CN114605257B - Purification method of L-lactic acid - Google Patents
Purification method of L-lactic acid Download PDFInfo
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- CN114605257B CN114605257B CN202210525607.6A CN202210525607A CN114605257B CN 114605257 B CN114605257 B CN 114605257B CN 202210525607 A CN202210525607 A CN 202210525607A CN 114605257 B CN114605257 B CN 114605257B
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- 238000000034 method Methods 0.000 title claims abstract description 114
- JVTAAEKCZFNVCJ-REOHCLBHSA-N L-lactic acid Chemical compound C[C@H](O)C(O)=O JVTAAEKCZFNVCJ-REOHCLBHSA-N 0.000 title claims abstract description 44
- 238000000746 purification Methods 0.000 title claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 130
- 239000003957 anion exchange resin Substances 0.000 claims abstract description 82
- 239000000463 material Substances 0.000 claims abstract description 77
- 238000004519 manufacturing process Methods 0.000 claims abstract description 63
- 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 abstract description 61
- 239000003729 cation exchange resin Substances 0.000 claims abstract description 60
- 238000011069 regeneration method Methods 0.000 claims abstract description 31
- 238000002386 leaching Methods 0.000 claims abstract description 25
- 238000011001 backwashing Methods 0.000 claims abstract description 24
- 230000008929 regeneration Effects 0.000 claims abstract description 24
- 238000000079 presaturation Methods 0.000 claims abstract description 14
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 98
- 239000002253 acid Substances 0.000 claims description 92
- 239000000243 solution Substances 0.000 claims description 62
- 239000003513 alkali Substances 0.000 claims description 60
- 239000011347 resin Substances 0.000 claims description 51
- 229920005989 resin Polymers 0.000 claims description 51
- 239000004310 lactic acid Substances 0.000 claims description 49
- 235000014655 lactic acid Nutrition 0.000 claims description 49
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 11
- 241001550224 Apha Species 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000010828 elution Methods 0.000 claims description 3
- 230000001172 regenerating effect Effects 0.000 claims description 2
- 239000011260 aqueous acid Substances 0.000 claims 1
- 238000005342 ion exchange Methods 0.000 description 157
- 150000001768 cations Chemical class 0.000 description 47
- 150000001450 anions Chemical class 0.000 description 44
- 239000010410 layer Substances 0.000 description 44
- 239000002699 waste material Substances 0.000 description 32
- -1 iron ions Chemical class 0.000 description 26
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 19
- 238000005349 anion exchange Methods 0.000 description 16
- 239000000047 product Substances 0.000 description 16
- 238000001179 sorption measurement Methods 0.000 description 16
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 12
- 239000011241 protective layer Substances 0.000 description 12
- 229920006395 saturated elastomer Polymers 0.000 description 12
- 150000002500 ions Chemical class 0.000 description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 11
- 229910052742 iron Inorganic materials 0.000 description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 229910052799 carbon Inorganic materials 0.000 description 9
- 238000005341 cation exchange Methods 0.000 description 9
- 238000007599 discharging Methods 0.000 description 9
- 238000005086 pumping Methods 0.000 description 9
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 8
- 239000002585 base Substances 0.000 description 8
- 238000002791 soaking Methods 0.000 description 8
- 238000002156 mixing Methods 0.000 description 6
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 description 4
- JVTAAEKCZFNVCJ-UHFFFAOYSA-M Lactate Chemical compound CC(O)C([O-])=O JVTAAEKCZFNVCJ-UHFFFAOYSA-M 0.000 description 4
- 150000001413 amino acids Chemical class 0.000 description 4
- 239000000460 chlorine Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- 238000000855 fermentation Methods 0.000 description 4
- 230000004151 fermentation Effects 0.000 description 4
- 239000000174 gluconic acid Substances 0.000 description 4
- 235000012208 gluconic acid Nutrition 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 230000003204 osmotic effect Effects 0.000 description 4
- 235000006408 oxalic acid Nutrition 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000000049 pigment Substances 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 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
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000005374 membrane filtration Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000000199 molecular distillation Methods 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 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
- 229920002261 Corn starch Polymers 0.000 description 1
- 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
- 229920002472 Starch Polymers 0.000 description 1
- 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
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000008120 corn starch Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- DQYBDCGIPTYXML-UHFFFAOYSA-N ethoxyethane;hydrate Chemical compound O.CCOCC DQYBDCGIPTYXML-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000013072 incoming material Substances 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000013379 molasses Nutrition 0.000 description 1
- 231100000957 no side effect Toxicity 0.000 description 1
- 238000004094 preconcentration Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 229960004793 sucrose Drugs 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
-
- 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
-
- 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
- C07C51/487—Separation; Purification; Stabilisation; Use of additives by treatment giving rise to chemical modification
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention discloses a purification method of L-lactic acid, which comprises the following steps: (1) a production process; (2) a circulating procedure; (3) a water material ejection process: water is adopted to carry out water jacking on the cation exchange resin column and the anion exchange resin column switched from the production process, and the jacked materials are recovered; (4) a backwashing process; (5) a regeneration step; (6) leaching; (7) a pre-saturation process; (8) a material top water process; the cation exchange resin column and the anion exchange resin column of the production process, the circulation process, the water ejection process, the backwashing process, the regeneration process, the leaching process, the pre-saturation process and the water ejection process are continuously switched.
Description
Technical Field
The invention relates to a lactic acid separation and purification technology, in particular to a purification method of L-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 its levorotatory character, it has very good biological compatibility, and can be combined with mammalDirectly 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 through acidolysis, filtration, preconcentration, decolorization, ion exchange, membrane filtration, concentration, molecular distillation and the like, and the cost of the subsequent membrane filtration, concentration and molecular distillation of the ion exchange is higher.
Disclosure of Invention
The invention aims to provide a novel method for purifying L-lactic acid, which adopts a multiple-time ion exchange method and can obtain higher yield.
