CN112471485A - Decolouring refining process for producing gourmet powder - Google Patents
Decolouring refining process for producing gourmet powder Download PDFInfo
- Publication number
- CN112471485A CN112471485A CN202011394934.XA CN202011394934A CN112471485A CN 112471485 A CN112471485 A CN 112471485A CN 202011394934 A CN202011394934 A CN 202011394934A CN 112471485 A CN112471485 A CN 112471485A
- Authority
- CN
- China
- Prior art keywords
- resin
- decoloring
- volume
- mother liquor
- monosodium glutamate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000007670 refining Methods 0.000 title claims abstract description 18
- 239000000843 powder Substances 0.000 title description 2
- 239000012452 mother liquor Substances 0.000 claims abstract description 51
- 238000000855 fermentation Methods 0.000 claims abstract description 39
- 230000004151 fermentation Effects 0.000 claims abstract description 39
- LPUQAYUQRXPFSQ-DFWYDOINSA-M monosodium L-glutamate Chemical compound [Na+].[O-]C(=O)[C@@H](N)CCC(O)=O LPUQAYUQRXPFSQ-DFWYDOINSA-M 0.000 claims abstract description 33
- 235000013923 monosodium glutamate Nutrition 0.000 claims abstract description 33
- 239000004223 monosodium glutamate Substances 0.000 claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 claims abstract description 21
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 10
- 239000011347 resin Substances 0.000 claims description 127
- 229920005989 resin Polymers 0.000 claims description 127
- 238000004042 decolorization Methods 0.000 claims description 34
- 239000003957 anion exchange resin Substances 0.000 claims description 27
- 238000002834 transmittance Methods 0.000 claims description 27
- 239000002585 base Substances 0.000 claims description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 238000006386 neutralization reaction Methods 0.000 claims description 19
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 19
- 239000012492 regenerant Substances 0.000 claims description 18
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical class OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 239000000706 filtrate Substances 0.000 claims description 16
- 239000004005 microsphere Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 12
- 238000001514 detection method Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 11
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 8
- 150000003440 styrenes Chemical class 0.000 claims description 7
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims description 6
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 claims description 6
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 6
- 238000005576 amination reaction Methods 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000002270 dispersing agent Substances 0.000 claims description 6
- 235000013922 glutamic acid Nutrition 0.000 claims description 6
- 239000004220 glutamic acid Substances 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000004806 packaging method and process Methods 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 4
- 239000011780 sodium chloride Substances 0.000 claims description 4
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 4
- 229910001948 sodium oxide Inorganic materials 0.000 claims description 4
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 3
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 3
- HRQGCQVOJVTVLU-UHFFFAOYSA-N bis(chloromethyl) ether Chemical compound ClCOCCl HRQGCQVOJVTVLU-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000003431 cross linking reagent Substances 0.000 claims description 3
- SLGWESQGEUXWJQ-UHFFFAOYSA-N formaldehyde;phenol Chemical compound O=C.OC1=CC=CC=C1 SLGWESQGEUXWJQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000003456 ion exchange resin Substances 0.000 claims description 3
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 3
- 239000000178 monomer Substances 0.000 claims description 3
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 claims description 3
- 229920001568 phenolic resin Polymers 0.000 claims description 3
- 230000000379 polymerizing effect Effects 0.000 claims description 3
- 229960004889 salicylic acid Drugs 0.000 claims description 3
- 238000010557 suspension polymerization reaction Methods 0.000 claims description 3
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 claims description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- 239000008346 aqueous phase Substances 0.000 claims 1
- 239000012071 phase Substances 0.000 claims 1
- 230000002194 synthesizing effect Effects 0.000 claims 1
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 17
- 229910052799 carbon Inorganic materials 0.000 description 12
- 238000002425 crystallisation Methods 0.000 description 7
- 230000008025 crystallization Effects 0.000 description 7
- 229920006395 saturated elastomer Polymers 0.000 description 4
- 239000012535 impurity Substances 0.000 description 3
- 230000001172 regenerating effect Effects 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000010828 elution Methods 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 238000004176 ammonification Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000009516 primary packaging Methods 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/20—Synthetic spices, flavouring agents or condiments
- A23L27/21—Synthetic spices, flavouring agents or condiments containing amino acids
- A23L27/22—Synthetic spices, flavouring agents or condiments containing amino acids containing glutamic acids
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/40—Colouring or decolouring of foods
- A23L5/41—Retaining or modifying natural colour by use of additives, e.g. optical brighteners
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Proteomics, Peptides & Aminoacids (AREA)
- Treatment Of Water By Ion Exchange (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention belongs to the technical field of biological fermentation, and discloses a novel decoloring and refining process in monosodium glutamate production, which comprises the following steps: neutralizing the fermentation liquor in the step 1), decoloring the fermentation liquor in the step 2), crystallizing and adjusting the mother liquor in the step 3), decoloring the mother liquor in the step 4), and preparing the finished product of monosodium glutamate in the step 5). The method has the advantages of high fermentation yield, simple process, high efficiency, environmental protection and low production cost.
