CN108191687B - Process for decoloring L-phenylglycine - Google Patents
Process for decoloring L-phenylglycine Download PDFInfo
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- CN108191687B CN108191687B CN201810031126.3A CN201810031126A CN108191687B CN 108191687 B CN108191687 B CN 108191687B CN 201810031126 A CN201810031126 A CN 201810031126A CN 108191687 B CN108191687 B CN 108191687B
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Abstract
A process for decoloring L-phenylglycine comprises the steps of decoloring a solution produced by L-phenylglycine through a glass column filled with a decoloring agent, heating the solution produced by L-phenylglycine to 50-100 ℃, then allowing the solution produced by L-phenylglycine to pass through the glass column, controlling the temperature of the glass column to be 55-80 ℃, controlling the outflow speed of the solution produced by L-phenylglycine from the glass column to be 7-9ml/min, and collecting the outflow solution from the glass column to finish the decoloring. The decoloring process disclosed by the invention has the advantages of more targeted removal of color development impurities and color-assisting impurities in the production of the L-phenylglycine, excellent removal effect, obvious better decoloring requirement than that of the production of the L-phenylglycine, environmental friendliness and low production cost.
Description
Technical Field
The invention belongs to the technical field of production of L-phenylglycine, and relates to a L-phenylglycine decoloring process.
Background
The chemical and pharmaceutical products generally have high requirements on color and luster, and in order to reach the color and luster of the products, the industrial decolorization process is generally adopted, and the activated carbon has wide pore size distribution and can adsorb color development impurities and color aiding impurities with various sizes, so that the activated carbon is widely used in the field of chemical and pharmaceutical products as a broad-spectrum decolorizer, but the use of the activated carbon has a great problem; secondly, because the activated carbon has poor thermal stability and is easy to burn at high temperature, the activated carbon can only be used once, the regeneration and the repeated use of the activated carbon cannot be realized by methods such as high-temperature roasting, the used activated carbon can only be treated as waste activated carbon, the waste activated carbon belongs to hazardous waste according to the national regulations, and the nation has strict legal regulations in the processes of storage, delivery, transportation and disposal, thereby not only causing great economic burden to enterprises, but also being often accompanied with serious environmental pollution risks.
The L-phenylglycine is an important pharmaceutical intermediate and a special chemical, the appearance of the L-phenylglycine is a white solid, currently, the L-phenylglycine is decolorized by using active carbon, 8 kilograms of active carbon are required for average decolorization of each ton of products, the comprehensive cost is high, and the L-phenylglycine is environment-friendly and resource-wasting, so that the development of a green environment-friendly decolorization process suitable for the L-phenylglycine production has great economic value and important environmental protection significance.
Disclosure of Invention
The invention provides the environment-friendly and good-decoloring technology of the L-phenylglycine, aiming at solving the problems of single decoloring technology and unsatisfactory decoloring effect of the existing L-phenylglycine.
The technical scheme adopted by the invention for realizing the purpose is as follows:
a process for decoloring L-phenylglycine comprises the steps of passing a solution produced by the L-phenylglycine through a glass column filled with a decoloring agent for decoloring, heating the solution produced by the L-phenylglycine to 50-100 ℃, passing the solution produced by the L-phenylglycine through the glass column, controlling the temperature of the glass column to be 55-80 ℃, controlling the outflow speed of the solution produced by the L-phenylglycine from the glass column to be 7-9ml/min, and collecting the outflow solution from the glass column to finish the decoloring.
The decolorizing agent comprises, by mass, 2-10% of a molecular sieve A, 5-20% of a molecular sieve B, 20-50% of a molecular sieve C and 30-70% of a molecular sieve D, wherein the molecular sieve A is selected from
Molecular sieves, AlPO4At least one of a 34 molecular sieve and a SAPO-34 molecular sieve, wherein the molecular sieve B is selected from at least one of NaZSM-11 molecular sieve with Si/Al more than 200, NaZSM-8 molecular sieve with Si/Al more than 200 and NaZSM-5 molecular sieve with Si/Al more than 200; the molecular sieve C is selected from mordenite and AlPO4At least one of-11 molecular sieve and Na β molecular sieve with Si/Al greater than 200, wherein the molecular sieve D is selected from NaY molecular sieve, USY molecular sieve and AlPO4-5 molecular sieves.
And the decolorant is regenerated and then is filled into the glass column for cyclic utilization.