The technical scheme of the invention is as follows: a method for purifying L-lactic acid comprises the following steps:
(1) the production process comprises the following steps: the crude lactic acid solution enters a cation exchange resin column unit and an anion exchange resin column unit which are arranged in series to obtain a lactic acid purification solution; filtering, evaporating, hydrolyzing and decoloring the L-lactic acid fermentation liquor by using a plate frame to obtain a crude lactic acid solution;
(2) and (3) a circulating process: the crude lactic acid solution enters an anion exchange resin column switched from the production process, effluent liquid circulates in the anion exchange resin column until sulfate ions are detected in the effluent liquid, and the circulation process is finished;
(3) a water material ejection process: respectively carrying out water jacking on the cation exchange resin column switched from the production process and the anion exchange resin column switched from the circulation process by adopting water, and recovering the jacked materials;
(4) and (3) backwashing: backwashing the cation exchange resin column and the anion exchange resin column switched in the water material jacking process by using water;
(5) a regeneration procedure: regenerating a cation exchange resin column and an anion exchange resin column which are switched out in a backwashing process by using a regeneration liquid, wherein the regeneration liquid of the cation exchange resin column is a dilute acid aqueous solution, and the regeneration liquid of the anion exchange resin column is a dilute alkali aqueous solution;
(6) leaching: leaching the anion exchange resin column and the cation exchange resin column switched in the regeneration process by adopting water;
(7) a pre-saturation process: replacing water in the leached anion exchange resin column and cation exchange resin column with weak acid solution; the presaturation procedure adopts weak acid to press out water with pH value or unqualified ion content, so as to reduce the dosage of the incoming material;
(8) and (3) material water ejection procedure: performing material water replacement on the cation exchange resin column after the presaturation procedure by adopting a crude lactic acid solution, and performing material water replacement on the anion exchange resin column by adopting the effluent of a cation exchange resin column unit in the production procedure;
the cation exchange resin column and the anion exchange resin column of the production process, the circulation process, the water ejection process, the backwashing process, the regeneration process, the leaching process, the pre-saturation process and the water ejection process are continuously switched.
The cation exchange resin column unit comprises three stages of cation exchange resin column subunits which are arranged in series, and each stage of cation exchange resin column subunit comprises at least two cation exchange resin columns which are connected in parallel; the anion exchange resin column unit comprises three stages of anion exchange resin column subunits which are arranged in series, and each stage of anion exchange resin column subunit comprises at least two anion exchange resin columns which are connected in parallel.
The anion exchange resin column is OH - Form D319 macroporous weakly basic anion exchange resin.
In the material top water process, liquid discharged from the cation exchange resin column and the anion exchange resin column is discharged according to sewage firstly, when the mass concentration of lactic acid in the liquid discharged from the cation exchange resin column and the anion exchange resin column is more than or equal to 0.5 percent, the drain valve is closed, the weak acid valve is opened to send the liquid discharged to the weak acid tank, and when the mass concentration of lactic acid in the liquid discharged from the cation exchange resin column and the anion exchange resin column is more than or equal to 2.5 percent, the weak acid valve is closed, and the discharge valve is opened.
And (4) feeding the discharged material in the water material lifting procedure into a weak acid tank.
The feeding pipes of the anion exchange resin column and the cation exchange resin column in the pre-saturation process are communicated with a weak acid tank.
The mass concentration of crude lactic acid fed in the production process is 17-22%, and the chroma is less than or equal to 300 APHA.
The feeding flow rate of the production process is controlled at 15-30 m/h.
The water material-lifting process adopts steam condensate water or hot pure water, and the temperature of the water is 45-50 ℃. The water at this temperature helps to strip the acid from the resin.
And when the mass concentration of lactic acid in the discharged solution of the water material ejecting process is less than or equal to 0.5 percent, the water material ejecting process is completed.
The dilute hydrochloric acid solution is 3.5-5% by mass.
The dilute alkali solution is sodium hydroxide solution, and the mass percent concentration of the sodium hydroxide solution is 5-6%.
The regeneration liquid added in the regeneration procedure is 1.5-2 times of the volume of the resin, and the resin is soaked for 2-4 hours.
Mixing the liquid acid from the leaching procedure with the concentrated acid solution in the regenerated liquid, adding the mixture into a cation exchange resin column in the regeneration procedure, and mixing the liquid alkali from the leaching procedure with the concentrated alkali solution in the regenerated liquid, and adding the mixture into an anion exchange resin column; directly backwashing the cation exchange column in the backwashing procedure by the leached water 3; and eluting the water from the elution step 3 to back wash the anion exchange column.
In the leaching procedure, leaching is completed when the pH value of the effluent of the cation exchange resin column is 3-4, and leaching is completed when the pH value of the anion exchange resin column is 8-9.
The weak acid solution is a solution with the content of lactic acid generated by the water jacking and the water jacking of the anion-cation column being less than 2.5 percent.
Drawings
FIG. 1 is a schematic flow diagram of the process of the present invention.
FIG. 2 is a process flow diagram of a manufacturing process.
FIG. 3 is a schematic of resin layering in an ion exchange resin column.
Detailed Description
The present invention will be described in detail with reference to the following examples and drawings.
An extraction method of a purified L-lactic acid solution, as shown in FIG. 1, comprises the following steps,
(1) the production process comprises
a. Primary crossing position: pumping the crude lactic acid solution which is pretreated by the carbon column and has the concentration of 17-22% and the chroma of less than or equal to 300APHA into a cation exchange resin column subunit and an anion exchange resin column subunit which are connected in series by a centrifugal pump for ion exchange, controlling the flow rate at 15-30m for each hour, and discharging the material to a primary ion exchange storage tank when the discharged material ions reach (the chroma of less than or equal to 50-100 APHA). One cation exchange resin subunit has multiple cation exchange resin columns connected in parallel, and one anion exchange resin subunit has multiple anion exchange resin columns connected in parallel.
b. Secondary crossing position: when the primary ion exchange discharge index is unqualified, a protection effect can be achieved. The secondary ion exchange is that two cation exchange resin column subunits are connected in series and then connected in series with two anion exchange resin column subunits which are connected in series.
c. Tertiary ion exchange position: ensuring that the discharge ions and the chroma (iron ions <2ppm, chloride ions <2ppm, sulfate radicals <5ppm and chroma <50-100APHA) of the ion exchange are qualified, wherein the three ion exchange positions are formed by connecting three cation exchange resin column subunits in series and then connecting three anion exchange resin column subunits in series.
