CN114702379B - Purification method of red lactic acid - Google Patents
Purification method of red lactic acid Download PDFInfo
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- CN114702379B CN114702379B CN202210631977.8A CN202210631977A CN114702379B CN 114702379 B CN114702379 B CN 114702379B CN 202210631977 A CN202210631977 A CN 202210631977A CN 114702379 B CN114702379 B CN 114702379B
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- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 title claims abstract description 346
- 235000014655 lactic acid Nutrition 0.000 title claims abstract description 173
- 239000004310 lactic acid Substances 0.000 title claims abstract description 173
- 238000000034 method Methods 0.000 title claims abstract description 39
- 238000000746 purification Methods 0.000 title claims abstract description 26
- 239000003957 anion exchange resin Substances 0.000 claims abstract description 170
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- 230000008929 regeneration Effects 0.000 claims abstract description 60
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- 238000001179 sorption measurement Methods 0.000 claims abstract description 60
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- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 33
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 32
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- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims abstract description 16
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- 239000000243 solution Substances 0.000 claims description 118
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- 239000000463 material Substances 0.000 claims description 49
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- 238000003795 desorption Methods 0.000 claims description 20
- 238000002386 leaching Methods 0.000 claims description 19
- 229920006395 saturated elastomer Polymers 0.000 claims description 10
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 9
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- 229920003303 ion-exchange polymer Polymers 0.000 claims description 9
- -1 lactate ions Chemical class 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 5
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- 239000000284 extract Substances 0.000 abstract 1
- 238000000855 fermentation Methods 0.000 description 12
- 230000004151 fermentation Effects 0.000 description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 11
- 239000008367 deionised water Substances 0.000 description 11
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- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 5
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- 238000000199 molecular distillation Methods 0.000 description 5
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- JVTAAEKCZFNVCJ-REOHCLBHSA-N L-lactic acid Chemical compound C[C@H](O)C(O)=O JVTAAEKCZFNVCJ-REOHCLBHSA-N 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 238000005374 membrane filtration Methods 0.000 description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
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- 235000000346 sugar Nutrition 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
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- KVZLHPXEUGJPAH-BXRBKJIMSA-N (2s)-2-oxidanylpropanoic acid Chemical compound C[C@H](O)C(O)=O.C[C@H](O)C(O)=O KVZLHPXEUGJPAH-BXRBKJIMSA-N 0.000 description 1
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- CZMRCDWAGMRECN-UHFFFAOYSA-N Rohrzucker Natural products OCC1OC(CO)(OC2OC(CO)C(O)C(O)C2O)C(O)C1O CZMRCDWAGMRECN-UHFFFAOYSA-N 0.000 description 1
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- 229930006000 Sucrose Natural products 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
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Classifications
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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
- C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Treatment Of Water By Ion Exchange (AREA)
Abstract
The invention discloses a purification method of red lactic acid, which comprises the following steps: (1) adsorption: adding the acidified red lactic acid solution into a weak-base anion exchange resin column; (2) and (3) analysis: adding a sulfuric acid solution into a weak-base anion exchange resin column which adsorbs lactate, and replacing the lactate on the resin with sulfate radicals to obtain a lactic acid solution; (3) regeneration: and adding ammonia water into the weak-base anion exchange resin column after the resolution is finished, and regenerating the resin. The invention separates the impurities such as pigment, salt, polysaccharide protein and the like in the waste red lactic acid from the lactic acid, extracts the lactic acid, and recycles the byproduct ammonium sulfate, thereby changing waste into valuable and reducing the treatment capacity of the waste red lactic acid. The method not only improves the yield of the lactic acid, but also protects the environment, is an environment-friendly purification method, and more importantly has the beneficial effects of energy conservation and environmental protection.
Description
Technical Field
The invention relates to a lactic acid separation and purification technology, in particular to a purification method of red lactic acid.
Background
L-Lactic acid (L-Lactic acid): molecular formula C 3 H 6 O 3 The boiling point is 125 ℃, the L-lactic acid is an organic acid which is prepared by taking corn starch, raw material cane sugar, beet sugar or molasses thereof and the like as raw materials through biological fermentation and refining, the organic acid is colorless clear viscous liquid, and the aqueous solution is acidic. Optionally mixed with water, ethanol or diethyl ether, and insoluble in chloroform. Because of the levorotatory characteristic, the compound has good biological compatibility, can be fused with mammals, can directly participate in human metabolism, has no side effect, and is widely applied to the fields of food, medicine and the like.
The L-lactic acid is prepared by saccharifying starch-containing raw materials and inoculating lactic acid strains for fermentation. After fermentation, the final product is obtained by acidolysis, filtration, preconcentration, decolorization, ion exchange, membrane filtration, concentration, molecular distillation and the like. The fermentation liquor is treated by molecular distillation to obtain a light phase and a heavy phase, and the concentrated liquor produced by membrane filtration and the heavy phase product produced by molecular distillation are generally called as red lactic acid. Although the lactic acid content of the red lactic acid is up to 60% or more, the red lactic acid also contains impurities such as sugars, pigments, proteins, salts, etc., and has a low utility value, and as shown in fig. 8, the color of the red lactic acid is very high. The traditional process is to mix a part of the red lactic acid back and a part of the red lactic acid is used as waste. Since the red lactic acid contains sugars, proteins, and the like, it is not easy to store and it is difficult to handle it as a waste.