The regeneration treatment comprises the following steps: after the decoloring treatment is finished, draining the decoloring agent in the glass column for 0.8-1.2h, pouring out the decoloring agent, placing the decoloring agent in a roasting furnace, drying at the temperature of 120-150 ℃ for 12-24h, heating to the temperature of more than 500 +/-1 ℃, roasting for 3-6h, and then cooling to room temperature to finish the regeneration treatment.
Heating to 550 ℃ and 600 ℃, and roasting for 3-6 h.
The retention time of the solution produced by the L-phenylglycine in the glass column is controlled to be more than or equal to 10 min.
The invention has the beneficial effects that:
in the production of L-phenylglycine, L-phenylglycine mother liquor used for decoloring is generally an acidic solution, and can cause damage to a decoloring agent to cause poor decoloring effect.
The decolorizing agent can be regenerated and reused, has a decolorizing effect superior to that of activated carbon, is combined with the selection and proportion collocation of molecular sieves, is mutually supported in function, can remove color-developing impurities and color-assisting impurities existing in the production of the L-phenylglycine in a more targeted manner, has an excellent removing effect, is obviously superior to the decolorizing requirement of the production of the L-phenylglycine, and has the advantages of environmental protection and low production cost.
In the prior art, the levo-phenylglycine is generally prepared by adopting processes of racemization, mixed rotation, resolution and the like, substances such as aromatic aldehydes, catalysts, racemization agents, racemization catalysts and the like are added in the preparation process, the substances are oxidized to generate colored impurities when the levo-phenylglycine is produced, and the color-assisting effect of the substances enables the levo-phenylglycine to generate certain color change, so that the removal of the colored impurities and the color-assisting impurities is the key for realizing the decoloration of the levo-phenylglycine, if active carbon is selected, although the active carbon has a macroporous structure and has a certain adsorption effect on the impurities, the limitation of adsorption is caused due to the particularity of the colored substances and the color-assisting impurities in the levo-phenylglycine, the irregularity of the pore structure and the non-ideal adsorption center, so that a large amount of active carbon is used for decoloration in practice, the increase of cost and the waste of energy are caused, and the decoloring effect is not satisfactory. According to long-term creative research, the molecular sieves of four schemes are selected for compounding, the mixing ratio of each molecular sieve is combined, a strong electrostatic field in a crystal cavity is utilized to play a role, the adsorption potential energy on the surface of a pore channel is improved, the diffusion and adsorption of colored substances are improved through reasonable matching of the crystallinity and the specific surface area of the molecular sieves, and the decolorizing speed and the decolorizing capacity are further improved; by controlling the temperature of the levorotatory phenylglycine solution and the temperature of the molecular sieve glass column, the probability of organic impurities entering the pore channel is improved, the spatial resistance of the organic impurities approaching the molecular sieve adsorption center is reduced, the organic impurities can more easily approach the molecular sieve adsorption center, the acting force between the organic impurities and the adsorption center is enhanced, and the decoloring capacity is further improved.
The selection and the matching proportion of the molecular sieve are the key for realizing high-efficiency decolorization and the key for improving the regeneration capacity, and on the basis of the regeneration process of the decolorizing agent, the molecular sieve is more targeted during adsorption and the selection of the adsorption substance to the pore channel is more stable due to the selection and the matching proportion of the molecular sieve, so that high desorption can be realized by combining the regeneration process, and the regeneration effect is good.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
Heating 1000ml of a solution produced by the L-phenylglycine (the pH is 9.5, and the absorbance (lambda is 410nm) is 1.305) to 50 ℃, then passing the solution produced by the L-phenylglycine through a 50mm glass column filled with a decolorizing agent, winding a heating belt outside the glass column, controlling the heating belt by a temperature control system, controlling the temperature of the glass column to be 60 +/-5 ℃, controlling the outflow speed of the solution produced by the L-phenylglycine from the glass column to be 7ml/min, collecting the outflow solution from the glass column, finishing decolorization treatment, and detecting the absorbance (lambda is 410nm) of the outflow L-phenylglycine solution to be 0.206.
The decolorizing agent is:
4g of molecular sieve, 7g of NaZSM-8(Si/Al is more than 200) molecular sieve, 25g of Na β (Si/Al is more than 200) molecular sieve and 64g of USY molecular sieve, wherein the used molecular sieves are all small balls with the diameter of 2-3 mm.