Description
Technical Field
The invention belongs to the field of monosodium glutamate production in the biological fermentation industry, and particularly provides a novel decoloring and refining process in monosodium glutamate production.
Background
In the traditional production, the monosodium glutamate fermentation liquor is precipitated by isoelectric point to obtain crystallized glutamic acid, and then neutralized by alkali liquor, and the transmittance of the neutralized liquid is only 10-20 without being decolorized by powdered carbon.
At present, the transmittance of the monosodium glutamate neutralization solution after being decolored by powdered carbon is generally between 83 and 89 (722 spectrophotometer, 430nm waveband and 1cm cuvette detection), then secondary decoloration is carried out by K-15 granular carbon columns, the transmittance of the monosodium glutamate neutralization solution after being decolored by granular carbon can be improved to 92 to 94 (722 spectrophotometer, 430nm waveband and 1cm cuvette detection), and as the adsorption pigment of K-15 granular carbon belongs to physical adsorption, the adsorption effect is poor and the speed is slow.
The neutralization solution enters a crystallization evaporator for crystallization after decolorization, the color of mother liquor becomes dark and impurities are increased after crystallization, in the traditional process, the mother liquor is centrifuged by a centrifuge, tap water is added to adjust the Baume degree to 24-28, then powdered carbon is added for decolorization, the decolorized mother liquor enters K-15 granular carbon for decolorization, and the light transmission energy of the decolorized mother liquor reaches 70-75 (722 spectrophotometer, 430nm waveband, 1cm cuvette detection), so that the process is complex and the cost is high. In the prior art, the method also comprises the step of decolorizing with the Dow resin, wherein carbon powder is firstly added into the neutralized solution, and the neutralized solution is stirred, filtered and decolorized with the Dow resin, and the filtered solution still contains trace carbon powder, so that a subsequent decolorization medium is blocked and saturated, the cleanliness of the solution is low, and the defects of complex structure, low production efficiency, low product quality and the like exist.
Disclosure of Invention
In order to solve the problems of the decoloring refining in the monosodium glutamate production, the invention provides a novel decoloring refining process in the monosodium glutamate production, and the method has the advantages of high fermentation yield, simple process, high efficiency, environmental protection and low production cost.
The invention is realized by the following technical scheme:
a new decoloring and refining process in monosodium glutamate production comprises the following steps: neutralizing the fermentation liquor in the step 1), decoloring the fermentation liquor in the step 2), crystallizing and adjusting the mother liquor in the step 3), decoloring the mother liquor in the step 4), and preparing the finished product of monosodium glutamate in the step 5).
