CN108456145A - A kind of DL-phenylalanine production technology of mother liquor recoverable - Google Patents
A kind of DL-phenylalanine production technology of mother liquor recoverable Download PDFInfo
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- CN108456145A CN108456145A CN201710833232.9A CN201710833232A CN108456145A CN 108456145 A CN108456145 A CN 108456145A CN 201710833232 A CN201710833232 A CN 201710833232A CN 108456145 A CN108456145 A CN 108456145A
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- phenylalanine
- racemization
- mother liquor
- production technology
- recoverable
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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
- C07C227/36—Racemisation of optical isomers
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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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- 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
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- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract
The invention discloses a kind of DL phenylalanine Production Technologies of mother liquor recoverable, it is characterised in that：By racemization, centrifugal drying and mother liquid recycle step, the DL phenylalanine Production Technologies are completed.It the advantage is that：The present invention prepares DL phenylalanines using L phenylalanine racemization methods, the mother liquor generated in building-up process is repeatedly applied to L phenylalanine Racemic of N, reduce the dosage of L phenylalanines during follow-up racemization, salicylide and sodium hydrosulfite, raw material is saved, and synthesis technology is simple, DL phenylalanine stable qualities are prepared, content is higher, is suitable for mass producing.
Description
Technical field
The invention belongs to chemosynthesis technical fields, and in particular to a kind of DL-phenylalanine life of mother liquor recoverable
Production. art.
Background technology
Phenylalanine is one of eight kinds of essential amino acids of human body, is used as the nutrition fortifier of food.Recently, DL- benzene
Alanine is proven to have the very good effectiveness such as refresh the mind, ease pain and lose weight.Currently, passing through chemical synthesis DL- benzene
There are many method of alanine, such as cyanamide process and L-phenylalanine racemization method.
Cyanamide process is that phenylacetaldehyde and Cymag is used to prepare DL-phenylalanine for raw material, and step is simple, this method raw material
It is expensive, and Cymag is severe toxicity, working condition requires height, and production cost is high, is also easy to produce a large amount of cyanide wastewater, difficulty
Reason.L-phenylalanine racemization method is to use L-phenylalanine for raw material, and LD- phenylalanines are prepared using racemization agent.Existing L-
Raw material dosage is more in phenylalanine racemization method technique so that production cost is higher, is not suitable for large-scale production.
Invention content
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to now provide, a kind of production cost is low, product purity is high, system
The DL-phenylalanine production technology of standby mother liquor recoverable simple for process.
In order to solve the above technical problems, the technical solution adopted by the present invention is：A kind of DL- phenylpropyl alcohols of mother liquor recoverable
Propylhomoserin production technology, innovative point are：By racemization, centrifugal drying and mother liquid recycle step, the DL- phenylpropyl alcohol ammonia is completed
Acid production process；It is described to be as follows：
（1）Racemization：L-phenylalanine, salicylide, sodium hydrosulfite and methanol is added by a certain percentage in clean reaction kettle, is warming up to
40-50 DEG C, after insulation reaction 5h, survey the content of DL-phenylalanine；
（2）Centrifugal drying：Above-mentioned DL-phenylalanine content is cooled to 20 DEG C more than 98% postcooling, filters, centrifugation, mother liquid obtained
It is applied mechanically for racemization, gained filter cake is dried after being washed with methanol, and the racemization together with mother liquor of the solution after gained washing is applied mechanically；
（3）Mother liquid recycle：It takes above-mentioned racemization to apply mechanically mother liquor and L-phenylalanine, salicylide, sodium hydrosulfite is added by a certain percentage, repeat
Above-mentioned processing step, recycles, and completes the production technology of the DL-phenylalanine.
Further, the step（1）Middle L-phenylalanine：Salicylide：Sodium hydrosulfite：Methanol is 5:0.08:0.05:10.
Further, the step（2）Middle methanol usage is 60Kg.
Further, the step（3）Middle mother liquor：L-phenylalanine：Salicylide：Sodium hydrosulfite is 12:4:0.05:0.01.
Beneficial effects of the present invention are as follows：The present invention prepares DL-phenylalanine using L-phenylalanine racemization method, synthesizes
The mother liquor generated in journey is repeatedly applied to L-phenylalanine Racemic of N, reduces L-phenylalanine, water during follow-up racemization
The dosage of poplar aldehyde and sodium hydrosulfite has saved raw material, and synthesis technology is simple, prepare DL-phenylalanine stable quality, content compared with
Height is suitable for producing on a large scale.
Specific implementation mode
Illustrate that embodiments of the present invention, those skilled in the art can be by this explanations by particular specific embodiment below
Content disclosed by book understands other advantages and effect of the present invention easily.
