CN105732662A - Process for recovering 6-APA and salt from 6-APA mother liquor - Google Patents
Process for recovering 6-APA and salt from 6-APA mother liquor Download PDFInfo
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- CN105732662A CN105732662A CN201610129123.4A CN201610129123A CN105732662A CN 105732662 A CN105732662 A CN 105732662A CN 201610129123 A CN201610129123 A CN 201610129123A CN 105732662 A CN105732662 A CN 105732662A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D499/00—Heterocyclic compounds containing 4-thia-1-azabicyclo [3.2.0] heptane ring systems, i.e. compounds containing a ring system of the formula:, e.g. penicillins, penems; Such ring systems being further condensed, e.g. 2,3-condensed with an oxygen-, nitrogen- or sulfur-containing hetero ring
- C07D499/21—Heterocyclic compounds containing 4-thia-1-azabicyclo [3.2.0] heptane ring systems, i.e. compounds containing a ring system of the formula:, e.g. penicillins, penems; Such ring systems being further condensed, e.g. 2,3-condensed with an oxygen-, nitrogen- or sulfur-containing hetero ring with a nitrogen atom directly attached in position 6 and a carbon atom having three bonds to hetero atoms with at the most one bond to halogen, e.g. an ester or nitrile radical, directly attached in position 2
- C07D499/42—Compounds with a free primary amino radical attached in position 6
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/16—Halides of ammonium
- C01C1/164—Ammonium chloride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D499/00—Heterocyclic compounds containing 4-thia-1-azabicyclo [3.2.0] heptane ring systems, i.e. compounds containing a ring system of the formula:, e.g. penicillins, penems; Such ring systems being further condensed, e.g. 2,3-condensed with an oxygen-, nitrogen- or sulfur-containing hetero ring
- C07D499/04—Preparation
- C07D499/18—Separation; Purification
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- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention relates to a method for recovering 6-APA and salt from a 6-APA mother liquor, belongs to the technical field of pharmaceuticals. The process comprises the following steps: using a nanofiltration membrane for concentrating the 6-APA mother liquor; recovering 6-APA from a nanofiltration concentrate; recovering ammonium chloride or sodium chloride from a 6-APA nanofiltration dialyzate; meanwhile, recovering condensation water in an evaporative crystallization process. Compared with the prior art, the invention has the advantages that 6-APA and sodium chloride or ammonium chloride are recovered from the 6-APA mother liquor, steam condensation water of feed liquid is obtained while evaporating the recovered salt, the condensation water can be recycled into the workshop, to achieve the resource utilization of 6-APA mother liquor.
Description
Technical field
The present invention relates to a kind of method reclaiming 6-APA and salt, particularly relate to a kind of reclaim from 6-APA mother solution 6-APA and
The method of salt, belongs to pharmaceutical technology field.
Background technology
The method preparing 6-APA has chemical cleavage method and catalyzed by biological enzyme.The process route of chemical cracking is: extremely low
Under temperature conditions, first the carboxyl of penicillin is transformed into estersil and protects, then make the amide on side chain activate, by being formed
Penicillin substituted imine ether derivant, then under conditions of extremely gentleness, selective hydrolysis obtains 6-APA.Enzyme is urged
Change method is with penicillin as raw material, and under the effect of PA ase, penicillin is cracked into 6-APA and phenylacetic acid.Pass through
6-APA is separated by solvent extraction with phenylacetic acid, then by crystallizing, washing and be dried to obtain 6-APA.Chemical method reaction bar
Part is harsh, produces the intractable organic wastewater with high concentration of environmental protection simultaneously, and therefore, chemical method is replaced by enzyme process substantially.