Disclosure of Invention
In order to improve the utilization rate of the red lactic acid, the invention adopts a valve array type continuous ion exchange system to purify the red lactic acid, thereby increasing the additional value of the red lactic acid, improving the yield of the lactic acid, reducing the treatment amount of waste materials and changing waste into valuable.
The technical scheme of the invention is as follows: a method for purifying red lactic acid comprises the following steps:
(1) adsorption: adding the red lactic acid solution into a weak-base anion exchange resin column, and automatically adsorbing lactate ions onto the ion exchange resin;
(2) and (3) analysis: adding a sulfuric acid solution into a weak-base anion exchange resin column which adsorbs lactate, and replacing the lactate on the resin with sulfate radicals to obtain a lactic acid solution;
(3) regeneration: and adding ammonia water into the analyzed weak base anion exchange resin column, regenerating the resin, and obtaining the weak base anion exchange resin column recovering the exchange capacity and a byproduct ammonium sulfate solution after the regeneration is finished.
The absorbed weak base anion exchange resin column forms an absorption area, the resolved weak base anion exchange resin column forms an resolving area, the regenerated weak base anion exchange resin column forms a regeneration area, the weak base anion exchange resin column in the absorption area is automatically switched to the resolving area after being absorbed and saturated, meanwhile, the weak base anion exchange resin column after the resolving area is resolved is automatically switched to the regeneration area, the weak base anion exchange resin column after the regeneration area is regenerated is automatically switched to the absorption area, and continuous ion exchange is formed.
The purification process of the red lactic acid is continuously operated by full-automatic control of PLC.
The red lactic acid is a heavy phase product obtained by membrane filtration and/or molecular distillation in the process of preparing lactic acid from lactic acid fermentation liquor. The continuous ion exchange method directly obtains lactic acid from red lactic acid, rather than purifying lactic acid by removing impurities from red lactic acid, unlike the conventional ion exchange method.
The purification method of the red lactic acid also comprises the following steps:
washing the materials with water: before the analysis, washing the weak base anion exchange resin column adsorbing lactate, and switching the weak base anion exchange resin column to analyze after the washing material is finished;
washing with water and acid: after the analysis, washing the analyzed weak base anion exchange resin column, and switching the weak base anion exchange resin column after the acid washing to back wash;
backwashing: after washing acid, backwashing the weak base anion exchange resin column after the acid washing is finished, and switching the weak base anion exchange resin column to regenerate after the backwashing is finished;
water leaching: and after regeneration, washing the regenerated weak base anion exchange resin column with water, and switching the weak base anion exchange resin column after washing with water to analyze.
The weak base anion exchange resin column of the water washing material forms a water washing material area, the weak base anion exchange resin column of the water washing acid forms a water washing acid area, the weak base anion exchange resin column of the water washing material area forms a water washing area, the weak base anion exchange resin column of the adsorption area is automatically switched to the water washing material area after being adsorbed and saturated, meanwhile, the weak base anion exchange resin column of the water washing material area is automatically switched to an analysis area, the weak base anion exchange resin column analyzed in the analysis area is automatically switched to the water washing acid area, the weak base anion exchange resin column of the water washing acid area is automatically switched to a backwashing area, the weak base anion exchange resin column of the backwashing area is automatically switched to a regeneration area, and the weak base anion exchange resin column regenerated in the regeneration area is automatically switched to the adsorption area to form continuous ion exchange. When one weak base anion exchange resin column is switched out from one area, the weak base anion exchange resin column in the next working procedure area can be switched in, so that the number of the columns in each area is kept relatively constant.
The mass concentration of the red lactic acid solution during feeding is 10-30%.
The mass concentration of the sulfuric acid solution is 10-40%.
The mass concentration of the ammonia water is 10-30%.
The adsorption zone comprises 2 or more than 2 weak base anion exchange resin columns which are connected in series.
And switching the resin columns when the pH value of the effluent of the last weak-base anion exchange resin column in the adsorption area is less than 3.
The resolving area comprises 2 or more than 2 weak base anion exchange resin columns which are connected in series.
And switching the resin columns when the sulfate radical concentration of the effluent of the last weak-base anion exchange resin column in the analysis area is greater than a set value.
The regeneration zone comprises 2 or more than 2 weak base anion exchange resin columns which are connected in series.