Carrying out regeneration treatment on the decolorizing agent:
after the decoloring treatment is finished, draining the decoloring agent in the glass column for 0.8h, pouring out the decoloring agent, placing in a roasting furnace, drying at 120 ℃ for 24h, heating to 520 ℃, roasting for 6h, and cooling to room temperature to obtain the regenerated decoloring agent.
The regenerated decolorizer was again subjected to the above decolorization treatment, and the absorbance (λ 410nm) of the discharged l-phenylglycine solution was measured to be 0.209.
Example 2
Heating 1000ml of a solution produced by the L-phenylglycine (the pH is 9.5, and the absorbance (lambda is 410nm) is 1.305) to 60 ℃, then passing the solution produced by the L-phenylglycine through a 50mm glass column filled with a decolorizing agent, winding a heating belt outside the glass column, controlling the heating belt by a temperature control system, controlling the temperature of the glass column to be 60 +/-3 ℃, controlling the outflow speed of the solution produced by the L-phenylglycine from the glass column to be 8ml/min, collecting the outflow solution from the glass column, completing the decolorization treatment, and detecting the absorbance (lambda is 410nm) of the outflow L-phenylglycine solution to be 0.207.
The decolorizing agent is: AlPO45g of-34 molecular sieve, 15g of NaZSM-5(Si/Al is more than 200) molecular sieve, 30g of Na β (Si/Al is more than 200) molecular sieve and 50g of NaY molecular sieve, wherein the molecular sieves are all small balls with the diameter of 2-3 mm.
Carrying out regeneration treatment on the decolorizing agent:
after the decoloring treatment is finished, draining the decoloring agent in the glass column for 0.9h, pouring out the decoloring agent, placing the decoloring agent in a roasting furnace, drying at 125 ℃ for 22h, heating to 530 ℃, roasting for 5.5h, and cooling to room temperature to obtain the regenerated decoloring agent.
The regenerated decolorizer was again subjected to the above decolorization treatment, and the absorbance (λ 410nm) of the discharged l-phenylglycine solution was measured to be 0.209.
Example 3
Heating 1000ml of a solution produced by the L-phenylglycine (the pH is 9.5, and the absorbance (lambda is 410nm) is 1.305) to 70 ℃, then passing the solution produced by the L-phenylglycine through a 50mm glass column filled with a decolorizing agent, winding a heating belt outside the glass column, controlling the heating belt by a temperature control system, controlling the temperature of the glass column to be 70 +/-5 ℃, controlling the outflow speed of the solution produced by the L-phenylglycine from the glass column to be 9ml/min, collecting the outflow solution from the glass column, finishing the decolorization treatment, and detecting the absorbance (lambda is 410nm) of the outflow L-phenylglycine solution to be 0.207.
The decolorizing agent is:
molecular sieves 2g, AlPO45g of-34 molecular sieve, 5g of NaZSM-8(Si/Al is more than 200) molecular sieve, 10g of NaZSM-11(Si/Al is more than 200) molecular sieve, 20g of mordenite (Si/Al is more than 100), 40g of USY molecular sieve and AlPO4-5 molecular sieves 18 g. The molecular sieves used are all small balls with the diameter of 2-3 mm.
Carrying out regeneration treatment on the decolorizing agent:
after the decoloring treatment is finished, draining the decoloring agent in the glass column for 1h, pouring out the decoloring agent, placing the decoloring agent in a roasting furnace, drying for 20h at the temperature of 130 ℃, then heating to 540 ℃, roasting for 5h, and then cooling to room temperature to obtain the regenerated decoloring agent.
The regenerated decolorizer was again subjected to the above decolorization treatment, and the absorbance (λ 410nm) of the discharged l-phenylglycine solution was measured to be 0.208.
Example 4
1000ml of a solution produced by the L-phenylglycine (pH 9.5 and absorbance ((lambda 410nm) 1.305)) is heated to 80 ℃, then the solution produced by the L-phenylglycine is passed through a 50mm glass column filled with a decolorizing agent, a heating belt is wound outside the glass column, the heating belt is controlled by a temperature control system, the temperature of the glass column is controlled to be 70 +/-3 ℃, the outflow speed of the solution produced by the L-phenylglycine from the glass column is controlled to be 7.5ml/min, the outflow solution from the glass column is collected, the decolorization treatment is completed, and the absorbance (lambda 410nm) of the outflow L-phenylglycine solution is detected to be 0.208.
