CN112457225B - Taurine coarse crystal optimization method - Google Patents
Taurine coarse crystal optimization method Download PDFInfo
- Publication number
- CN112457225B CN112457225B CN202011288989.2A CN202011288989A CN112457225B CN 112457225 B CN112457225 B CN 112457225B CN 202011288989 A CN202011288989 A CN 202011288989A CN 112457225 B CN112457225 B CN 112457225B
- Authority
- CN
- China
- Prior art keywords
- taurine
- crystallization
- mother liquor
- crystal
- decoloring
- 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.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/42—Separation; Purification; Stabilisation; Use of additives
- C07C303/44—Separation; Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a taurine coarse crystal optimization method, which comprises the following steps: firstly, extracting a small amount of mother liquor from a reaction kettle for preliminary examination, judging whether the mother liquor is springed or not, adding a decoloring agent into the reaction kettle for high-temperature stirring and decoloring if the mother liquor is yellowed, adding an adsorbent into the reaction kettle for adsorbing impurity particles in the mother liquor after decoloring, performing circulating filtration, introducing the mother liquor into a crystallization kettle for crystallization after the mother liquor for crystallizing taurine is completely clear and transparent, separating out taurine crystals in a centrifugal separation mode, and finally washing with cold water to remove salt attached to the crystals. Through the mode, the invention can remove the phenomenon of yellowing of taurine crystals caused by polysulfide remaining in reaction liquid due to raw materials, so that the taurine crude crystal finished product has good quality, high purity, white and transparent whole body and good appearance, and the process difficulty of subsequent further refining is reduced.
Description
Technical Field
The invention relates to the field of taurine fabrics, in particular to a taurine coarse crystal optimization method.
Background
Taurine (Taurine), also known as taurocholic acid, is a sulfur-containing non-protein amino acid with a chemical name of 2-aminoethanesulfonic acid, is a sulfur-containing amino acid with multiple physiological functions existing in a human body, has the effects of promoting brain development, enhancing eyesight, resisting inflammation, relieving fever, reducing blood pressure, reducing blood sugar, strengthening liver, benefiting gallbladder and the like, and is one of the most important amino acids in the human body. Taurine has no toxic side effect, so developed countries pay attention to the research and application of taurine. In recent years, along with the intensive research on physiological action and nutritional value, the application of the taurine is very wide, and the taurine is widely used as a nutritional health product and a food additive in foreign countries;
taurine has been discovered, and synthetic pathways have been continuously explored. To date, there are not dozens of methods for synthesizing taurine. At present, the industrial production method of taurine in China mainly comprises an ethanolamine method and an ethylene oxide method, crystallization and precipitation are very critical steps in the process of preparing taurine by using the method, in some cases, the crystallized taurine crystals obviously turn yellow and need to be decolored and refined again, and analysis shows that the phenomenon of the yellowing of the taurine is mainly due to polysulfide impurities contained in raw materials, and the polysulfide impurities can enter the crystals during the crystallization process to cause the discoloration of the crystals.
Disclosure of Invention
The invention mainly solves the technical problem of providing the method, which can solve the problem of yellowing in the process of preparing the coarse crystal of the taurine.
In order to solve the technical problems, the invention adopts a technical scheme that: the taurine coarse crystal optimization method comprises the following steps:
step 1, a pre-detection step, namely extracting a small amount of taurine crystallization mother liquor from a reaction kettle, sending the small amount of taurine crystallization mother liquor into a laboratory for rapid cooling crystallization, observing the crystal character, sending the taurine crystallization mother liquor in the reaction kettle into a crystallization kettle for crystallization if the crystal is normal, and entering a decoloration step if the whole crystal is yellow;
step 2, a decoloring step, namely adding a decoloring agent into the reaction kettle, stirring and decoloring at a high temperature for 5-10 min under an acidic condition, and then adding an adsorbent into taurine crystallization mother liquor for adsorption while keeping a stirring state;
step 3, filtering and crystallizing, namely continuously filtering the decolored taurine crystallization mother liquor in a circulating filtration mode under a stirring state until the solution is clear and transparent, and introducing the solution into a crystallization kettle for cooling and crystallizing to obtain a solution mixed with taurine crystals;
step 4, centrifugal separation, namely introducing the solution in the crystallization kettle into a centrifugal separator for centrifugal separation to obtain solid taurine crystals;
and 5, washing the crystal, namely washing the crystal by using cold water to remove inorganic salts mixed on the surface of the crystal.
In a preferred embodiment of the invention, the decolorizing agent is sulfur dioxide gas or sulfite, and the addition amount of the decolorizing agent is 0.1-2% of the total amount of the taurine crystallization mother liquor.
