CN108191687A - L-Phenylglycine decoloration process - Google Patents
L-Phenylglycine decoloration process Download PDFInfo
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- CN108191687A CN108191687A CN201810031126.3A CN201810031126A CN108191687A CN 108191687 A CN108191687 A CN 108191687A CN 201810031126 A CN201810031126 A CN 201810031126A CN 108191687 A CN108191687 A CN 108191687A
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- phenylglycine
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- decolorising agent
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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
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/07—Optical isomers
Abstract
L-Phenylglycine decoloration process, belong to the technical field of L-Phenylglycine production, to the solution that L-Phenylglycine produces decolorization is carried out by being equipped with the glass column of decolorising agent, the solution that L-Phenylglycine produces is heated to 50 100 DEG C, then the solution that L-Phenylglycine produces is passed through into glass column, the temperature for controlling glass column is 55 80 DEG C, control the solution of L-Phenylglycine production from the rate of outflow of glass column be 7 9ml/min, collected from the outflow solution of glass column, that is, complete decolorization.Decoloration process of the present invention is to color-causing impurity present in L-Phenylglycine production and helps the more targeted removal of colored foreign, and removal effect is excellent, hence it is evident that better than the decoloration requirement of L-Phenylglycine production, has the advantage environmentally protective, production cost is low.
Description
Technical field
The invention belongs to the technical fields of L-Phenylglycine production, are related to L-Phenylglycine decoloration process, the present invention
Decoloration process is easy to operate, and decolorization is stablized, to the good decolorizing effect of L-Phenylglycine.
Background technology
Chemical industry and pharmaceutical products are generally very high to color and luster requirement, in order to which product color can be up to standard, industrially generally will
It is decolourized using decoloration process, since activated carbon has very wide pore-size distribution, it is miscellaneous that color development of all sizes can be adsorbed
Matter and colored foreign is helped, therefore activated carbon is widely used as a kind of wide spectrum decolorising agent in field of chemical pharmacy, but activity
Charcoal, which uses, has very big problem, and common product contains one or more of color-causing impurities of different sizes and helps colored foreign first, living
Property charcoal can only there is the hole in the apertures of one or more of corresponding sizes to play decolorization, and the holes of the overwhelming majority of activated carbon are not
It is utilized, therefore usually usage amount is larger for activated carbon；Secondly because activated carbon thermal stability is poor, easily burn under high temperature,
Therefore it is used only once, it is impossible to which the methods of passing through high-temperature roasting realizes that regenerating active carbon is reused, and used activated carbon is only
It can be handled as waste active carbon, belong to hazardous waste according to national regulation waste active carbon, in storage, delivery, transport, disposal process
In, there is stringent laws and regulations regulation in country, and larger financial burden can be not only caused to enterprise, but also is frequently accompanied by tight
Weight risk of environmental pollution.
L-Phenylglycine is a kind of important pharmaceutical intermediate and special chemical article, and appearance is white solid, left at present
Phenylglycine is revolved in process of production using activated carbon decolorizing, and average product decoloration per ton needs 8 kilograms of activated carbons, not only integrates
It is of high cost, and be a kind of environmental pollution and the wasting of resources, therefore develop needed for a kind of suitable L-Phenylglycine production
Environmentally protective decoloration process has larger economic value and important environment protection significance.
Invention content
The present invention is provided to solve the problems, such as that existing L-Phenylglycine decoloration process is single, decolorizing effect is undesirable
A kind of decoloration process of environmentally protective, good decolorizing effect L-Phenylglycine.
The present invention for realize its purpose the technical solution adopted is that：
L-Phenylglycine decoloration process, to the solution that L-Phenylglycine produces by be equipped with the glass column of decolorising agent into
The solution that L-Phenylglycine produces is heated to 50-100 DEG C by row decolorization, then by the molten of L-Phenylglycine production
For liquid by glass column, the temperature for controlling glass column is 55-80 DEG C, controls the solution of L-Phenylglycine production from the stream of glass column
Go out speed for 7-9ml/min, collected from the outflow solution of glass column, that is, complete decolorization.