Embodiment 1
A kind of DL-phenylalanine production technology of mother liquor recoverable, it is characterised in that：By racemization, centrifugal drying and mother
Liquid applies mechanically step, completes the DL-phenylalanine production technology；It is as follows：
（1）Racemization：Be added in clean reaction kettle 265kgL- phenylalanines, 4.24kg salicylides, 2.65kg sodium hydrosulfites and
530kg methanol, is warming up to 40-50 DEG C, after insulation reaction 5h, surveys the content of DL-phenylalanine；
（2）Centrifugal drying：Above-mentioned DL-phenylalanine content is cooled to 20 DEG C more than 98% postcooling, filters, centrifugation, mother liquid obtained
It is applied mechanically for racemization, gained filter cake is dried after being washed with 60kg methanol, solution racemization together with mother liquor after gained washing
It applies mechanically；
（3）Mother liquid recycle：The above-mentioned mother liquors of 648kg, 216KgL- phenylalanines, 2.70kg salicylides, 0.53kg sodium hydrosulfites are taken, weight
Multiple above-mentioned processing step, recycles, completes the production technology of the DL-phenylalanine.
Embodiment 2
A kind of DL-phenylalanine production technology of mother liquor recoverable, it is characterised in that：By racemization, centrifugal drying and mother
Liquid applies mechanically step, completes the DL-phenylalanine production technology；It is as follows：
（1）Racemization：Be added in clean reaction kettle 1322kgL- phenylalanines, 21.15kg salicylides, 13.22kg sodium hydrosulfites and
2644kg methanol, is warming up to 40-50 DEG C, after insulation reaction 5h, surveys the content of DL-phenylalanine；
（2）Centrifugal drying：Above-mentioned DL-phenylalanine content is cooled to 20 DEG C more than 98% postcooling, filters, centrifugation, mother liquid obtained
It is applied mechanically for racemization, gained filter cake is dried after being washed with 60kg methanol, solution racemization together with mother liquor after gained washing
It applies mechanically；
（3）Mother liquid recycle：The above-mentioned mother liquors of 3172.8kg, 1057.6kgL- phenylalanines, 13.22kg salicylides, 2.64kg is taken to protect
Dangerous powder repeats above-mentioned processing step, recycles, complete the production technology of the DL-phenylalanine.
Embodiment 3
A kind of DL-phenylalanine production technology of mother liquor recoverable, it is characterised in that：By racemization, centrifugal drying and mother
Liquid applies mechanically step, completes the DL-phenylalanine production technology；It is as follows：
（1）Racemization：Be added in clean reaction kettle 794kgL- phenylalanines, 12.7kg salicylides, 7.94kg sodium hydrosulfites and
1588kg methanol, is warming up to 40-50 DEG C, after insulation reaction 5h, surveys the content of DL-phenylalanine；
（2）Centrifugal drying：Above-mentioned DL-phenylalanine content is cooled to 20 DEG C more than 98% postcooling, filters, centrifugation, mother liquid obtained
It is applied mechanically for racemization, gained filter cake is dried after being washed with 60kg methanol, solution racemization together with mother liquor after gained washing
It applies mechanically；
（3）Mother liquid recycle：Take the above-mentioned mother liquors of 1905.6kg, 635.2KgL- phenylalanines, 7.94kg salicylides, 1.59kg insurances
Powder repeats above-mentioned processing step, recycles, complete the production technology of the DL-phenylalanine.
Physical and chemical index by the DL-phenylalanine obtained by embodiment 1-3 is as shown in table 1.
The physical and chemical index table of table 1DL- phenylalanines
Note：Appearance is tested with eyesight；Specific rotatory power GB/T613-2007 standard tests；Acidity presses GB5009.237-2016 standards
It measures chloride content and presses GB/9729-2007 standard tests；Amounts of ammonium salt presses GB5009.234-2016 standard tests；Sulfate
Content presses GBT9728-2007 standard tests；Content of beary metal presses GB 31604.9-2016 standard tests；Molysite content presses GB/
T4324.6-2012 standard tests；Arsenic salt content presses GB5009.11-2014 standard tests；Loss on drying rate presses DB13T1236-
1010 standard tests；Residue on ignition presses GB 31604.6-2016 standard tests；Cadmium content is surveyed by GB5009.15-2014 standards
It is fixed；Mercury content presses GB5009.17-2014 standard tests.
As shown in Table 1, in the DL-phenylalanine product obtained by embodiment 1-3, the content of DL-phenylalanine is higher reachable
99% or more, chloride, sulfate, heavy metal, molysite, arsenic, cadmium, the content of mercury are less in product, it is dry after product weightlessness
Rate is relatively low, and DL-phenylalanine stable quality, content is higher, is suitable for mass producing.