Specifically, step 1) neutralizing the fermentation liquor, adding glutamic acid and 0.5-2 times of water into a neutralization tank, then adding a sodium hydroxide solution in a flowing manner for neutralization, wherein the neutralization temperature is 40-50 ℃, and when the pH value is 6.8-7, the addition of the sodium oxide solution is stopped, so as to obtain the neutralized fermentation liquor;
step 2), decoloring the fermentation liquor, decoloring for the first time, heating the neutralized fermentation liquor to 50-55 ℃, passing through a macroporous phenolic amphoteric resin column, wherein the diameter of resin microspheres in the resin column is 0.35-1.4mm, the flow rate of material passing is 1-2 times of the volume of the resin per hour, and the light transmittance of the neutralized liquid after being decolored by the macroporous phenolic amphoteric resin is not less than 85;
performing secondary decolorization, namely cooling the neutralized liquid after primary decolorization to 30-35 ℃, passing through a styrene series macroporous strong base anion exchange resin column, wherein the diameter of resin microspheres in the resin column is 0.315-1.25mm, the resin filtration flow rate is 1-3 times the volume of the resin per hour, and the light transmittance of the decolorized filtrate is not less than 97 (722 spectrophotometer, 430nm waveband, 1cm cuvette detection);
step 3), crystallizing and adjusting mother liquor, concentrating and crystallizing the filtrate obtained in the step 2, centrifuging the mother liquor by using a centrifugal machine, and adding water into the filtered mother liquor to adjust the Baume degree to 24-28;
step 4), mother liquor is decolorized, the temperature of the mother liquor is controlled to be 50-60 ℃, the mother liquor passes through an acrylic acid series macroporous weak-base anion exchange resin column, the diameter of resin microspheres in the resin column is 0.22-0.85mm, the resin filtration flow rate is 1-2 times of the resin volume per hour, and the light transmittance of the mother liquor is not less than 85 after passing through the acrylic acid series macroporous weak-base anion exchange resin (722 spectrophotometer, 430nm waveband, 1cm cuvette detection);
and 5) preparing finished monosodium glutamate, concentrating and crystallizing the mother liquor decolorized in the step 4), and drying, grading and packaging crystals after twice filtration.
Further, in the step 2), the macroporous phenolic amphoteric resin is synthesized by phenol formaldehyde and salicylic acid in oil phase in the presence of a dispersing agent and a pore-forming agent, and is subjected to oil phase synthesis, balling and amination to synthesize an alkaline group.
Further, in the step 2), when the light transmittance of the solution after primary decolorization is less than 85, the decolorization is stopped, the macroporous phenolic amphoteric resin is eluted and regenerated, firstly, 3-5% of alkali liquor is used for flowing into the resin in an amount which is 2-3 times of the volume of the resin, the flow rate is 1-2 times of the volume of the resin per hour, then 3-5% of hydrochloric acid is used for adding into the resin in an amount which is 2-3 times of the volume of the resin per hour, the flow rate is 1-2 times of the volume of the resin per hour, and finally, the solution is washed by water until the ph is neutral, and the solution can be continuously used for primary decoloriz.
Further, in the step 2), the styrene series macroporous strong base anion exchange resin is synthesized by polymerizing styrene and divinylbenzene in water phase in the presence of a dispersing agent and a pore-forming agent to form microspheres, and then chloromethylating with chloromethyl ether and quaternary ammonification of dimethylamine.
Further, in the step 2), when the light transmittance of the filtrate after the secondary decolorization is less than 97, the decolorization is stopped, the resin column is eluted by using a regenerant, the proportion of the regenerant is 3-5% of hydrochloric acid, the volume of the regenerant is 3 times that of the resin, and the flow rate is 1 time that of the resin per hour.
Further, in the step 4), the acrylic macroporous weakly basic anion exchange resin column takes methyl acrylate or methyl methacrylate as a monomer and divinylbenzene as a cross-linking agent, and the macroporous weakly basic acrylic acid ion exchange resin is synthesized by performing suspension polymerization and then performing amination reaction with tetraethylenepentamine.
Further, in the step 4), when the light transmittance of the filtrate after decolorization is less than 85, the decolorization is stopped, the resin column is eluted by using a regenerant, the regenerant is regenerated by using 3-5% of sodium hydroxide in an amount which is 3 times the volume of the resin at a flow rate which is 1 time the volume of the resin per hour, and then regenerated by using 2 times the volume of the resin with 3% of sodium chloride in a concentration at a flow rate which is 1 time the volume of the resin per hour.
The technical scheme of the invention has the following outstanding advantages and uniqueness:
in the fermentation process, macroporous phenolic amphoteric resin is added to replace carbon powder; styrene series macroporous strong base anion exchange resin replaces K-15 granular carbon to decolor the neutralization solution; the acrylic acid series macroporous alkalescent anion exchange resin column replaces powdered carbon and K-15 granular carbon to decolor the mother liquor, so that links such as filtration, filter pressing and the like are saved, and macromolecular impurities are removed. The invention adopts specific resin to decolorize the feed liquid, greatly removes impurities and pigments, and greatly improves the purity and yield of the product.