The decolorising agent by mass percentage, the molecular sieve-4 A including 2-10%, the molecular sieve B, 20- of 5-20%
The molecular sieve D of 50% molecular sieve C, 30-70%, the molecular sieve-4 A are selected fromMolecular sieve, AlPO4- 34 molecular sieves,
At least one of SAPO-34 molecular sieves, the molecular sieve B is selected from NaZSM-11 molecular sieves of the Si/Al more than 200, Si/Al is more than
At least one of the 200 NaZSM-5 molecular sieves of NaZSM-8 molecular sieves, Si/Al more than 200；The molecular sieve C is selected from mercerising
Zeolite, AlPO4At least one of the Na beta-molecular sieves of -11 molecular sieves, Si/Al more than 200；Molecular sieve D is selected from NaY molecular sieve,
USY molecular sieve, AlPO4At least one of -5 molecular sieves.
The decolorising agent, which is again loaded into after regeneration treatment in glass column, to be recycled.
The regeneration treatment includes the following steps：After completing decolorization, the decolorising agent in glass column is drained into solution
Then 0.8-1.2h pours out decolorising agent, be placed in roaster, prior to 120-150 DEG C at dry 12-24h, then heat to 500
± 1 DEG C or more, 3-6h is roasted, then near room temperature, that is, complete regeneration treatment.
550-600 DEG C is warming up to, roasts 3-6h.
Control residence time >=10min of the solution of L-Phenylglycine production in glass column.
The beneficial effects of the invention are as follows：
In the production of L-Phenylglycine, acid solution is generally for the left-handed benzene thuja acid mother liquor of decoloration, to decoloration
Agent can generate harm and cause decolorizing effect poor, and the present invention controls left-handed benzene by the way that the molecular sieve of different structure is selected to be mixed
The temperature of glycin mother liquid and the temperature of molecular sieve glass column, reduce to decolorising agent structural damage, and then prevent acidity
Damage of the solution to decolorising agent, so as to fulfill excellent decolorizing effect.
The renewable reuse of decolorising agent of the present invention, and decolorizing effect is better than activated carbon, the selection of binding molecule sieve and
Ratio is arranged in pairs or groups so that functionally mutually support to color-causing impurity present in L-Phenylglycine production and helps colored foreign more
It targetedly removes, and removal effect is excellent, hence it is evident that better than the decoloration requirement of L-Phenylglycine production, there is green ring
It protects, the advantage that production cost is low.
It is generally prepared, prepared using techniques such as racemization, mixed, fractionations in the production of prior art L-Phenylglycine
Cheng Zhonghui adds in the substances such as aromatic aldehydes, catalyst, racemization agent, racemization catalyst, and the addition of these substances is producing left-handed benzene
Oxidation can generate foreign pigment during glycine, while such substance helps color to act on so that L-Phenylglycine generates certain color
Become, thus to above-mentioned foreign pigment and help colored foreign removing be the key that realize L-Phenylglycine decoloration, if selection live
Property charcoal, although there is certain adsorption effect to these impurity with macroporous structure, due to colored substance in L-Phenylglycine
Matter and the particularity of colored foreign and the irregular of pore structure and adsorption site undesirable are helped, cause the limitation of absorption, from
And to be decolourized with a large amount of activated carbon in practice, the increase of cost and the waste of the energy are caused, and decolorizing effect is not so good as
Meaning.The present invention passes through long-term creative research, is compounded by the molecular sieve for selecting four kinds of schemes, with reference to each molecular sieve
Mix ratio is worked using electrostatic field powerful inside bug hole, improves the absorption potential energy of channel surfaces, pass through molecular sieve crystallinity
It is reasonably combined with specific surface area, diffusion and absorption to coloring matter are improved, and then improve decolorization rate and decoloring ability；
By controlling the temperature of L-Phenylglycine solution and the temperature of molecular sieve glass column, improve organic impurities and enter duct
Probability, the space resistance for making organic impurities close to molecular sieve adsorption site reduce, it is easier to close to the adsorption site of molecular sieve,
Enhance with the active force of adsorption site, further improve decoloring ability.