The method of the invention utilizes the porous structure of the anion resin and the groups on the resin skeleton to carry out ion exchange, for example, in an adsorption zone, ionic lactate ions in a red lactic acid solution can be adsorbed on the resin, thereby separating protein, polysaccharide and salts from lactic acid; after the resin is adsorbed and saturated, cutting the resin into an analysis area, adding a sulfuric acid solution into the resin column in the analysis area, and replacing lactate adsorbed on the resin by sulfate radicals to obtain a relatively pure lactic acid product; cutting the resolved resin column to a regeneration area; in the regeneration zone, the resin column is regenerated by feeding ammonia water, and the sulfate radical on the resin is replaced by hydroxide radical to combine with the ionic ammonium radical to produce ammonium sulfate as by-product. In the ion exchange process, impurities such as pigments, salts, polysaccharide proteins and the like in the waste red lactic acid are separated from the lactic acid, the lactic acid is extracted, a byproduct ammonium sulfate is recovered, waste materials are changed into valuable materials, the treatment capacity of the waste red lactic acid is reduced, the yield of the lactic acid is improved, the environment is protected, the method is an environment-friendly purification method, more importantly, the beneficial effects of energy conservation and environmental protection are achieved, and the method has great significance for environmental protection.
Drawings
FIG. 1 is a schematic diagram of the main flow of a red lactic acid purification process.
Fig. 2 is a schematic structural diagram of a valve array type continuous ion exchange system for purification of red lactic acid of example 1.
Fig. 3 is a schematic structural diagram of a valve array type continuous ion exchange system for purification of red lactic acid of example 2.
FIG. 4 is a schematic diagram of the structure of a valve-matrix continuous ion-exchange system for purification of red lactic acid according to example 3.
FIG. 5 is a schematic diagram of the structure of a valve-matrix continuous ion-exchange system for purification of red lactic acid of example 4.
FIG. 6 is a schematic diagram of the structure of a valve matrix type continuous ion exchange system for purification of red lactic acid of example 5.
FIG. 7 is a schematic diagram of the structure of the valve matrix type continuous ion exchange system for purification of red lactic acid of example 6.
FIG. 8 is a schematic diagram of the red lactic acid starting material used in example 6.
Figure 9 is a physical comparison of the product prepared using the red lactic acid purification process of example 6 with the incoming red lactic acid solution.
Detailed Description
The present invention will be described in detail with reference to the following examples and drawings.
The red lactic acid is a heavy phase product obtained by molecular distillation in the process of preparing lactic acid from lactic acid fermentation liquor and/or a concentrated solution obtained by membrane filtration, and contains a small amount of impurities such as sugar, pigment, protein, salt and the like besides lactic acid. The mass concentration of lactic acid in the red lactic acid is 30-70%.
As shown in fig. 1, the purification method of red lactic acid is to exchange the red lactic acid solution obtained by diluting, acid hydrolyzing and decolorizing red lactic acid with weak base group of ion exchange resin, then to analyze with sulfuric acid solution to obtain lactic acid solution, and to regenerate the resin with ammonia water to obtain ammonium sulfate solution. The red lactic acid solution passes through an ion exchange resin column to achieve the refining purpose, and impurities such as salt, pigment, and mixed acid generated in the fermentation and acidification processes in the red lactic acid solution are separated. Since the bonding capacity of lactate and sulfate with resin is different, sulfate can resolve lactate. Finally, lactate exists in the analysis solution, and ammonium sulfate exists in the regeneration solution.
The red lactic acid is diluted with pure water.
Diluting the red lactic acid, and carrying out acidolysis by using concentrated sulfuric acid, wherein the amount of the sulfuric acid solution is 1-5 per mill of the feeding mass of the red lactic acid solution, and the concentration of the sulfuric acid solution is 98%.
The mass concentration of the feed of the red lactic acid solution is 10-30%. The concentration of the lactic acid solution needs to be controlled in the range, and the lactic acid solution is difficult to separate due to too high viscosity when the concentration is too high; the water consumption and the sewage discharge amount are increased when the concentration is too low, and the water consumption is correspondingly increased by 1% when the concentration is reduced by 1%.
The feed temperature of the red lactic acid solution is preferably 30 to 80 ℃.
The mass concentration of the sulfuric acid solution is 10-40%.
The mass concentration of the regenerated liquid ammonia water is 10-40%.
The purification process of the red lactic acid adopts PLC full-automatic control continuous operation.
Example 1
The purification method of the red lactic acid comprises the following steps:
(1) adsorption: feeding a solution of the red lactic acid with the temperature of 30 ℃ into a weak-base anion exchange resin column of the adsorption zone 1; the red lactic acid solution is waste red lactic acid generated in the process of producing lactic acid by fermentation and refining, is diluted, is subjected to acidolysis, is decolorized by active carbon and is filtered by a plate frame to obtain filtrate, and the feeding mass concentration of the red lactic acid solution is 10 percent;
(2) and (3) analysis: using a normal-temperature dilute sulfuric acid solution as an analysis agent, analyzing the lactic acid adsorbed by the weak-base anion exchange resin column in the analysis area 2 to obtain a refined lactic acid solution, wherein the concentration of the fed dilute sulfuric acid solution is 15%;
(3) regeneration: and (3) regenerating the resin in the weak base anion exchange resin column in the regeneration zone 3 by using a normal-temperature dilute ammonia solution as a regenerant to obtain an ammonium sulfate solution and a regenerated weak base anion exchange resin column, wherein the mass concentration of the ammonia water is 20%.
