CN102659564A - Method for extracting lactic acid from wastewater generated in lactic acid production - Google Patents
Method for extracting lactic acid from wastewater generated in lactic acid production Download PDFInfo
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- CN102659564A CN102659564A CN2012101527164A CN201210152716A CN102659564A CN 102659564 A CN102659564 A CN 102659564A CN 2012101527164 A CN2012101527164 A CN 2012101527164A CN 201210152716 A CN201210152716 A CN 201210152716A CN 102659564 A CN102659564 A CN 102659564A
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Abstract
The invention provides a method for extracting lactic acid from wastewater generated in lactic acid production. The lactic acid is extracted by a method of combining nanofiltration membrane filtration, reverse osmosis membrane filtration and anion exchange resin adsorption. The method has a few process steps, and is easy to operate and master. In all process steps, the wastage rate of lactic acid is low, the yield of the lactic acid by the method is high, and the purity of the obtained lactic acid is high.
Description
Technical field
The present invention relates to a kind of method of from the waste water of lactic acid-producing, extracting lactic acid.
Background technology
Lactic acid is a kind of very important organic acid, is widely used in food, medicine and chemical industry.Industrial production lactic acid mainly is to adopt microbe fermentation method, and in China, fermentation raw material is main with corn, sweet potato starch carbohydrate mostly.The composition of lactic acid fermentation liquid is very complicated, except that lactic acid, also comprises plurality of impurities such as mycelium, residual sugar, protein, pigment, other organic acid, inorganic salt.Because using lactic acid many is main with the food medical treatment, therefore extremely strict to the specification of quality of lactic acid, need pass through a lot of processes from lactic acid fermentation liquid to the lactic acid finished product, improve constantly the requirement that lactic acid purity could satisfy the market user.In each process steps that fermented liquid is purified to finished product; More or less all can there be the lactic acid loss; Generally speaking; Require difference according to the lactic acid final product quality, lactic acid factory has only 80%-90% from fermenting to product yield, that is to say that corn or the Dian Fentang in the sweet potato that our lactobacillus ferment is used have 10%-18% to lose.500,000 tons of lactic acid of the annual consumption of lactic acid market scale at present, the yield with 85% calculates, and the Dian Fentang of annual waste just has 7.5 ten thousand tons, is worth about 2.8 hundred million yuans.China is populous nation, and all government attaches great importance to food problem all the time, is that the cost of raw material production lactic acid receives the influence of provision price very big with grain; Therefore; Improve the lactic acid yield, the lactic acid that reclaims in the waste water has very profound significance, but just ten minutes is complicated originally because of the lactobacillus ferment composition; Cause the composition in the waste water same very complicated, bring very big difficulty for the lactic acid recovery operation.
Existing traditional and improved lactic acid ca crystallization and acid hydrolysis method exist extraction yield low; The used extraction agent of extraction process is poisonous, and lactic acid is difficult to from organic phase, separate efficiently; The macromolecule resin absorption method exists the selectivity of macromolecule resin, the problem that the static exchange capacity is low; Molecular distillation method exists the lactic acid loss that bottoms is coloured, gunk-squeeze process causes more behind the distillation lactic acid big.And these methods all can't be extracted the lactic acid of lower concentration in the waste water.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method of from the waste water of lactic acid-producing, extracting lactic acid, require to use the yield of this method extraction lactic acid high, and the purity of the lactic acid that obtains is high.
For solving the problems of the technologies described above, the invention provides a kind of method of from the waste water of lactic acid-producing, extracting lactic acid, extract lactic acid through the method for using nf membrane filtration, reverse osmosis membrane filtration and anionite-exchange resin absorption to combine.
Specifically, may further comprise the steps:
(1) waste water with lactic acid-producing filters through Plate Filtration and filter stick core, obtains cleaner liquid;
(2) will cross cleaner liquid and filter, and obtain nanofiltration and be detained material and nanofiltration feed liquid through nf membrane;
(3) the nanofiltration feed liquid that obtains of step (2) is filtered through reverse osmosis filter membrane, obtains that reverse osmosis filter membrane is detained material and reverse osmosis filter membrane penetrates material;
(4) anionite-exchange resin is crossed in the materials flow of reverse osmosis filter membrane retentate, can be obtained being attracted to the lactic acid solution in the anionite-exchange resin.