The selection of molecular sieve of the present invention and mixing ratio are the key that realize efficient decolorizing, while are also to improve power of regeneration
Key, on the basis of decolorising agent regeneration technology of the present invention, selection and mixing ratio due to molecular sieve so that in absorption
When it is more targeted, adsorbate is more stable to the selection in duct, therefore with reference to regeneration technology, can realize high desorption, regenerates
Effect is good.
Specific embodiment
With reference to specific embodiment, the present invention is further illustrated.
Embodiment 1
(pH=9.5, absorbance ((λ=410nm) 1.305) are heated to the solution that 1000ml L-Phenylglycines are produced
50 DEG C, then by the solution of L-Phenylglycine production by being equipped with the 50mm glass columns of decolorising agent, be tied with outside glass column plus
The torrid zone, heating are controlled with temperature-controlling system, and the temperature for controlling glass column is 60 ± 5 DEG C, control the molten of L-Phenylglycine production
Liquid is 7ml/min from the rate of outflow of glass column, collected from the outflow solution of glass column, that is, completes decolorization.Detection outflow
L-Phenylglycine solution absorbance (λ=410nm) be 0.206.
The decolorising agent is：(Si/Al is more than molecular sieve 7g, Na β by molecular sieve 4g, NaZSM-8 (Si/Al is more than 200)
200) molecular sieve 25g, USY molecular sieve 64g.Molecular sieve used is the bead of diameter 2-3mm.
Above-mentioned decolorising agent is subjected to regeneration treatment：
After completing decolorization, the decolorising agent in glass column is drained into solution 0.8h, then pours out decolorising agent, is placed in roasting
In stove, prior to 120 DEG C at it is dry then heat to 520 DEG C for 24 hours, roast 6h, then near room temperature is to get regeneration decolorising agent.
Regenerated decolorising agent is subjected to above-mentioned decolorization again, detects the absorbance of the L-Phenylglycine solution of outflow
(λ=410nm) is 0.209.
Embodiment 2
(pH=9.5, absorbance ((λ=410nm) 1.305) are heated to the solution that 1000ml L-Phenylglycines are produced
60 DEG C, then by the solution of L-Phenylglycine production by being equipped with the 50mm glass columns of decolorising agent, be tied with outside glass column plus
The torrid zone, heating are controlled with temperature-controlling system, and the temperature for controlling glass column is 60 ± 3 DEG C, control the molten of L-Phenylglycine production
Liquid is 8ml/min from the rate of outflow of glass column, collected from the outflow solution of glass column, that is, completes decolorization.Detection outflow
L-Phenylglycine solution absorbance (λ=410nm) be 0.207.
The decolorising agent is：AlPO4- 34 molecular sieve 5g, NaZSM-5 (Si/Al is more than 200) molecular sieve 15g, Na β (Si/
Al is more than 200) molecular sieve 30g, NaY molecular sieve 50g.Molecular sieve used is the bead of diameter 2-3mm.
Above-mentioned decolorising agent is subjected to regeneration treatment：
After completing decolorization, the decolorising agent in glass column is drained into solution 0.9h, then pours out decolorising agent, is placed in roasting
In stove, prior to 125 DEG C at dry 22h, then heat to 530 DEG C, roast 5.5h, then near room temperature is to get regeneration decolorising agent.
Regenerated decolorising agent is subjected to above-mentioned decolorization again, detects the absorbance of the L-Phenylglycine solution of outflow
(λ=410nm) is 0.209.