Containing a certain amount of 6-APA in 6-APA mother solution, if by this direct discharging of waste water, on the one hand make waste discharge
COD is higher, on the other hand causes the waste of resource.Patent CN101041663A reports and reclaims crystalline mother solution with nanofiltration
The method of middle 6-APA, first the pH of regulation 6-APA crystalline mother solution is 5.0-8.5, then coarse filtration, carries out nanofiltration afterwards,
Cycles of concentration is 5-20 times, obtains nanofiltration concentrated solution and nanofiltration dialysis solution.Concentrated solution through methyl iso-butyl ketone (MIBK) extract, crystallization,
Sucking filtration and dry prepared 6-APA finished product.Although this patent has been reported for work and reclaimed the 6-APA in mother solution by NF membrane, but to dialysis
The recovery of the salt in liquid is not reported.
Summary of the invention
The present invention, on the basis of above research, has reclaimed 6-APA, salt and condensed water from 6-APA mother solution, has not had 6-APA
The discharge of crystalline mother solution, alleviates environmental protection pressure.In order to realize the object of the invention, the technical scheme is that and use NF membrane
6-APA mother solution is concentrated, from nanofiltration concentrated solution, reclaims 6-APA, from 6-APA nanofiltration dialysis solution, reclaim ammonium chloride
(or sodium chloride), reclaims condensed water in evaporation and crystal process simultaneously.
A kind of recovery 6-APA and technique of salt from 6-APA mother solution that the present invention provides, comprises the steps:
(1) removing of solvent in 6-APA mother solution
By the solvent in decompression distillation removing 6-APA mother solution, feed temperature controls at 30-50 DEG C, vacuum >=0.085MPa,
Sampling and measuring solvent residual in subtractive process, as content of acetone≤50ppm in 6-APA mother solution, levels of n-butanol≤200ppm,
When n-butyl acetate content≤200ppm, the content≤10ppm of methyl iso-butyl ketone (MIBK), stop decompression distillation；
(2) regulation of 6-APA mother solution pH
6-APA mother solution after above-mentioned removing solvent is lowered the temperature, when temperature reduces to 10 DEG C, in this mother solution, adds 30% hydrogen-oxygen
Changing sodium solution (or 20% ammonia), the pH of regulation feed liquid is 6.5-7.0；
(3) nanofiltration of 6-APA mother solution concentrates
Above-mentioned 6-APA mother solution, through the cartridge filter of 5 μm, processes subsequently into one-level nanofiltration, and one-level nanofiltration dialysis solution enters
Entering to nanofiltration dialysis solution storage tank, one-level nanofiltration concentrated solution enters into two grades of nanofiltrations and processes, and two grades of nanofiltration dialysis solution enter into nanofiltration
Dialysis solution storage tank, two grades of nanofiltration concentrated solutions carry out processing into three grades of nanofiltrations, and three grades of nanofiltration dialysis solution enter into dialysis solution storage tank,
Three grades of nanofiltration concentrated solutions carry out the recovery of follow-up 6-APA；Control during 6-APA mother solution being concentrated by NF membrane
Feed temperature is 5-10 DEG C, enters film pressure≤2.5MPa, and cycles of concentration is 8-10 times, and the molecular cut off of NF membrane is 200；
(4) from concentrated solution, 6-APA is reclaimed
Take above-mentioned three grades of nanofiltration concentrated solutions, lower the temperature in ice-water bath so that it is temperature≤8 DEG C, be subsequently adding methyl iso-butyl ketone (MIBK),
Dosage is the 1/3-1/2 of nanofiltration concentrated solution volume, under stirring, adds the hydrochloric acid of 20-30% in this feed liquid, controls the pH of feed liquid
For 0.8-1.5；Then this feed liquid is poured into standing split-phase in separatory funnel, separates lower floor's aqueous phase；This aqueous phase is placed in ice-water bath
In, controlling feed temperature≤8 DEG C, be subsequently adding activated carbon and decolour, activated carbon dosage is 1-5 ‰, stirs 15-30min,
Sucking filtration；Filtrate is placed in ice-water bath, under stirring, is added thereto to 15-30% sodium hydroxide solution (or 10-20% ammonia),
The pH of feed liquid is adjusted to 3.8-4.2, growing the grain 90min, sucking filtration, washs with purified water and acetone respectively；By gained 6-APA
Wet-milling is placed in vacuum drying oven and is dried, and baking temperature is 40-60 DEG C, vacuum >=0.085MPa, and dry end obtains
6-APA dry powder.