Detailed Description
Embodiment 1, a new decoloring and refining process in monosodium glutamate production, which comprises the following steps: neutralizing the fermentation liquor in the step 1), decoloring the fermentation liquor in the step 2), crystallizing and adjusting the mother liquor in the step 3), decoloring the mother liquor in the step 4), and preparing the finished product of monosodium glutamate in the step 5).
Step 1) neutralizing fermentation liquor, namely adding glutamic acid and 0.5-2 times of water into a neutralization tank, then adding a sodium hydroxide solution in a flowing manner for neutralization, stopping adding the sodium oxide solution when the neutralization temperature is 40-50 ℃ and the pH value is 6.8-7, and obtaining neutralized fermentation liquor;
step 2) decoloring the fermentation liquor, decoloring for the first time, heating the neutralized fermentation liquor to 50-55 ℃, passing through a macroporous phenolic amphoteric resin column, wherein the diameter of resin microspheres in the resin column is 0.35-1.4mm, the flow rate of material passing is 1-2 times of the volume of the resin per hour, and the light transmittance of the neutralized liquid after being decolored by the macroporous phenolic amphoteric resin is not less than 85;
performing secondary decolorization, namely keeping the temperature of the neutralized liquid after primary decolorization to 50-60 ℃, passing through a styrene series macroporous strong base anion exchange resin column, wherein the diameter of resin microspheres in the resin column is 0.315-1.25mm, the resin filtration flow rate is 1-3 times the resin volume per hour, and the light transmittance of the decolorized filtrate is not less than 97 (722 spectrophotometer, 430nm waveband, 1cm cuvette detection);
step 3) crystallizing and adjusting mother liquor, concentrating and crystallizing the filtrate obtained in the step 2, centrifuging the mother liquor by using a centrifugal machine, and adding water into the filtered mother liquor to adjust the Baume degree to 24-28;
step 4) mother liquor is decolorized, the mother liquor is heated to 55-60 ℃, and is passed through an acrylic acid series macroporous weak base anion exchange resin column, the diameter of resin microspheres in the resin column is 0.315-1.25mm, the resin filtration flow rate is 1-2 times of the resin volume per hour, and the light transmittance of the mother liquor is not less than 85 after passing through the acrylic acid series macroporous weak base anion exchange resin (722 spectrophotometer, 430nm waveband, 1cm cuvette detection);
and 5) preparing finished monosodium glutamate, concentrating and crystallizing the mother liquor decolorized in the step 4), and drying, grading and packaging the filtered crystal.
In the step 2), the macroporous phenolic amphoteric resin is synthesized by phenol formaldehyde and salicylic acid in an oil phase, and after balling, alkaline groups are synthesized through amination.
In the step 2, when the light transmittance of the solution after primary decolorization is less than 85, the decolorization is stopped, the macroporous phenolic amphoteric resin is eluted and regenerated, the solution flows into the resin by using 3-5% of alkali liquor in an amount which is 2-3 times the volume of the resin, the flow rate is 1-2 times the volume of the resin per hour, then the solution is added into the resin by using 3-5% of hydrochloric acid in an amount which is 2-3 times the volume of the resin per hour, the flow rate is 1-2 times the volume of the resin per hour, and finally the solution is washed by using water until the ph is neutral, so that the solution can be continuously used for primary.
In the step 2), the styrene series macroporous strong base anion exchange resin is synthesized by polymerizing styrene and divinylbenzene in water phase in the presence of a dispersant and a pore-making agent to form microspheres, and then chloromethylating with chloromethyl ether and quaternizing with dimethylamine.
In the step 2), when the light transmittance of the filtrate after the secondary decolorization is less than 93, the decolorization is stopped, the resin column is eluted by using a regenerant, the proportion of the regenerant is 3-5% of the amount of 3 times of the resin volume of hydrochloric acid for regeneration, and the flow rate is 1 time of the resin volume per hour.
