CN115872482B - Normal-temperature desalting and resource utilization method and device for glutamic acid concentrated mother solution - Google Patents
Normal-temperature desalting and resource utilization method and device for glutamic acid concentrated mother solution Download PDFInfo
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- CN115872482B CN115872482B CN202211350141.7A CN202211350141A CN115872482B CN 115872482 B CN115872482 B CN 115872482B CN 202211350141 A CN202211350141 A CN 202211350141A CN 115872482 B CN115872482 B CN 115872482B
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- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 235000013922 glutamic acid Nutrition 0.000 title claims abstract description 65
- 239000004220 glutamic acid Substances 0.000 title claims abstract description 65
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000011033 desalting Methods 0.000 title claims abstract description 21
- 239000010413 mother solution Substances 0.000 title claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 81
- 239000012452 mother liquor Substances 0.000 claims abstract description 51
- 239000003960 organic solvent Substances 0.000 claims abstract description 37
- 238000001556 precipitation Methods 0.000 claims abstract description 37
- 239000007788 liquid Substances 0.000 claims abstract description 33
- 239000002351 wastewater Substances 0.000 claims abstract description 33
- 239000003792 electrolyte Substances 0.000 claims abstract description 18
- 238000004064 recycling Methods 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000000855 fermentation Methods 0.000 claims abstract description 10
- 230000004151 fermentation Effects 0.000 claims abstract description 10
- 238000010979 pH adjustment Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 235000018102 proteins Nutrition 0.000 claims abstract description 9
- 102000004169 proteins and genes Human genes 0.000 claims abstract description 9
- 108090000623 proteins and genes Proteins 0.000 claims abstract description 9
- 238000011084 recovery Methods 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 4
- 239000007791 liquid phase Substances 0.000 claims abstract 2
- 239000007790 solid phase Substances 0.000 claims abstract 2
- 239000000243 solution Substances 0.000 claims description 56
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 33
- 239000012071 phase Substances 0.000 claims description 28
- -1 compound salt Chemical class 0.000 claims description 27
- 238000003860 storage Methods 0.000 claims description 23
- 239000010865 sewage Substances 0.000 claims description 19
- 239000012074 organic phase Substances 0.000 claims description 17
- 238000002425 crystallisation Methods 0.000 claims description 15
- 230000008025 crystallization Effects 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 150000003839 salts Chemical class 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 239000003337 fertilizer Substances 0.000 claims description 8
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 6
- 239000000395 magnesium oxide Substances 0.000 claims description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 5
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 5
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 3
- 239000001099 ammonium carbonate Substances 0.000 claims description 3
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 3
- 239000000920 calcium hydroxide Substances 0.000 claims description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000292 calcium oxide Substances 0.000 claims description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 3
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 3
- 238000010612 desalination reaction Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- 235000019441 ethanol Nutrition 0.000 description 47
- 239000013078 crystal Substances 0.000 description 8
- 235000021049 nutrient content Nutrition 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 235000001014 amino acid Nutrition 0.000 description 5
- 150000001413 amino acids Chemical class 0.000 description 5
- 238000005469 granulation Methods 0.000 description 5
- 230000003179 granulation Effects 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000013049 sediment Substances 0.000 description 4
- 238000007599 discharging Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000011552 falling film Substances 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 2
- 235000011130 ammonium sulphate Nutrition 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- LPUQAYUQRXPFSQ-DFWYDOINSA-M monosodium L-glutamate Chemical compound [Na+].[O-]C(=O)[C@@H](N)CCC(O)=O LPUQAYUQRXPFSQ-DFWYDOINSA-M 0.000 description 2
- 235000013923 monosodium glutamate Nutrition 0.000 description 2
- 239000004223 monosodium glutamate Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 235000013379 molasses Nutrition 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- 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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
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- Fertilizers (AREA)
Abstract
The invention discloses a normal-temperature desalting and recycling method and a device for glutamic acid concentrated mother solution, wherein the method comprises the following steps: (1) preheating and heating: raising the temperature of the glutamic acid concentrated mother liquor wastewater to 30-80 ℃; (2) electrolyte addition, pH adjustment: adding alkaline electrolyte into the wastewater, stirring, and adjusting the pH value; (3) cooling: cooling the glutamic acid concentrated mother liquor wastewater subjected to pH adjustment to below 20 ℃, and transferring to an alcohol precipitation tank; (4) desalting: injecting an alcohol organic solvent into an alcohol precipitation tank, stirring, and standing to separate into solid and liquid phases; (5) solid-liquid separation; (6) recovery of organic solvent: and collecting the organic solvent, so that the organic solvent can be recycled, and the low-salt liquid remained after rectification can be used for biological fermentation raw materials or protein feeds. The invention also relates to a device for carrying out the method. Compared with the prior art, the method is simple, mass production is easy to realize, and carbon emission is effectively reduced.