Embodiment 3
(pH=9.5, absorbance ((λ=410nm) 1.305) are heated to the solution that 1000ml L-Phenylglycines are produced
70 DEG C, then by the solution of L-Phenylglycine production by being equipped with the 50mm glass columns of decolorising agent, be tied with outside glass column plus
The torrid zone, heating are controlled with temperature-controlling system, and the temperature for controlling glass column is 70 ± 5 DEG C, control the molten of L-Phenylglycine production
Liquid is 9ml/min from the rate of outflow of glass column, collected from the outflow solution of glass column, that is, completes decolorization.Detection outflow
L-Phenylglycine solution absorbance (λ=410nm) be 0.207.
The decolorising agent is：Molecular sieve 2g, AlPO4- 34 molecular sieve 5g, NaZSM-8 (Si/Al is more than 200) molecular sieve
5g, NaZSM-11 (Si/Al is more than 200) molecular sieve 10g, modenite (Si/Al is more than 100) 20g, USY molecular sieve 40g,
AlPO4- 5 molecular sieve 18g.Molecular sieve used is the bead of diameter 2-3mm.
Above-mentioned decolorising agent is subjected to regeneration treatment：
After completing decolorization, the decolorising agent in glass column is drained into solution 1h, decolorising agent is then poured out, is placed in roaster
In, prior to 130 DEG C at dry 20h, then heat to 540 DEG C, roast 5h, then near room temperature is to get regeneration decolorising agent.
Regenerated decolorising agent is subjected to above-mentioned decolorization again, detects the absorbance of the L-Phenylglycine solution of outflow
(λ=410nm) is 0.208.
Embodiment 4
(pH=9.5, absorbance ((λ=410nm) 1.305) are heated to the solution that 1000ml L-Phenylglycines are produced
80 DEG C, then by the solution of L-Phenylglycine production by being equipped with the 50mm glass columns of decolorising agent, be tied with outside glass column plus
The torrid zone, heating are controlled with temperature-controlling system, and the temperature for controlling glass column is 70 ± 3 DEG C, control the molten of L-Phenylglycine production
Liquid is 7.5ml/min from the rate of outflow of glass column, collected from the outflow solution of glass column, that is, completes decolorization.Detection stream
The absorbance (λ=410nm) of the L-Phenylglycine solution gone out is 0.208.
The decolorising agent is：AlPO4- 34 molecular sieve 5g, NaZSM-5 (Si/Al is more than 200) molecular sieve 5g, NaZSM-11
(Si/Al is more than 200) molecular sieve 5g, AlPO4- 11 molecular sieve 8g, modenite (Si/Al is more than 100) 17g, NaY molecular sieve
70g.Molecular sieve used is the bead of diameter 2-3mm.
Above-mentioned decolorising agent is subjected to regeneration treatment：
After completing decolorization, the decolorising agent in glass column is drained into solution 1.1h, then pours out decolorising agent, is placed in roasting
In stove, prior to 135 DEG C at dry 16h, then heat to 550 DEG C, roast 4h, then near room temperature is to get regeneration decolorising agent.
Regenerated decolorising agent is subjected to above-mentioned decolorization again, detects the absorbance of the L-Phenylglycine solution of outflow
(λ=410nm) is 0.209.
Embodiment 5
(pH=9.5, absorbance ((λ=410nm) 1.305) are heated to the solution that 1000ml L-Phenylglycines are produced
90 DEG C, then by the solution of L-Phenylglycine production by being equipped with the 50mm glass columns of decolorising agent, be tied with outside glass column plus
The torrid zone, heating are controlled with temperature-controlling system, and the temperature for controlling glass column is 75 ± 5 DEG C, control the molten of L-Phenylglycine production
Liquid is 8.5ml/min from the rate of outflow of glass column, collected from the outflow solution of glass column, that is, completes decolorization.Detection stream
The absorbance (λ=410nm) of the L-Phenylglycine solution gone out is 0.207.