The production process can adopt a primary ion exchange position, a secondary ion exchange position or a tertiary ion exchange position according to the situation, preferably a tertiary ion exchange position, and the tertiary ion exchange position is specifically as follows (as shown in figure 2): subjecting decolorized crude lactic acid solution to primary cation column ion exchange, secondary cation column ion exchange and tertiary cation column ion exchange at a flow rate of 15-30 m/h by using a centrifugal pump, then discharging the product to a transit tank, and then pumping the product into primary anion column ion exchange, secondary anion column ion exchange and tertiary anion column ion exchange at a flow rate of 15-30 m/h by using a centrifugal pump (in one embodiment, a cation column 5 column parallel column is primary cation column ion exchange, a series cation column 5 column parallel column is secondary cation column ion exchange, a series cation column 5 column parallel column is tertiary cation column ion exchange, and after tertiary cation column ion exchange, the product enters anion column ion exchange, a anion column 4 column parallel column is primary anion column ion exchange, a series anion column 4 column parallel column is secondary anion column ion exchange, and a series anion column 4 column parallel column is tertiary anion column ion exchange), wherein the columns are controlled by an intelligent control system.
(2) And (3) a circulating process: in practiceThe anion exchange resin column selected in the production process is OH - The D319 macroporous weak-base anion exchange resin has larger physical pores, higher exchange speed, large exchange capacity, high regeneration rate, good organic pollution resistance, osmotic pressure resistance, impact change resistance and high physical strength. Besides a large amount of lactate, a small amount of organic acid radicals such as oxalic acid and gluconic acid, sulfate radicals, chloride ions, amino acids, pigments with negative charges and the like exist in the crude lactic acid solution. According to the adsorption selection sequence of the weak base anion exchange resin to acid radical as OH - >SO 4 2- >Lactate radical>NO 3 - >Cl - >F - During the production process, a large amount of lactate ions can be adsorbed on the anion resin, and then the lactate ions adsorbed on the anion resin are exchanged with H in the material through sulfate ions in the feed lactic acid solution + And combining to generate lactic acid. However, in the production process, the failure of the ion exchange column is judged by the existence of the outflow of chloride ions at the outlet of the ion exchange column, and the resin layer can be divided into three layers (as shown in figure 3) in the material passing process of the ion exchange column according to the adsorption capacity of the resin, namely, the first layer is a saturated layer, the second layer is an ion exchange layer, and the third layer is a protective layer. After the materials continuously flow in, the adsorption capacity of the resin is gradually saturated, the saturated layer moves to the exchange layer, the exchange layer moves to the protective layer (the resin cannot really move, and only the change of the adsorption capacity of the resin is vividly expressed), the ion exchange column loses the protection of the protective layer and can generate a phenomenon of chlorine ion leakage, the failure of the ion exchange column is judged, but lactate ions on the resin of the exchange layer are not exchanged, at this time, the anion exchange resin column is started to circulate until sulfate radicals flow out from the outlet of the ion exchange column, the complete failure of the ion exchange column is judged, and therefore the yield of the ion exchange column can be improved.
(3) A water material ejection process: three serial columns are adopted to jack the completely failed ion exchange column into a tank before ion exchange or a next standby column by using steam condensate water or hot pure water (the temperature is 45-50 ℃), the concentration change condition of the outlet of the failed column needs to be noticed during water jacking, a weak acid tank needs to be switched in when the concentration is less than or equal to 2.5 percent, and the water jacking is completed when the concentration is less than or equal to 0.5 percent.
(4) And (3) backwashing: the column, completed with the water top, is backwashed with steam condensate for the purpose of loosening the resin bed and backwashing out broken resin particles and some impurities.
(5) A regeneration procedure: the waste acid and the waste alkali are used for mixing concentrated acid and concentrated alkali, and the eluted waste acid and the waste alkali are directly connected to a concentrated acid and concentrated alkali pipeline in series and mixed by a mixer, wherein three series-connected columns are also adopted, so that the utilization rate of acid and alkali is improved, and the production cost of a factory is reduced. Adding 3.5-5% hydrochloric acid into positive column, adding 5-6% sodium hydroxide into negative column, adding 1.5-2 times of acid and alkali, and soaking for 2-4 hr. Acid and alkali are recycled and concentrated acid and alkali are mixed, so that the consumption of acid and alkali is reduced.
(6) Leaching: the method also adopts three columns in series connection, the columns after soaking are washed by hot pure water, leached waste acid and waste alkali are reused by being directly connected to the inlet of a regeneration column and mixed with concentrated acid and concentrated alkali, the leaching process is divided into two steps, the first step is to leach the waste acid and waste alkali out of the columns, the pH value of a positive column is washed to 3-4, the pH value of a negative column is washed to 8-9, the second step is to carry out, the leached water is directly series-connected to the columns in the backwashing process, the step also fully utilizes the water, and the use and production cost of the water is reduced. And after the leaching of the anion and cation columns is finished, the iron ions are detected to be less than or equal to 2ppm, and the chloride ions are detected to be less than or equal to 2ppm, so that the ion exchange column can be put into production. The amount of water used is about 4-8 times the volume of the resin.
(7) A pre-saturation process: the washed column is replaced by the water of the ion exchange column by using a weak acid solution (the concentration is less than or equal to 2.5 percent), so that the burden of a concentration post is reduced, and the production cost is reduced.