Description
Technical Field
The invention relates to a normal-temperature desalting and recycling method for glutamic acid concentrated mother liquor, in particular to a method for treating glutamic acid concentrated mother liquor and recycling the glutamic acid concentrated mother liquor by utilizing electrolyte strengthening and an organic solvent extraction method, and also relates to a device for the method. The invention belongs to the technical field of wastewater treatment.
Background
The glutamic acid industry is one of main industries of fermentation industry in China, the production of glutamic acid in China is gradually increased along with the development of society, 300 ten thousand tons or more are achieved in 2020, the annual sales income is about 270 hundred million yuan, and the profit is about 40 hundred million yuan. The production of monosodium glutamate is usually carried out by taking rice, starch and molasses as main raw materials, saccharifying, fermenting, separating and extracting glutamic acid, and refining to obtain monosodium glutamate product.
The glutamic acid concentration mother liquor is mainly waste liquor generated by falling film concentration after glutamic acid and mycoprotein are extracted from glutamic acid fermentation liquor. It is a high-concentration organic waste water, and has the characteristics of strong acidity, high COD, high BOD, high sulfate radical, high thallus content, low temperature and the like. The wastewater contains a large amount of glutamic acid, reducing sugar, SS and ammonia nitrogen, and any emission of the wastewater not only wastes precious resources, but also causes serious environmental pollution and destroys ecological balance, and if the wastewater enters a sewage treatment system, the cost is high and the operation in winter is difficult.
At present, the main flow process of most glutamic acid production enterprises in China adopts concentrated mother liquor slurry spraying granulation, fluidized bed granulation and high-temperature falling film concentration crystallization technology for extracting ammonium sulfate. The guniting granulated fertilizer is destroyed by a plurality of active ingredients at high temperature in the production process, the pH is about 3.5, the excessive carbonization water solubility is poor, and the problem of smoke pollution exists at the same time; the fluidized bed granulation technology has high granulation cost and small granularity, and can not be mixed with chemical fertilizers; the high-temperature falling film concentration crystallization technology for extracting ammonium sulfate can reduce the amount of concentrated solution, but the residual concentrated mother solution is required to be treated by spraying granulation.
Therefore, the prior art cannot completely meet the requirements of healthy development of the glutamic acid industry due to the limitations of product shape, cost, environmental protection standard and process integrity, and how to efficiently treat the glutamic acid concentrated mother solution without pollution has become an important problem for limiting sustainable development of the glutamic acid industry.
Disclosure of Invention
The invention aims to provide a normal-temperature desalting and recycling method and device for glutamic acid concentrated mother liquor, which can realize recycling of glutamic acid mother liquor and meet the requirement of zero pollutant emission.
In order to solve the technical problems, the invention adopts the following technical means:
the invention relates to a normal-temperature desalting and resource utilization method of glutamic acid concentrated mother liquor, which comprises the following steps:
(1) Preheating and heating: placing glutamic acid concentrated mother liquor wastewater into a reaction kettle, and heating to 30-80 ℃;
(2) Electrolyte addition, pH adjustment: adding alkaline electrolyte into the glutamic acid concentrated mother liquor wastewater, stirring, reacting for 30-90min, and adjusting the pH value of the glutamic acid concentrated mother liquor wastewater to be 3.5-6.5;
(3) And (3) cooling: cooling the glutamic acid concentrated mother liquor wastewater subjected to pH adjustment to below 20 ℃ by adopting a heat exchanger, and transferring to an alcohol precipitation tank;
(4) Desalting: injecting an alcohol organic solvent into an alcohol precipitation tank according to the volume ratio of the alcohol organic solvent to the glutamic acid concentrated mother liquor wastewater of 0.5-1.5:1, stirring at the stirring speed of 60-150r/min for 10-15min, standing for more than 1 hour, separating into solid-liquid two phases, wherein the upper layer is an organic phase solution, and the lower layer is a compound salt crystalline phase;
(5) Solid-liquid separation: sucking out the compound salt crystallization phase from the bottom of the alcohol precipitation tank by utilizing a sewage pump, removing liquid in the compound salt crystallization phase by utilizing a centrifugal machine, recovering the liquid into an organic solution storage tank, and directly using the dehydrated compound salt crystallization as a compound fertilizer raw material;
(6) And (3) organic solvent recovery: the organic phase solution in the alcohol precipitation tank is stored in an organic solution storage tank, the organic solution storage tank enters a rectifying tower, alcohol organic solvent is collected, the alcohol organic solvent returns to the alcohol precipitation tank, so that the recycling of the alcohol organic solvent is realized, and the residual low-salt liquid after rectification is used for preparing biological fermentation raw materials or protein feed.