For the purpose of the concise description problem, below the method for from the waste water of lactic acid-producing, extracting lactic acid according to the invention is all abbreviated as present method.
About nf membrane and the reverse osmosis membrane rejection to different substances sees the following form:
The waste water of lactic acid-producing after Plate Filtration and filter stick core filter, is left and taken cleaner liquid, can remove some bigger impurity particles such as free suspended particulate matter, colloidalmaterial in the waste water of lactic acid-producing; Nf membrane has the very strong interception of damming to carbohydrate, protein, pigment, macromolecule organic acid material, mycelium, so these materials nf membrane capable of using is removed; Reverse osmosis membrane has the very strong effect of damming again to materials such as lactic acid, to other anionic effect deviation of damming of part, has removed other negatively charged ion of part; Again anionite-exchange resin is crossed in the materials flow of reverse osmosis filter membrane retentate, anionite-exchange resin is adsorbable lactic acid, negatively charged ion, and positively charged ion is separated goes out.Can reach the purpose of from the waste water of lactic acid-producing, removing impurity, extracting lactic acid, the yield that extracts lactic acid is high, and the purity of the lactic acid that obtains is high.
As the optimization of present method, the filter cloth aperture of Plate Filtration is 20-25um described in the said step (1), and feed pressure is not higher than 4.5bar; Said filter stick core is filtered into the filter stick core that adopts 0.45um and filters, and filter pressure is not higher than 2.5bar.
It is 15-18 bar that the filtering temperature of charge of the said employing nf membrane of said step (2) is not higher than 30 ℃, feed pressure, and the circulating pressure of nf membrane is controlled to be 18-22 bar, and nf membrane retentate general export flow is 1/6-1/18 of an import total flux.
Said: it is 15-18 bar that the filtering temperature of charge of the said employing reverse osmosis filter membrane of step (4) is not higher than 30 ℃, feed pressure; The circulating pressure of reverse osmosis filter membrane is 18-21bar, and reverse osmosis filter membrane retentate rate of discharge is 1/10-1/15 of an import total flux.
Said anionite-exchange resin is 315 type anionite-exchange resin.
The said anionite-exchange resin of said step (3) carries out wet method dress post; The reverse osmosis filter membrane retentate is with the flow velocity upper prop of 1.2BV-1.5BV/h; Detect the specific conductivity of effluent in the upper prop process simultaneously, when the specific conductivity of anion column effluent is 1.4-1.8 ms/cm, stop upper prop.
The elutriant of said anionite-exchange resin is that concentration is 2-6% sulphuric acid soln; The consumption of elutriant is 1.2-1.5 times of feed volume of described anion-exchange column; Behind said anionite-exchange resin wash-out; Adopt air to press empty resin anion(R.A), obtain containing the lactic acid solution of elutriant.
Present method is extracted lactic acid through the method for using nf membrane filtration, reverse osmosis membrane filtration and anionite-exchange resin absorption to combine, and process step is few, simple to operate, is easy to grasp.In the whole process step, the turnover rate of lactic acid is few, makes to utilize present method to extract the yield height of lactic acid.For the waste water complicated component, contain carbohydrate, colloidalmaterials such as a large amount of COD in the waste water, and the less waste water of lactic acid content, especially be fit to adopt present method to reclaim lactic acid.In the method; Plate Filtration, filter core rod filter and do not lose lactic acid, nf membrane filter loss lactic acid about 7%, osmosis filtration loss lactic acid about 22%; Resin absorption loss lactic acid about 25%; Therefore, even even the lactic acid content in the waste water under the lower concentration of 5-8g/L, still can reach 50%-55% total adopt the lactic acid recovery of present method to get rate; The technology that present method adopts is the physics mode separating impurity; Do not bring any pollution, behind the resin anion(R.A) absorb-elute, though need sodium hydroxide solution to regenerate during the anion regenerant resin; But do not have chemical oxygen demand COD, biological oxygen demand BOD to pollute, environmental protection pressure is little.
Nf membrane described in present method, reverse osmosis membrane and anionite-exchange resin are commercially available article.