A valve array type continuous ion exchange system used for purifying the red lactic acid is shown in figure 2 and comprises an adsorption zone 1, a desorption zone 2 and a regeneration zone 3, wherein each zone comprises an anion exchange resin column; the feeding of the anion exchange resin column of the adsorption zone 1 is a red lactic acid solution, the anion exchange resin column of the desorption zone 2 adsorbs lactate, the feeding is a sulfuric acid solution, the anion exchange resin column of the regeneration zone 3 adsorbs sulfate, and the feeding is an ammonia water solution; the anion exchange resin in the adsorption zone 1 is saturated to adsorb lactate and then is switched to the desorption zone 2, the lactate ions on the anion exchange resin column in the desorption zone 2 are switched to the regeneration zone 3 after being desorbed, and the anion exchange resin column in the regeneration zone 3 is switched to the adsorption zone 1 after being regenerated. The valve array type continuous ion exchange system is controlled to continuously operate by a PLC (programmable logic controller) in a full-automatic mode. The ion exchange resin in the system is weak-base acrylic anion exchange resin.
Example 2
The purification method of the red lactic acid comprises the following steps:
(1) adsorption: feeding a 50 ℃ red lactic acid solution into a weak-base anion exchange resin column in an adsorption zone 1; the red lactic acid solution is waste red lactic acid generated in the process of producing lactic acid by fermentation and refining, is diluted, is subjected to acidolysis, is decolorized by active carbon and is filtered by a plate frame to obtain filtrate, and the feeding mass concentration of the red lactic acid solution is 25 percent;
(2) and (3) analysis: using a normal-temperature dilute sulfuric acid solution as an analysis agent, analyzing the lactic acid adsorbed by the weak-base anion exchange resin column in the analysis area 2 to obtain a refined lactic acid solution, wherein the mass concentration of the fed dilute sulfuric acid solution is 10%;
(3) regeneration: and (3) regenerating the resin in the weak base anion exchange resin column in the regeneration zone 3 by using a normal-temperature dilute ammonia solution as a regenerant to obtain an ammonium sulfate solution and a regenerated weak base anion exchange resin column, wherein the mass concentration of ammonia water is 25%.
A valve array type continuous ion exchange system used for purifying the red lactic acid is shown in figure 3 and comprises an adsorption zone 1, a desorption zone 2 and a regeneration zone 3, wherein each zone comprises two anion exchange resin columns; the feeding of the anion exchange resin column of the adsorption zone 1 is a red lactic acid solution, the anion exchange resin column of the desorption zone 2 adsorbs lactate, the feeding is a sulfuric acid solution, the anion exchange resin column of the regeneration zone 3 adsorbs sulfate, and the feeding is an ammonia water solution; the anion exchange resin in the adsorption zone 1 is saturated to adsorb lactate and then is switched to the desorption zone 2, the lactate ions on the anion exchange resin column in the desorption zone 2 are switched to the regeneration zone 3 after being desorbed, and the anion exchange resin column in the regeneration zone 3 is switched to the adsorption zone 1 after being regenerated. The valve array type continuous ion exchange system is controlled to continuously operate by a PLC (programmable logic controller) in a full-automatic mode. The ion exchange resin in the system is weak-base acrylic anion exchange resin.
Example 3
The purification method of the red lactic acid comprises the following steps:
(1) adsorption: feeding a red lactic acid solution with the temperature of 70 ℃ into a weak-base anion exchange resin column in an adsorption zone 1; the red lactic acid solution is waste red lactic acid generated in the process of producing lactic acid by fermentation and refining, is diluted, is subjected to acidolysis, is decolorized by active carbon and is filtered by a plate frame to obtain filtrate, and the feeding mass concentration of the red lactic acid solution is 30%;
(2) and (3) analysis: using a normal-temperature dilute sulfuric acid solution as an analysis agent, analyzing the lactic acid adsorbed by the weak-base anion exchange resin column in the analysis area 2 to obtain a refined lactic acid solution, wherein the concentration of the fed dilute sulfuric acid solution is 40%;
(3) regeneration: and (3) regenerating the weak-base anion exchange resin column in the regeneration zone 3 by using a normal-temperature dilute ammonia solution as a regenerant to obtain an ammonium sulfate solution and a regenerated anion exchange resin column, wherein the mass concentration of ammonia is 30%.
The valve array type continuous ion exchange system used for purifying the red lactic acid is shown in figure 4 and comprises an adsorption zone 1, a desorption zone 2 and a regeneration zone 3, wherein each zone comprises more than two anion exchange resin columns; the feeding of the anion exchange resin column of the adsorption zone 1 is a red lactic acid solution, the anion exchange resin column of the desorption zone 2 adsorbs lactate, the feeding is a sulfuric acid solution, the anion exchange resin column of the regeneration zone 3 adsorbs sulfate, and the feeding is an ammonia water solution; the anion exchange resin in the adsorption zone 1 is saturated to adsorb lactate and then is switched to the desorption zone 2, the lactate ions on the anion exchange resin column in the desorption zone 2 are switched to the regeneration zone 3 after being desorbed, and the anion exchange resin column in the regeneration zone 3 is switched to the adsorption zone 1 after being regenerated. The valve array type continuous ion exchange system is controlled to continuously operate by PLC in a full-automatic way. The ion exchange resin in the system is weak-base acrylic anion exchange resin.