Wherein, preferably, the alkaline electrolyte in the step (2) is at least one selected from potassium hydroxide, potassium carbonate, calcium oxide, calcium hydroxide, calcium carbonate, magnesium oxide or ammonium carbonate.
Preferably, the cooling in the step (3) is to cool the glutamic acid concentrated mother liquor wastewater with the pH adjusted to below 20 ℃ by adopting a plate heat exchanger.
Preferably, the alcohol organic solvent in the step (4) is an ethanol solution or a methanol solution, wherein the purity of the ethanol solution is >90%, and the purity of the methanol solution is >95%.
Wherein, preferably, the sewage pump in the step (5) is an explosion-proof self-priming sewage pump.
Preferably, the centrifuge in the step (5) is a filter cloth centrifuge or a decanter centrifuge.
Furthermore, in order to cooperate with the method, the invention also provides a normal-temperature desalting device for concentrating the mother liquor of glutamic acid, which comprises a reaction kettle, a heat exchanger, an alcohol precipitation tank, an organic solution storage tank and a rectifying tower which are connected in sequence through pipelines, wherein a sewage pump is further arranged at the bottom of the organic solution storage tank, the sewage pump is connected with a centrifugal machine through a pipeline, the other end of the centrifugal machine is connected with the organic solution storage tank, and the other end of the rectifying tower is connected with the alcohol precipitation tank;
wherein the reaction kettle is used for accommodating glutamic acid concentrated mother liquor wastewater and alkaline electrolyte and enabling the glutamic acid concentrated mother liquor wastewater and alkaline electrolyte to react;
the heat exchanger is used for cooling the glutamic acid concentrated mother liquor wastewater;
wherein the alcohol precipitation tank contains an alcohol organic solvent and is used for desalting treatment of glutamic acid concentrated mother liquor wastewater, and the alcohol precipitation tank is divided into solid-liquid two phases, wherein the upper layer is an organic phase solution, and the lower layer is a compound salt crystalline phase;
wherein the organic solution storage tank is used for storing organic phase solution and liquid separated from the compound salt crystal phase;
the rectification tower is used for rectifying the organic phase solution stored in the organic solution storage tank, the organic solvent obtained by rectification is returned to the alcohol precipitation tank, so that the recycling of the organic solvent is realized, and the residual low-salt liquid after rectification is used for preparing biological fermentation raw materials or protein feed;
wherein, the sewage pump is used for sucking out the compound salt crystalline phase from the bottom of the alcohol precipitation tank;
the centrifugal machine is used for removing liquid in the compound salt crystallization phase, the liquid is recovered to the organic solution storage tank, and the dehydrated compound salt crystallization is directly used as a compound fertilizer raw material.
Preferably, the heat exchanger is a plate heat exchanger.
Preferably, the sewage pump is an explosion-proof self-priming sewage pump.
Preferably, the centrifugal machine is a flat scraper lower discharging centrifugal machine or a horizontal decanter centrifugal machine.
Preferably, the reaction kettle and the alcohol precipitation tank are provided with stirring devices.
It will be understood that terms, such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
Compared with the prior art, the invention has the beneficial effects that:
1. realizes the normal temperature removal of the salt of the glutamic acid mother solution: the electrolyte is fully utilized to increase the dissolving polarity, the dissolving capacity of the organic solvent, water molecules and organic matters is utilized to reduce the solubility of salt, the salt is crystallized out, the efficiency is high, and the energy input is not needed;
2. the full-scale recycling of the glutamic acid concentrated mother liquor can be realized, and zero pollution emission is realized: the solid compound salt produced by the method contains rich nitrogen and potassium elements, the total nutrient content is more than 20%, the nitrogen content is more than 16.5%, the potassium content is more than 3.5%, and the solid compound salt is a high-quality compound fertilizer raw material and has large market demand; the liquid (the water content is about 50%) remained after the rectification of the organic solution phase contains more than 20% of true protein, wherein the content of free amino acid is more than 12%, and the organic solution phase can be used as a biological fermentation matrix and a high-quality protein feed;
3. the recovery rate of the organic solvent is high, and the energy consumption for rectification recovery is small: the organic solvent ethanol or methanol used in the technology has a large boiling point difference from water, is easy to recycle, has no chemical reaction loss in the mother solution, and has a recycling rate of more than 98.5%.