In the step 4), the acrylic macroporous weak-base anion exchange resin column takes methyl acrylate or methyl methacrylate as a monomer and divinylbenzene as a cross-linking agent, and the acrylic macroporous weak-base anion exchange resin is synthesized by amination reaction with tetraethylenepentamine after suspension polymerization.
In the step 4), when the light transmittance of the decolorized filtrate is less than 85, stopping decolorizing, eluting the resin column with a regenerant, regenerating the regenerant by 3-5% of sodium hydroxide by 3 times the volume of the resin at a flow rate of 1 time the volume of the resin per hour, and then regenerating the resin column with 3% of sodium chloride by 2 times the volume of the resin at a flow rate of 1 time the volume of the resin per hour.
The method comprises the steps of decoloring and filtering macroporous phenolic amphoteric resin, secondarily decoloring a neutralized decoloring solution by an exchange column containing anion exchange resin, filtering a mother solution after adding water to adjust the baume degree, and secondarily decoloring by the exchange column containing macroporous weak base anion exchange resin with an acrylic acid skeleton.
Embodiment 2, a new decoloring and refining process in monosodium glutamate production, which comprises the following steps: step 1) neutralizing fermentation liquor; step 2), primary decolorization of fermentation liquor, secondary decolorization of the fermentation liquor, and saturated elution; step 3), crystallizing and adjusting mother liquor; step 4), mother liquor is decolorized and is eluted in a saturated mode; and 5) preparing finished monosodium glutamate.
Step 1) neutralizing fermentation liquor, namely adding glutamic acid and 0.5 times of water into a neutralization tank, then adding a sodium hydroxide solution in a flowing manner for neutralization, wherein the neutralization temperature is 40 ℃, and when the pH value is 7, the addition of the sodium oxide solution is stopped, so as to obtain neutralized fermentation liquor;
step 2) primary decolorization of fermentation liquor, heating the neutralized fermentation liquor to 50 ℃, passing through a macroporous phenolic amphoteric resin column, wherein the diameter of resin microspheres in the resin column is 0.315-1.25mm, the flow rate of material passing is 1 time of the volume of the resin per hour, and the light transmittance of the neutralized liquid decolorized by the macroporous phenolic amphoteric resin is not less than 85;
performing secondary decolorization on fermentation liquor, cooling the neutralized liquid after primary decolorization to 30 ℃, passing through a styrene series macroporous strong base anion exchange resin column, wherein the diameter of a resin microsphere in the resin column is 0.315-1.25mm, the resin filtration flow rate is 1-2 times the resin volume per hour, and the light transmittance of the decolorized filtrate is not less than 93 (722 spectrophotometer, 430nm waveband, 1cm cuvette detection);
saturated elution, stopping decoloring when the light transmittance of the solution after primary decoloring of the fermentation liquor is less than 85, and eluting and regenerating the macroporous phenolic amphoteric resin; firstly, 3 percent of alkali liquor is used for flowing into the resin by 3 times of the volume of the resin, and the flow rate is 2 times of the volume of the resin per hour; then adding 5% hydrochloric acid 3 times of the resin volume into the resin, wherein the flow rate is 1 time of the resin volume per hour, and finally washing with water until ph is neutral;
when the light transmittance of the filtrate after the secondary decolorization of the fermentation liquor is less than 93, stopping decolorization, and eluting the resin column by using a regenerant, wherein the proportion of the regenerant is 3 percent of hydrochloric acid and 3 times of the volume of the resin, and the flow rate is 1 time of the volume of the resin per hour;
step 3) crystallizing and adjusting mother liquor, concentrating and crystallizing the filtrate obtained in the step 2, centrifuging the mother liquor by using a centrifugal machine, and adding water into the filtered mother liquor to adjust the Baume degree to 24-28;
step 4) mother liquor decoloration, heating the mother liquor to 60 ℃, and passing through
The diameter of a resin microsphere in the resin column is 0.22-0.85mm, the filtering flow rate of the resin is 1-2 times of the volume of the resin per hour, and the light transmittance of the mother liquor is not less than 85 after passing through the acrylic macroporous weak base anion exchange resin (722 spectrophotometer, 430nm waveband, 1cm cuvette detection);
when the light transmittance of the filtrate after the mother liquor is decolorized is less than 85, the decolorization is stopped, the resin column is eluted by using a regenerant, the proportioning of the regenerant is 5 percent of sodium hydroxide with the amount of 3 times the volume of the resin, the flow rate is 1 time the volume of the resin per hour, and then the regenerant is regenerated by using 3 percent of sodium chloride with the amount of 2 times the volume of the resin per hour, and the flow rate is 1 time the volume of the resin per hour.
