CN104045665B - A kind of isolation and purification method of Phytin - Google Patents
A kind of isolation and purification method of Phytin Download PDFInfo
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- CN104045665B CN104045665B CN201410259930.9A CN201410259930A CN104045665B CN 104045665 B CN104045665 B CN 104045665B CN 201410259930 A CN201410259930 A CN 201410259930A CN 104045665 B CN104045665 B CN 104045665B
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- phytin
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- eluent
- semen maydis
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Abstract
The present invention relates to the isolation and purification method of a kind of Phytin, specifically include following steps: (1) settlement treatment；(2) resin absorption；(3) eluting is resolved；(4) neutralize, precipitate；(5) plate-and-frame filtration.The present invention greatly reduces insoluble protein content in Semen Maydis water, thoroughly solves the Semen Maydis water slug problem from friendship post, and reduces protein content in Phytin, improves quality and the yield of Phytin further.Have employed novel adsorbent resin simultaneously, significantly improve product yield.
Description
Technical field
The present invention relates to the production method of a kind of Phytin, be specifically related to a kind of isolation and purification method producing Phytin from soak water of maize.
Background technology
Utilizing Semen Maydis water or rice bran extract is the main method that current domestic industry produces inositol raw material to produce Phytin.Its concrete production method is broadly divided into Traditional Method and adsorbing separation two kinds.
Traditional Method uses the direct quick lime that adds in Semen Maydis water to generate Phytin, causes waste water to continue with, pollutes big.Although and general resin adsorption method overcomes some pollution problems of Traditional Method, but owing to the great amount of soluble albumen in Semen Maydis water easily causes the blocking of adsorbent resin, need substantial amounts of manually to clean with the time, also bring along the decline of Phytin yield yield simultaneously.Albumen in Semen Maydis water will also result in starch factory subsequent concentration operation easily fouling, needs every day to clean concentration and evaporation equipment, and work efficiency is relatively low.
The present invention uses Semen Maydis water by fast stream tank, settles impurity, can be substantially reduced insoluble protein content in Semen Maydis water, thoroughly solves the Semen Maydis water slug problem from friendship post, and reduces protein content in Phytin, improves quality and the yield of Phytin further.Owing to the reduction of protein content makes follow-up Waste water concentrating scale problems significantly improve in Semen Maydis water, reduce waste water to the pollution to environment.The present invention have employed novel adsorbent resin simultaneously, significantly improves product yield.
Summary of the invention
For solving current production technology problem, the invention provides a kind of Phytin isolation and purification method, Semen Maydis water is processed by the method by early stage sedimentation albumen, uses New Polymeric Adsorbent to improve product yield.Solve follow-up Semen Maydis water simultaneously and concentrate difficult problem.
The invention provides the isolation and purification method of a kind of Phytin, concrete steps include:
(1) settlement treatment: by Semen Maydis waste water by speed stream tank, settle impurity, 8 ~ 10 hours sedimentation times, bottom underflow is separated by horizontal screw centrifuge, removing water-insoluble protein and particulate matter, this partial material, rich in nutritional labelings such as albumen, can be further processed into feedstuff.
Speed stream tank operation principle: feed liquid is entered with tangential direction by cylindrical portions, rotates and produces centrifugal force, comes downwards to tapered segment more violent.Solids in feed liquid or the bigger liquid of density are thrown to wall by the effect of centrifugal force, and press helix downstream to outlet (underflow) along wall.The relatively fine particle carried in the liquid of clarification or liquid then rises, the outlet overflows at center go out.
(2) resin absorption: the corn soaking waste water after sedimentation enters resin column, resin model is D315, flow speed control is at per hour 2 ~ 3 times of column volumes and resin Contact-sorption, resin and ratio of adsorption scope 1:15 ~ 20 of waste water, corn soaking waste water after resin absorption returns corn soaking waste water back pool, then come back to the enrichment facility of Semen Maydis waste water, continue evaporation and concentration.Phytic acid is only extracted by this process, does not change the content of effective ingredient in original corn soaking waste water.
(3) eluting is resolved: by the resin hydrochloric acid eluent of mass concentration 5 ~ 8% after absorption, elution speed controls in per hour 2 ~ 3 times of column volumes, elution time 2 ~ 3 hours.Clean resin with 1 ~ 2 times of column volume tap water, be mixed to get eluent.
(4) neutralize, precipitate: in eluent, add the nertralizer Ca (OH) of mass concentration 10-20%2Solution, is neutralized to eluent ph value 7, obtains Phytin precipitation mixed liquor.
(5) plate-and-frame filtration: it is by the Phytin solid content initial gross separation in Phytin mixed liquor out that filtration is divided into two-stage, one-level filter pressing, primary filtrate recycle is in preparation eluant, nertralizer；Sending into two grades of filter pressings after the isolated Phytin of one-level filter pressing washs again with 2 ~ 4 times of clear water, isolate the Phytin that comparison is pure, two grades of filtrates are reclaimed equally for preparing eluant, nertralizer.Filtrate recycle advantageously reduces fresh water usage amount, additionally can be by ion effective recycling.Phytin after two grades of filter pressings i.e. can be used for the hydrolysis of inositol and produces.
