CN104045665A - Separation and purification method for phytine - Google Patents
Separation and purification method for phytine Download PDFInfo
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- CN104045665A CN104045665A CN201410259930.9A CN201410259930A CN104045665A CN 104045665 A CN104045665 A CN 104045665A CN 201410259930 A CN201410259930 A CN 201410259930A CN 104045665 A CN104045665 A CN 104045665A
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- phytin
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Abstract
The invention relates to a separation and purification method for phytine, which specially comprises the following steps: (1) sedimentation processing; (2) resin adsorption; (3) desorption elution; (4) neutralization and precipitation; and (5) sheet frame filtering. According to the invention, the insoluble protein content of corn water is greatly reduced, the problem the hybridization column is blocked by corn water is completely solved, the protein content of phytine is reduced, and the quality and yield of phytine are further improved. And through the adoption of a novel adsorption resin, the yield of products is significantly improved.
Description
Technical field
The present invention relates to a kind of production method of Phytin, be specifically related to a kind of separation purification method of producing Phytin from soak water of maize.
Background technology
Utilizing corn water or rice bran extract to produce Phytin is the main method that current domestic industry is produced inositol raw material.Its concrete production method is mainly divided into two kinds of Traditional Method and fractionation by adsorption.
Traditional Method adopts and directly in corn water, adds unslaked lime to generate Phytin, causes waste water cannot continue to utilize, and pollutes large.And although general resin adsorption method has overcome some pollution problems of Traditional Method, but because the great amount of soluble albumen in corn water very easily causes the obstruction of polymeric adsorbent, need a large amount of artificial and time to clean, also can bring the decline of Phytin output yield simultaneously.Albumen in corn water also can cause the very easily fouling of the follow-up enrichment process of starch factory, and need to clean concentration and evaporation equipment every day, and working efficiency is lower.
The present invention adopts corn water is flowed to tank by speed, and sedimentation impurity, can reduce insoluble protein content in corn water greatly, thoroughly solves corn water slug from the problem of handing over post, and reduces protein content in Phytin, further improves quality and the yield of Phytin.Because the reduction of protein content in corn water significantly improves follow-up Waste water concentrating scale problems, reduced waste water to the pollution to environment.The present invention has adopted novel polymeric adsorbent simultaneously, significantly improves product yield.
Summary of the invention
For solving current production technique problem, the invention provides a kind of Phytin separation purification method, the method is processed corn water by sedimentation in early stage albumen, adopt New Polymeric Adsorbent to improve product yield.Solve the concentrated difficult problem of follow-up corn water simultaneously.
The separation purification method that the invention provides a kind of Phytin, concrete steps comprise:
(1) sedimentation is processed: corn waste water is flowed to tank by speed, sedimentation impurity, 8 ~ 10 hours settling times, bottom underflow is separated by horizontal screw centrifuge, remove water-insoluble protein and particulate matter, this partial material is rich in the nutritive ingredients such as albumen, can further be processed as feed.
Speed stream tank principle of work: feed liquid is entered with tangential direction by cylindrical portions, rotates and produces centrifugal force, comes downwards to tapered segment more violent.The liquid that solids in feed liquid or density are larger is subject to the effect of centrifugal force to be thrown to wall, and presses spiral-line downstream to outlet (underflow) along wall.That in the liquid of clarification or liquid, carries rises compared with fine particle, by the outlet overflow at center, is gone out.
(2) resin absorption: the corn soaking waste water after sedimentation enters resin column, resin model is D315, flow rate control is at 2 ~ 3 times of column volumes per hour and resin Contact-sorption, ratio of adsorption scope 1:15 ~ 20 of resin and waste water, corn soaking waste water after resin absorption returns to corn soaking waste water back pool, then come back to the concentrating unit of corn waste water, continue evaporation concentration.This process only extracts phytic acid, does not change the content of effective constituent in original corn soaking waste water.
(3) resolve wash-out: the hydrochloric acid eluent wash-out by the resin after absorption by mass concentration 5 ~ 8%, elution speed is controlled at 2 ~ 3 times of column volumes per hour, elution time 2 ~ 3 hours.With 1 ~ 2 times of column volume tap water, clean resin, be mixed to get elutriant.
(4) neutralization, precipitation: the neutralizing agent Ca (OH) that adds mass concentration 10-20% in elutriant
2solution, is neutralized to elutriant ph value 7, obtains Phytin precipitation mixed solution.