And 5) preparing finished monosodium glutamate, concentrating and crystallizing the mother liquor obtained after the resin is decolorized in the step 4), and drying, grading and packaging the filtered crystals.
Example 3, a new process for decoloring and refining in monosodium glutamate production, which comprises a macroporous phenolic amphoteric resin column, a styrene macroporous strong base anion exchange resin column and an acrylic macroporous weak base anion exchange resin column.
Example 4, the present application compares the decolorization amount of the neutralization fermentation broth and the mother liquor with the prior art, and the experimental group is example 2; the control group of the Dow resin had a resin amount of 50 liters.
| Neutralizing the fermentation broth | Mother liquor | Carbon powder | |
| Experimental group | 10000- | 5000 and 10000 l | - |
| Control group | 5000 and 10000 l | 3000- | 15-30Kg |
In conclusion, the present application has about 1 times higher decolorization amount for neutralized fermentation broth and about 0.5 to 1 times higher decolorization amount for mother liquor compared to prior art dow resin decolorization, and no carbon powder consumption.
The method comprises the steps of secondary decolorization of glutamic acid neutralization and macroporous phenolic amphoteric resin, secondary decolorization of neutralization decolorized liquid by an exchange column containing anion exchange resin, crystallization of monosodium glutamate, separation of monosodium glutamate, drying of monosodium glutamate, primary packaging, inspection, packaging of monosodium glutamate and the like to obtain a final monosodium glutamate finished product, wherein the anion exchange resin is macroporous quaternary ammonium base strong base anion exchange resin, and meanwhile, a manufacturing process for realizing crystallization through recycling of crystallization mother liquor is also provided, namely after the baume degree of the crystallization mother liquor is adjusted, powdery carbon does not need to be added, and the crystallized mother liquor directly passes through macroporous weak base acrylic acid series ion exchange resin through K15 granular carbon.
The foregoing list is only illustrative of the preferred embodiments of the present invention. It is obvious that the invention is not limited to the above embodiments, but that many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.
Claims (8)
1. A new decoloring and refining process in monosodium glutamate production comprises the following steps: neutralizing the fermentation liquor in the step 1), decoloring the fermentation liquor in the step 2), crystallizing and adjusting the mother liquor in the step 3), decoloring the mother liquor in the step 4), and preparing the finished product of monosodium glutamate in the step 5).
2. The new decoloring and refining process in monosodium glutamate production according to claim 1, wherein in the step 1) neutralizing the fermentation broth, glutamic acid and 0.5-2 times of water are added into a neutralization tank, then sodium hydroxide solution is fed for neutralization, and when the neutralization temperature is 40-50 ℃ and the pH value is 6.8-7, the addition of sodium oxide solution is stopped, so as to obtain the neutralized fermentation broth;
step 2) decoloring the fermentation liquor, decoloring for the first time, heating the neutralized fermentation liquor to 50-55 ℃, passing through a macroporous phenolic amphoteric resin column, wherein the diameter of resin microspheres in the resin column is 0.35-1.4mm, the flow rate of material passing is 1-2 times of the volume of the resin per hour, and the light transmittance of the neutralized liquid after being decolored by the macroporous phenolic amphoteric resin is not less than 85;
performing secondary decolorization, namely cooling the neutralized liquid after primary decolorization to 30-35 ℃, passing through a styrene series macroporous strong base anion exchange resin column, wherein the diameter of resin microspheres in the resin column is 0.315-1.25mm, the resin filtration flow rate is 1-3 times the volume of the resin per hour, and the light transmittance of the decolorized filtrate is not less than 97 (722 spectrophotometer, 430nm waveband, 1cm cuvette detection);
step 3) crystallizing and adjusting mother liquor, concentrating and crystallizing the filtrate obtained in the step 2, centrifuging the mother liquor by using a centrifugal machine, and adding water into the filtered mother liquor to adjust the Baume degree to 24-28;
step 4) mother liquor is decolorized for one time, the mother liquor is heated to 55-60 ℃, and is filtered by an acrylic acid series macroporous weak base anion exchange resin column, the diameter of resin microspheres in the resin column is 0.22-0.85mm, the resin filtration flow rate is 1-2 times of the resin volume per hour, and the light transmittance of the mother liquor is not less than 85 after passing through the acrylic acid series macroporous weak base anion exchange resin (722 spectrophotometer, 430nm waveband, 1cm cuvette detection);
and 5) preparing finished monosodium glutamate, concentrating and crystallizing the mother liquor decolorized in the step 4), and drying, grading and packaging the filtered crystals.