4. Compared with the prior art, the treatment process is simple, is easy to realize mass production, and effectively reduces carbon emission.
Drawings
FIG. 1 is a schematic diagram of the device connection of the present invention;
FIG. 2 is a flow chart of the method of the present invention;
FIG. 3 is a graph showing the effect of the initial pH of the mother liquor on the yield of crystallized complex salts;
FIG. 4 is a graph showing the effect of the initial pH of the mother liquor on the morphology of the crystalline complex salt;
FIG. 5 shows the precipitation yields obtained by adding different volumes of anhydrous methanol.
Detailed Description
The invention will be further described with reference to specific embodiments, and advantages and features of the invention will become apparent from the description. These examples are merely exemplary and do not limit the scope of the invention in any way. It will be understood by those skilled in the art that various changes and substitutions of details and forms of the technical solution of the present invention may be made without departing from the spirit and scope of the present invention, but these changes and substitutions fall within the scope of the present invention.
Example 1
A schematic diagram of the device connection of the present invention is shown in fig. 1. The invention relates to a normal-temperature desalting device for concentrated glutamic acid mother liquor, which comprises a reaction kettle, a heat exchanger, an alcohol precipitation tank, an organic solution storage tank and a rectifying tower which are sequentially connected through pipelines, wherein a sewage pump is further arranged at the bottom of the organic solution storage tank, the sewage pump is connected with a centrifugal machine through a pipeline, the other end of the centrifugal machine is connected with the organic solution storage tank, and the other end of the rectifying tower is connected with the alcohol precipitation tank;
wherein the reaction kettle is used for accommodating glutamic acid concentrated mother liquor wastewater and alkaline electrolyte and enabling the glutamic acid concentrated mother liquor wastewater and alkaline electrolyte to react;
the heat exchanger is used for cooling the glutamic acid concentrated mother liquor waste liquid;
wherein the alcohol precipitation tank contains an alcohol organic solvent for desalting treatment of glutamic acid concentrated mother liquor, and the alcohol precipitation tank is divided into solid-liquid two phases, wherein the upper layer is an organic phase solution, and the lower layer is a compound salt crystalline phase;
wherein the organic solution storage tank is used for storing organic phase solution and liquid separated from the compound salt crystal phase;
the rectification tower is used for rectifying the organic phase solution stored in the organic solution storage tank, the organic solvent obtained by rectification is returned to the alcohol precipitation tank, so that the recycling of the organic solvent is realized, and the residual low-salt liquid after rectification is used for preparing biological fermentation raw materials or protein feed;
wherein, the sewage pump is used for sucking out the compound salt crystalline phase from the bottom of the alcohol precipitation tank;
the centrifugal machine is used for removing liquid in the compound salt crystallization phase, the liquid is recovered to the organic solution storage tank, and the dehydrated compound salt crystallization is directly used as a compound fertilizer raw material.
Wherein the heat exchanger is a plate heat exchanger.
Wherein, the sewage pump is an explosion-proof self-priming sewage pump.
Wherein, the centrifugal machine is a flat scraper lower discharging centrifugal machine or a horizontal decanter centrifuge.
Wherein, the reaction kettle and the alcohol precipitation tank are provided with a stirring device.