The decolorizing agent is: AlPO45g of-34 molecular sieve, 5g of NaZSM-5(Si/Al is more than 200) molecular sieve, 5g of NaZSM-11(Si/Al is more than 200) molecular sieve and AlPO48g of-11 molecular sieve, 17g of mordenite (Si/Al is more than 100) and 70g of NaY molecular sieve. The molecular sieves used are all small balls with the diameter of 2-3 mm.
Carrying out regeneration treatment on the decolorizing agent:
after the decoloring treatment is finished, draining the decoloring agent in the glass column for 1.1h, pouring out the decoloring agent, placing in a roasting furnace, drying at 135 ℃ for 16h, heating to 550 ℃, roasting for 4h, and cooling to room temperature to obtain the regenerated decoloring agent.
The regenerated decolorizer was again subjected to the above decolorization treatment, and the absorbance (λ 410nm) of the discharged l-phenylglycine solution was measured to be 0.209.
Example 5
Heating 1000ml of a solution produced by the L-phenylglycine (pH 9.5 and absorbance ((lambda 410nm)1.305) to 90 ℃, then passing the solution produced by the L-phenylglycine through a 50mm glass column filled with a decolorizing agent, winding a heating belt outside the glass column, controlling the heating belt by a temperature control system, controlling the temperature of the glass column to be 75 +/-5 ℃, controlling the outflow speed of the solution produced by the L-phenylglycine from the glass column to be 8.5ml/min, collecting the outflow solution from the glass column, finishing decolorization treatment, and detecting the absorbance (lambda 410nm) of the outflow L-phenylglycine solution to be 0.207.
The decolorizing agent is: 4AlPO4-34 g of a molecular sieve (2 g),
2g of molecular sieve, 5g of NaZSM-11(Si/Al is more than 200) molecular sieve and AlPO48g of-11 molecular sieve, 17g of mordenite (Si/Al is more than 100), 50g of NaY molecular sieve and AlPO4-5 molecular sieves 16 g. Used ofThe molecular sieves are all small balls with the diameter of 2-3 mm.
Carrying out regeneration treatment on the decolorizing agent:
after the decoloring treatment is finished, draining the decoloring agent in the glass column for 1h, pouring out the decoloring agent, placing the decoloring agent in a roasting furnace, drying for 14h at the temperature of 140 ℃, heating to 560 ℃, roasting for 4.5h, and cooling to room temperature to obtain the regenerated decoloring agent.
The regenerated decolorizer was again subjected to the above decolorization treatment, and the absorbance (λ 410nm) of the discharged l-phenylglycine solution was measured to be 0.209.
Example 6
Heating 1000ml of a solution produced by L-phenylglycine (pH 9.5 and absorbance ((lambda 410nm)1.305) to 100 ℃, then passing the solution produced by L-phenylglycine through a 50mm glass column filled with a decolorizing agent, winding a heating belt outside the glass column, controlling the heating belt by a temperature control system, controlling the temperature of the glass column to be 70 +/-5 ℃, controlling the outflow speed of the solution produced by L-phenylglycine from the glass column to be 9ml/min, collecting the outflow solution from the glass column, namely completing decolorization treatment, and detecting the absorbance (lambda 410nm) of the outflow L-phenylglycine solution to be 0.202.
The decolorizing agent is:
molecular sieves 2g, AlPO41g of-34 molecular sieve, 1g of SAPO-34 molecular sieve, 5g of NaZSM-11(Si/Al is more than 200) molecular sieve, 2g of NaZSM-8(Si/Al is more than 200) molecular sieve, 3g of NaZSM-5(Si/Al is more than 200) molecular sieve, AlPO46g of-11 molecular sieve, 10g of mordenite (Si/Al is more than 100), 5g of Na β (Si/Al is more than 200) molecular sieve, 20g of USY molecular sieve and AlPO425g of-5 molecular sieve and 20g of NaY molecular sieve. The molecular sieves used are all small balls with the diameter of 2-3 mm.
Carrying out regeneration treatment on the decolorizing agent:
after the decoloring treatment is finished, draining the decoloring agent in the glass column for 0.9h, pouring out the decoloring agent, placing in a roasting furnace, drying at 145 ℃ for 19h, heating to 570 ℃, roasting for 3h, and cooling to room temperature to obtain the regenerated decoloring agent.
The regenerated decolorizer was again subjected to the above decolorization treatment, and the absorbance (λ 410nm) of the discharged l-phenylglycine solution was measured to be 0.203.