3. The new decolorizing and refining process for monosodium glutamate production as claimed in claim 2, wherein in step 2), said macroporous phenolic amphoteric resin is prepared by oil phase synthesis of phenol formaldehyde and salicylic acid in the presence of pore-forming agent and dispersant, balling, amination, and synthesizing basic groups.
4. The new decoloring and refining process in monosodium glutamate production according to claim 2, wherein in step 2), when the light transmittance of the solution after primary decoloring is less than 85, decoloring is stopped, the macroporous phenolic amphoteric resin is eluted and regenerated, the solution is first flowed into the resin with 3-5% alkali solution in an amount 2-3 times the volume of the resin at a flow rate of 1-2 times the volume of the resin per hour, then added into the resin with 3-5% hydrochloric acid in an amount 2-3 times the volume of the resin at a flow rate of 1-2 times the volume of the resin per hour, and finally washed with water until ph is neutral, and the solution can be continuously used for primary decoloring.
5. The new decoloring and refining process as claimed in claim 2, wherein in step 2), the styrene-based macroporous strong base anion exchange resin is synthesized by polymerizing styrene and divinylbenzene in the presence of a dispersant and a pore-forming agent in an aqueous phase to form microspheres, chloromethylating with chloromethyl ether, and quaternizing with dimethylamine.
6. The new decoloring and refining process in monosodium glutamate production according to claim 2, wherein in the step 2), when the transmittance of the filtrate after the secondary decoloring is less than 97, the decoloring is stopped, the resin column is eluted with a regenerant, the ratio of the regenerant is 3-5% of the amount of the hydrochloric acid regenerated by 3 times the volume of the resin, and the flow rate is 1 time of the amount of the resin by volume per hour.
7. The new decoloring and refining process in monosodium glutamate production as claimed in claim 2, wherein in said step 4), said acrylic macroporous weak base anion exchange resin column is prepared by using methyl acrylate or methyl methacrylate as monomer, divinylbenzene as cross-linking agent, and then subjecting to suspension polymerization in the presence of dispersant and pore-forming agent, followed by amination reaction with tetraethylenepentamine to synthesize macroporous weak base acrylic acid ion exchange resin.
8. The new decoloring refining process in monosodium glutamate production according to claim 2, wherein in the step 4), when the light transmittance of the decolored filtrate is less than 85, decoloring is stopped, the resin column is eluted with a regenerant, the regenerant is regenerated at a ratio of 3-5% by volume of sodium hydroxide 3 times the volume of the resin at a flow rate of 1 time by volume of the resin per hour, and then regenerated at a ratio of 3% by volume of sodium chloride 2 times the volume of the resin at a flow rate of 1 time by volume of the resin per hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011394934.XA CN112471485B (en) | 2020-12-03 | New decolorizing and refining process in monosodium glutamate production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011394934.XA CN112471485B (en) | 2020-12-03 | New decolorizing and refining process in monosodium glutamate production |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112471485A true CN112471485A (en) | 2021-03-12 |
| CN112471485B CN112471485B (en) | 2024-06-25 |
Family
ID=
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101033284A (en) * | 2006-12-07 | 2007-09-12 | 沈阳化工学院 | Synthesis for resorcin-containing coarse-pore sphere type adsorption resin and application method thereof |
| CN102020745A (en) * | 2010-11-05 | 2011-04-20 | 山东鲁抗立科药物化学有限公司 | Acrylic decolorization resin and preparation method thereof |