Example 4
The purification method of the red lactic acid comprises the following steps:
(1) adsorption: feeding a red lactic acid solution with the temperature of 80 ℃ into a weak-base anion exchange resin column in an adsorption zone 1; the red lactic acid solution is waste red lactic acid generated in the process of producing lactic acid by fermentation and refining, is diluted, is subjected to acidolysis, is decolorized by active carbon and is filtered by a plate frame to obtain filtrate, and the feeding mass concentration of the red lactic acid solution is 15%;
(2) washing the materials with water: eluting the residual red lactic acid solution in the weak-base anion exchange resin column of the water washing material area 4 by using the evaporated condensate water or the steam condensate water or the deionized water as an eluent, and refluxing the eluent to a crude lactic acid tank;
(3) and (3) analysis: using normal temperature dilute sulfuric acid solution as an analysis agent, analyzing the lactic acid adsorbed by the weak base anion exchange resin column in the analysis area 2 to obtain an analysis solution which is refined lactic acid solution, wherein the concentration of the dilute sulfuric acid solution is 20%;
(4) washing with water and acid: washing the weak base anion exchange resin column in the water washing acid area 5 with the evaporated condensate water or steam condensate water or deionized water as the feed material to wash out the residual sulfuric acid solution;
(5) backwashing: backwashing the weak base anion exchange resin column switched to the backwashing area 7, and switching the weak base anion exchange resin column of the backwashing area 7 from the water washing acid area 5;
(6) regeneration: regenerating the weak base anion exchange resin column in the regeneration area 3 by using normal temperature weak ammonia water solution as a regenerant to obtain ammonium sulfate solution and a regenerated weak base anion exchange resin column, wherein the mass concentration of ammonia water is 15%;
(7) water leaching: and (3) cleaning the weak base anion exchange resin column in the water leaching area 6 by taking the evaporated condensate water or the steam condensate water or the deionized water as a feeding material, washing out the residual ammonia water solution, and switching to the adsorption area 1 for another period of operation after the weak base anion exchange resin column in the water leaching area 6 is leached.
The valve array type continuous ion exchange system used for purifying the red lactic acid is shown in figure 5 and comprises an adsorption area 1, an analysis area 2, a regeneration area 3, a water washing material area 4, a water acid washing area 5, a water leaching area 6 and a backwashing area 7, wherein each area is provided with an anion exchange resin column; the feeding of the anion exchange resin column of the adsorption area 1 is a red lactic acid solution, the anion exchange resin column of the analysis area 2 adsorbs lactate, the feeding is a sulfuric acid solution, the anion exchange resin column of the regeneration area 3 adsorbs sulfate radicals, the feeding is an ammonia water solution, the water washing material area 4, the water washing acid area 5 and the water leaching area 6 all feed water, and the feeding of the backwashing area 7 is water.
When the resin columns are switched every time, the adsorption area 1 is switched to the water washing material area 4 through one anion exchange resin column, the water washing material area 4 is switched to the analysis area 2 through one anion exchange resin column, the analysis area 2 is switched to the water washing acid area 5 through one anion exchange resin column, the water washing acid area 5 is switched to the backwashing area 7 through one anion exchange resin column, the backwashing area 7 is switched to the regeneration area 3 through one anion exchange resin column, the regeneration area 3 is switched to the water washing area 6 through one anion exchange resin column, the water washing area 6 is switched to the adsorption area 1 through one anion exchange resin column, and the valve array type continuous ion exchange system runs continuously. The valve array type continuous ion exchange system is controlled to continuously operate by a PLC (programmable logic controller) in a full-automatic mode. The ion exchange resin in the system is weak-base acrylic anion exchange resin.
Example 5
The purification method of the red lactic acid comprises the following steps:
(1) adsorption: feeding a 60 ℃ red lactic acid solution into a weak-base anion exchange resin column in an adsorption zone 1; the red lactic acid solution is waste red lactic acid generated in the process of producing lactic acid by fermentation and refining, is diluted, is subjected to acidolysis, is decolorized by active carbon and is filtered by a plate frame to obtain filtrate, and the feeding mass concentration of the red lactic acid solution is 20%;
(2) washing the materials with water: eluting the residual red lactic acid solution in the weak-base anion exchange resin column of the water washing material area 4 by using the evaporated condensate water or the steam condensate water or the deionized water as an eluent, and refluxing the eluent to a crude lactic acid tank;
(3) and (3) analysis: using a normal-temperature dilute sulfuric acid solution as an analysis agent, analyzing the lactic acid adsorbed by the weak-base anion exchange resin column in the analysis area 2 to obtain an analysis solution which is a refined lactic acid solution, wherein the concentration of the dilute sulfuric acid solution is 15%;
(4) washing with water and acid: washing the weak-base anion exchange resin column in the water washing acid zone 5 by using the evaporated condensate water or the steam condensate water or the deionized water as a feed material, and washing out the residual sulfuric acid solution;
(5) backwashing: backwashing the weak base anion exchange resin column switched to the backwashing area 7, and switching the weak base anion exchange resin column in the backwashing area from the water washing acid area 5;
(6) regeneration: regenerating the weak base anion exchange resin column in the regeneration area 3 by using normal temperature weak ammonia water solution as a regenerant to obtain ammonium sulfate solution and a regenerated weak base anion exchange resin column, wherein the mass concentration of ammonia water is 10%;
(7) water leaching: and (3) cleaning the weak base anion exchange resin column in the water leaching area 6 by taking the evaporated condensate water or the steam condensate water or the deionized water as a feeding material, washing out the residual ammonia water solution, and switching to the adsorption area 1 for another period of operation after the weak base anion exchange resin column in the water leaching area 6 is leached.