In a preferred embodiment of the present invention, the decoloring temperature in the decoloring step is 90 to 100 ℃.
In a preferred embodiment of the present invention, in the decolorizing step, the pH value of the taurine crystallization mother liquor is maintained between 1 and 3.
In a preferred embodiment of the present invention, the adsorbent is activated carbon or diatomaceous earth.
In a preferred embodiment of the present invention, the amount of the adsorbent added in the decoloring step is 0.1 to 2%.
In a preferred embodiment of the present invention, the size of the filter bag used in the adsorbent circulation filtration in the filtration and crystallization step is 1-50 um.
In a preferred embodiment of the present invention, the number of times of the adsorbent circulation filtration in the filtration and crystallization step is 3 to 8 cycles.
In a preferred embodiment of the present invention, the liquid separated in the centrifugation step is concentrated under reduced pressure and then introduced into the taurine reaction solution for reuse.
In a preferred embodiment of the present invention, the cold water used in the crystal washing step is distilled water having a temperature of not more than 10 ℃.
The invention has the beneficial effects that: according to the invention, by adjusting the pH value of the solution and adding sulfur dioxide or sulfite into the taurine crystallization mother liquor to react with polysulfide in the solution, polysulfide in the solution is effectively eliminated under the condition of not influencing the crystallization yield of taurine, the decoloring cost is low, the crude taurine crystals have good quality and high purity, the appearance is transparent and white, and the process conditions for subsequent refining and purification of the crystals are reduced.
Detailed Description
The following detailed description of the preferred embodiments of the present invention is provided to enable those skilled in the art to more readily understand the advantages and features of the present invention, and to clearly and unequivocally define the scope of the present invention.
The embodiment of the invention comprises the following steps:
example 1
A taurine crude crystal optimization method comprises the following steps:
step 1, a pre-detection procedure, namely extracting a small amount of taurine crystallization mother liquor in a reaction kettle, sending the small amount of taurine crystallization mother liquor into a laboratory for rapid cooling crystallization, observing the crystal character, sending the taurine crystallization mother liquor in the reaction kettle into a crystallization kettle for crystallization if the crystal is normal, and entering a decoloration step if the whole crystal is yellow;
step 2, a decoloring step, namely firstly adding ammonium sulfite into the reaction kettle according to 2% of the total mass of the taurine crystallization mother liquor, continuously stirring and decoloring at a high temperature of 90-100 ℃ under an acidic condition that the pH value of the solution is 1-3, and after continuously stirring for 5min, adding active carbon accounting for 0.1% of the total mass into the taurine crystallization mother liquor in a stirring state to be used as an adsorbent for adsorption;
step 3, filtering and crystallizing, namely continuously and circularly filtering the taurine crystallization mother liquor subjected to the decoloring treatment in the step 2 for 3 times by using a filter bag with the specification of 1um under the stirring state until the solution is clarified, and introducing the solution into a crystallization kettle for cooling and crystallizing to obtain a solution rich in taurine crystals;
step 4, centrifugal separation, namely introducing the liquid in the crystallization kettle into a centrifugal separator for centrifugal separation to obtain solid taurine crystals, and introducing the liquid centrifugally separated in the step into taurine reaction liquid for recycling after pressure reduction and concentration, so that the waste of materials is reduced and the discharge of waste water is reduced;
and 5, washing the crystal, namely washing the crystal by using distilled water with the temperature of not more than 10 ℃, and removing inorganic salts mixed on the surface of the crystal while reducing the loss of taurine in the washing process by utilizing the characteristic of low solubility of the taurine at low temperature.
Example 2
A taurine crude crystal optimization method comprises the following steps:
step 1, a pre-detection procedure, namely extracting a small amount of taurine crystallization mother liquor in a reaction kettle, sending the small amount of taurine crystallization mother liquor into a laboratory for rapid cooling crystallization, observing the crystal character, sending the taurine crystallization mother liquor in the reaction kettle into a crystallization kettle for direct crystallization if the crystal is normal, and entering a decoloration step if the whole crystal is yellow;
step 2, a decoloring step, namely adding sodium sulfite accounting for 1 percent of the total amount of the taurine crystallization mother liquor into a reaction kettle as a decoloring agent, keeping the mixture at a high temperature of 90-100 ℃ under an acidic condition that the pH value of the solution is 1-3, continuously stirring and decoloring, keeping the stirring state after continuously stirring for 8min, and adding diatomite accounting for 1 percent of the total amount into the taurine crystallization mother liquor as an adsorbent to adsorb;
step 3, filtering and crystallizing, namely continuously and circularly filtering the taurine crystallization mother liquor subjected to the decoloring treatment in the step 2 for 5 times by using a filter bag with the specification of 25um under the stirring state until the solution is completely clarified, and introducing the solution into a crystallization kettle for cooling and crystallizing to obtain a solution rich in taurine crystals;
step 4, centrifugal separation, namely introducing the solution in the crystallization kettle into a centrifugal separator for centrifugal separation to obtain solid taurine crystals, and introducing the liquid centrifugally separated in the step into taurine reaction liquid for recycling after pressure reduction and concentration, so that the waste of materials is reduced and the discharge of waste water is reduced;
and 5, washing the crystal, namely washing the crystal by using distilled water with the temperature of not more than 10 ℃, and removing inorganic salts mixed on the surface of the crystal while reducing the loss of taurine in the washing process by utilizing the characteristic of low solubility of the taurine at low temperature.