(5) Plate Filtration: filter and be divided into two-stage, one-level press filtration is by the Phytin solid substance initial gross separation in Phytin mixed solution out, elementary filtrate recycle is in preparation eluent, neutralizing agent; After the isolated Phytin of one-level press filtration washs again with 2 ~ 4 times of clear water, send into secondary press filtration, isolate purer Phytin, the same recovery of secondary filtrate is used for preparing eluent, neutralizing agent.Filtrate recycle is conducive to reduce fresh water usage quantity, in addition can be by ion effective recycling.Phytin after secondary press filtration can be used for the hydrolysis of inositol and produces.
The present invention prepares Phytin not changing under the nature of corn soaking waste water and the prerequisite of purposes, greatly reduce insoluble protein content in corn water, thoroughly solve the problem of corn water slug ion exchange resin, and reduce protein content in Phytin, further improve the quality of Phytin, improve the yield of inositol, reduce waste water to the pollution to environment.
Embodiment
Further illustrate detailed content of the present invention and embodiment thereof below.Should be appreciated that specific embodiment described herein is only for explaining the present invention, and be not used in restriction invention.
embodiment 1:
Corn water directly enters ion exchange resin column without the removal of impurities of speed stream tank, in turn includes the following steps:
absorption: get the soak water of maize 105m3 of organophosphorus content 0.6%, enter 7 tons of anionite-exchange resin of handling well are housed, resin model D305, loading flow rate control is at 2 times of column volumes per hour.
resolve wash-out: with pressurized air, blow off the corn water remaining in pillar, enter 1 times of column volume tap water in the other direction, the hydrochloric acid of preparation 5% is with the speed wash-out resin of 2 times of column volumes per hour, elution time 2 hours, with pressurized air, blow off the elutriant in pillar again, with 1 times of column volume tap water, clean resin, be mixed to get elutriant.
neutralization: the suspension liquid with calcium hydroxide preparation 10%, progressively regulates elutriant to pH7.
plate Filtration is divided into two-stage, and one-level press filtration is by the Phytin solid substance initial gross separation in Phytin mixed solution out, and the recovery of elementary filtrate is used for preparing eluent, neutralizing agent; After the isolated Phytin of one-level press filtration washs again with 2 times of clear water, send into secondary press filtration, isolate purer Phytin.Oven dry obtains Phytin 1502.96kg, detects organophosphorus content 37.21%, protein content 2.1%, yield 88.77%.
embodiment 2:
Corn water first enters ion exchange resin column again through the removal of impurities of speed stream tank, in turn includes the following steps:
get the soak water of maize 105m3 of organophosphorus content 0.6%, through speed stream tank sedimentation 8 hours.
absorption: supernatant liquor enters 7 tons of anionite-exchange resin of handling well are housed, resin model D305, loading flow rate control is at 2 times of column volumes per hour.
resolve wash-out: with pressurized air, blow off the corn water remaining in pillar, enter 1 times of column volume tap water in the other direction, the hydrochloric acid of preparation 5% is with the speed wash-out resin of 2 times of column volumes per hour, elution time 2 hours, with pressurized air, blow off the elutriant in pillar again, with 1 times of column volume tap water, clean resin, be mixed to get elutriant.
neutralization: the suspension liquid with calcium hydroxide preparation 10%, progressively regulates elutriant to pH7.
5. Plate Filtration is divided into two-stage, and one-level press filtration is by the Phytin solid substance initial gross separation in Phytin mixed solution out, and the recovery of elementary filtrate is used for preparing eluent, neutralizing agent; After the isolated Phytin of one-level press filtration washs again with 2 times of clear water, send into secondary press filtration, isolate purer Phytin.Oven dry obtains Phytin 1492.79kg, detects organophosphorus content 39.35%, protein content 0.56%, yield 93.24%.
embodiment 3:
Corn water first enters ion exchange resin column again through the removal of impurities of speed stream tank, in turn includes the following steps:
get the soak water of maize 105m3 of organophosphorus content 0.6%, through speed stream tank sedimentation 8 hours.
absorption: supernatant liquor enters 7 tons of anionite-exchange resin of handling well are housed, resin model D315, loading flow rate control is at 2 times of column volumes per hour.
resolve wash-out: with pressurized air, blow off the corn water remaining in pillar, enter 1 times of column volume tap water in the other direction, the hydrochloric acid of preparation 5% is with the speed wash-out resin of 2 times of column volumes per hour, elution time 2 hours, with pressurized air, blow off the elutriant in pillar again, with 1 times of column volume tap water, clean resin, be mixed to get elutriant.
neutralization: the suspension liquid with calcium hydroxide preparation 10%, progressively regulates elutriant to pH7.