(8) A step of material top water, in which during the material top water of the positive column, crude lactic acid solution which is pretreated by a carbon column and has the color of less than or equal to 300APHA is pumped into a positive ion exchange column by a centrifugal pump to carry out the material water replacement process; when the material of the anion column is subjected to water jacking, the concentration of the lactic acid solution which is processed by the third ion exchange treatment of the cation column is 20 percent, iron ions with the concentration less than 5ppm are pumped into the anion exchange column through a centrifugal pump to carry out material water replacement, when the concentration of the material jacking water outlet of the cation and anion exchange column is more than or equal to 0.5 percent, the blowoff valve is switched to a weak acid valve, the effluent is sent to a weak acid tank, when the concentration of the material jacking water outlet of the cation and anion exchange column is more than or equal to 2.5 percent, the weak acid valve is closed and switched to a three-time discharge valve, and the process enters the formal production process.
The automatic control system realizes real-time display, alarm, valve opening, state, operation time and the like of the starting, the stopping, the flow control, the current, the power, the frequency, the state and the like of the pump.
Improves the working efficiency, reduces the consumption of water, alkali, acid and steam in the production and improves the yield of the product.
Example 1
An extraction method of a purified L-lactic acid solution, as shown in FIG. 1, comprises the following steps,
(1) the production process comprises
a. Primary crossing position: pumping the crude lactic acid solution which is pretreated by the carbon column and has the concentration of 22% and the chromaticity of less than or equal to 300APHA into a cation exchange resin column subunit and an anion exchange resin column subunit which are connected in series by a centrifugal pump for ion exchange, controlling the flow rate at 15m for each hour, and discharging the material to a primary ion exchange storage tank when the discharged material ions reach (the chromaticity of less than or equal to 50-100 APHA). One cation exchange resin subunit has multiple cation exchange resin columns connected in parallel, and one anion exchange resin subunit has multiple anion exchange resin columns connected in parallel.
b. Secondary crossing position: when the primary ion exchange discharge index is unqualified, a protection effect can be achieved. The secondary ion exchange is that two cation exchange resin column subunits are connected in series and then connected in series with two anion exchange resin column subunits which are connected in series.
c. Tertiary ion exchange position: ensuring that the ion and chromaticity of the ion exchange discharge material are qualified, wherein the third ion exchange position is formed by connecting three cation exchange resin column subunits in series and then connecting three anion exchange resin column subunits in series.
The three ion exchange positions of the production process are specifically as follows (as shown in FIG. 2): subjecting the decolorized crude lactic acid solution to primary cation column ion exchange, secondary cation column ion exchange and tertiary cation column ion exchange at a flow rate of 15 m/h by using a centrifugal pump, then discharging the product to a transit tank, and then pumping the product into primary anion column ion exchange, secondary anion column ion exchange and tertiary anion column ion exchange at a flow rate of 15 m/h by using the centrifugal pump (in one embodiment, a positive column 5 column parallel column is primary cation column ion exchange, a positive column 5 column parallel column is secondary cation column ion exchange, a positive column 5 column parallel column is tertiary cation column ion exchange, and after the tertiary cation column ion exchange, the product enters anion column ion exchange again, a negative column 4 column parallel column is primary anion column ion exchange, a negative column 4 column parallel column is secondary anion column ion exchange, and a negative column 4 column parallel column is tertiary anion exchange), wherein the columns are controlled by an intelligent control system.
(2) And (3) a circulating process: the anion exchange resin column selected in the actual production process is OH - The D319 macroporous weak-base anion exchange resin has larger physical pores, higher exchange speed, large exchange capacity, high regeneration rate, good organic pollution resistance, osmotic pressure resistance, impact change resistance and high physical strength. Besides a large amount of lactate, a small amount of organic acid radicals such as oxalic acid and gluconic acid, sulfate radicals, chloride ions, amino acids, negatively charged pigments and the like exist in the crude lactic acid solution. According to the adsorption selection sequence of the weak base anion exchange resin to acid radical as OH - >SO 4 2- >Lactate radical>NO 3 - >Cl - >F - During the production process, a large amount of lactate ions can be adsorbed on the anion resin, and then the lactate ions adsorbed on the anion resin are exchanged with H in the material through sulfate ions in the feed lactic acid solution + And combining to generate lactic acid. However, in the production process, the failure of the ion exchange column is judged by the existence of the outflow of chloride ions at the outlet of the ion exchange column, and the resin layer can be divided into three layers (as shown in figure 3) in the material passing process of the ion exchange column according to the adsorption capacity of the resin, namely, the first layer is a saturated layer, the second layer is an ion exchange layer, and the third layer is a protective layer. When the materials continuously flow in, the adsorption capacity of the resin is gradually saturated, the saturated layer moves to the exchange layer, the exchange layer moves to the protective layer (the resin does not really move, only the change of the adsorption capacity of the resin is vividly expressed), the ion exchange column loses the protection of the protective layer and the phenomenon of chlorine ion leakage occurs, the failure of the ion exchange column is judged, but the resin of the exchange layer also contains lactic acidThe ions are not exchanged, and at the moment, the circulation of the anion exchange resin column is started until sulfate radicals flow out from an outlet of the ion exchange column, and the ion exchange column is judged to be completely invalid, so that the yield of the ion exchange column can be improved.
(3) A water material ejection process: three series columns are adopted to jack the completely failed ion exchange column into a pre-ion exchange tank or a next standby column by using steam condensate water or hot pure water (the temperature is 45 ℃), the concentration change condition of the outlet of the failed column needs to be noticed during water jacking, a weak acid tank is switched in when the concentration is less than or equal to 2.5 percent, and the water jacking is completed when the concentration is less than or equal to 0.5 percent.
(4) And (3) backwashing: the column, completed with the water top, is backwashed with steam condensate for the purpose of loosening the resin bed and backwashing out broken resin particles and some impurities.
(5) A regeneration procedure: the waste acid and the waste alkali are used for mixing concentrated acid and concentrated alkali, and the eluted waste acid and the waste alkali are directly connected to a concentrated acid and concentrated alkali pipeline in series and mixed by a mixer, wherein three series-connected columns are also adopted, so that the utilization rate of acid and alkali is improved, and the production cost of a factory is reduced. Adding 3.5% hydrochloric acid into positive column, adding 5% sodium hydroxide into negative column, adding 1.5-2 times of acid and alkali, and soaking for 2-4 hr. Acid and alkali are recycled and concentrated acid and alkali are mixed, so that the consumption of acid and alkali is reduced.