Example 7
Heating 1000ml of a solution produced by L-phenylglycine (pH 9.5 and absorbance ((lambda 410nm)1.305) to 3 ℃, then passing the solution produced by L-phenylglycine through a 50mm glass column filled with a decolorizing agent, winding a heating belt outside the glass column, controlling the heating belt by a temperature control system, controlling the temperature of the glass column to be 60 +/-2 ℃, controlling the outflow speed of the solution produced by L-phenylglycine from the glass column to be 8ml/min, collecting the outflow solution from the glass column, namely completing decolorization treatment, and detecting the absorbance (lambda 410nm) of the outflow L-phenylglycine solution to be 0.201.
The decolorizing agent is:
2g of molecular sieve, 3g of SAPO-34 molecular sieve, 6g of NaZSM-8(Si/Al is more than 200) molecular sieve, 6g of NaZSM-5(Si/Al is more than 200) molecular sieve, 20g of mordenite (Si/Al is more than 100), 23g of Na β (Si/Al is more than 200) molecular sieve, 15g of USY molecular sieve and 25g of NaY molecular sieve, wherein the used molecular sieves are all small balls with the diameter of 2-3 mm.
Carrying out regeneration treatment on the decolorizing agent:
after the decoloring treatment is finished, draining the decoloring agent in the glass column for 0.8h, pouring out the decoloring agent, placing in a roasting furnace, drying at 120 ℃ for 17h, heating to 580 ℃, roasting for 3.5h, and cooling to room temperature to obtain the regenerated decoloring agent.
The regenerated decolorizer was again subjected to the above decolorization treatment, and the absorbance (λ 410nm) of the discharged l-phenylglycine solution was measured to be 0.202.
Example 8
Heating 1000ml of a solution produced by L-phenylglycine (pH 9.5 and absorbance ((lambda 410nm)1.305) to 76 ℃, then passing the solution produced by L-phenylglycine through a 50mm glass column filled with a decolorizing agent, winding a heating belt outside the glass column, controlling the heating belt by a temperature control system, controlling the temperature of the glass column to be 70 +/-5 ℃, controlling the outflow speed of the solution produced by L-phenylglycine from the glass column to be 7ml/min, collecting the outflow solution from the glass column, namely completing decolorization treatment, and detecting the absorbance (lambda 410nm) of the outflow L-phenylglycine solution to be 0.203.
The decolorizing agent is: AlPO44g of-34 molecular sieve, 2g of SAPO-34 molecular sieve, 5g of NaZSM-11(Si/Al is more than 200) molecular sieve, 4g of NaZSM-5(Si/Al is more than 200) molecular sieve and AlPO415g of-11 molecular sieve, 15g of Na β (Si/Al is more than 200) molecular sieve and AlPO4-5 molecular sieves 55 g. The used sub-sieves are all small balls with the diameter of 2-3 mm.
Carrying out regeneration treatment on the decolorizing agent:
after the decoloring treatment is finished, draining the decoloring agent in the glass column for 1.1h, pouring out the decoloring agent, placing the decoloring agent in a roasting furnace, drying at 130 ℃ for 15h, heating to 590 ℃, roasting for 3h, and cooling to room temperature to obtain the regenerated decoloring agent.
The regenerated decolorizer was again subjected to the above decolorization treatment, and the absorbance (λ 410nm) of the discharged l-phenylglycine solution was measured to be 0.204.
Example 9
Heating 1000ml of a solution produced by L-phenylglycine (pH 9.5 and absorbance ((lambda 410nm)1.305) to 74 ℃, then passing the solution produced by L-phenylglycine through a 50mm glass column filled with a decolorizing agent, winding a heating belt outside the glass column, controlling the heating belt by a temperature control system, controlling the temperature of the glass column to be 75 +/-5 ℃, controlling the outflow speed of the solution produced by L-phenylglycine from the glass column to be 7ml/min, collecting the outflow solution from the glass column, namely completing decolorization treatment, and detecting the absorbance (lambda 410nm) of the outflow L-phenylglycine solution to be 0.203.