The valve array type continuous ion exchange system used for purifying the red lactic acid is shown in figure 6 and comprises an adsorption area 1, an analysis area 2, a regeneration area 3, a water washing material area 4, a water washing acid area 5, a water washing area 6 and a backwashing area 7, wherein the adsorption area 1, the analysis area 2, the regeneration area 3, the water washing material area 4, the water washing acid area 5 and the water washing area 6 are all provided with two anion exchange resin columns, and the backwashing area 7 is provided with 1 anion exchange resin column; the feeding of the anion exchange resin column of the adsorption area 1 is a red lactic acid solution, the anion exchange resin column of the analysis area 2 adsorbs lactate, the feeding is a sulfuric acid solution, the anion exchange resin column of the regeneration area 3 adsorbs sulfate radicals, the feeding is an ammonia water solution, the water washing material area 4, the water washing acid area 5 and the water leaching area 6 all feed water, and the feeding of the backwashing area 7 is water.
When the resin columns are switched every time, the adsorption area 1 is switched to the water washing material area 4 through one anion exchange resin column, the water washing material area 4 is switched to the analysis area 2 through one anion exchange resin column, the analysis area 2 is switched to the water washing acid area 5 through one anion exchange resin column, the water washing acid area 5 is switched to the backwashing area 7 through one anion exchange resin column, the backwashing area 7 is switched to the regeneration area 3 through one anion exchange resin column, the regeneration area 3 is switched to the water washing area 6 through one anion exchange resin column, the water washing area 6 is switched to the adsorption area 1 through one anion exchange resin column, and the valve array type continuous ion exchange system runs continuously. The valve array type continuous ion exchange system is controlled to continuously operate by a PLC (programmable logic controller) in a full-automatic mode. The ion exchange resin in the system is weak-base acrylic anion exchange resin.
Example 6
The purification method of the red lactic acid comprises the following steps:
(1) adsorption: feeding the red lactic acid solution with the temperature of 40 ℃ into a weak-base anion exchange resin column in the adsorption zone 1; as shown in fig. 8, the concentration of lactic acid is about 60%, the red lactic acid is diluted and subjected to acidolysis, decolorized by activated carbon and filtered by a plate frame to obtain a filtrate which is a red lactic acid solution, and the feed mass concentration of the red lactic acid solution is 25.6%; the object is shown in figure 9 as the first bottle.
(2) Washing the materials with water: eluting the residual red lactic acid solution in the weak-base anion exchange resin column of the water washing material area 4 by using the evaporated condensate water or the steam condensate water or the deionized water as an eluent, and refluxing the eluent to a crude lactic acid tank;
(3) and (3) analysis: using a normal-temperature dilute sulfuric acid solution as an analysis agent, analyzing the lactic acid adsorbed by the weak-base anion exchange resin column in the analysis area 2 to obtain an analysis solution which is a refined lactic acid solution, wherein the concentration of the dilute sulfuric acid solution is 25%;
(4) washing with water and acid: washing the weak-base anion exchange resin column in the water washing acid zone 5 by using the evaporated condensate water or the steam condensate water or the deionized water as a feed material, and washing out the residual sulfuric acid solution;
(5) backwashing: backwashing the anion exchange resin column switched to the backwashing area 7, and switching the weak-base anion exchange resin column in the backwashing area from the water washing acid area 5;
(6) regeneration: regenerating the weak base anion exchange resin column in the regeneration area 3 by using normal temperature weak ammonia water solution as a regenerant to obtain ammonium sulfate solution and a regenerated weak base anion exchange resin column, wherein the mass concentration of ammonia water is 20%;
(7) water leaching: and (3) cleaning the weak base anion exchange resin column in the water leaching area 6 by taking the evaporated condensate water or the steam condensate water or the deionized water as a feeding material, washing out the residual ammonia water solution, and switching to the adsorption area 1 for another period of operation after the weak base anion exchange resin column in the water leaching area 6 is leached.
The valve array type continuous ion exchange system used for purifying the red lactic acid is shown in figure 7 and comprises an adsorption area 1, an analysis area 2, a regeneration area 3, a water washing material area 4, a water acid washing area 5, a water leaching area 6 and a backwashing area 7; the feeding material of the anion exchange resin column of the adsorption area 1 is a red lactic acid solution, the anion exchange resin column of the analysis area 2 adsorbs lactate, the feeding material is a sulfuric acid solution, the anion exchange resin column of the regeneration area 3 adsorbs sulfate radicals, the feeding material is an ammonia water solution, the water washing material area 4, the water washing acid area 5 and the water spraying area 6 all feed water, and the feeding material of the backwashing area 7 is dilute ammonia water.