(6) Leaching: the method also adopts three columns in series connection, the columns after soaking are washed by hot pure water, leached waste acid and waste alkali are reused by being directly connected to the inlet of a regeneration column and mixed with concentrated acid and concentrated alkali, the leaching process is divided into two steps, the first step is to leach the waste acid and waste alkali out of the columns, the pH value of a positive column is washed to 3-4, the pH value of a negative column is washed to 8-9, the second step is to carry out, the leached water is directly series-connected to the columns in the backwashing process, the step also fully utilizes the water, and the use and production cost of the water is reduced. And after the leaching of the anion and cation columns is finished, the iron ions are detected to be less than or equal to 2ppm, and the chloride ions are detected to be less than or equal to 2ppm, so that the ion exchange column can be put into production. The amount of water used is about 4-8 times the volume of the resin.
(7) A pre-saturation process: the washed column is replaced by the water of the ion exchange column by using a weak acid solution (the concentration is less than or equal to 2.5 percent), so that the burden of a concentration post is reduced, and the production cost is reduced.
(8) A step of material top water, in which during the material top water of the positive column, 17 percent of crude lactic acid solution which is pretreated by a carbon column and has the chromaticity less than or equal to 300APHA is pumped into a positive ion exchange column by a centrifugal pump to carry out the material water replacement process; when the material of the anion column is subjected to water jacking, the concentration of the lactic acid solution which is processed by the third ion exchange treatment of the cation column is 20 percent, iron ions with the concentration less than 5ppm are pumped into the anion exchange column through a centrifugal pump to carry out material water replacement, when the concentration of the material jacking water outlet of the cation and anion exchange column is more than or equal to 0.5 percent, the blowoff valve is switched to a weak acid valve, the effluent is sent to a weak acid tank, when the concentration of the material jacking water outlet of the cation and anion exchange column is more than or equal to 2.5 percent, the weak acid valve is closed and switched to a three-time discharge valve, and the process enters the formal production process.
The automatic control system realizes real-time display, alarm, valve opening, state, operation time and the like of the starting, the stopping, the flow control, the current, the power, the frequency, the state and the like of the pump.
Improves the working efficiency, reduces the consumption of water, alkali, acid and steam in the production and improves the yield of the product.
Example 2
An extraction method of a purified L-lactic acid solution, as shown in FIG. 1, comprises the following steps,
(1) the production process comprises
a. Primary crossing position: pumping the crude lactic acid solution which is pretreated by the carbon column and has the concentration of 22% and the chromaticity of less than or equal to 300APHA into a cation exchange resin column subunit and an anion exchange resin column subunit which are connected in series by a centrifugal pump for ion exchange, controlling the flow rate at 30m for each hour of cultivation, and discharging the material to a primary ion exchange storage tank when the discharged material ions reach (the chromaticity of less than or equal to 50-100 APHA). One cation exchange resin subunit has multiple cation exchange resin columns connected in parallel, and one anion exchange resin subunit has multiple anion exchange resin columns connected in parallel.
b. Secondary crossing position: when the primary ion exchange discharge index is unqualified, a protection effect can be achieved. The secondary ion exchange is that two cation exchange resin column subunits are connected in series and then connected in series with two anion exchange resin column subunits which are connected in series.
c. Tertiary ion exchange position: ensuring that the discharge ions and the chroma (iron ions <2ppm, chloride ions <2ppm, sulfate radicals <5ppm and chroma <50-100APHA) of the ion exchange are qualified, wherein the three ion exchange positions are formed by connecting three cation exchange resin column subunits in series and then connecting three anion exchange resin column subunits in series.
The production process adopts three times of ion exchange positions, and the three times of ion exchange positions are specifically as follows (as shown in figure 2): subjecting the decolorized crude lactic acid solution to primary cation column ion exchange, secondary cation column ion exchange and tertiary cation column ion exchange at the flow rate of 30 m/h by using a centrifugal pump, then discharging the product to a transit tank, and then pumping the product into primary anion column ion exchange, secondary anion column ion exchange and tertiary anion column ion exchange at the flow rate of 30 m/h by using the centrifugal pump (in one embodiment, a positive column 5 column parallel column is primary cation column ion exchange, a positive column 5 column parallel column is secondary cation column ion exchange, a positive column 5 column parallel column is tertiary cation column ion exchange, and after the tertiary cation column ion exchange, the product enters anion column ion exchange, a negative column 4 column parallel column is primary anion column ion exchange, a negative column 4 column parallel column is secondary anion column ion exchange, and a negative column 4 column parallel column is tertiary anion exchange), wherein the columns are controlled by an intelligent control system.
(2) And (3) a circulating process: the anion exchange resin column selected in the actual production process is OH - The D319 macroporous weak-base anion exchange resin has larger physical pores, higher exchange speed, large exchange capacity, high regeneration rate, good organic pollution resistance, osmotic pressure resistance, impact change resistance and high physical strength. Besides a large amount of lactate, a small amount of organic acid radicals such as oxalic acid and gluconic acid, sulfate radicals, chloride ions, amino acids, pigments with negative charges and the like exist in the crude lactic acid solution. According to the adsorption selection sequence of the weak base anion exchange resin to acid radical as OH - >SO 4 2- >Lactate radical>NO 3 - >Cl - >F - During the production process, a large amount of lactate ions can be adsorbed on the anion resin, and then the lactate ions adsorbed on the anion resin are exchanged with H in the material through sulfate ions in the feed lactic acid solution + And combining to generate lactic acid. But in the production process IThe failure of the ion exchange column is judged by the existence of the outflow of chloride ions at the outlet of the ion exchange column, and the resin layer can be divided into three layers (as shown in figure 3) in the material passing process of the ion exchange column according to the adsorption capacity of the resin, namely, the first layer is a saturated layer, the second layer is an ion exchange layer, and the third layer is a protective layer. After the materials continuously flow in, the adsorption capacity of the resin is gradually saturated, the saturated layer moves to the exchange layer, the exchange layer moves to the protective layer (the resin cannot really move, and only the change of the adsorption capacity of the resin is vividly expressed), the ion exchange column loses the protection of the protective layer and can generate a phenomenon of chlorine ion leakage, the failure of the ion exchange column is judged, but lactate ions on the resin of the exchange layer are not exchanged, at this time, the anion exchange resin column is started to circulate until sulfate radicals flow out from the outlet of the ion exchange column, the complete failure of the ion exchange column is judged, and therefore the yield of the ion exchange column can be improved.