5. Plate Filtration is divided into two-stage, and one-level press filtration is by the Phytin solid substance initial gross separation in Phytin mixed solution out, and the recovery of elementary filtrate is used for preparing eluent, neutralizing agent; After the isolated Phytin of one-level press filtration washs again with 2 times of clear water, send into secondary press filtration, isolate purer Phytin.Oven dry obtains Phytin 1400.1kg, detects organophosphorus content 43.26%, protein content 0.54%, yield 96.14%.
embodiment 4:
Corn water first enters ion exchange resin column again through the removal of impurities of speed stream tank, in turn includes the following steps:
get the soak water of maize 140m3 of organophosphorus content 0.6%, through speed stream tank sedimentation 10 hours.
absorption: supernatant liquor enters 7 tons of anionite-exchange resin of handling well are housed, resin model D315, loading flow rate control is at 3 times of column volumes per hour.
resolve wash-out: with pressurized air, blow off the corn water remaining in pillar, enter 1 times of column volume tap water in the other direction, the hydrochloric acid of preparation 8% is with the speed wash-out resin of 3 times of column volumes per hour, elution time 3 hours, with pressurized air, blow off the elutriant in pillar again, with 1 times of column volume tap water, clean resin, be mixed to get elutriant.
neutralization: the suspension liquid with calcium hydroxide preparation 20%, progressively regulates elutriant to pH7.
5. Plate Filtration is divided into two-stage, and one-level press filtration is by the Phytin solid substance initial gross separation in Phytin mixed solution out, and the recovery of elementary filtrate is used for preparing eluent, neutralizing agent; After the isolated Phytin of one-level press filtration washs again with 4 times of clear water, send into secondary press filtration, isolate purer Phytin.Oven dry obtains Phytin 1900.32kg, detects organophosphorus content 42.93%, protein content 0.51%, yield 97.12%.
embodiment 5:
Corn water first enters ion exchange resin column again through the removal of impurities of speed stream tank, in turn includes the following steps:
get the soak water of maize 119m3 of organophosphorus content 0.6%, through speed stream tank sedimentation 10 hours.
absorption: supernatant liquor enters 7 tons of anionite-exchange resin of handling well are housed, resin model D315, the ratio of adsorption scope 1:17 of resin and waste water, loading flow rate control is at 3 times of column volumes per hour.
resolve wash-out: with pressurized air, blow off the corn water remaining in pillar, enter 1 times of column volume tap water in the other direction, preparation, 6.5% hydrochloric acid is with the speed wash-out resin of 2 times of column volumes per hour, elution time 3 hours, with pressurized air, blow off the elutriant in pillar again, with 1 times of column volume tap water, clean resin, be mixed to get elutriant.
neutralization: the suspension liquid with calcium hydroxide preparation 16%, progressively regulates elutriant to pH7.
5. Plate Filtration is divided into two-stage, and one-level press filtration is by the Phytin solid substance initial gross separation in Phytin mixed solution out, and the recovery of elementary filtrate is used for preparing eluent, neutralizing agent; After the isolated Phytin of one-level press filtration washs again with 3 times of clear water, send into secondary press filtration, isolate purer Phytin.Oven dry obtains Phytin 1593.93kg, detects organophosphorus content 44.15%, protein content 0.49%, yield 98.56%.
By speed, being flowed tank sedimentation processing and adopted model is the resin of D315 model, and quality product and yield are significantly improved.
Claims (7)
1. a separation purification method for Phytin, is characterized in that: comprise the steps:
(1) sedimentation is processed; (2) resin absorption; (3) resolve wash-out; (4) neutralization, precipitation;
(5) Plate Filtration.
2. method for purifying and separating as claimed in claim 1, it is characterized in that: described step (1) sedimentation is flowed tank by corn waste water by speed, sedimentation impurity, 8 ~ 10 hours settling times in processing, bottom underflow is separated by horizontal screw centrifuge, removes water-insoluble protein and particulate matter.