A flow chart of the method of the present invention is shown in fig. 2. When the device is used for normal-temperature desalination and recycling of glutamic acid concentrated mother liquor, the device comprises the following steps:
(1) Preheating and heating: placing glutamic acid concentrated mother liquor wastewater into a reaction kettle, and heating to 30-80 ℃;
(2) Electrolyte addition, pH adjustment: adding alkaline electrolyte into the glutamic acid concentrated mother liquor wastewater, stirring, reacting for 30-90min, and adjusting the pH value of the glutamic acid concentrated mother liquor wastewater to be 3.5-6.5;
(3) Cooling the plate heat exchanger: cooling the glutamic acid concentrated mother liquor wastewater subjected to pH adjustment to below 20 ℃ by adopting a heat exchanger, and transferring to an alcohol precipitation tank;
(4) Desalting: injecting an alcohol organic solvent into an alcohol precipitation tank according to the volume ratio of the alcohol organic solvent to the glutamic acid concentrated mother liquor wastewater of 0.5-1.5:1, stirring at the stirring speed of 60-150r/min for 10-15min, standing for more than 1 hour, separating into solid-liquid two phases, wherein the upper layer is an organic phase solution, and the lower layer is a compound salt crystalline phase;
(5) Solid-liquid separation: sucking out the compound salt crystallization phase from the bottom of the alcohol precipitation tank by utilizing a sewage pump, removing liquid in the compound salt crystallization phase by utilizing a centrifugal machine, recovering the liquid into an organic solution storage tank, and directly using the dehydrated compound salt crystallization as a compound fertilizer raw material;
(6) And (3) organic solvent recovery: the organic phase solution in the alcohol precipitation tank is stored in an organic solution storage tank, the organic solution storage tank enters a rectifying tower, alcohol organic solvent is collected, the alcohol organic solvent returns to the alcohol precipitation tank, so that the recycling of the alcohol organic solvent is realized, and the residual low-salt liquid after rectification is used for preparing biological fermentation raw materials or protein feed.
Wherein the alkaline electrolyte in the step (2) is at least one selected from potassium hydroxide, potassium carbonate, calcium oxide, calcium hydroxide, calcium carbonate, magnesium oxide and ammonium carbonate.
Wherein the alcohol organic solvent in the step (4) is ethanol solution or methanol solution, wherein the purity of the ethanol solution is more than 90%, and the purity of the methanol solution is more than 95%.
Example 2 application of the method and apparatus of the invention in the treatment of glutamic acid concentrated mother liquor wastewater
The characteristics of glutamic acid concentrated mother liquor wastewater of a certain enterprise are shown in table 1:
TABLE 1 physicochemical Properties of glutamic acid concentrated mother liquor of certain enterprises
The normal temperature desalting apparatus for the glutamic acid-concentrated mother liquor was as described in example 1. The normal-temperature desalting and resource utilization method of the glutamic acid concentrated mother solution comprises the following steps:
(1) Preheating and heating: placing glutamic acid concentrated mother liquor wastewater into a reaction kettle, and heating to 45 ℃;
(2) Electrolyte addition, pH adjustment: adding magnesium oxide with different contents, adjusting pH to respectively treat 4.5, 5.0, 5.5 and 6.0 without adding magnesium oxide as control, and stirring in a reaction kettle for 30min;
(3) Cooling the plate heat exchanger: cooling the glutamic acid concentrated mother liquor wastewater subjected to pH adjustment to 15 ℃ by adopting a plate heat exchanger, and transferring to an alcohol precipitation tank;
(4) Desalting: adding absolute ethyl alcohol according to the volume ratio of the absolute ethyl alcohol to the glutamic acid concentrated mother solution of 1:1, stirring at the speed of 120r/min, standing for 1 hour, separating into solid-liquid two phases, wherein the upper layer is an organic phase solution, and the lower layer is a compound salt crystalline phase;
(5) The lower compound salt crystal phase is sucked into a discharging centrifugal machine at the lower part of a flat plate type scraper by an explosion-proof self-priming sewage pump, 2000r/min is carried out, dehydration is carried out for 20min, and compound salt crystal sediment with the water content of 33% is obtained, the sediment yield of the water-containing compound salt crystal is shown as a figure 3, and experimental results show that different initial pH values cannot influence the precipitation amount of sediment, but the pH value can influence the crystal particle size in the precipitation sediment through crystal size analysis (figure 4). The nutrient content of the crystallized composite salt is shown in Table 2, and the total nutrient content of the crystallized composite salt is highest at the pH of 5.0.
(6) And (3) organic solvent recovery: the organic phase solution in the alcohol precipitation tank is stored in an organic solution storage tank, the organic solution enters a rectifying tower from the storage tank, and the organic solvent is collected, and experimental results show that the ethanol recovery rate reaches more than 98.1%, the residual liquid characteristics after ethanol rectification recovery are shown in table 3, the total amino acid content exceeds 22% under the most conditional condition, the total amino acid content in dry matters exceeds 40%, sulfate radical and ammonium nitrogen content are greatly reduced compared with concentrated mother liquor, and the organic phase solution has good biochemical performance and can be directly used as protein feed or microbial fermentation matrix.