The decolorizing agent is:
molecular sieves 4g, AlPO44g of-34 molecular sieve, 4g of SAPO-34 molecular sieve, 6g of NaZSM-11(Si/Al is more than 200) molecular sieve, 7g of NaZSM-8(Si/Al is more than 200) molecular sieve, 7g of NaZSM-5(Si/Al is more than 200) molecular sieve, AlPO410g of-11 molecular sieves, 12g of mordenite (Si/Al is more than 100)g, Na β (Si/Al is more than 200) molecular sieve 13g, USY molecular sieve 11g, AlPO411g of-5 molecular sieve and 11g of NaY molecular sieve. The molecular sieves used are all small balls with the diameter of 2-3 mm.
Carrying out regeneration treatment on the decolorizing agent:
after the decoloring treatment is finished, draining the decoloring agent in the glass column for 1.2h, pouring out the decoloring agent, placing the decoloring agent in a roasting furnace, drying at 140 ℃ for 13h, heating to 600 ℃, roasting for 3h, and cooling to room temperature to obtain the regenerated decoloring agent.
The regenerated decolorizer was again subjected to the above decolorization treatment, and the absorbance (λ 410nm) of the discharged l-phenylglycine solution was measured to be 0.204.
Example 10
Heating 1000ml of a solution produced by L-phenylglycine (pH 9.5 and absorbance ((lambda 410nm)1.305) to 67 ℃, then passing the solution produced by L-phenylglycine through a 50mm glass column filled with a decolorizing agent, winding a heating belt outside the glass column, controlling the heating belt by a temperature control system, controlling the temperature of the glass column to be 70 +/-5 ℃, controlling the outflow speed of the solution produced by L-phenylglycine from the glass column to be 8ml/min, collecting the outflow solution from the glass column, namely completing decolorization treatment, and detecting the absorbance (lambda 410nm) of the outflow L-phenylglycine solution to be 0.207.
The decolorizing agent is:
12g of molecular sieve, 8g of SAPO-34 molecular sieve, 7g of NaZSM-11(Si/Al is more than 200) molecular sieve, 10g of NaZSM-5(Si/Al is more than 200) molecular sieve, and AlPO411g of-11 molecular sieve, 11g of mordenite (Si/Al is more than 100), 11g of Na β (Si/Al is more than 200) molecular sieve, 10g of USY molecular sieve and AlPO410g of-5 molecular sieve and 10g of NaY molecular sieve. The molecular sieves used are all small balls with the diameter of 2-3 mm.
1. Carrying out regeneration treatment on the decolorizing agent:
① after the decoloring treatment is finished, draining the solution of the decoloring agent in the glass column for 1.2h, pouring out the decoloring agent, placing in a roasting furnace, drying at 150 ℃ for 12h, heating to 610 ℃, roasting for 3h, and cooling to room temperature to obtain the regenerated decoloring agent.
The regenerated decolorizer was again subjected to the above decolorization treatment, and the absorbance (λ 410nm) of the discharged l-phenylglycine solution was measured to be 0.208.
The decolorizers of examples 1 to 10 were subjected to continuous regeneration treatment and decolorized with the regenerated decolorizer, and the decolorization effect was as follows:
TABLE 1
The above absorbance (λ ═ 410nm) test was performed by a spectrophotometer method; all of the above molecular sieves are available from the great works science and technology limited of North Heibo Huamao.
② regeneration effect controlled by different regeneration conditions
The effect of the regenerated decolorizing agent of the invention is that besides the collocation and proportion control of the decolorizing agent to enhance the use of the decolorizing agent, the control of the regeneration condition can play a promoting role, the decolorizing agent is dried for 12-24h at the temperature of 120-150 ℃ to protect the pore structure of the molecular sieve, the preparation is made for the subsequent roasting at the temperature of more than 500 ℃, the damage of the pore structure of the molecular sieve is avoided, the drying temperature cannot be less than 120 ℃, the protection effect cannot be played, the temperature cannot exceed 150 ℃, otherwise, the regeneration effect of the regenerated molecular sieve is poor, the time length needs to be strictly controlled, the time is too short, the protection effect is not obvious, and the subsequent regeneration reduction is influenced by too long
③ decolorization effect of decolorizer
| Item | Absorbance of the solution | Amount of adsorbed L-phenylglycine |
| Example 1 | 0.206 | 0.12％ |
| Example 2 | 0.209 | 0.13％ |
| Example 3 | 0.207 | 0.12％ |
| Example 4 | 0.208 | 0.10％ |
| Example 5 | 0.207 | 0.11％ |
| Example 6 | 0.202 | 0.12％ |
| Example 7 | 0.201 | 0.13％ |
| Example 8 | 0.203 | 0.12％ |
| Example 9 | 0.203 | 0.12％ |
| Example 10 | 0.207 | 0.13％ |
| Comparative example 1 | 0.876 | 5.78％ |
| Comparison 2 (average) | 0.819 | 4.67％ |
Note: comparative 1 is the same amount of activated carbon. Comparison 2 is the same amount of other built molecular sieves (e.g., small grain Y-type or nano Y-type molecular sieves are built with one of A-type, X-type, Y-type, ZSM-type, mordenite, aluminum phosphate molecular sieves).