The specific structure of the valve array type continuous ion exchange system for purifying the red lactic acid is as follows:
adsorption zone 1: the number of anion exchange resin columns in this zone is preferably 2 or more, and in this embodiment, the unit comprises 8 to 13#6 ion exchange columns, but the number of resin columns may be set as the case may be.
The red lactic acid solution sequentially enters the ion resin exchange columns of the adsorption zone 1 in a downstream column-string mode, and the ionic lactic acid is exchanged to the groups of the resin framework.
Washing material area 4: the water-washing material zone 4 has 1 anion exchange resin column which is switched from the adsorption zone 1. Specifically, the outlet of the 13# column (the last anion exchange resin column in the adsorption zone 1) is detected, when the pH value is less than 3, the 8# column is saturated by adsorption, the column cutting operation is performed at the moment, the 8# column is cut to the water washing material zone 4 where the 7# column is located for water washing, the residual material in the column is washed out to a crude lactic acid tank, and when the 8# column is switched, the 7# column is switched to an analysis zone.
Detecting the effluent of the anion exchange resin column in the water washing material zone 4, wherein the effluent is qualified when the pH value is more than or equal to 3, and switching to the next analysis zone 2;
analysis area 2: the number of anion exchange resin columns in the desorption zone 2 is preferably more than 2, and the anion exchange resin columns in the zone are switched from the water washing material zone 4, namely, after the water washing material is finished, the resin columns are switched to the desorption zone 2. In this example, the analysis zone 2 is composed of 3 resin columns (such as column # 4-6 in FIG. 6), and the resin columns in the analysis zone 2 are all resin columns saturated by lactic acid adsorption cut one by the water wash zone 4. Sulfuric acid solution is fed from the No. 4 column and sequentially flows in the column to the No. 5 and No. 6 columns, the sulfate radicals in the column displace lactic acid on the resin, and the lactic acid is discharged from the No. 6 column to a lactic acid recovery tank, so that a required cleaner lactic acid product is obtained. And (3) taking an outlet sample of the 6# column to detect sulfate radicals, stopping feeding sulfuric acid solution into the 4# column when the detected value of the sulfate radicals is larger than a set value, and switching the resin column (the sulfate radicals are titrated by barium chloride solution of 0.25g/ml, and the set value is reached when white precipitates appear).
Water washing acid zone 5: consists of 3 resin columns (as shown in figures 1-3 #) (the number of resin columns can be set according to actual conditions). The resolved column is cut into a water washing acid zone 5, residual sulfuric acid in the column is washed out by water, water is fed from the 1# column, the column is sequentially connected to the 2# column and the 3# column, the discharged acid is discharged from the 3# column, and the discharged acid enters a sulfuric acid tank, wherein the standard of water washing completion is that the pH value of the discharged water of the current column such as the 1# column is more than 3.5.
A backwashing zone 7: contains 20# of the one column. And after the anion exchange resin column in the water washing acid zone 5 finishes water washing, switching to a backwashing zone 7 for backwashing.
The backwashing area can be independently supplied with water, diluted ammonia water generated when the 14# column in the water leaching area 6 is quickly leached can be connected to the 20# column through a backwashing inlet valve in series, the anion exchange resin column in the backwashing area is of a lower-in-upper-out structure, impurities in the column are washed out, and the discharged water is clear.
Regeneration zone 3: the column after backwashing in the backwashing area is switched into a regeneration area, the regeneration area comprises 3 columns, namely 17-19 columns (the number of resin columns can be set according to actual conditions), ammonia water solution is fed into the 17# columns and sequentially connected to the 18# and 19# columns, the ammonia water replaces sulfate radicals on the resins to recover the exchange capacity of the resins, and the sulfate radicals and the ammonia radicals are combined to generate ammonium sulfate which is discharged to an ammonium sulfate tank from the 19# column.
A water leaching area 6: comprises 3 resin columns, namely 14-16# columns. The resin columns regenerated in the regeneration zone 3 are sequentially transferred into a water spraying zone 6, deionized water is fed from a 14# column and sequentially flows to a 15# column and a 16# column, and the deionized water is discharged from the 16# column. The standard for completion of the elution is that the pH of the effluent from the current column, e.g., column # 14, is < 10 and the anion exchange resin column after completion of the elution is switched to adsorption zone 1. The discharged water is recycled to the ammonia water tank.
The flow speed of the leaching water in the leaching area is 5-8 BV/h.
When the system runs, all the zones run the parameters set by each zone simultaneously, one resin column is switched every period, one resin column is cut out from one zone, and one resin column is cut in from the adjacent zone, so that the reciprocating circulation realizes the continuous running.