(3) A water material ejection process: three serial columns are adopted to jack the completely failed ion exchange column to a pre-ion exchange tank or a next standby column by using steam condensate water or hot pure water (the temperature is 50 ℃), the concentration change condition of the outlet of the failed column needs to be noticed during water jacking, a weak acid tank needs to be cut when the concentration is less than or equal to 2.5 percent, and the water jacking is completed when the concentration is less than or equal to 0.5 percent.
(4) And (3) backwashing: the column, completed with the water top, is backwashed with steam condensate for the purpose of loosening the resin bed and backwashing out broken resin particles and some impurities.
(5) A regeneration procedure: the waste acid and the waste alkali are used for mixing concentrated acid and concentrated alkali, and the eluted waste acid and the waste alkali are directly connected to a concentrated acid and concentrated alkali pipeline in series and mixed by a mixer, wherein three series-connected columns are also adopted, so that the utilization rate of acid and alkali is improved, and the production cost of a factory is reduced. Adding 5% hydrochloric acid into positive column, adding 6% sodium hydroxide into negative column, adding 1.5-2 times of acid and alkali volume of resin volume, and soaking for 2-4 hr. Acid and alkali are recycled and concentrated acid and alkali are mixed, so that the consumption of acid and alkali is reduced.
(6) Leaching: the method also adopts three columns in series connection, the columns after soaking are washed by hot pure water, leached waste acid and waste alkali are reused by being directly connected to the inlet of a regeneration column and mixed with concentrated acid and concentrated alkali, the leaching process is divided into two steps, the first step is to leach the waste acid and waste alkali out of the columns, the pH value of a positive column is washed to 3-4, the pH value of a negative column is washed to 8-9, the second step is to carry out, the leached water is directly series-connected to the columns in the backwashing process, the step also fully utilizes the water, and the use and production cost of the water is reduced. And after the leaching of the anion and cation columns is finished, the iron ions are detected to be less than or equal to 2ppm, and the chloride ions are detected to be less than or equal to 2ppm, so that the ion exchange column can be put into production. The amount of water used is about 4-8 times the volume of the resin.
(7) A pre-saturation process: the washed column is replaced by the water of the ion exchange column by using a weak acid solution (the concentration is less than or equal to 2.5 percent), so that the burden of a concentration post is reduced, and the production cost is reduced.
(8) A step of material top water, in which during the material top water of the positive column, crude lactic acid solution which is pretreated by a carbon column and has the color of less than or equal to 300APHA is pumped into a positive ion exchange column by a centrifugal pump to carry out the material water replacement process; when the material of the anion column is subjected to water jacking, the concentration of the lactic acid solution which is processed by the third ion exchange treatment of the cation column is 20 percent, iron ions with the concentration less than 5ppm are pumped into the anion exchange column through a centrifugal pump to carry out material water replacement, when the concentration of the material jacking water outlet of the cation and anion exchange column is more than or equal to 0.5 percent, the blowoff valve is switched to a weak acid valve, the effluent is sent to a weak acid tank, when the concentration of the material jacking water outlet of the cation and anion exchange column is more than or equal to 2.5 percent, the weak acid valve is closed and switched to a three-time discharge valve, and the process enters the formal production process.
The automatic control system realizes real-time display, alarm, valve opening, state, operation time and the like of the starting, the stopping, the flow control, the current, the power, the frequency, the state and the like of the pump.
Improves the working efficiency, reduces the consumption of water, alkali, acid and steam in the production and improves the yield of the product.
Example 3
An extraction method of a purified L-lactic acid solution, as shown in FIG. 1, comprises the following steps,
(1) the production process comprises
a. Primary crossing position: pumping the crude lactic acid solution which is pretreated by the carbon column and has the concentration of 20 percent and the chroma of less than or equal to 300APHA into a cation exchange resin column subunit and an anion exchange resin column subunit which are connected in series by a centrifugal pump for ion exchange, controlling the flow rate at 25m for each hour, and discharging the material to a primary ion exchange storage tank when the discharged material ions reach (the chroma of less than or equal to 50-100 APHA). One cation exchange resin subunit has multiple cation exchange resin columns connected in parallel, and one anion exchange resin subunit has multiple anion exchange resin columns connected in parallel.
b. Secondary crossing position: when the primary ion exchange discharge index is unqualified, a protection effect can be achieved. The secondary ion exchange is that two cation exchange resin column subunits are connected in series and then connected in series with two anion exchange resin column subunits which are connected in series.
c. Tertiary ion exchange position: ensuring that the discharge ions and the chroma (iron ions <2ppm, chloride ions <2ppm, sulfate radicals <5ppm and chroma <50-100APHA) of the ion exchange are qualified, wherein the three ion exchange positions are formed by connecting three cation exchange resin column subunits in series and then connecting three anion exchange resin column subunits in series.
The production process adopts three times of ion exchange positions, and the three times of ion exchange positions are specifically as follows (as shown in figure 2): subjecting the decolorized crude lactic acid solution to primary cation column ion exchange, secondary cation column ion exchange and tertiary cation column ion exchange at a flow rate of 15-30 m/h by using a centrifugal pump, then discharging the product to a transit tank, and then pumping the product into primary anion column ion exchange, secondary anion column ion exchange and tertiary anion column ion exchange at a flow rate of 25 m/h by using a centrifugal pump (in one embodiment, a positive column 5 column parallel column is primary cation column ion exchange, a positive column 5 column series parallel column is secondary cation column ion exchange, a positive column 5 column series parallel column is tertiary cation column ion exchange, and after the tertiary cation column ion exchange, the product enters anion column ion exchange again, a negative column 4 column parallel column is primary anion column ion exchange, a negative column 4 column series parallel column is secondary anion column ion exchange, and a negative column 4 column series parallel column is tertiary anion exchange), wherein the columns and the columns are controlled by an intelligent control system.