3. the method for purifying and separating as described in claim 1-2 any one, is characterized in that: described step (2)
In resin absorption, resin model is D315, and the corn soaking waste water after sedimentation enters resin column, and flow rate control is at 2 ~ 3 times of column volumes per hour and resin Contact-sorption, ratio of adsorption scope 1:15 ~ 20 of resin and waste water.
4. the method for purifying and separating as described in claim 1-3 any one, is characterized in that: described step (3)
The hydrochloric acid eluent of mass concentration 5 ~ 8% for resin in parsing wash-out after absorption, elution speed is controlled at 2 ~ 3 times of column volumes per hour, and elution time 2 ~ 3 hours is cleaned resin with 1 ~ 2 times of column volume tap water, is mixed to get elutriant.
5. the method for purifying and separating as described in claim 1-4 any one, is characterized in that: described step (4)
In neutralization, precipitation, neutralizing agent is the Ca (OH) of mass concentration 10 ~ 20%
2solution adds neutralizing agent solution in elutriant, is neutralized to elutriant ph value 7, obtains Phytin precipitation mixed solution.
6. the method for purifying and separating as described in claim 1-5 any one, is characterized in that: described step (5)
Plate Filtration is divided into two-stage, and one-level press filtration is by the Phytin solid substance initial gross separation in Phytin mixed solution out, and the recovery of elementary filtrate is used for preparing eluent, neutralizing agent; After the isolated Phytin of one-level press filtration washs again with 2 ~ 4 times of clear water, send into secondary press filtration, isolate purer Phytin.
7. a separation purification method for Phytin, is characterized in that: comprise the steps:
get the soak water of maize 119m3 of organophosphorus content 0.6%, through speed stream tank sedimentation 10 hours;
absorption: supernatant liquor enters 7 tons of anionite-exchange resin of handling well are housed, resin model D315, the ratio of adsorption scope 1:17 of resin and waste water, loading flow rate control is at 3 times of column volumes per hour;
resolve wash-out: with pressurized air, blow off the corn water remaining in pillar, enter 1 times of column volume tap water in the other direction, preparation, 6.5% hydrochloric acid is with the speed wash-out resin of 2 times of column volumes per hour, elution time 3 hours, with pressurized air, blow off the elutriant in pillar again, with 1 times of column volume tap water, clean resin, be mixed to get elutriant;
neutralization: the suspension liquid with calcium hydroxide preparation 16%, progressively regulates elutriant to pH7;
5. Plate Filtration is divided into two-stage, and one-level press filtration is by the Phytin solid substance initial gross separation in Phytin mixed solution out, and the recovery of elementary filtrate is used for preparing eluent, neutralizing agent; After the isolated Phytin of one-level press filtration washs again with 3 times of clear water, send into secondary press filtration, isolate purer Phytin.
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| CN201410259930.9A CN104045665B (en) | 2014-06-12 | 2014-06-12 | A kind of isolation and purification method of Phytin |
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| CN201410259930.9A CN104045665B (en) | 2014-06-12 | 2014-06-12 | A kind of isolation and purification method of Phytin |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106986749A (en) * | 2017-05-05 | 2017-07-28 | 吉林富利生物科技开发有限公司 | A kind of preparation method for crystallizing inositol |
| CN107416787A (en) * | 2017-05-15 | 2017-12-01 | 吉林富利生物科技开发有限公司 | A kind of method that calcium monohydrogen phosphate is produced using renewable plant phosphorus source |
| CN113135954A (en) * | 2021-04-24 | 2021-07-20 | 诸城市浩天药业有限公司 | Process method for preparing calcium phytate and calcium lactate by using corn soaking water |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106986749A (en) * | 2017-05-05 | 2017-07-28 | 吉林富利生物科技开发有限公司 | A kind of preparation method for crystallizing inositol |
| CN107416787A (en) * | 2017-05-15 | 2017-12-01 | 吉林富利生物科技开发有限公司 | A kind of method that calcium monohydrogen phosphate is produced using renewable plant phosphorus source |
| CN107416787B (en) * | 2017-05-15 | 2019-12-27 | 吉林富利生物科技开发有限公司 | Method for producing calcium hydrophosphate by utilizing renewable plant phosphorus source |
| CN113135954A (en) * | 2021-04-24 | 2021-07-20 | 诸城市浩天药业有限公司 | Process method for preparing calcium phytate and calcium lactate by using corn soaking water |
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