The decolorising agent is：4AlPO4- 34 molecular sieve 2g,Molecular sieve 2g, NaZSM-11 (Si/Al is more than 200) point
Son sieve 5g, AlPO4- 11 molecular sieve 8g, modenite (Si/Al is more than 100) 17g, NaY molecular sieve 50g, AlPO4- 5 molecular sieves
16g.Molecular sieve used is the bead of diameter 2-3mm.
Above-mentioned decolorising agent is subjected to regeneration treatment：
After completing decolorization, the decolorising agent in glass column is drained into solution 1h, decolorising agent is then poured out, is placed in roaster
In, prior to 140 DEG C at dry 14h, then heat to 560 DEG C, roast 4.5h, then near room temperature is to get regeneration decolorising agent.
Regenerated decolorising agent is subjected to above-mentioned decolorization again, detects the absorbance of the L-Phenylglycine solution of outflow
(λ=410nm) is 0.209.
Embodiment 6
(pH=9.5, absorbance ((λ=410nm) 1.305) are heated to the solution that 1000ml L-Phenylglycines are produced
100 DEG C, then by the solution of L-Phenylglycine production by being equipped with the 50mm glass columns of decolorising agent, be tied with outside glass column plus
The torrid zone, heating are controlled with temperature-controlling system, and the temperature for controlling glass column is 70 ± 5 DEG C, control the molten of L-Phenylglycine production
Liquid is 9ml/min from the rate of outflow of glass column, collected from the outflow solution of glass column, that is, completes decolorization.Detection outflow
L-Phenylglycine solution absorbance (λ=410nm) be 0.202.
The decolorising agent is：Molecular sieve 2g, AlPO4- 34 molecular sieve 1g, SAPO-34 molecular sieve 1g, NaZSM-11
(Si/Al is more than 200) molecular sieve 5g, NaZSM-8 (Si/Al is more than 200) molecular sieve 2g, NaZSM-5 (Si/Al is more than 200) point
Son sieve 3g, AlPO4- 11 molecular sieve 6g, modenite (Si/Al is more than 100) 10g, Na β (Si/Al is more than 200) molecular sieve 5g,
USY molecular sieve 20g, AlPO4- 5 molecular sieve 25g, NaY molecular sieve 20g.Molecular sieve used is the bead of diameter 2-3mm.
Above-mentioned decolorising agent is subjected to regeneration treatment：
After completing decolorization, the decolorising agent in glass column is drained into solution 0.9h, then pours out decolorising agent, is placed in roasting
In stove, prior to 145 DEG C at dry 19h, then heat to 570 DEG C, roast 3h, then near room temperature is to get regeneration decolorising agent.
Regenerated decolorising agent is subjected to above-mentioned decolorization again, detects the absorbance of the L-Phenylglycine solution of outflow
(λ=410nm) is 0.203.
Embodiment 7
(pH=9.5, absorbance ((λ=410nm) 1.305) are heated to 3 to the solution that 1000ml L-Phenylglycines are produced
DEG C, the solution of L-Phenylglycine production is then tied with heating by being equipped with the 50mm glass columns of decolorising agent outside glass column
Band, heating are controlled with temperature-controlling system, and the temperature for controlling glass column is 60 ± 2 DEG C, the solution of control L-Phenylglycine production
It is 8ml/min from the rate of outflow of glass column, collected from the outflow solution of glass column, that is, completes decolorization.Detection outflow
The absorbance (λ=410nm) of L-Phenylglycine solution is 0.201.
The decolorising agent is：Molecular sieve 2g, SAPO-34 molecular sieve 3g, NaZSM-8 (Si/Al is more than 200) molecular sieve
6g, NaZSM-5 (Si/Al is more than 200) molecular sieve 6g, modenite (Si/Al is more than 100) 20g, Na β (Si/Al is more than 200)
Molecular sieve 23g, USY molecular sieve 15g, NaY molecular sieve 25g.Molecular sieve used is the bead of diameter 2-3mm.