Embodiment
Further specify the present invention through embodiment below.
Embodiment 1:
From the waste water of lactic acid-producing, extract the method for lactic acid, may further comprise the steps:
(1) will contain lactic acid concn is that the waste water of the lactic acid-producing of 5.2g/L is the Plate Filtration of 20um through the filter cloth aperture; The control feed pressure is not higher than 4.5bar; Then the filter stick core of the filtrating behind the Plate Filtration through 0.45um filtered, controlled filter pressure is not higher than 2.5bar, obtains cleaner liquid;
(2) will cross cleaner liquid filters through nf membrane: when adopting nf membrane to filter; It is 15 bar that the temperature of controlled filter clear liquid is not higher than 30 ℃, feed pressure; The circulating pressure of nf membrane is controlled to be 18 bar, and nf membrane retentate general export flow is 1/18 of an import total flux.After nf membrane is filtered, obtain nanofiltration and be detained material and nanofiltration feed liquid;
(3) the nanofiltration feed liquid that step (2) is obtained is filtered through reverse osmosis filter membrane: it is 15 bar that the filtering temperature of charge of reverse osmosis filter membrane is not higher than 30 ℃, feed pressure; The circulating pressure of reverse osmosis filter membrane is 18bar, and reverse osmosis filter membrane retentate rate of discharge is 1/15 of an import total flux.After reverse osmosis filter membrane filtered, the reverse osmosis filter membrane that obtains lactic acid concn and be 59.8g/L is detained material and reverse osmosis filter membrane penetrates material;
(4) with the materials flow of reverse osmosis filter membrane retentate cross 315 type anionite-exchange resin, with the flow velocity upper prop of 1.2BV/h; Detect the specific conductivity of effluent in the upper prop process simultaneously; When the specific conductivity of anion column effluent is 1.4 ms/cm; Stop upper prop, the feed volume of minute book step anion-exchange column;
(5) stop upper prop after, adopting concentration is that 2% sulphuric acid soln is an elutriant, and said anionite-exchange resin is carried out wash-out, the consumption of elutriant is 1.2 times of feed volume of described anion-exchange column.Adopt air to press empty resin anion(R.A) then, obtain containing the lactic acid solution of elutriant, lactic acid concn is 37.4 g/L.The sulfuric acid solution operation that this lactic acid solution that contains elutriant can be back to lactic acid is utilized again.
Embodiment 2:
From the waste water of lactic acid-producing, extract the method for lactic acid, may further comprise the steps:
(1) will contain lactic acid concn is that the waste water of the lactic acid-producing of 6.5g/L is the Plate Filtration of 22um through the filter cloth aperture; The control feed pressure is not higher than 4.5bar; Then the filter stick core of the filtrating behind the Plate Filtration through 0.45um filtered, controlled filter pressure is not higher than 2.5bar, obtains cleaner liquid;
(2) will cross cleaner liquid filters through nf membrane: when adopting nf membrane to filter; It is 16 bar that the temperature of controlled filter clear liquid is not higher than 30 ℃, feed pressure; The circulating pressure of nf membrane is controlled to be 20 bar, and nf membrane retentate general export flow is 1/12 of an import total flux.After nf membrane is filtered, obtain nanofiltration and be detained material and nanofiltration feed liquid;
(3) the nanofiltration feed liquid that step (2) is obtained is filtered through reverse osmosis filter membrane: it is 16 bar that the filtering temperature of charge of reverse osmosis filter membrane is not higher than 30 ℃, feed pressure; The circulating pressure of reverse osmosis filter membrane is 20bar, and reverse osmosis filter membrane retentate rate of discharge is 1/13 of an import total flux.After reverse osmosis filter membrane filtered, the reverse osmosis filter membrane that obtains lactic acid concn and be 68.9g/L is detained material and reverse osmosis filter membrane penetrates material;
(4) with the materials flow of reverse osmosis filter membrane retentate cross 315 type anionite-exchange resin, with the flow velocity upper prop of 1.3BV/h; Detect the specific conductivity of effluent in the upper prop process simultaneously; When the specific conductivity of anion column effluent is 1.6 ms/cm; Stop upper prop, the feed volume of minute book step anion-exchange column;
(5) stop upper prop after, adopting concentration is that 4% sulphuric acid soln is an elutriant, and said anionite-exchange resin is carried out wash-out, the consumption of elutriant is 1.3 times of feed volume of described anion-exchange column.Adopt air to press empty resin anion(R.A) then, obtain containing the lactic acid solution of elutriant, lactic acid concn is 43.1g/L.The sulfuric acid solution operation that this lactic acid solution that contains elutriant can be back to lactic acid is utilized again.