| CN107594467A (en) * | 2017-08-05 | 2018-01-19 | 广州奥桑味精食品有限公司 | A kind of manufacturing process for lifting monosodium glutamate quality |
| CN107759719A (en) * | 2017-11-04 | 2018-03-06 | 李华玲 | A kind of weak-base anion-exchange resin and preparation method thereof |
| CN109077289A (en) * | 2018-07-13 | 2018-12-25 | 广州奥桑味精食品有限公司 | The method that anion exchange resin regenerated liquid recycles production monosodium glutamate |
| CN111909299A (en) * | 2020-08-24 | 2020-11-10 | 皖东高科(天长)股份有限公司 | Novel alkalescent styrene ion exchange resin |
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101033284A (en) * | 2006-12-07 | 2007-09-12 | 沈阳化工学院 | Synthesis for resorcin-containing coarse-pore sphere type adsorption resin and application method thereof |
| CN102020745A (en) * | 2010-11-05 | 2011-04-20 | 山东鲁抗立科药物化学有限公司 | Acrylic decolorization resin and preparation method thereof |
| CN107594467A (en) * | 2017-08-05 | 2018-01-19 | 广州奥桑味精食品有限公司 | A kind of manufacturing process for lifting monosodium glutamate quality |
| CN107759719A (en) * | 2017-11-04 | 2018-03-06 | 李华玲 | A kind of weak-base anion-exchange resin and preparation method thereof |
| CN109077289A (en) * | 2018-07-13 | 2018-12-25 | 广州奥桑味精食品有限公司 | The method that anion exchange resin regenerated liquid recycles production monosodium glutamate |
| CN111909299A (en) * | 2020-08-24 | 2020-11-10 | 皖东高科(天长)股份有限公司 | Novel alkalescent styrene ion exchange resin |
Non-Patent Citations (1)
| Title |
|---|
| 危冬梅: "大孔酚醛吸附树脂的合成与应用研究", 《工程科技Ⅰ辑》, pages 1 - 9 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4523959A (en) | Purification of sugarcane juice | |
| KR950009318B1 (en) | Process for recovering l-amino acids from fermentation liquors | |
| CN102976923B (en) | New process for extracting lactic acid from lactic acid fermentation liquid | |
| CN105154499B (en) | The preparation method of L-aspartic acid-L-ornithine | |
| LU505449B1 (en) | Sucrose decoloring method and system | |
| CN112225762A (en) | Process for extracting xylose | |
| WO2023124395A1 (en) | System and method for co-producing xylitol and caramel color by using xylose mother liquor | |
| CN110183519B (en) | Separation and purification method of dalbavancin key intermediate A40926 | |
| US4331483A (en) | Ion exchange purification of sugar beet juice | |
| WO2013026313A1 (en) | New additive for sugar manufacturing with cane, and preparation method therefor and application method thereof in sugar manufacturing | |
| CN112471485B (en) | New decolorizing and refining process in monosodium glutamate production | |
| CN112471485A (en) | Decolouring refining process for producing gourmet powder | |
| CN113248551A (en) | System and method for preparing refined xylose by utilizing xylose mother liquor chromatographic extract | |
| CN104560707B (en) | The process of a kind of Enzyme catalyzed synthesis AA 2G and process system | |
| CN109553650B (en) | Water phase extraction method of erythromycin fermentation liquor | |
| CS241479B2 (en) | Method of sorbents' regeneration by means of alkaline aqueous solution | |
| CN108640816B (en) | Refining process for inositol filtrate by high-temperature rapid ion exchange | |
| CN114699801B (en) | Valve array type continuous ion exchange system for purification of red lactic acid | |
| CN102924551B (en) | A kind of method extracting guanosine from fermented liquid | |
| CN108774273B (en) | Trehalose crystallization process | |
| CN115073539B (en) | Method for separating and purifying 2' -fucosyllactose | |
| CN115785174A (en) | Preparation method of high-purity arabinose crystal | |
| US4997754A (en) | Process for recovering L-amino acids from fermentation liquors containing them | |
| CN105061196B (en) | Method for extracting potassium citrate from last potassium citrate mother solution | |
| CN108929248B (en) | Preparation method of L-arginine hydrochloride |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant |