CN112521291A - Glutamic acid crystal transformation method for shortening crystal transformation time - Google Patents
Glutamic acid crystal transformation method for shortening crystal transformation time Download PDFInfo
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- 239000013078 crystal Substances 0.000 title claims abstract description 141
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- 235000013922 glutamic acid Nutrition 0.000 title claims abstract description 74
- 239000004220 glutamic acid Substances 0.000 title claims abstract description 74
- 230000009466 transformation Effects 0.000 title claims abstract description 44
- 238000011426 transformation method Methods 0.000 title claims abstract description 15
- 238000004904 shortening Methods 0.000 title claims description 14
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 claims abstract description 121
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims abstract description 84
- 239000000725 suspension Substances 0.000 claims abstract description 57
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims abstract description 52
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 claims abstract description 42
- 235000010262 sodium metabisulphite Nutrition 0.000 claims abstract description 42
- 235000010265 sodium sulphite Nutrition 0.000 claims abstract description 42
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- LPUQAYUQRXPFSQ-DFWYDOINSA-M monosodium L-glutamate Chemical compound [Na+].[O-]C(=O)[C@@H](N)CCC(O)=O LPUQAYUQRXPFSQ-DFWYDOINSA-M 0.000 abstract description 6
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/44—Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
- C07C227/42—Crystallisation
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Abstract
The invention discloses a glutamic acid crystal transformation method, belonging to the technical field of monosodium glutamate processing, which comprises the steps of adjusting the pH value of suspension containing alpha-glutamic acid crystals to 4.5-4.8, heating to 70-90 ℃, and carrying out crystal transformation under the stirring condition to obtain transformation mother liquor and beta-glutamic acid crystals, and is characterized in that: after the pH value is adjusted to 4.5-4.8, sodium metabisulfite or sodium sulfite or a mixture of the sodium metabisulfite and the sodium sulfite are added into the suspension, or sulfur dioxide is introduced into the suspension, and the invention has the beneficial effects that: reaction reagents, namely sodium pyrosulfite, sodium sulfite or sulfur dioxide, are added into the suspension of the alpha-glutamic acid crystals, so that the crystal transformation time from the alpha-glutamic acid crystals to the beta-crystal form glutamic acid can be shortened; the overall glutamic acid yield can be improved from 91.60% (mean value) to 95.10% (mean value) of the overall glutamic acid.
Description
The technical field is as follows:
the invention belongs to the technical field of monosodium glutamate processing, and particularly relates to a glutamic acid crystal transformation method.
Background art:
along with economic development and technical progress, China has become a country with great demands for monosodium glutamate production, and fermentation liquor in the monosodium glutamate production process can generate a large amount of high-concentration waste liquor after isoelectric and ion exchange extraction, and the waste liquor is rich in amino acid, thallus, protein and other solid matter suspended matters, various inorganic salts, organic acids, biotin, reducing sugar and the like, and has the characteristics of five high and one low, namely COD, BOD, COD, Cl + SO4、NH3N, high thallus content, low pH value and great treatment difficulty, and is one of the largest pollution sources in glutamic acid production. At present, monosodium glutamate production enterprises generally adopt polyacrylamide flocculation and plate-and-frame filter pressing to extract mycoprotein, and clear liquid contains a large amount of ammonium sulfate, and then is concentrated and sprayed with slurry to granulate so as to prepare organic fertilizer (a fermentation byproduct ammonium sulfate).
However, as the productivity of the fertilizer industry rapidly expands, the agricultural demand decreases, and the content of the produced ammonium sulfate is low, the sale is difficult, so that the product is overstocked in a large amount, and the stability and the continuity of the production are seriously affected. Meanwhile, smoke generated in the process of guniting granulation is discharged to form a large amount of white smoke, contains pollutants such as smoke dust and the like, has unpleasant smell, and greatly influences the environment.
The company develops a process for obtaining alpha-glutamic acid crystal suspension by directly carrying out concentration, isoelectric treatment and centrifugation on glutamic acid fermentation liquor, and carrying out crystal transformation at high temperature to obtain beta-crystal form glutamic acid, so that impurities mixed in the crystals are separated out, and the purity of the glutamic acid is improved; however, the crystal transformation time of the crystal transformation process is long, generally more than 180min is needed, so that the alpha-glutamic acid crystal is transformed into pyroglutamic acid under the condition of high temperature regulation for a long time, thereby influencing the refining yield, causing the unit consumption of each raw and auxiliary material to be increased, the cost of monosodium glutamate to be increased and other serious problems.
Moreover, the preparation of the glutamic acid belongs to the traditional process, and is quite mature after years of development, and the overall yield of the glutamic acid is difficult to exceed 95 percent, which is a technical bottleneck.
The invention content is as follows:
in order to solve the problems and overcome the defects of the prior art, the invention provides a glutamic acid crystal transformation method with short crystal transformation time, which can effectively solve the problems.
The specific technical scheme for solving the technical problems comprises the following steps: a glutamic acid crystal transformation method for shortening crystal transformation time is characterized in that pH of turbid liquid containing alpha-glutamic acid crystals is adjusted to 4.5-4.8, the temperature is raised to 70-90 ℃, crystal transformation is carried out under the stirring condition, and transformation mother liquor and beta-glutamic acid crystals are obtained, and the method is characterized in that: adjusting the pH value to 4.5-4.8, adding sodium metabisulfite or sodium sulfite or a mixture of the sodium metabisulfite and the sodium sulfite into the suspension, or introducing sulfur dioxide into the suspension.
Further, the mass ratio of the volume of the suspension to the sodium metabisulfite or sodium sulfite or the mixture of the sodium metabisulfite and the sodium sulfite is as follows: 0.8-1g of 100 mL.
Further, the molar ratio of the volume of the suspension to the sulfur dioxide is 100mL: 0.008 to 0.01 mol.
Further, the suspension containing the alpha-glutamic acid crystals is prepared from the alpha-glutamic acid crystals, and the specific steps are adding the alpha-glutamic acid crystals into water, and uniformly stirring.
Further, the Baume degree of the suspension of the alpha-glutamic acid crystals is 24 to 26.
Further, the suspension containing the alpha-glutamic acid crystals is prepared from glutamic acid fermentation liquor, and the glutamic acid fermentation liquor is directly obtained after concentration, isoelectric treatment and centrifugation.
Further, sodium metabisulfite or sodium sulfite or a mixture of sodium metabisulfite and sodium sulfite is added into the glutamic acid fermentation liquor in a continuous isoelectric tank for isoelectric treatment.
Further, sulfur dioxide is introduced into the glutamic acid fermentation liquor in a continuous isoelectric tank for isoelectric treatment.
The invention has the beneficial effects that:
(1) the invention creatively adds a reaction reagent, namely sodium pyrosulfite, sodium sulfite or sulfur dioxide, into the suspension of the alpha-glutamic acid crystal, and can shorten the crystal transformation time from the alpha-glutamic acid crystal to the beta-crystal form glutamic acid;
(2) the invention creatively adds a reaction reagent, namely sodium pyrosulfite, sodium sulfite or sulfur dioxide, into the suspension of the alpha-glutamic acid crystal, and can improve the overall yield of the glutamic acid from 91.60 percent (mean value) to 95.10 percent (mean value) of the overall yield of the glutamic acid.
Description of the drawings:
FIG. 1 is a crystal structure diagram of a high crystal density beta-form glutamic acid of the present invention;
FIG. 2 is a crystal structure diagram of a low crystal density beta-form glutamic acid of the present invention; in the drawings:
the specific implementation mode is as follows:
in the description of the invention, specific details are given only to enable a full understanding of the embodiments of the invention, but it should be understood by those skilled in the art that the invention is not limited to these details for the implementation. In other instances, well-known structures and functions have not been described or shown in detail to avoid obscuring the points of the embodiments of the invention. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
The specific implementation mode of the invention is as follows:
a glutamic acid crystal transformation method for shortening crystal transformation time is characterized in that pH of turbid liquid containing alpha-glutamic acid crystals is adjusted to 4.5-4.8, the temperature is raised to 70-90 ℃, crystal transformation is carried out under the stirring condition, and transformation mother liquor and beta-glutamic acid crystals are obtained, and the method is characterized in that: adjusting the pH value to 4.5-4.8, adding sodium metabisulfite or sodium sulfite or a mixture of the sodium metabisulfite and the sodium sulfite into the suspension, or introducing sulfur dioxide into the suspension.
Further, the mass ratio of the volume of the suspension to the sodium metabisulfite or sodium sulfite or the mixture of the sodium metabisulfite and the sodium sulfite is as follows: 0.8-1g of 100 mL.
Further, the molar ratio of the volume of the suspension to the sulfur dioxide is 100mL: 0.008 to 0.01 mol.
Further, the suspension containing the alpha-glutamic acid crystals is prepared from the alpha-glutamic acid crystals, and the specific steps are adding the alpha-glutamic acid crystals into water, and uniformly stirring.
Further, the Baume degree of the suspension of the alpha-glutamic acid crystals is 24 to 26.
Further, the suspension containing the alpha-glutamic acid crystals is prepared from glutamic acid fermentation liquor, and the glutamic acid fermentation liquor is directly obtained after concentration, isoelectric treatment and centrifugation.
Further, sodium metabisulfite or sodium sulfite or a mixture of sodium metabisulfite and sodium sulfite is added into the glutamic acid fermentation liquor in a continuous isoelectric tank for isoelectric treatment.
Further, sulfur dioxide is introduced into the glutamic acid fermentation liquor in a continuous isoelectric tank for isoelectric treatment.
The glutamic acid crystal transformation method for shortening the crystal transformation time realizes the technical effect of shortening the crystal transformation time by adding sodium metabisulfite or sodium sulfite or a mixture of the sodium metabisulfite and the sodium sulfite into the turbid liquid or introducing sulfur dioxide into the turbid liquid;
the invention also comprises a glutamic acid transcrystallization method, which solves the problems of poor crystal density and low yield of glutamic acid crystals; in order to solve the problems, the method comprises the following specific steps:
specifically, the method comprises the steps of adjusting the pH of suspension containing alpha-glutamic acid crystals to 4.5-4.8, heating to 70-90 ℃, and carrying out crystal transformation under the stirring condition to obtain transformation mother liquor and beta-glutamic acid crystals, and is characterized in that: adjusting the pH value to 4.5-4.8, adding sodium metabisulfite or sodium sulfite or a mixture of the sodium metabisulfite and the sodium sulfite into the suspension, or introducing sulfur dioxide into the suspension;
specifically, the method also comprises the steps of adding sodium metabisulfite or sodium sulfite or a mixture of the sodium metabisulfite and the sodium sulfite into the suspension, or introducing sulfur dioxide into the suspension; then, an aqueous polyacrylamide solution is further added to the suspension.
Furthermore, the volume ratio of the suspension to the polyacrylamide aqueous solution is 100mL:3-8mL, and the concentration of the polyacrylamide aqueous solution is 0.01-0.03%.
Further, the mass ratio of the volume of the suspension to the sodium metabisulfite or sodium sulfite or the mixture of the sodium metabisulfite and the sodium sulfite is as follows: 0.8-1g of 100 mL.
Further, the molar ratio of the volume of the suspension to the sulfur dioxide is 100mL: 0.008 to 0.01 mol.
Further, the mass ratio of the volume of the suspension to the polyacrylamide is as follows: 0.8-1g of 100 mL.
Further, the suspension containing the alpha-glutamic acid crystals is prepared from the alpha-glutamic acid crystals, and the specific steps are adding the alpha-glutamic acid crystals into water, and uniformly stirring.
Further, the Baume degree of the suspension of the alpha-glutamic acid crystals is 24 to 26.
Further, the suspension containing the alpha-glutamic acid crystals is prepared from glutamic acid fermentation liquor, and the glutamic acid fermentation liquor is directly obtained after concentration, isoelectric treatment and centrifugation.
Further, sodium metabisulfite or sodium sulfite or a mixture of sodium metabisulfite and sodium sulfite is added into the glutamic acid fermentation liquor in a continuous isoelectric tank for isoelectric treatment.
Further, sulfur dioxide is introduced into the glutamic acid fermentation liquor in a continuous isoelectric tank for isoelectric treatment.
Adding sodium metabisulfite or sodium sulfite or a mixture of sodium metabisulfite and sodium sulfite into the suspension, or adding polyacrylamide into the suspension after introducing sulfur dioxide; the realized effects are as follows:
(1) the crystal density of the beta-glutamic acid crystal is improved; (2) the overall yield of beta-glutamic acid crystals is improved; (3) the unexpected discovery shows that the accelerating effect of polyacrylamide on sodium metabisulfite, sodium sulfite or sulfur dioxide further shortens the crystal transfer time 1/3 and further improves the yield on the basis of the crystal transfer time after the glutamic acid crystal transfer method shortens the crystal transfer time.
Table 1: experimental data of reaction reagents for crystal transformation time
| Source of suspension of alpha-glutamic acid crystals | Reaction reagent | Time to crystallize/min | |
| Example one | Glutamic acid fermentation liquor | Sodium metabisulfite | 120 |
| Example two | Pure product configuration | Sodium metabisulfite | 120 |
| EXAMPLE III | Glutamic acid fermentation liquor | Sodium sulfite | 121 |
| Example four | Pure product configuration | Sodium sulfite | 122 |
| EXAMPLE five | Glutamic acid fermentation liquor | Mixture of | 119 |
| EXAMPLE six | Glutamic acid fermentation liquor | Mixture of | 119 |
| EXAMPLE seven | Glutamic acid fermentation liquor | Sulfur dioxide | 118 |
| Example eight | Pure product configuration | Sulfur dioxide | 118 |
According to the data analysis in the table 1, the following results are obtained: the first to eighth embodiments of the present invention are different only in the reaction reagents, and perform crystal transformation using a suspension of α -glutamic acid crystals of a glutamic acid fermentation broth and a suspension of α -glutamic acid crystals prepared as a pure product, respectively, under different reaction reagent conditions,
the timing end point of the crystal transformation is the complete transformation from the alpha-crystal form to the beta-crystal form, namely the crystal transformation is completed when the alpha-crystal form is 100 percent transformed into the beta-crystal form by observing through a microscope.
The results of the above examples show that the difference of the crystal transfer time of different reagents is not great, the mean value of the crystal transfer time is 120min,
in addition, the alpha-glutamic acid crystal suspension of the glutamic acid fermentation liquor and the alpha-glutamic acid crystal suspension prepared in a pure product have no difference under the condition of the same reaction reagent, which is mainly because the impurities in the fermentation liquor are removed by the concentration, isoelectric treatment and centrifugation processes before the alpha-glutamic acid crystal transformation process of the glutamic acid fermentation liquor disclosed by the invention, and the impurities have no difference with the alpha-glutamic acid crystal suspension prepared in a pure product.
In order to more intuitively show the process advantages of the reaction reagent of the present invention, i.e. sodium metabisulfite or sodium sulfite or sulfur dioxide, the present invention is compared with the same process by replacing the above reaction reagent equivalently, table 2: control experiment data of reaction reagent for crystal transformation time
| Source of suspension of alpha-glutamic acid crystals | Reaction reagent | Time to crystallize/min | |
| Comparative example 1 | Glutamic acid fermentation liquor | Is free of | 180 |
| Comparative example No. two | Pure product configuration | Is free of | 180 |
| Comparative example No. three | Glutamic acid fermentation liquor | Is free of | 180 |
| Comparative example No. four | Pure product configuration | Is free of | 180 |
| Comparative example five | Glutamic acid fermentation liquor | Is free of | 180 |
| Comparative example six | Glutamic acid fermentation liquor | Is free of | 180 |
| Comparative example seven | Glutamic acid fermentation liquor | Is free of | 180 |
| Comparative example eight | Pure product configuration | Is free of | 180 |
According to the data analysis of the table 2, the following results are obtained: comparative examples one to eight of the present invention are different from the examples of the present invention in that there is no reactive agent, and the suspension of alpha-glutamic acid crystals of glutamic acid fermentation broth and the suspension of pure alpha-glutamic acid crystals are separately used to perform crystal transformation under different reactive agent conditions,
the timing end point of the crystal transformation time is the complete transformation from the alpha-crystal form to the beta-crystal form, namely the crystal transformation is completed when the alpha-crystal form is 100 percent transformed into the beta-crystal form by observing through a microscope;
the results of the comparative example show that the crystal transfer time is not different when the crystal transfer time of different reaction reagents is not available, and the average value is 180min, so that the reaction reagents can have the effect of shortening the crystal transfer time for the crystal transfer process of the suspension of the alpha-glutamic acid crystals; can be shortened from 180min of the mean value to 120min of the mean value.
In order to more intuitively show the advantages of the polyacrylamide process, the method is specially compared with a method for equivalent replacement of the same process by using a single variable.
Table 3: polyacrylamide transcrystallization test data of suspension of alpha-glutamic acid crystals
Remarking: the conventional low crystal density of beta-form glutamic acid is 1.570g/cm3(ii) a While the high crystal density of the beta-form glutamic acid is 1.625g/cm3。
Analysis from the data in table 3:
(1) the comparison of the first and second examples with the first and second comparative examples shows that: the reaction reagent can shorten the crystal transformation time from 180min to 120min, and the addition of the reaction reagent can increase the yield from 91.60% (mean) to 95.10% (mean), but the addition of the reaction reagent has no significant influence on the crystal density of the beta-crystalline glutamic acid;
(2) the first and second embodiments are compared with the ninth and tenth embodiments to find that: the reaction reagent is added, and then the polyacrylamide is added, so that the crystal transformation time can be further shortened from 120min to 90min, particularly, the polyacrylamide is added, the higher crystal density of beta-crystal form glutamic acid can be obtained, and the yield can be improved from 95.10% (mean value) to 98.50% (mean value).