Above-mentioned decolorising agent is subjected to regeneration treatment：
After completing decolorization, the decolorising agent in glass column is drained into solution 0.8h, then pours out decolorising agent, is placed in roasting
In stove, prior to 120 DEG C at dry 17h, then heat to 580 DEG C, roast 3.5h, then near room temperature is to get regeneration decolorising agent.
Regenerated decolorising agent is subjected to above-mentioned decolorization again, detects the absorbance of the L-Phenylglycine solution of outflow
(λ=410nm) is 0.202.
Embodiment 8
(pH=9.5, absorbance ((λ=410nm) 1.305) are heated to the solution that 1000ml L-Phenylglycines are produced
76 DEG C, then by the solution of L-Phenylglycine production by being equipped with the 50mm glass columns of decolorising agent, be tied with outside glass column plus
The torrid zone, heating are controlled with temperature-controlling system, and the temperature for controlling glass column is 70 ± 5 DEG C, control the molten of L-Phenylglycine production
Liquid is 7ml/min from the rate of outflow of glass column, collected from the outflow solution of glass column, that is, completes decolorization.Detection outflow
L-Phenylglycine solution absorbance (λ=410nm) be 0.203.
The decolorising agent is：AlPO4- 34 molecular sieve 4g, SAPO-34 molecular sieve 2g, NaZSM-11 (Si/Al is more than 200)
Molecular sieve 5g, NaZSM-5 (Si/Al is more than 200) molecular sieve 4g, AlPO4- 11 molecular sieve 15g, Na β (Si/Al is more than 200) point
Son sieve 15g, AlPO4- 5 molecular sieve 55g.Used point of son sieve is the bead of diameter 2-3mm.
Above-mentioned decolorising agent is subjected to regeneration treatment：
After completing decolorization, the decolorising agent in glass column is drained into solution 1.1h, then pours out decolorising agent, is placed in roasting
In stove, prior to 130 DEG C at dry 15h, then heat to 590 DEG C, roast 3h, then near room temperature is to get regeneration decolorising agent.
Regenerated decolorising agent is subjected to above-mentioned decolorization again, detects the absorbance of the L-Phenylglycine solution of outflow
(λ=410nm) is 0.204.
Embodiment 9
(pH=9.5, absorbance ((λ=410nm) 1.305) are heated to the solution that 1000ml L-Phenylglycines are produced
74 DEG C, then by the solution of L-Phenylglycine production by being equipped with the 50mm glass columns of decolorising agent, be tied with outside glass column plus
The torrid zone, heating are controlled with temperature-controlling system, and the temperature for controlling glass column is 75 ± 5 DEG C, control the molten of L-Phenylglycine production
Liquid is 7ml/min from the rate of outflow of glass column, collected from the outflow solution of glass column, that is, completes decolorization.Detection outflow
L-Phenylglycine solution absorbance (λ=410nm) be 0.203.
The decolorising agent is：Molecular sieve 4g, AlPO4- 34 molecular sieve 4g, SAPO-34 molecular sieve 4g, NaZSM-11
(Si/Al is more than 200) molecular sieve 6g, NaZSM-8 (Si/Al is more than 200) molecular sieve 7g, NaZSM-5 (Si/Al is more than 200) point
Son sieve 7g, AlPO4- 11 molecular sieve 10g, modenite (Si/Al is more than 100) 12g, Na β (Si/Al is more than 200) molecular sieve
13g, USY molecular sieve 11g, AlPO4- 5 molecular sieve 11g, NaY molecular sieve 11g.Molecular sieve used is the small of diameter 2-3mm
Ball.
Above-mentioned decolorising agent is subjected to regeneration treatment：
After completing decolorization, the decolorising agent in glass column is drained into solution 1.2h, then pours out decolorising agent, is placed in roasting
In stove, prior to 140 DEG C at dry 13h, then heat to 600 DEG C, roast 3h, then near room temperature is to get regeneration decolorising agent.
