CN105399622A - Method for producing potassium lactate from heavy-component lactic acid - Google Patents
Method for producing potassium lactate from heavy-component lactic acid Download PDFInfo
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- CN105399622A CN105399622A CN201510811624.6A CN201510811624A CN105399622A CN 105399622 A CN105399622 A CN 105399622A CN 201510811624 A CN201510811624 A CN 201510811624A CN 105399622 A CN105399622 A CN 105399622A
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- lactic acid
- potassium lactate
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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Abstract
The invention discloses a method for producing potassium lactate from heavy-component lactic acid. Particularly, the heavy-component lactic acid is pumped into a reaction tank, potassium hydroxide is pumped in a stirring state for a reaction, the temperature of a reaction system is kept at the temperature of 40-60 DEG C, adding of potassium hydroxide is stopped when the pH (potential of hydrogen) value of a reaction liquid is 6.5-7.5, and potassium lactate is obtained; deionized water is added to a completely reacted potassium lactate solution, the mass concentration of potassium lactate is controlled to range from 20% to 25%, and a roughly filtered potassium lactate solution is pumped into a nanofiltration membrane unit for filtration; during filtration by the nanofiltration membrane unit, penetrating fluids are collected independently and then continuously pumped into a triple-effect concentration section for concentration, trapped fluids flow back to a raw material container, the feeding speed is controlled, when the content of discharged potassium lactate is controlled in the range from 60% to 63%, discharged potassium lactate is pumped into a finished product tank, and a production process of potassium lactate can be completed. The technological process is mild, the material loss is small, and the comprehensive preparation cost (not containing the cost of heavy-component lactic acid and potassium hydroxide raw material) is smaller than 300 yuan per ton.
Description
Technical field
The present invention relates to a kind of method of lactic acid-producing potassium lactate, specifically with the method for heavy constituent lactic acid for the exquisite potassium lactate of Material synthesis.
Background technology
Heavy constituent lactic acid is the byproduct of domestic lactic acid-producing enterprise (comprise this patent and declare Gu De company of unit) final product processing short-range molecular distillation operation.The basic procedure of lactic acid-fermenting manufacture is, take glucose as basic raw material, and through fermentation, calcium oxide neutralization generates calcium lactate, sulfuric acid replacement(metathesis)reaction becomes rare lactic acid, ion-exchange is removed inorganic salt impurities, is concentrated into the operations such as content 100%, short-range molecular distillation.Wherein short-range molecular distillation operation, makes the mixture separation of pure lactic acid molecules and lactylic anhydride and organic impurities open by molecular distillation.That is to say while obtaining pure lactic acid, the by-product mixture of lactylic anhydride and organic impurities, be referred to as heavy constituent lactic acid.In short-range molecular distillation operation, the heavy constituent lactic acid of lactic acid total amount 30% is had to produce (lactic acid of another lactic acid total amount 30% is pure lactic acid).Be enriched with the impurity such as pigment, water-soluble protein and β-amylose in heavy constituent lactic acid, and most of lactic acid is macromolecular polymeric state, material is tawny, can not sell as food lactic acid, as technical grade lactic acid selling market finite capacity.
The treatment process traditional to this part heavy constituent lactic acid mainly contains two kinds, one is adopt activated carbon adsorption bleaching repeatedly, progressively remove the impurity such as pigment wherein, water-soluble protein and β-amylose, before the lactic acid of relative clean (containing polymerization lactic acid) returns back to short-range molecular distillation operation, again carry out short-range molecular distillation operation together with new work in-process.The representative manufacturers of this kind for the treatment of process is Jindan, Henan company, shortcoming is the powdered activated carbon that will consume volume in process, and final product per ton consumes activated carbon about 70-80 kilograms, and processing efficiency is low, lactic acid loss is comparatively large, comprehensive treating process expense about 700-800 yuan/ton of lactic acid.Two is application organic solvent extracting taking equipments, take isopropyl ether as extraction agent, by relatively pure lactic acid from, be mixed in heavy constituent lactic acid aqueous solution, isopropyl ether and lactic acid miscible after, be separated with water stratification.The impurity etc. such as organic pigment, water-soluble protein and β-amylose reside in the aqueous solution, due to the solubleness of lactic acid in isopropyl ether less (6%), need the lactic acid that repeated multiple times extraction could have been extracted in heavy constituent lactic acid.Isopropyl ether and lactic acid miscible after extraction liquid, distill, lactic acid be separated with isopropyl ether, collect isopropyl ether reuse and obtain relatively pure lactic acid simultaneously.The representative manufacturers of this kind for the treatment of process is Feng Yuan Ge Late company, and shortcoming is that extraction equipment is huge, invests high, and extractant in process isopropyl ether is high harmful influence, there is potential safety hazard, and at lactic acid final product easily residual isopropyl ether.Isopropyl ether and lactic acid miscible after extraction liquid carry out fractionation by distillation, high water consumption electricity vapour.More than comprehensive treating process expense 800 yuan/ton of lactic acid.
