: add alkali, the pH value that makes faint yellow luxuriant and rich with fragrance fourth solution is 6, after stirring suction filtration, gets luxuriant and rich with fragrance butyrin product.
Three, lipositol is produced
Comprise ion-exchange, decolouring, cryoconcentration three operations.
7, ion-exchange: add the storng-acid cation exchange resin of about equivalent, behind the luxuriant and rich with fragrance butyrin product of stirring and dissolving, make its clear liquid get weak yellow liquid by ion exchange column.
8, decolouring: use activated carbon decolorizing.
9, cryoconcentration: in the temperature evaporation concentration of 60-90 ℃ or 70-75 ℃ (better), (seeing Table four) more than 75% until finished product mysoinositol phosphoric acid fat content than the former with the rotation vacuum concentrator.
Table four has also shown the salt acid system that " I, II, III " of the present invention method all is better than the book from aspects such as extraction yield, output and augmentation ratio being carried with mass data, after combining this effect aspect three, its order of excellence is " II " method>" III " method>" I " method successively〉〉 the salt acid system.
Table one. dilute acid concentration (%) and luxuriant and rich with fragrance fourth extraction yield relation
Method Dilute acid concentration (%) Luxuriant and rich with fragrance fourth extraction yield (%)
Scope Optimum value Scope Optimum value
I method (rare nitric acid) 0.5-1 0.7 75-83.3 83.3
II method (nitration mixture) 0.5-1.5 1 78-86 86
III method (nitration mixture) 0.5-1.5 1 76-85 85
Table two, the composition of mixed acid process and luxuriant and rich with fragrance fourth extraction yield relation
Figure 911115943_IMG1
Table three. luxuriant and rich with fragrance fourth deposition rate and pH value relation
Method The pH value territory Deposition rate (%)
1 2 3 10%(milk of lime+sodium hydroxide) 10% milk of lime, 10% sodium hydroxide 5-8 5-8 6-9 90-95.7 90-96.3 85-89.5
The salt acid system of table four, the present invention and prior art relatively
The item description Salt acid system (carrying in the book) Nitrate method (I method) Nitration mixture II method Nitration mixture III method
Raw rice bran heavy (g) 1700 1700 1700 1700
Luxuriant and rich with fragrance fourth content (average g) 200 200 200 200
Phytic acid content (average g) 91 91 91 91
Luxuriant and rich with fragrance fourth Extraction yield (%) 66.7 83.3 86 85
Output (g) 133.2 166.6 172 170
Phytic acid Extraction yield (%) 70 88.4 91 90.4
Output (g) 93.1 147.3 156.5 153.7
Augmentation ratio (%) 1 17.1 19.4 18.4

Claims (8)

1, a kind of method of extracting lipositol, be to carry raw material with acidleach, raw material is through rice bran after pulverizing or the kind subclass of other farm crop, it is characterized in that earlier with rare nitric acid or by the mixing acid of rare nitric acid and another diluted acid compatibility lixiviate raw material at room temperature, De Feiding crude product behind the alkaline purification sedimentation and filtration, acidolysis again, neutralization filters out luxuriant and rich with fragrance butyrin product, then by behind ion-exchange and decolouring processing and the cryoconcentration, promptly get the lipositol liquid product of 75% above concentration, some processing parameter is in leaching process, the acidleach pH value is less than 4, and pH value should be controlled at 5-8 during precipitation, and the cryoconcentration temperature should be controlled at 60-90 ℃.
2, method according to claim 1 is characterized in that described mixing acid is made up of rare nitric acid and dilute hydrochloric acid, and its percentage concentration is 0.5-1.5, and both blended volume percent are (10-90): (90-10).
3, method according to claim 1 is characterized in that described mixing acid is made up of the acid of rare nitric acid and thin planting, and its percentage concentration is 0.5-1.5, and both blended volume percent are (90-10): (10-90).
4, method according to claim 1, when it is characterized in that adopting separately rare nitric acid, the percentage concentration of rare nitric acid is 0.5-1.
5, method according to claim 4, the percentage concentration that it is characterized in that rare nitric acid is 0.7.
6, method according to claim 1, the pH value when it is characterized in that precipitating is 6.5.
7, method according to claim 1 is characterized in that the cryoconcentration temperature is 70-75 ℃.
8, method according to claim 1, the kind subclass that it is characterized in that described other farm crop is another name for Sichuan Province, grain, beans, or their wheat bran.
CN 91111594 1991-12-11 1991-12-11 A kind of method of extracting lipositol Pending CN1073178A (en)

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CN 91111594 CN1073178A (en) 1991-12-11 1991-12-11 A kind of method of extracting lipositol

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CN 91111594 CN1073178A (en) 1991-12-11 1991-12-11 A kind of method of extracting lipositol

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101602776B (en) * 2009-02-23 2011-07-27 杜江 Method for producing high-purity solid phytic acid
CN103450256A (en) * 2013-09-11 2013-12-18 无锡群硕谷唐生物科技有限公司 Comprehensive utilization method of defatted rice bran
WO2015089686A1 (en) * 2013-12-16 2015-06-25 刘登富 Preparation method for extracting calcium phytate from rice bran

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101602776B (en) * 2009-02-23 2011-07-27 杜江 Method for producing high-purity solid phytic acid
CN103450256A (en) * 2013-09-11 2013-12-18 无锡群硕谷唐生物科技有限公司 Comprehensive utilization method of defatted rice bran
WO2015089686A1 (en) * 2013-12-16 2015-06-25 刘登富 Preparation method for extracting calcium phytate from rice bran

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