Embodiment 3:
From the waste water of lactic acid-producing, extract the method for lactic acid, may further comprise the steps:
(1) will contain lactic acid concn is that the waste water of the lactic acid-producing of 8.6g/L is the Plate Filtration of 25um through the filter cloth aperture; The control feed pressure is not higher than 4.5bar; Then the filter stick core of the filtrating behind the Plate Filtration through 0.45um filtered, controlled filter pressure is not higher than 2.5bar, obtains cleaner liquid;
(2) will cross cleaner liquid filters through nf membrane: when adopting nf membrane to filter; It is 18 bar that the temperature of controlled filter clear liquid is not higher than 30 ℃, feed pressure; The circulating pressure of nf membrane is controlled to be 22 bar, and nf membrane retentate general export flow is 1/6 of an import total flux.After nf membrane is filtered, obtain nanofiltration and be detained material and nanofiltration feed liquid;
(3) the nanofiltration feed liquid that step (2) is obtained is filtered through reverse osmosis filter membrane: it is 18 bar that the filtering temperature of charge of reverse osmosis filter membrane is not higher than 30 ℃, feed pressure; The circulating pressure of reverse osmosis filter membrane is 21bar, and reverse osmosis filter membrane retentate rate of discharge is 1/10 of an import total flux.After reverse osmosis filter membrane filtered, the reverse osmosis filter membrane that obtains lactic acid concn and be 90.1g/L is detained material and reverse osmosis filter membrane penetrates material;
(4) with the materials flow of reverse osmosis filter membrane retentate cross 315 type anionite-exchange resin, with the flow velocity upper prop of 1.5BV/h; Detect the specific conductivity of effluent in the upper prop process simultaneously; When the specific conductivity of anion column effluent is 1.8 ms/cm; Stop upper prop, the feed volume of minute book step anion-exchange column;
(5) stop upper prop after, adopting concentration is that 6% sulphuric acid soln is an elutriant, and said anionite-exchange resin is carried out wash-out, the consumption of elutriant is 1.5 times of feed volume of described anion-exchange column.Adopt air to press empty resin anion(R.A) then, obtain containing the lactic acid solution of elutriant, lactic acid concn 56.3 g/L.The sulfuric acid solution operation that this lactic acid solution that contains elutriant can be back to lactic acid is utilized again.
In the method, anionite-exchange resin can also adopt other anionite-exchange resin except that 315 type anionite-exchange resin, when the anionite-exchange resin multiple adsorb need be regenerated, can adopt sodium hydroxide solution to regenerate.Nf membrane can adopt U.S. NF2-8040EN nf membrane, and reverse osmosis filter membrane can adopt RO2-8040-80N reverse osmosis filter membrane.
The lactic acid solution that contains elutriant that finally obtains can directly be back to the sulfuric acid solution operation of lactic acid and utilize, has practiced thrift production cost, has improved the utilization ratio of the lactic acid that from the waste water of lactic acid-producing, extracts.
Above-described only is three kinds of embodiments of the present invention.Should be pointed out that for the person of ordinary skill of the art under the prerequisite that does not break away from the principle of the invention, can also make some modification and improvement, these also should be regarded as belonging to protection scope of the present invention.
Claims (8)
1. a method of from the waste water of lactic acid-producing, extracting lactic acid is characterized in that: through the method extraction lactic acid that uses nf membrane filtration, reverse osmosis membrane filtration and anionite-exchange resin absorption to combine.