In heavy constituent lactic acid, be mixed with the lactylic anhydride compared with macromolecular structure and lact-acid oligomer, molecular weight is worked as with there being the impurity phases such as pigment, water-soluble protein and β-amylose, and it is very difficult with being separated of organic impurities that direct using nanofiltration film unit carries out lactic acid to heavy constituent lactic acid.
Summary of the invention
A kind of method main contents of heavy constituent lactic acid-producing potassium lactate that adopt of the present invention are: heavy constituent lactic acid (containing more macromolecular lactylic anhydride and lact-acid oligomer) and potassium hydroxide such as to carry out at mole combination reaction, unit molecule lactic acid in heavy constituent lactic acid, lactylic anhydride, lact-acid oligomer, under alkaline environment, are easy to separate coalescence and generate monomolecular potassium lactate.Potassium lactate solution after the balance that reacts completely is in neutral, adding after deionized water is adjusted to the aqueous solution of potassium lactate content 20-25% retains in a fixed container, middle pressure is introduced in the film pipe of NF type nanofiltration membrane unit, permeate is the potassium lactate solution after the decolorizing purification of molecular weight, trapped fluid contains potassium lactate and organic pigment, the impurity such as water-soluble protein and β-amylose passes back into container, repeatedly be filtered to the potassium lactate solution permeate after decolorizing purification and account for 98% of total amount, containing potassium lactate and organic pigment, the trapped fluid of the impurity such as water-soluble protein and β-amylose stops when remaining 2% of not enough total amount, the permeate of collecting is colourless or faint yellow potassium lactate solution, after multiple-effect evaporator is concentrated, physical and chemical index meets GB GB28305-2012.The trapped fluid collected is chocolate, is enriched the impurity such as the organic pigment of in raw material more than 99.9%, water-soluble protein and β-amylose, otherwise processed.By this nanofiltration membrane decoloring process, reach heavy constituent lactic acid and transform the technique object of producing commodity potassium lactate.
Concrete technical scheme is as follows
Adopt a method for heavy constituent lactic acid-producing potassium lactate, comprise the steps
1) heavy constituent lactic acid is pumped in retort, under whipped state, pump into potassium hydroxide react, maintenance temperature of reaction system is 40-60 DEG C, when reacting liquid pH value is 6.5-7.5, stop adding potassium hydroxide, can obtain the potassium lactate reacted completely, described lactic acid and potassium hydroxide mol ratio are 1:1;
2) potassium lactate solution reacted completely is added deionized water, controlling potassium lactate mass concentration is 20%-25%, after filtration, coarse filtration potassium lactate solution is pumped into nanofiltration membrane unit and filters;
3) when nanofiltration membrane unit Filtration Filtration, permeate is continuously pumped into triple effect concentration section and concentrates after collecting separately, trapped fluid passes back in material container, by controlling input speed, discharging potassium lactate content controls when 60-63%, pump into finished pot, the production technique of potassium lactate can be completed.
Technological process is as follows:
---------------triple effect concentrates---blending---finished product to nanofiltration membrane to 20% potassium lactate to potassium lactate+deionized water to heavy constituent lactic acid+potassium hydroxide in coarse filtration
Technique correlated response formula:
In lactic acid and potassium hydroxide and generate potassium lactate:
CH
3CHOHCOOH+KOH→CH
3CHOHCOOK+H
2O
The mol ratio that heavy constituent lactic acid solution and potassium hydroxide solution carry out reacting is 1:1.When coarse filtration potassium lactate solution pumps into the filtration of nanofiltration membrane unit, hydrodynamicpressure maintains 2.0MPa-2.5MPa, and permeate flow and trapped fluid flow ratio control system are 1:100-110; And the hierarchy of control stabilizes to 30 DEG C-40 DEG C.Time concentrated, Steam pressure control is 1.0MPa-2.0MPa, and concentrated material temperature is 50 DEG C-75 DEG C.