Regenerated decolorising agent is subjected to above-mentioned decolorization again, detects the absorbance of the L-Phenylglycine solution of outflow
(λ=410nm) is 0.204.
Embodiment 10
(pH=9.5, absorbance ((λ=410nm) 1.305) are heated to the solution that 1000ml L-Phenylglycines are produced
67 DEG C, then by the solution of L-Phenylglycine production by being equipped with the 50mm glass columns of decolorising agent, be tied with outside glass column plus
The torrid zone, heating are controlled with temperature-controlling system, and the temperature for controlling glass column is 70 ± 5 DEG C, control the molten of L-Phenylglycine production
Liquid is 8ml/min from the rate of outflow of glass column, collected from the outflow solution of glass column, that is, completes decolorization.Detection outflow
L-Phenylglycine solution absorbance (λ=410nm) be 0.207.
The decolorising agent is：Molecular sieve 12g, SAPO-34 molecular sieve 8g, NaZSM-11 (Si/Al is more than 200) molecule
Sieve 7g, NaZSM-5 (Si/Al is more than 200) molecular sieve 10g, AlPO4- 11 molecular sieve 11g, modenite (Si/Al is more than 100)
11g, Na β (Si/Al is more than 200) molecular sieve 11g, USY molecular sieve 10g, AlPO4- 5 molecular sieve 10g, NaY molecular sieve 10g.Institute
Molecular sieve is the bead of diameter 2-3mm.
1st, above-mentioned decolorising agent is subjected to regeneration treatment：
1. after completing decolorization, the decolorising agent in glass column is drained into solution 1.2h, then pours out decolorising agent, is placed in roasting
Burn in stove, prior to 150 DEG C at dry 12h, then heat to 610 DEG C, roast 3h, then near room temperature is to get regeneration decolorising agent.
Regenerated decolorising agent is subjected to above-mentioned decolorization again, detects the absorbance of the L-Phenylglycine solution of outflow
(λ=410nm) is 0.208.
By the decolorising agent of above-described embodiment 1-10 through constantly regenerating processing, decolorization is carried out with regenerated decolorising agent, is taken off
Color effect is as follows：
Table 1
More than absorbance (λ=410nm) test is using spectrophotometer method；All of above molecular sieve is by Hebei Hua Mao great achievements
Science and Technology Ltd. provides.
2. the regeneration effect of different regeneration condition controls
Effect after decolorising agent regeneration of the present invention is other than the collocation of itself and ratio control enhance its use, then the carded sliver
The control of part can play facilitation, be first the pore passage structure for protecting molecular sieve the purpose of dry 12-24h at 120-150 DEG C,
For follow-up 500 DEG C it is baked above prepare, avoid molecular sieve pore passage structure destroy, drying temperature cannot be less than 120 DEG C, otherwise not
It can play the role of protection, temperature is also no more than 150 DEG C, and the regenerating molecular sieve effect after otherwise regenerating is poor, the length of time
It must strictly control, the time is too short, protecting effect unobvious, long to influence subsequent regeneration reducing instead
3. the decolorizing effect of decolorising agent
| Project | Absorbance | Adsorb the amount of L-Phenylglycine |
| Embodiment 1 | 0.206 | 0.12% |
| Embodiment 2 | 0.209 | 0.13% |
| Embodiment 3 | 0.207 | 0.12% |
| Embodiment 4 | 0.208 | 0.10% |
| Embodiment 5 | 0.207 | 0.11% |
| Embodiment 6 | 0.202 | 0.12% |
| Embodiment 7 | 0.201 | 0.13% |
| Embodiment 8 | 0.203 | 0.12% |
| Embodiment 9 | 0.203 | 0.12% |
| Embodiment 10 | 0.207 | 0.13% |
| Comparison 1 | 0.876 | 5.78% |
| Compare 2 (average values) | 0.819 | 4.67% |
Note：Comparison 1 is the activated carbon of same amount.Comparison 2 is other compounding molecular sieve (such as small-grain Ys of same amount
Type or nano Y-shaped molecular sieve and a kind of compounding in A types, X-type, Y types, ZSM types, modenite, aluminium phosphate molecular sieve).