2. the method for from the waste water of lactic acid-producing, extracting lactic acid according to claim 1 is characterized in that: may further comprise the steps:
(1) waste water with lactic acid-producing filters through Plate Filtration and filter stick core, obtains cleaner liquid;
(2) will cross cleaner liquid and filter, and obtain nanofiltration and be detained material and nanofiltration feed liquid through nf membrane;
(3) the nanofiltration feed liquid that obtains of step (2) is filtered through reverse osmosis filter membrane, obtains that reverse osmosis filter membrane is detained material and reverse osmosis filter membrane penetrates material;
(4) anionite-exchange resin is crossed in the materials flow of reverse osmosis filter membrane retentate, can be obtained being attracted to the lactic acid solution in the anionite-exchange resin.
3. the method for from the waste water of lactic acid-producing, extracting lactic acid according to claim 2, it is characterized in that: the filter cloth aperture of Plate Filtration is 20-25um described in the step (1), and feed pressure is not higher than 4.5bar; Said filter stick core is filtered into the filter stick core that adopts 0.45um and filters, and filter pressure is not higher than 2.5bar.
4. the method for from the waste water of lactic acid-producing, extracting lactic acid according to claim 2; It is characterized in that: it is 15-18 bar that the filtering temperature of charge of the said employing nf membrane of step (2) is not higher than 30 ℃, feed pressure; The circulating pressure of nf membrane is controlled to be 18-22 bar, and nf membrane retentate general export flow is 1/6-1/18 of an import total flux.
5. the method for from the waste water of lactic acid-producing, extracting lactic acid according to claim 2; It is characterized in that: it is 15-18 bar that the filtering temperature of charge of the said employing reverse osmosis filter membrane of step (4) is not higher than 30 ℃, feed pressure; The circulating pressure of reverse osmosis filter membrane is 18-21bar, and reverse osmosis filter membrane retentate rate of discharge is 1/10-1/15 of an import total flux.
6. the method for from the waste water of lactic acid-producing, extracting lactic acid according to claim 2, it is characterized in that: said anionite-exchange resin is 315 type anionite-exchange resin.
7. the method for from the waste water of lactic acid-producing, extracting lactic acid according to claim 6; It is characterized in that: the said anionite-exchange resin of step (3) carries out wet method dress post; The reverse osmosis filter membrane retentate is with the flow velocity upper prop of 1.2BV-1.5BV/h; Detect the specific conductivity of effluent in the upper prop process simultaneously, when the specific conductivity of anion column effluent is 1.4-1.8 ms/cm, stop upper prop.
8. the method for from the waste water of lactic acid-producing, extracting lactic acid according to claim 6; It is characterized in that: the elutriant of said anionite-exchange resin is that concentration is 2-6% sulphuric acid soln; The consumption of elutriant is 1.2-1.5 times of feed volume of described anion-exchange column; Behind said anionite-exchange resin wash-out, adopt air to press empty resin anion(R.A), obtain containing the lactic acid solution of elutriant.
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Cited By (3)
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| CN103450007A (en) * | 2013-09-02 | 2013-12-18 | 西安通鑫半导体辅料有限公司 | Method for recovering lactic acid from waste lactic acid generated in silicon slice degumming procedure |
| CN104557515A (en) * | 2015-01-12 | 2015-04-29 | 河南金丹乳酸科技股份有限公司 | Method for extracting and separating L-lactic acid from ammonium lactate fermentation material liquid |
| CN106565465A (en) * | 2016-10-27 | 2017-04-19 | 广西轻工业科学技术研究院 | Method for extracting lactic acid from yellow water as by-product of Daqu liquor |
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| CN1348992A (en) * | 2001-10-31 | 2002-05-15 | 徐昌洪 | Continuous single-tank fermentation process of bacillus in membrane coupled clear liquid for producing levolactic acid |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103450007A (en) * | 2013-09-02 | 2013-12-18 | 西安通鑫半导体辅料有限公司 | Method for recovering lactic acid from waste lactic acid generated in silicon slice degumming procedure |
| CN104557515A (en) * | 2015-01-12 | 2015-04-29 | 河南金丹乳酸科技股份有限公司 | Method for extracting and separating L-lactic acid from ammonium lactate fermentation material liquid |
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| CN106565465A (en) * | 2016-10-27 | 2017-04-19 | 广西轻工业科学技术研究院 | Method for extracting lactic acid from yellow water as by-product of Daqu liquor |
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Application publication date: 20120912 |