(3) Comparison of comparative example one and comparative example two with comparative example nine and comparative example ten reveals that: on the basis of not adding a reaction reagent, only polyacrylamide is added, and the polyacrylamide used alone has no significant improvement on the crystal transformation time of glutamic acid, the crystal density of beta-crystal form glutamic acid and the overall yield of glutamic acid.
In summary, the following steps:
(1) the invention creatively adds a reaction reagent, namely sodium pyrosulfite, sodium sulfite or sulfur dioxide, into the suspension of the alpha-glutamic acid crystal, and can shorten the crystal transformation time from the alpha-glutamic acid crystal to the beta-crystal form glutamic acid;
(2) the invention creatively adds a reaction reagent, namely sodium pyrosulfite, sodium sulfite or sulfur dioxide, into the suspension of the alpha-glutamic acid crystal, and can improve the overall yield of the glutamic acid from 91.60 percent (mean value) to 95.10 percent (mean value) of the overall yield of the glutamic acid;
(3) the invention also creatively adds a reaction reagent, namely sodium pyrosulfite, sodium sulfite or sulfur dioxide, into the suspension of the alpha-glutamic acid crystal, and then adds polyacrylamide, and unexpectedly discovers that the polyacrylamide can promote the reaction reagent in the overall yield of the glutamic acid and the crystal density of the beta-crystal form glutamic acid.
Claims (8)
1. A glutamic acid crystal transformation method for shortening crystal transformation time is characterized in that pH of turbid liquid containing alpha-glutamic acid crystals is adjusted to 4.5-4.8, the temperature is raised to 70-90 ℃, crystal transformation is carried out under the stirring condition, and transformation mother liquor and beta-glutamic acid crystals are obtained, and the method is characterized in that: adjusting the pH value to 4.5-4.8, adding sodium metabisulfite or sodium sulfite or a mixture of the sodium metabisulfite and the sodium sulfite into the suspension, or introducing sulfur dioxide into the suspension.
2. The glutamic acid crystal transformation method for shortening the crystal transformation time according to claim 1, wherein the volume ratio of the suspension to the sodium metabisulfite or the sodium sulfite or the mixture of the sodium metabisulfite and the sodium sulfite is as follows: 0.8-1g of 100 mL.
3. The glutamic acid crystal transformation method for shortening the crystal transformation time according to claim 1, wherein the molar ratio of the volume of the suspension to the sulfur dioxide is 100mL: 0.008 to 0.01 mol.
4. The glutamic acid crystal transformation method for shortening the crystal transformation time according to any one of claims 1 to 3, wherein the suspension containing the alpha-glutamic acid crystals is prepared from the alpha-glutamic acid crystals, and the specific steps are adding the alpha-glutamic acid crystals into water, and uniformly stirring.
5. The method for glutamic acid crystallization with shortened crystallization time according to claim 4, wherein the Baume degree of the suspension of the α -glutamic acid crystals is 24 to 26.
6. The glutamic acid transformation method for shortening the transformation time according to any one of claims 1 to 3, wherein the suspension containing the α -glutamic acid crystals is prepared from a glutamic acid fermentation broth, and the glutamic acid fermentation broth is directly obtained by concentration, isoelectric treatment, and centrifugation.
7. The glutamic acid crystal transformation method for shortening the crystal transformation time according to claim 6, wherein sodium pyrosulfite or sodium sulfite or a mixture of the sodium pyrosulfite and the sodium sulfite is further added into the continuous isoelectric tank for isoelectric treatment.
8. The glutamic acid transformation method for shortening the transformation time according to claim 6, wherein sulfur dioxide is further introduced into the glutamic acid fermentation broth in a continuous isoelectric tank for isoelectric treatment.
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| CN118206462A (en) * | 2024-05-20 | 2024-06-18 | 内蒙古阜丰生物科技有限公司 | Technology for improving glutamic acid crystal transformation quality by utilizing ultrasonic technology |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB654629A (en) * | 1946-06-12 | 1951-06-27 | Int Minerals & Chem Corp | Improvements in the manufacture of glutamic acid |
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| CN118206462A (en) * | 2024-05-20 | 2024-06-18 | 内蒙古阜丰生物科技有限公司 | Technology for improving glutamic acid crystal transformation quality by utilizing ultrasonic technology |
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