The present invention prepares Phytin on the premise of the nature not changing corn soaking waste water and purposes, it is substantially reduced insoluble protein content in Semen Maydis water, the problem thoroughly solving Semen Maydis water slug ion exchange resin, and reduce protein content in Phytin, improve the quality of Phytin further, improve the yield of inositol, reduce waste water to the pollution to environment.
Detailed description of the invention
Detailed content and the detailed description of the invention thereof of the present invention are further illustrated below.Should be appreciated that specific embodiment described herein is only used for explaining the present invention, be not used to limit invention.
Embodiment 1:
Semen Maydis water directly enters ion exchange resin column without speed stream tank remove impurity, in turn includes the following steps:
Absorption: take the soak water of maize 105m of organic phosphorous content 0.6%, enters equipped with 7 tons of anion exchange resin handled well, resin model D305, and loading flow speed control is at per hour 2 times of column volumes.
Resolve eluting: blow off the Semen Maydis water remained in pillar by compressed air, opposite direction enters 1 times of column volume tap water, the hydrochloric acid of preparation 5% is with the speed eluting resin of per hour 2 times of column volumes, elution time 2 hours, the eluent in pillar is blown off again by compressed air, clean resin with 1 times of column volume tap water, be mixed to get eluent.
Neutralize: with the suspension of calcium hydroxide preparation 10%, progressively regulation eluent is to pH7.
Plate-and-frame filtration is divided into two-stage, one-level filter pressing to be by the Phytin solid content initial gross separation in Phytin mixed liquor out, and primary filtrate is reclaimed and is used for preparing eluant, nertralizer；After the isolated Phytin of one-level filter pressing washs again with 2 times of clear water, send into two grades of filter pressings, isolate the Phytin that comparison is pure.Drying obtains Phytin 1502.96kg, detects organic phosphorous content 37.21%, protein content 2.1%, yield 88.77%.
Embodiment
2
:
Semen Maydis water first enters ion exchange resin column again through speed stream tank remove impurity, in turn includes the following steps:
Take the soak water of maize 105m of organic phosphorous content 0.6%, settle 8 hours through speed stream tank.
Absorption: supernatant enters equipped with 7 tons of anion exchange resin handled well, resin model D305, and loading flow speed control is at per hour 2 times of column volumes.
Resolve eluting: blow off the Semen Maydis water remained in pillar by compressed air, opposite direction enters 1 times of column volume tap water, the hydrochloric acid of preparation 5% is with the speed eluting resin of per hour 2 times of column volumes, elution time 2 hours, the eluent in pillar is blown off again by compressed air, clean resin with 1 times of column volume tap water, be mixed to get eluent.
Neutralize: with the suspension of calcium hydroxide preparation 10%, progressively regulation eluent is to pH7.
5. plate-and-frame filtration is divided into two-stage, one-level filter pressing to be by the Phytin solid content initial gross separation in Phytin mixed liquor out, and primary filtrate is reclaimed and is used for preparing eluant, nertralizer；After the isolated Phytin of one-level filter pressing washs again with 2 times of clear water, send into two grades of filter pressings, isolate the Phytin that comparison is pure.Drying obtains Phytin 1492.79kg, detects organic phosphorous content 39.35%, protein content 0.56%, yield 93.24%.
Embodiment
3
:
Semen Maydis water first enters ion exchange resin column again through speed stream tank remove impurity, in turn includes the following steps:
Take the soak water of maize 105m of organic phosphorous content 0.6%, settle 8 hours through speed stream tank.
Absorption: supernatant enters equipped with 7 tons of anion exchange resin handled well, resin model D315, and loading flow speed control is at per hour 2 times of column volumes.
Resolve eluting: blow off the Semen Maydis water remained in pillar by compressed air, opposite direction enters 1 times of column volume tap water, the hydrochloric acid of preparation 5% is with the speed eluting resin of per hour 2 times of column volumes, elution time 2 hours, the eluent in pillar is blown off again by compressed air, clean resin with 1 times of column volume tap water, be mixed to get eluent.
Neutralize: with the suspension of calcium hydroxide preparation 10%, progressively regulation eluent is to pH7.
5. plate-and-frame filtration is divided into two-stage, one-level filter pressing to be by the Phytin solid content initial gross separation in Phytin mixed liquor out, and primary filtrate is reclaimed and is used for preparing eluant, nertralizer；After the isolated Phytin of one-level filter pressing washs again with 2 times of clear water, send into two grades of filter pressings, isolate the Phytin that comparison is pure.Drying obtains Phytin 1400.1kg, detects organic phosphorous content 43.26%, protein content 0.54%, yield 96.14%.
Embodiment
4
:
Semen Maydis water first enters ion exchange resin column again through speed stream tank remove impurity, in turn includes the following steps:
Take the soak water of maize 140m of organic phosphorous content 0.6%, settle 10 hours through speed stream tank.
Absorption: supernatant enters equipped with 7 tons of anion exchange resin handled well, resin model D315, and loading flow speed control is at per hour 3 times of column volumes.