Example 3
A taurine crude crystal optimization method comprises the following steps:
step 1, a pre-detection procedure, namely extracting a small amount of taurine crystallization mother liquor in a reaction kettle, sending the small amount of taurine crystallization mother liquor into a laboratory for rapid cooling crystallization, observing the crystal character, sending the taurine crystallization mother liquor in the reaction kettle into a crystallization kettle for crystallization if the crystal is normal, and entering a decoloration step if the whole crystal is yellow;
step 2, a decoloring step, namely introducing sulfur dioxide gas into a reaction kettle for decoloring, keeping high temperature of 90-100 ℃ under an acidic condition with the pH value of 1-3, continuously stirring for decoloring, wherein the introduced sulfur dioxide gas accounts for 0.1% of the total mass of the taurine crystallization mother liquor, continuously stirring for 10min after the gas is added, keeping the stirring state, and adding active carbon accounting for 2% of the total mass into the taurine crystallization mother liquor to be used as an adsorbent for adsorption;
step 3, filtering and crystallizing, namely continuously and circularly filtering the decolored taurine crystallization mother liquor for 8 times by using a filter bag with the specification of 50um under the stirring state until the solution is clarified, and introducing the solution into a crystallization kettle for cooling and crystallizing to obtain a solution rich in taurine crystals;
step 4, centrifugal separation, namely introducing the solution in the crystallization kettle into a centrifugal separator for centrifugal separation to obtain solid taurine crystals, and introducing the liquid centrifugally separated in the step into taurine reaction liquid for recycling after pressure reduction and concentration, so that the waste of materials is reduced and the discharge of waste water is reduced;
and 5, washing the crystal, namely washing the crystal by using distilled water with the temperature of not more than 10 ℃, and removing inorganic salts mixed on the surface of the crystal while reducing the loss of taurine in the washing process by utilizing the characteristic of low solubility of the taurine at low temperature.
In the above embodiments 1 to 3, yellow polysulfide in the solution is removed by using the characteristic that sulfite and polysulfide react under an acidic condition to produce elemental sulfur and sulfate ions, and the generated elemental S is removed by a filtration and adsorption manner, so that the color purity of the crude taurine crystal is ensured, and the condition of advanced treatment at a later stage is reduced.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (9)
1. The taurine crude crystal optimization method is characterized by comprising the following steps of:
step 1, a pre-detection step, namely extracting a small amount of taurine crystallization mother liquor from a reaction kettle, sending the small amount of taurine crystallization mother liquor into a laboratory for rapid cooling crystallization, observing the crystal character, and entering a decoloring step if the whole crystal is yellow;
step 2, a decoloring step, namely adding a decoloring agent into the reaction kettle, stirring and decoloring at a high temperature for 5-10 min under an acidic condition, and then adding an adsorbent into taurine crystallization mother liquor for adsorption while keeping a stirring state; the decolorizing agent is sulfur dioxide gas or sulfite; the adsorbent is active carbon or diatomite;
step 3, filtering and crystallizing, namely continuously filtering the decolored taurine crystallization mother liquor in a circulating filtration mode under a stirring state until the solution is clear and transparent, and introducing the solution into a crystallization kettle for cooling and crystallizing to obtain a solution mixed with taurine crystals;
step 4, centrifugal separation, namely introducing the solution in the crystallization kettle into a centrifugal separator for centrifugal separation to obtain solid taurine crystals;
and 5, washing the crystal, namely washing the crystal by using cold water to remove inorganic salts mixed on the surface of the crystal.
2. The method for optimizing the crude taurine crystals according to claim 1, wherein the addition amount of the decoloring agent is 0.1-2% of the total amount of the mother liquid for taurine crystallization.
3. The taurine crude crystal optimization method according to claim 1, wherein the decolorizing temperature in the decolorizing step is 90-100 ℃.
4. The method for optimizing taurine crude crystals according to claim 1, wherein in the decoloring step, the pH value of the taurine crystallization mother liquor is maintained between 1 and 3.