TABLE 2 Effect of different pH values on nutrient content of crystalline complex salts
TABLE 3 liquid Properties after rectification of the upper organic phase
Example 3
By using the glutamic acid concentration mother liquor, the apparatus and the method used in example 2, when the initial pH is 5.0, different volumes of anhydrous methanol are added to obtain obvious difference of precipitation yield (figure 5); the nutrient content of the crystallized complex salt gradually increases when the volume ratio of the anhydrous methanol to the concentrated solution is less than 100%, the organic matter content gradually decreases, and the nutrient content in the complex salt crystals increases but the increase is not remarkable when the volume ratio is more than 100% (table 4); the amino acid content in the organic solution phase gradually increased when the volume ratio of the anhydrous methanol to the concentrate was less than 110%, and the organic content also gradually increased, and when it was more than 110%, the amino acid content increased, but the increase was not significant (table 5).
TABLE 4 influence of different pH values on nutrient content of crystalline complex salts
TABLE 5 liquid Properties after rectification of the upper organic phase
Although embodiments of the present invention have been disclosed above, it is not limited to the details and embodiments shown, it is well suited to various fields of use for which the invention is suited, and further modifications may be readily made by one skilled in the art, and the invention is therefore not to be limited to the particular details and examples shown and described herein, without departing from the general concepts defined by the claims and the equivalents thereof.
Claims (5)
1. The normal-temperature desalting and recycling method for the glutamic acid concentrated mother solution is characterized by comprising the following steps of:
(1) Preheating and heating: placing glutamic acid concentrated mother liquor wastewater into a reaction kettle, and heating to 30-80 ℃;
(2) Electrolyte addition, pH adjustment: adding alkaline electrolyte into the glutamic acid concentrated mother liquor wastewater, stirring, reacting for 30-90min, and adjusting the pH value of the glutamic acid concentrated mother liquor wastewater to 5.0; the alkaline electrolyte is at least one selected from potassium hydroxide, potassium carbonate, calcium oxide, calcium hydroxide, calcium carbonate, magnesium oxide or ammonium carbonate;
(3) And (3) cooling: cooling the glutamic acid concentrated mother liquor wastewater subjected to pH adjustment to below 20 ℃ by adopting a heat exchanger, and transferring to an alcohol precipitation tank;
(4) Desalting: injecting an alcohol organic solvent into an alcohol precipitation tank according to the volume ratio of the alcohol organic solvent to the glutamic acid concentrated mother liquor wastewater of 0.5-1.5:1, stirring at the stirring speed of 60-150r/min for 10-15min, standing for more than 1 hour, and separating into solid-liquid two phases, wherein the liquid phase is an organic phase solution, and the solid phase is a composite salt crystalline phase;
(5) Solid-liquid separation: sucking out the compound salt crystallization phase from the bottom of the alcohol precipitation tank by utilizing a sewage pump, removing liquid in the compound salt crystallization phase by utilizing a centrifugal machine, recovering the liquid into an organic solution storage tank, and directly using the dehydrated compound salt crystallization as a compound fertilizer raw material;
(6) And (3) organic solvent recovery: the organic phase solution in the alcohol precipitation tank is stored in an organic solution storage tank, the organic solution storage tank enters a rectifying tower, alcohol organic solvent is collected, the alcohol organic solvent returns to the alcohol precipitation tank, so that the recycling of the alcohol organic solvent is realized, and the residual low-salt liquid after rectification is used for preparing biological fermentation raw materials or protein feed.
2. The method for desalting and recycling glutamic acid concentrated mother liquor at normal temperature according to claim 1, wherein the cooling in the step (3) is to cool the glutamic acid concentrated mother liquor wastewater with the pH adjusted to below 20 ℃ by adopting a plate heat exchanger.
3. The method for desalting and recycling glutamic acid concentrated mother solution at normal temperature according to claim 1, wherein the alcohol organic solvent in the step (4) is ethanol solution or methanol solution, wherein the purity of the ethanol solution is >90%, and the purity of the methanol solution is >95%.
4. The method for normal temperature desalination and resource utilization of glutamic acid concentrated mother solution according to claim 1, wherein the sewage pump in the step (5) is an explosion-proof self-priming sewage pump.
5. The method for desalting and recycling the concentrated glutamic acid mother liquor at normal temperature according to claim 1, wherein the centrifuge in the step (5) is a flat scraper lower discharge centrifuge or a decanter centrifuge.
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