The advantage of the invention:
Pigment is enriched with in heavy constituent lactic acid, the impurity such as water-soluble protein and β-amylose, and most of lactic acid is macromolecular polymeric state, material is tawny, can not sell as food lactic acid, after reacting be depolymerized to unit molecule potassium lactate with potassium hydroxide, utilize potassium lactate molecule and organic pigment, the impurity such as water-soluble protein and β-amylose divides the difference of strength, adopt Nanofiltration Membrane Separation Technology, obtain relatively pure commodity potassium lactate, finished product quality equivalent food products level lactic acid and potassium hydroxide react the commodity potassium lactate produced, technological process is gentle, material loss is little, at the bottom of comprehensive manufacturing cost, larger cost advantage is had with the process ration of foregoing active carbon decoloring method and organic solvent extractionprocess process heavy constituent lactic acid.Present invention process process is gentle, and material loss is little, and comprehensive manufacturing cost (not containing heavy constituent lactic acid and potassium hydroxide raw material) is less than 300 yuan/ton.
Embodiment
Embodiment 1
By the heavy constituent lactic acid (content 80%) 1000 kilograms of application batch, disposablely pump into 5m
3in 316L stainless steel reaction tank and accurate-metering; Under whipped state, pump into potassium hydroxide solution (35%) carry out combination reaction, react with the pH value of on-line checkingi reaction solution for benchmark foundation, after 45 minutes the pH value of reaction solution reach and stablize to 7.0 time, reaction reach terminal, stop add potassium hydroxide.In reaction process, retort chuck passes into water coolant, ensures that reacting liquid temperature is no more than 75 degree.
The potassium lactate solution reacted completely totally 2423 kilograms, adds deionized water in retort, adjustment potassium lactate content about 20%.Obtain 5690 kilograms of potassium lactate solution.Deionized water is mainly derived from steam water coolant reuse when product concentrates, and insufficient section supplements with fresh deionized water.
By the potassium lactate solution of content about 20%, from retort, be transferred to 5m
3storage tank in, from 5m
3storage tank in, before input nanofiltration membrane unit, flow through cloth envelop collector, to remove the mechanical impurity that may surprisingly be mixed into.
Potassium lactate solution after coarse filtration is pumped into the NF type nanofiltration membrane unit of filtration area 305 square metres, hydrodynamicpressure maintains 2.0-2.5MPa, permeate flow and trapped fluid flow ratio adjust between 1:100 to 1:110, by the impact of seasonal climate temperature, before trapped fluid backflow, flow through interchanger, ensure that temperature of charge is no more than 40 degree.
During nanofiltration membrane unit operation, permeate pumps into Multi-effect concentration workshop section after collecting separately.Trapped fluid passes back in material container.In the nanofiltration membrane unit operation later stage, trapped fluid potassium lactate content slightly increases, and supplements deionized water 220 kilograms successively.
After the continuous operation of 42 hours, collect the potassium lactate solution 5807 kilograms that permeate is relatively pure, follow-up feeding triple-effect evaporator.Collect trapped fluid 95 kilograms, because being rich in organic impurities, otherwise processed.
By the permeate potassium lactate solution after purification, be continuously pumped into triple-effect evaporator and concentrate.Time concentrated, Steam pressure control is at below 2.0MPa, and material temperature is not higher than 75 degree, and by feeding rate, discharging potassium lactate content controls, 60-63%, to pump into finished pot.Steam condensate collects reuse.
By Sodium.alpha.-hydroxypropionate concentrated solution adjustment content 60.5%, obtain potassium lactate final product 1844 kilograms.Carry out physical and chemical index total analysis qualified rear filling.