As aromatic aldehydes, catalysts, racemization agents, racemization catalysts and other substances are added in the process of preparing the L-phenylglycine, the substances are oxidized to generate colored impurities when the L-phenylglycine is produced, and the color-assisting effect of the substances enables the L-phenylglycine to generate certain color change, so that the colored impurities and the color-assisting impurities exist in the L-phenylglycine, aiming at the colored impurities and the color-assisting impurities, the adsorption effect of active carbon is limited, and the molecular sieve can realize adsorption, but the problem of poor adsorption effect and even large amount of L-phenylglycine adsorption can be caused if the molecular sieve is improperly used. In order to reduce the absorption of the L-phenylglycine, a further process of controlling the outflow speed of the solution to be 7-9ml/min and enabling the solution to stay in the column for at least 10 minutes is required, so that the L-phenylglycine is decolorized, and the L-phenylglycine is hardly absorbed.
Claims (5)
1. The method is characterized in that the solution produced by the L-phenylglycine is heated to 50-100 ℃, then the solution produced by the L-phenylglycine passes through a glass column, the temperature of the glass column is controlled to be 55-80 ℃, the outflow speed of the solution produced by the L-phenylglycine from the glass column is controlled to be 7-9ml/min, and the outflow solution from the glass column is collected, namely the decoloring treatment is completed;
the decolorizing agent comprises, by mass, 2-10% of a molecular sieve A, 5-20% of a molecular sieve B, 20-50% of a molecular sieve C and 30-70% of a molecular sieve D, wherein the molecular sieve A is selected from
Molecular sieves, AlPO4At least one of a 34 molecular sieve and a SAPO-34 molecular sieve, wherein the molecular sieve B is selected from at least one of NaZSM-11 molecular sieve with Si/Al more than 200, NaZSM-8 molecular sieve with Si/Al more than 200 and NaZSM-5 molecular sieve with Si/Al more than 200; the molecular sieve C is selected from mordenite and AlPO4At least one of-11 molecular sieve and Na β molecular sieve with Si/Al greater than 200, wherein the molecular sieve D is selected from NaY molecular sieve, USY molecular sieve and AlPO4-5 molecular sieves.
2. The levo-phenylglycine decolorizing process according to claim 1, characterized in that the decolorizing agent is regenerated and then placed in a glass column again for recycling.
3. The levo-phenylglycine decolorizing process according to claim 2, characterized in that said regeneration treatment comprises the following steps: after the decoloring treatment is finished, draining the decoloring agent in the glass column for 0.8-1.2h, pouring out the decoloring agent, placing the decoloring agent in a roasting furnace, drying at the temperature of 120-150 ℃ for 12-24h, heating to the temperature of more than 500 +/-1 ℃, roasting for 3-6h, and then cooling to room temperature to finish the regeneration treatment.
4. The process for decoloring L-phenylglycine according to claim 3, wherein the temperature is raised to 550 ℃ and 600 ℃ and the mixture is calcined for 3-6 h.
5. The levo-phenylglycine decolorizing process according to claim 1, characterized in that the residence time of the solution produced by levo-phenylglycine in the glass column is controlled to be not less than 10 min.
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| CN1185991A (en) * | 1996-12-27 | 1998-07-01 | 韩国化学研究所 | Manufacturing method of granulated complex molecular sieve composition having multi-functions |
| CN102851332A (en) * | 2012-09-07 | 2013-01-02 | 石药集团中诺药业（石家庄）有限公司 | Recovery method for D(-)phenylglycine in ampicillin mother liquid by using enzyme method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1185991A (en) * | 1996-12-27 | 1998-07-01 | 韩国化学研究所 | Manufacturing method of granulated complex molecular sieve composition having multi-functions |
| CN102851332A (en) * | 2012-09-07 | 2013-01-02 | 石药集团中诺药业（石家庄）有限公司 | Recovery method for D(-)phenylglycine in ampicillin mother liquid by using enzyme method |
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