Since aromatic aldehydes, catalyst, racemization agent, racemization catalyst etc. can be added in during L-Phenylglycine is prepared
Substance, the addition of these substances is aoxidized when producing L-Phenylglycine can generate foreign pigment, while such substance helps color
Effect is so that L-Phenylglycine generates certain discoloration, therefore there are above-mentioned foreign pigment and helps color in L-Phenylglycine
Impurity for above-mentioned foreign pigment and helps colored foreign, and the adsorption effect of activated carbon is limited, although molecular sieve can realize absorption,
Be if the problem of improper use can cause adsorption effect difference or even a large amount of absorption L-Phenylglycine, to solve the above problems,
The present invention devises the decolorising agent of L-Phenylglycine production, and compounding solution is carried out with the molecular sieve of four kinds of schemes.In order to subtract
Few absorption to L-Phenylglycine needs further to be 7-9ml/min, make solution at least with reference to the control solution rate of outflow
The process that 10 minutes are stopped in column not only realizes the decoloration to L-Phenylglycine, while L-Phenylglycine is adsorbed
Seldom.
Claims (6)
1. L-Phenylglycine decoloration process is carried out to the solution that L-Phenylglycine produces by being equipped with the glass column of decolorising agent
Decolorization, which is characterized in that the solution that L-Phenylglycine produces is heated to 50-100 DEG C, then by L-Phenylglycine
For the solution of production by glass column, the temperature for controlling glass column is 55-80 DEG C, controls the solution that L-Phenylglycine produces from glass
The rate of outflow of glass column is 7-9ml/min, collected from the outflow solution of glass column, that is, completes decolorization.
2. L-Phenylglycine decoloration process according to claim 1, which is characterized in that the decolorising agent presses quality hundred
Divide than meter, the molecular sieve-4 A including 2-10%, the molecular sieve D of the molecular sieve C of the molecular sieve B of 5-20%, 20-50%, 30-70%,
The molecular sieve-4 A is selected fromMolecular sieve, AlPO4At least one of -34 molecular sieves, SAPO-34 molecular sieves, the molecular sieve B
Selected from NaZSM-11 molecular sieves of the Si/Al more than 200, NaZSM-8 molecular sieves of the Si/Al more than 200, Si/Al more than 200
At least one of NaZSM-5 molecular sieves；The molecular sieve C is selected from modenite, AlPO4- 11 molecular sieves, Si/Al are more than 200
At least one of Na beta-molecular sieves；Molecular sieve D is selected from NaY molecular sieve, USY molecular sieve, AlPO4At least one of -5 molecular sieves.
3. L-Phenylglycine decoloration process according to claim 2, which is characterized in that the decolorising agent is through regeneration treatment
After be again loaded into glass column and recycled.
4. L-Phenylglycine decoloration process according to claim 3, which is characterized in that the regeneration treatment includes following
Step：After completing decolorization, the decolorising agent in glass column is drained into solution 0.8-1.2h, then pours out decolorising agent, is placed in roasting
Burn in stove, prior to 120-150 DEG C at dry 12-24h, then heat to 500 ± 1 DEG C or more, roast 3-6h, then near room
Temperature completes regeneration treatment.
5. L-Phenylglycine decoloration process according to claim 4, which is characterized in that be warming up to 550-600 DEG C, roasting
3-6h。
6. L-Phenylglycine decoloration process according to claim 1, which is characterized in that control L-Phenylglycine production
Residence time >=10min of the solution in glass column.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
|---|---|---|---|---|
| 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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