Resolve eluting: blow off the Semen Maydis water remained in pillar by compressed air, opposite direction enters 1 times of column volume tap water, the hydrochloric acid of preparation 8% is with the speed eluting resin of per hour 3 times of column volumes, elution time 3 hours, the eluent in pillar is blown off again by compressed air, clean resin with 1 times of column volume tap water, be mixed to get eluent.
Neutralize: with the suspension of calcium hydroxide preparation 20%, progressively regulation eluent is to pH7.
5. plate-and-frame filtration is divided into two-stage, one-level filter pressing to be by the Phytin solid content initial gross separation in Phytin mixed liquor out, and primary filtrate is reclaimed and is used for preparing eluant, nertralizer；After the isolated Phytin of one-level filter pressing washs again with 4 times of clear water, send into two grades of filter pressings, isolate the Phytin that comparison is pure.Drying obtains Phytin 1900.32kg, detects organic phosphorous content 42.93%, protein content 0.51%, yield 97.12%.
Embodiment
5
:
Semen Maydis water first enters ion exchange resin column again through speed stream tank remove impurity, in turn includes the following steps:
Take the soak water of maize 119m of organic phosphorous content 0.6%, settle 10 hours through speed stream tank.
Absorption: supernatant enters ratio of adsorption scope 1:17 equipped with 7 tons of anion exchange resin handled well, resin model D315, resin and waste water, and loading flow speed control is at per hour 3 times of column volumes.
Resolve eluting: blow off the Semen Maydis water remained in pillar by compressed air, opposite direction enters 1 times of column volume tap water, preparation, the hydrochloric acid of 6.5% is with the speed eluting resin of per hour 2 times of column volumes, elution time 3 hours, blow off the eluent in pillar again by compressed air, clean resin with 1 times of column volume tap water, be mixed to get eluent.
Neutralize: with the suspension of calcium hydroxide preparation 16%, progressively regulation eluent is to pH7.
5. plate-and-frame filtration is divided into two-stage, one-level filter pressing to be by the Phytin solid content initial gross separation in Phytin mixed liquor out, and primary filtrate is reclaimed and is used for preparing eluant, nertralizer；After the isolated Phytin of one-level filter pressing washs again with 3 times of clear water, send into two grades of filter pressings, isolate the Phytin that comparison is pure.Drying obtains Phytin 1593.93kg, detects organic phosphorous content 44.15%, protein content 0.49%, yield 98.56%.
By speed stream tank settlement treatment and to use model be the resin of D315 model, product quality and yield are significantly improved.
Claims (1)
1. the isolation and purification method of a Phytin, it is characterised in that: comprise the steps:
1. the soak water of maize 119m of organic phosphorous content 0.6% is taken3, settle 10 hours through speed stream tank；
2. absorption: supernatant enters equipped with 7 tons of anion exchange resin handled well, resin model D315,
Resin and ratio of adsorption scope 1:17 of waste water, loading flow speed control is at per hour 3 times of column volumes；
3. resolving eluting: blow off the Semen Maydis water remained in pillar by compressed air, opposite direction enters 1 times of column volume
Tap water, the hydrochloric acid of preparation 6.5% is with the speed eluting resin of per hour 2 times of column volumes, and elution time 3 is little
Time, then the eluent in pillar is blown off by compressed air, clean resin with 1 times of column volume tap water, mix
To eluent；
4. neutralize: with the suspension of calcium hydroxide preparation 16%, progressively regulation eluent is 7 to pH；
5. plate-and-frame filtration is divided into two-stage, one-level filter pressing to be the Phytin solid content initial gross separation in Phytin mixed liquor to be gone out
Coming, primary filtrate is reclaimed and is used for preparing eluant, nertralizer；Clear with 3 times through the isolated Phytin of one-level filter pressing
Water sends into two grades of filter pressings after again washing, and isolates Phytin.
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| Application Number | Priority Date | Filing Date | Title |
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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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| CN104045665A CN104045665A (en) | 2014-09-17 |
| CN104045665B true CN104045665B (en) | 2016-08-10 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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 |
| CN111592136A (en) * | 2019-12-30 | 2020-08-28 | 江苏久吾高科技股份有限公司 | Method and device for efficiently utilizing components of corn soaking water |
| CN113135954B (en) * | 2021-04-24 | 2023-05-09 | 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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| CN101445514A (en) * | 2008-11-21 | 2009-06-03 | 西安皓天生物工程技术有限责任公司 | Method for manufacturing raw material phenanthrene tincture for synthesizing phaseomannite |
| CN101602777B (en) * | 2009-07-03 | 2011-09-14 | 安徽丰原生物化学股份有限公司 | Method for extracting phytic acid |
| CN102093413A (en) * | 2010-11-14 | 2011-06-15 | 河南永昌飞天淀粉糖有限公司 | New process for extracting phytin from corn soaking water |
| CN102127108A (en) * | 2010-12-08 | 2011-07-20 | 东北电力大学 | Method for extracting phytic acid from rice bran |
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