(2) And (3) a circulating process: the anion exchange resin column selected in the actual production process is OH - The D319 macroporous weak-base anion exchange resin has larger physical pores, higher exchange speed, large exchange capacity, high regeneration rate, good organic pollution resistance, osmotic pressure resistance, impact change resistance and high physical strength. Due to the fact thatThe crude lactic acid solution contains a large amount of lactate, and also contains a small amount of organic acid radicals such as oxalic acid and gluconic acid, sulfate radicals, chloride ions, amino acids, negatively charged pigments and the like. According to the adsorption selection sequence of the weak base anion exchange resin to acid radical as OH - >SO 4 2- >Lactate radical>NO 3 - >Cl - >F - During the production process, a large amount of lactate ions can be adsorbed on the anion resin, and then the lactate ions adsorbed on the anion resin are exchanged with H in the material through sulfate ions in the feed lactic acid solution + And combining to generate lactic acid. However, in the production process, the failure of the ion exchange column is judged by the existence of the outflow of chloride ions at the outlet of the ion exchange column, and the resin layer can be divided into three layers (as shown in figure 3) in the material passing process of the ion exchange column according to the adsorption capacity of the resin, namely, the first layer is a saturated layer, the second layer is an ion exchange layer, and the third layer is a protective layer. After the materials continuously flow in, the adsorption capacity of the resin is gradually saturated, the saturated layer moves to the exchange layer, the exchange layer moves to the protective layer (the resin cannot really move, and only the change of the adsorption capacity of the resin is vividly expressed), the ion exchange column loses the protection of the protective layer and can generate a phenomenon of chlorine ion leakage, the failure of the ion exchange column is judged, but lactate ions on the resin of the exchange layer are not exchanged, at this time, the anion exchange resin column is started to circulate until sulfate radicals flow out from the outlet of the ion exchange column, the complete failure of the ion exchange column is judged, and therefore the yield of the ion exchange column can be improved.
(3) A water material ejection process: three series columns are adopted to jack the completely failed ion exchange column into a tank before ion exchange or a next standby column by using steam condensate water or hot pure water (the temperature is 47 ℃), the concentration change condition of the outlet of the failed column needs to be noticed during water jacking, a weak acid tank needs to be switched in when the concentration is less than or equal to 2.5 percent, and the water jacking is completed when the concentration is less than or equal to 0.5 percent.
(4) And (3) backwashing: the water-topped column was backwashed with steam condensate for the purpose of loosening the resin bed and backwashing out broken resin particles and some impurities.
(5) A regeneration procedure: the waste acid and the waste alkali are used for mixing concentrated acid and concentrated alkali, and the eluted waste acid and the waste alkali are directly connected to a concentrated acid and concentrated alkali pipeline in series and mixed by a mixer, wherein three series-connected columns are also adopted, so that the utilization rate of acid and alkali is improved, and the production cost of a factory is reduced. Adding 4% hydrochloric acid into positive column, adding 5.5% sodium hydroxide into negative column, adding 1.5-2 times of acid and alkali, and soaking for 2-4 hr. Acid and alkali are recycled and concentrated acid and alkali are mixed, so that the consumption of acid and alkali is reduced.
(6) Leaching: the method also adopts three columns in series connection, the columns after soaking are washed by hot pure water, leached waste acid and waste alkali are reused by being directly connected to the inlet of a regeneration column and mixed with concentrated acid and concentrated alkali, the leaching process is divided into two steps, the first step is to leach the waste acid and waste alkali out of the columns, the pH value of a positive column is washed to 3-4, the pH value of a negative column is washed to 8-9, the second step is to carry out, the leached water is directly series-connected to the columns in the backwashing process, the step also fully utilizes the water, and the use and production cost of the water is reduced. And after the leaching of the anion and cation columns is finished, the iron ions are detected to be less than or equal to 2ppm, and the chloride ions are detected to be less than or equal to 2ppm, so that the ion exchange column can be put into production. The amount of water used is about 4-8 times the volume of the resin.
(7) A pre-saturation process: the washed column is replaced by the water of the ion exchange column by using a weak acid solution (the concentration is less than or equal to 2.5 percent), so that the burden of a concentration post is reduced, and the production cost is reduced.
(8) A step of material top water, in which during the material top water of the positive column, crude lactic acid solution which is pretreated by a carbon column and has the color of less than or equal to 300APHA is pumped into a positive ion exchange column by a centrifugal pump to carry out the material water replacement process; when the material of the anion column is subjected to water jacking, the concentration of the lactic acid solution which is processed by the third ion exchange treatment of the cation column is 20 percent, iron ions with the concentration less than 5ppm are pumped into the anion exchange column through a centrifugal pump to carry out material water replacement, when the concentration of the material jacking water outlet of the cation and anion exchange column is more than or equal to 0.5 percent, the blowoff valve is switched to a weak acid valve, the effluent is sent to a weak acid tank, when the concentration of the material jacking water outlet of the cation and anion exchange column is more than or equal to 2.5 percent, the weak acid valve is closed and switched to a three-time discharge valve, and the process enters the formal production process.
The automatic control system realizes real-time display, alarm, valve opening, state, operation time and the like of the starting, the stopping, the flow control, the current, the power, the frequency, the state and the like of the pump.
Improves the working efficiency, reduces the consumption of water, alkali, acid and steam in the production and improves the yield of the product.
Comparative example 1
A method for extracting an L-lactic acid solution,
m-a production process comprising
Primary crossing position: pumping the crude lactic acid solution which is pretreated by a carbon column and has the concentration of 22% and the chromaticity of less than or equal to 300APHA into a cation exchange resin column subunit and an anion exchange resin column subunit which are connected in series by a centrifugal pump for ion exchange, controlling the flow rate at 15m for each hour, and discharging when discharged ions reach (the chromaticity of less than or equal to 50-100APHA) to obtain the L-lactic acid solution of the comparison example I. One cation exchange resin subunit has 15 cation exchange resin columns connected in parallel, and one anion exchange resin subunit has 12 anion exchange resin columns connected in parallel.