Above-described embodiment is presently preferred embodiments of the present invention, is not the limitation to technical solution of the present invention, as long as
Without the technical solution that creative work can be realized on the basis of the above embodiments, it is regarded as falling into patent of the present invention
Rights protection scope in.
Claims (4)
1. a kind of DL-phenylalanine production technology of mother liquor recoverable, it is characterised in that：By racemization, centrifugal drying and
Mother liquid recycle step completes the DL-phenylalanine production technology；It is described to be as follows：
（1）Racemization：L-phenylalanine, salicylide, sodium hydrosulfite and methanol is added by a certain percentage in clean reaction kettle, is warming up to
40-50 DEG C, after insulation reaction 5h, survey the content of DL-phenylalanine；
（2）Centrifugal drying：Above-mentioned DL-phenylalanine content is cooled to 20 DEG C more than 98% postcooling, filters, centrifugation, mother liquid obtained
It is applied mechanically for racemization, gained filter cake is dried after being washed with methanol, and the racemization together with mother liquor of the solution after gained washing is applied mechanically；
（3）Mother liquid recycle：It takes above-mentioned racemization to apply mechanically mother liquor and L-phenylalanine, salicylide, sodium hydrosulfite is added by a certain percentage, repeat
Above-mentioned processing step, recycles, and completes the production technology of the DL-phenylalanine.
2. a kind of DL-phenylalanine production technology of mother liquor recoverable according to claim 1, it is characterised in that：
The step（1）Middle L-phenylalanine：Salicylide：Sodium hydrosulfite：Methanol is 5:0.08:0.05:10.
3. a kind of DL-phenylalanine production technology of mother liquor recoverable according to claim 1, it is characterised in that：
The step（2）Middle methanol usage is 60Kg.
4. a kind of DL-phenylalanine production technology of mother liquor recoverable according to claim 1, it is characterised in that：
The step（3）Middle mother liquor：L-phenylalanine：Salicylide：Sodium hydrosulfite is 12:4:0.05:0.01.
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| CN201710833232.9A CN108456145A (en) | 2017-09-15 | 2017-09-15 | A kind of DL-phenylalanine production technology of mother liquor recoverable |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4401820A (en) * | 1981-01-23 | 1983-08-30 | Tanabe Seiyaku Co., Ltd. | Process for racemizing optically active α-amino acids or a salt thereof |
| CN1418862A (en) * | 2002-11-22 | 2003-05-21 | 东南大学 | Method for preparing dextrorotary phenylalanine by asymmetric conversion method |
| CN1680282A (en) * | 2005-01-24 | 2005-10-12 | 南京大学 | Microwave racemization method of optically active amino acid or its salt |
| CN1839156A (en) * | 2003-08-21 | 2006-09-27 | 诺沃挪第克公司 | Isolation of polypeptides containing racemized amino acids |
| CN101289410A (en) * | 2008-06-06 | 2008-10-22 | 山东奥克特化工有限公司 | A kind of preparation method of D-phenylalanine |
| CN101863818A (en) * | 2010-06-30 | 2010-10-20 | 宜兴市前成生物有限公司 | Method for preparing DL-proline |
| CN106187799A (en) * | 2016-06-30 | 2016-12-07 | 宜兴市前成生物有限公司 | A kind of method preparing DL lysine hydrochloride |
-
2017
- 2017-09-15 CN CN201710833232.9A patent/CN108456145A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4401820A (en) * | 1981-01-23 | 1983-08-30 | Tanabe Seiyaku Co., Ltd. | Process for racemizing optically active α-amino acids or a salt thereof |
| CN1418862A (en) * | 2002-11-22 | 2003-05-21 | 东南大学 | Method for preparing dextrorotary phenylalanine by asymmetric conversion method |
| CN1839156A (en) * | 2003-08-21 | 2006-09-27 | 诺沃挪第克公司 | Isolation of polypeptides containing racemized amino acids |
| CN1680282A (en) * | 2005-01-24 | 2005-10-12 | 南京大学 | Microwave racemization method of optically active amino acid or its salt |
| CN101289410A (en) * | 2008-06-06 | 2008-10-22 | 山东奥克特化工有限公司 | A kind of preparation method of D-phenylalanine |
| CN101863818A (en) * | 2010-06-30 | 2010-10-20 | 宜兴市前成生物有限公司 | Method for preparing DL-proline |
| CN106187799A (en) * | 2016-06-30 | 2016-12-07 | 宜兴市前成生物有限公司 | A kind of method preparing DL lysine hydrochloride |
Non-Patent Citations (1)
| Title |
|---|
| 唐玲: "一种氨基酸衍生物消旋的新方法", 《合成化学》 * |
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Application publication date: 20180828 |