5. The method for optimizing taurine crude crystals according to claim 1, wherein the amount of the adsorbent added in the decoloring step is 0.1 to 2%.
6. The taurine coarse crystal optimization method according to claim 1, wherein the size of a filter bag used in the adsorbent circulation filtration in the filtration and crystallization step is 1-50 um.
7. The method for optimizing taurine crude crystals according to claim 1, wherein the number of times of the adsorbent cycle filtration in the step of filtration and crystallization is 3-8 cycles.
8. The method for optimizing taurine crude crystals according to claim 1, wherein the liquid separated in the centrifugal separation step is introduced into the taurine reaction liquid for reuse after being concentrated under reduced pressure.
9. The method for optimizing taurine crude crystals according to claim 1, wherein the cold water used in the step of washing the crystals is distilled water having a temperature of not more than 10 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011288989.2A CN112457225B (en) | 2020-11-17 | 2020-11-17 | Taurine coarse crystal optimization method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011288989.2A CN112457225B (en) | 2020-11-17 | 2020-11-17 | Taurine coarse crystal optimization method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112457225A CN112457225A (en) | 2021-03-09 |
| CN112457225B true CN112457225B (en) | 2022-04-19 |
Family
ID=74837611
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011288989.2A Active CN112457225B (en) | 2020-11-17 | 2020-11-17 | Taurine coarse crystal optimization method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112457225B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101486669A (en) * | 2009-01-09 | 2009-07-22 | 沙洋天一药业有限公司 | Method for synthesizing taurine |
| CN102659644A (en) * | 2012-05-10 | 2012-09-12 | 南京优科生物医药有限公司 | Crystal forms of 2-aminoethyl sulfonic acid and preparation processes for crystal forms |
| CN104628609A (en) * | 2013-11-07 | 2015-05-20 | 山东方明药业集团股份有限公司 | Separation and extraction method of taurine |
-
2020
- 2020-11-17 CN CN202011288989.2A patent/CN112457225B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101486669A (en) * | 2009-01-09 | 2009-07-22 | 沙洋天一药业有限公司 | Method for synthesizing taurine |
| CN102659644A (en) * | 2012-05-10 | 2012-09-12 | 南京优科生物医药有限公司 | Crystal forms of 2-aminoethyl sulfonic acid and preparation processes for crystal forms |
| CN104628609A (en) * | 2013-11-07 | 2015-05-20 | 山东方明药业集团股份有限公司 | Separation and extraction method of taurine |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112457225A (en) | 2021-03-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104003830B (en) | Amino acid separation and the method for iminodicarboxylic acid from the aqueous solution of amino acid whose alkali metal salt | |
| CN112158858A (en) | Method for preparing ammonium bifluoride by using BOE waste liquid | |
| CN103710470A (en) | Process for preparing sugar by two-step method and device thereof | |
| FI102620B (en) | Process for decolorizing solutions | |
| EP2516683A1 (en) | Compositions and processes for clarification of sugar juices and syrups | |
| CN112457225B (en) | Taurine coarse crystal optimization method | |
| CN114287603A (en) | Method for improving color intensity of monosodium glutamate product | |
| CN112661674A (en) | Optimized process for preparing taurine by ethylene oxide method | |
| JPH11500005A (en) | Crude sugar purification process | |
| CN112480032A (en) | Method for recycling secondary mother liquor in acesulfame potassium production | |
| KR101134502B1 (en) | Production process for phytic acid | |
| CN110655547A (en) | Adenosine extraction method for reducing content of single related impurities | |
| CN103012509B (en) | Method of separating and purifying sucrose-6-acetate mother liquor by salt fractionation | |
| BR112012011635B1 (en) | METHOD FOR THE PRODUCTION OF WHITE SUGAR, SUGAR | |
| EP2630119A1 (en) | Use of an acetic acid wash to prepare low-sulfate 5-sulfoisophthalic acid, mono-lithium salt | |
| US2929839A (en) | Process for recovering glutamic acid | |
| CN108948017B (en) | Purification method of folic acid | |
| CN112239413A (en) | Purification and closed production method of glycine | |
| CN101068938A (en) | Method for producing refining sugar | |
| CN111518057A (en) | Acesulfame potassium crystal liquid purification treatment method | |
| CN110407871A (en) | Glyphosate crystal device and method for crystallising | |
| CN105502769B (en) | A kind of method of esterified acid waste water in recycling treatment cyan-acetic ester production | |
| SU1578201A1 (en) | Method of separating fillmass | |
| CN115368321B (en) | Purification method, system and detection method of N-methylmorpholine-N-oxide and N-methylmorpholine-N-oxide obtained by same | |
| RU2155814C1 (en) | Method of producing sugar from raw sugar cane |
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 | ||
| GR01 | Patent grant |