Discharge detection indexes are as follows: the concentration of the analysis solution (lactic acid) is 10-18%, the sulfate radical content is 0, and the chroma is 400-500 APHA; the concentration of the byproduct ammonium sulfate is 6-8%. A comparison of the red lactic acid solution with the lactic acid solution after treatment with a valve array type continuous ion exchange system is shown in FIG. 9. The material liquid filled in the bottle with the label of fig. 9 as the red lactic acid is the filtrate of the red lactic acid raw material after dilution, acidolysis, activated carbon decolorization and plate-and-frame filtration, although the chromaticity is reduced, compared with the red lactic acid raw material in fig. 8, the color change can hardly be seen by naked eyes, which shows that although the impurity content is very high after the activated carbon decolorization treatment, the product with the label of fig. 9 as the recovered lactic acid can be obtained after the treatment of the valve array type multi-unit continuous ion exchange system, and the liquid is clear and transparent and meets the requirement of refined lactic acid. Therefore, the invention solves the important problem that the red milk has high acid content but cannot be utilized due to a large amount of pigment and impurities, and generates great economic benefit and environmental benefit.
TABLE 1 comparison of pre-and post-red lactic acid indices for the system of example 6
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. A method for purifying red lactic acid is characterized by comprising the following steps:
(1) adsorption: adding a red lactic acid solution obtained after dilution, acidolysis and decoloration into a weak-base anion exchange resin column, wherein lactate ions are automatically adsorbed onto the ion exchange resin, and the mass concentration of the red lactic acid solution is 10-30% during feeding;
diluting the red lactic acid, and carrying out acidolysis by using concentrated sulfuric acid, wherein the amount of a sulfuric acid solution is 1-5 per mill of the feeding mass of the red lactic acid solution, and the concentration of the sulfuric acid solution is 98%;
(2) and (3) analysis: adding a sulfuric acid solution into a weak-base anion exchange resin column which adsorbs lactate, and replacing the lactate on the resin with sulfate radicals to obtain a lactic acid solution, wherein the mass concentration of the sulfuric acid solution is 10-40%;
(3) regeneration: and adding ammonia water into the analyzed weak base anion exchange resin column, regenerating the resin, and obtaining the weak base anion exchange resin column with the recovered exchange capacity and a byproduct ammonium sulfate solution after the regeneration is finished.
2. The method for purifying red lactic acid according to claim 1, wherein the adsorbed weakly basic anion exchange resin column constitutes an adsorption zone, the desorbed weakly basic anion exchange resin column constitutes an desorption zone, the regenerated weakly basic anion exchange resin column constitutes a regeneration zone, the weakly basic anion exchange resin column in the adsorption zone is automatically switched to the desorption zone after being adsorbed and saturated, the weakly basic anion exchange resin column in the desorption zone is automatically switched to the regeneration zone, and the weakly basic anion exchange resin column in the regeneration zone is automatically switched to the adsorption zone to form continuous ion exchange.
3. The method of purifying red lactic acid according to claim 1, further comprising the steps of:
washing the materials with water: before the analysis, washing the weak base anion exchange resin column adsorbing lactate, and switching the weak base anion exchange resin column after the washing material is completed to analyze;
washing with water and acid: after the analysis, washing the analyzed weak base anion exchange resin column, and switching the weak base anion exchange resin column after the acid washing to back wash;
backwashing: after washing acid, backwashing the weak base anion exchange resin column after the acid washing is finished, and switching the weak base anion exchange resin column to regenerate after the backwashing is finished;
water leaching: and after regeneration, washing the regenerated weak base anion exchange resin column with water, and switching the weak base anion exchange resin column after washing with water to analyze.
4. The method for purifying red lactic acid according to claim 3, wherein the weak base anion exchange resin column of the washing material constitutes a washing material zone, the weak base anion exchange resin column of the washing acid constitutes a washing acid zone, the weak base anion exchange resin column of the washing water constitutes a washing water zone, the weak base anion exchange resin column of the adsorption zone is saturated and then automatically switched to the washing material zone, the weak base anion exchange resin column of the washing material zone is then automatically switched to the desorption zone, the weak base anion exchange resin column of the desorption zone is automatically switched to the washing acid zone, the weak base anion exchange resin column of the washing acid zone is automatically switched to the backwashing zone, the weak base anion exchange resin column of the backwashing zone is automatically switched to the regeneration zone, the weak base anion exchange resin column of the regeneration zone is automatically switched to the adsorption zone, continuous ion exchange is formed.
5. The method for purifying red lactic acid according to any one of claims 1 to 4, wherein the mass concentration of the aqueous ammonia is 10% to 30%.
6. A process for the purification of lactic acid according to any of claims 2 or 4, wherein the adsorption zone comprises 2 or more than 2 columns of weakly basic anion exchange resin connected in series.
7. The method for purifying red lactic acid according to any one of claims 2 or 4, wherein the resin column switching is performed when the pH of the effluent from the last weak base anion exchange resin column in the adsorption zone is less than 3.
8. The method for purifying red lactic acid according to any one of claims 2 or 4, wherein the resin column is switched when the sulfate concentration of the last weak base anion exchange resin column effluent in the desorption zone is greater than a predetermined value.
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