Claims (5)
1. adopt a method for heavy constituent lactic acid-producing potassium lactate, it is characterized in that, comprise the steps
1) pump in retort by heavy constituent lactic acid, pump into potassium hydroxide and react under whipped state, maintenance temperature of reaction system is 40-60 DEG C, when reacting liquid pH value is 6.5-7.5, stops adding potassium hydroxide, can obtain the potassium lactate reacted completely;
2) potassium lactate solution reacted completely is added deionized water, controlling potassium lactate mass concentration is 20%-25%, after filtration, coarse filtration potassium lactate solution is pumped into nanofiltration membrane unit and filters;
3) when nanofiltration membrane unit Filtration Filtration, permeate is continuously pumped into triple effect concentration section and concentrates after collecting separately, trapped fluid passes back in material container, by controlling input speed, discharging potassium lactate content controls when 60-63%, pump into finished pot, the production technique of potassium lactate can be completed.
2. the method for employing heavy constituent lactic acid-producing potassium lactate according to claim 1, it is characterized in that, the mol ratio that heavy constituent lactic acid and potassium hydroxide carry out reacting is 1:1.
3. the method for employing heavy constituent lactic acid-producing potassium lactate according to claim 1, it is characterized in that, heavy constituent lactic acid is the byproduct of lactic acid short-range molecular distillation process for refining, be enriched with pigment, water-soluble protein and β-amylose impurity, and most of lactic acid is macromolecular polymeric state, material is tawny, the lactic acid can not sold as food lactic acid.
4. the method for employing heavy constituent lactic acid-producing potassium lactate according to claim 1, it is characterized in that, when coarse filtration potassium lactate solution pumps into the filtration of nanofiltration membrane unit, hydrodynamicpressure maintains 2.0MPa-2.5MPa, and permeate flow and trapped fluid flow ratio control system are 1:100-110; And the hierarchy of control stabilizes to 30 DEG C-40 DEG C.
5. the method for employing heavy constituent lactic acid-producing potassium lactate according to claim 1, is characterized in that, time concentrated, Steam pressure control is 1.0MPa-2.0MPa, and concentrated material temperature is 50 DEG C-75 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110551018A (en) * | 2019-07-29 | 2019-12-10 | 武汉新奇华清膜分离技术工程有限公司 | Method for preparing sodium lactate by using lactic acid distillation residual liquid |
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| CN1270953A (en) * | 2000-03-20 | 2000-10-25 | 湖北省广水市民族化工有限公司 | Short-path molecular distillation process for refining lactic acid |
| CN101130795A (en) * | 2007-07-26 | 2008-02-27 | 武汉三江航天固德生物科技有限公司 | Technique for producing acrylic ester during lactic acid production by zymotechnics |
| CN101265179A (en) * | 2008-04-18 | 2008-09-17 | 南京工业大学 | Technique for purifying lactate |
| CN102225891A (en) * | 2011-05-10 | 2011-10-26 | 武汉三江航天固德生物科技有限公司 | Method for removing impurities from potassium lactate solution |
| CN102225892A (en) * | 2011-05-10 | 2011-10-26 | 武汉三江航天固德生物科技有限公司 | Preparation method of low-sodium potassium lactate |
| CN102517346A (en) * | 2011-12-16 | 2012-06-27 | 安徽中粮生化格拉特乳酸有限公司 | Method for preparing L-lactic acid and/or L-lactate |
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2015
- 2015-11-20 CN CN201510811624.6A patent/CN105399622B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1270953A (en) * | 2000-03-20 | 2000-10-25 | 湖北省广水市民族化工有限公司 | Short-path molecular distillation process for refining lactic acid |
| CN101130795A (en) * | 2007-07-26 | 2008-02-27 | 武汉三江航天固德生物科技有限公司 | Technique for producing acrylic ester during lactic acid production by zymotechnics |
| CN101265179A (en) * | 2008-04-18 | 2008-09-17 | 南京工业大学 | Technique for purifying lactate |
| CN102225891A (en) * | 2011-05-10 | 2011-10-26 | 武汉三江航天固德生物科技有限公司 | Method for removing impurities from potassium lactate solution |
| CN102225892A (en) * | 2011-05-10 | 2011-10-26 | 武汉三江航天固德生物科技有限公司 | Preparation method of low-sodium potassium lactate |
| CN102517346A (en) * | 2011-12-16 | 2012-06-27 | 安徽中粮生化格拉特乳酸有限公司 | Method for preparing L-lactic acid and/or L-lactate |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110551018A (en) * | 2019-07-29 | 2019-12-10 | 武汉新奇华清膜分离技术工程有限公司 | Method for preparing sodium lactate by using lactic acid distillation residual liquid |
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