In the comparative example 1, 15 positive columns are connected in parallel and 12 negative columns are connected in parallel, so that the material passing amount is small, unqualified discharge is easy to occur, the discharge chromaticity is high, the column cutting is frequent, the lactic acid yield is low, the consumption of regenerated acid and alkali is high, and the water consumption is large compared with three times of ion exchange.
The three-time ion exchange is that more than 5 positive columns are connected in parallel, more than 4 negative columns are connected in parallel, the switching columns are not frequent, the yield of lactic acid is high, the consumption of regenerated acid and alkali is low, the water consumption is low, the material passing amount is large, the qualified rate of discharged materials can be effectively guaranteed, and the discharged material color is low.
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 L-lactic acid is characterized by comprising the following steps:
(1) the production process comprises the following steps: the crude lactic acid solution enters a cation exchange resin column unit and an anion exchange resin column unit which are arranged in series to obtain a lactic acid purification solution; the cation exchange resin column unit comprises three stages of cation exchange resin column subunits which are arranged in series, and each stage of cation exchange resin column subunit comprises at least two cation exchange resin columns which are connected in parallel; the anion exchange resin column unit comprises three stages of anion exchange resin column subunits which are arranged in series, and each stage of anion exchange resin column subunit comprises at least two anion exchange resin columns which are connected in parallel; the anion exchange resin column is OH - Form D319 macroporous weakly basic anion exchange resin;
(2) and (3) a circulating process: the crude lactic acid solution enters an anion exchange resin column switched from the production process, effluent liquid circulates in the anion exchange resin column until sulfate ions are detected in the effluent liquid, and the circulation process is finished;
(3) a water material ejection process: respectively carrying out water jacking on the cation exchange resin column switched from the production process and the anion exchange resin column switched from the circulation process by adopting water, and recovering the jacked materials;
(4) and (3) backwashing: backwashing the cation exchange resin column and the anion exchange resin column switched in the water material jacking process by using water;
(5) a regeneration process: regenerating a cation exchange resin column and an anion exchange resin column which are switched out in a backwashing process by using a regeneration liquid, wherein the regeneration liquid of the cation exchange resin column is a dilute acid aqueous solution, and the regeneration liquid of the anion exchange resin column is a dilute alkali aqueous solution;
(6) leaching: leaching the anion exchange resin column and the cation exchange resin column switched in the regeneration process by adopting water;
(7) a pre-saturation process: replacing water in the leached anion exchange resin column and cation exchange resin column with weak acid solution;
(8) and (3) material water ejection procedure: performing material water replacement on the cation exchange resin column after the presaturation procedure by adopting a crude lactic acid solution, and performing material water replacement on the anion exchange resin column by adopting the effluent of a cation exchange resin column unit in the production procedure;
the cation exchange resin column and the anion exchange resin column of the production process, the circulation process, the water ejection process, the backwashing process, the regeneration process, the leaching process, the pre-saturation process and the water ejection process are continuously switched.
2. The method for purifying L-lactic acid according to claim 1, wherein the crude lactic acid fed to the production process has a mass concentration of 17-22% and a color of not more than 300 APHA.
3. The method of claim 1, wherein the throughput of the production process is 15-30 m/h.
4. The method of purifying L-lactic acid as claimed in claim 1, wherein the water-lifting step uses steam condensate or hot pure water, and the temperature of the water is 45-50 ℃.
5. The method of purifying L-lactic acid according to claim 1, wherein the water topping step is completed when the mass concentration of lactic acid in the discharged solution of the water topping step is 0.5% or less.
6. The method for purifying L-lactic acid according to claim 1, wherein the dilute aqueous acid solution is a dilute hydrochloric acid solution, and the mass percentage concentration of the dilute hydrochloric acid solution is 3.5-5%; the dilute alkali solution is sodium hydroxide solution, and the mass percent concentration of the sodium hydroxide solution is 5-6%.
7. The method of purifying L-lactic acid as claimed in claim 1, wherein the regeneration liquid added in the regeneration step is 1.5 to 2 times the volume of the resin, and the resin is soaked for 2 to 4 hours.
8. The method for purifying L-lactic acid as claimed in claim 1, wherein the elution is completed when the pH of the effluent from the cation exchange resin column is 3 to 4 and the elution is completed when the pH of the anion exchange resin column is 8 to 9.
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| PCT/CN2023/076141 WO2023155797A1 (en) | 2022-02-16 | 2023-02-15 | Method for purifying l-lactic acid |
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| CN111269107B (en) * | 2020-04-09 | 2021-08-03 | 安徽固德生物工程有限公司 | L-lactic acid purification and refining method |
| CN111592458B (en) * | 2020-05-25 | 2022-12-23 | 中粮营养健康研究院有限公司 | Method for separating lactic acid |
| CN113527085A (en) * | 2021-07-23 | 2021-10-22 | 厦门世达膜工程有限公司 | Production method for purifying lactic acid from lactic acid fermentation liquor |
| CN114409530A (en) * | 2022-02-16 | 2022-04-29 | 欧尚元(天津)有限公司 | Purification method of L-lactic acid |
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2022
- 2022-02-16 CN CN202210140354.0A patent/CN114409530A/en active Pending
- 2022-05-16 CN CN202210525607.6A patent/CN114605257B/en active Active
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2023
- 2023-02-15 WO PCT/CN2023/076141 patent/WO2023155797A1/en unknown
- 2023-02-15 LU LU505290A patent/LU505290B1/en active IP Right Grant
Also Published As
| Publication number | Publication date |
|---|---|
| CN114605257A (en) | 2022-06-10 |
| WO2023155797A1 (en) | 2023-08-24 |
| LU505290A1 (en) | 2023-10-26 |
| LU505290B1 (en) | 2024-02-19 |
| CN114409530A (en) | 2022-04-29 |
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