(5) salt is reclaimed in the evaporation of dialysis solution
6-APA mother solution nanofiltration dialysis solution is carried out decompression distillation, controls feed temperature and be 40-80 DEG C, vacuum >=0.085MPa,
Stop distillation when feed liquid occurs crystal, concentrated solution is cooled down in ice-water bath 60-90min, sucking filtration, obtains solid chlorine
Ammonium (or sodium chloride).
The method of a kind of effective process 6-APA mother solution of the present invention, due in 6-APA crystalline mother solution containing a small amount of molten
Matchmaker, in order to reduce the solvent infringement to NF membrane, with before nanofiltration membrane treatment 6-APA mother solution, this mother solution first must remove solvent；
Due to 6-APA less stable at high temperature, in order to reduce the degraded of 6-APA, improve the quality reclaiming 6-APA product,
So selecting removed under reduced pressure solvent at a lower temperature；In order to prevent the precipitation of 6-APA in nanofiltration concentration process, so
The pH of feed liquid is adjusted to 6.5-7.0, increases 6-APA dissolubility in water；Feed temperature is controlled in nanofiltration concentration process
For 5-10 DEG C, prevent under higher temperature conditions, the degraded of 6-APA；Along with the carrying out concentrated, 6-APA in nanofiltration concentrated solution
All increase with the concentration of phenylacetic acid, so the phenylacetic acid in concentrated solution and 6-APA being separated by solvent extraction；To extraction
Aqueous phase activated carbon decolorizing after taking, goes the removal of impurity further, then crystallization, sucking filtration, wash and be dried to obtain 6-APA and do
Powder, the secondary mother liquid of gained returns to front end circular treatment；In order to be recovered to, from 6-APA nanofiltration dialysis solution, the salt that composition is single,
Single bronsted lowry acids and bases bronsted lowry is used in the preparation process from filtrate to 6-APA.Butyl acetate containing penicillin is alkalized
Shi Suoyong alkali be ammonia, lysate extraction process used by acid alkali for hydrochloric acid, 6-APA crystallization process used by be ammonia, regulate
Alkali used by mother solution pH is ammonia, then the salt reclaimed 6-APA nanofiltration dialysis solution by evaporative crystallization is ammonium chloride；If
By above-mentioned used during alkali replace with sodium hydroxide, then salt 6-APA nanofiltration dialysis solution reclaimed by evaporative crystallization
For sodium chloride.The condensed water produced in evaporation process can be back to use workshop.
Compared with prior art, it is an advantage of the current invention that: from 6-APA mother solution, reclaimed 6-APA, sodium chloride or chlorine
Changing ammonium, while reclaiming salt by evaporation, obtained the steam condensation water of feed liquid simultaneously, this solidifying water can be back to use workshop, real
Show the recycling of 6-APA mother solution.
Accompanying drawing explanation
Fig. 1 is to reclaim 6-APA and the technological process of salt from 6-APA mother solution.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in further detail.
Embodiment 1
RBA (the butyl acetate phase containing penicillin after activated carbon decolorizing and washing), splits alkalization, the cracking of penicillin
Used in the process of the regulation of the solution extraction of liquid, the crystallization of 6-APA and 6-APA mother solution pH, alkali is ammonia, and acid used is hydrochloric acid.
(1) removing of solvent in 6-APA mother solution
By the solvent in decompression distillation removing 6-APA mother solution, feed temperature is 45 DEG C, and vacuum is 0.087MPa, de-
After solvent, in 6-APA mother solution the content of acetone, n-butyl alcohol, n-butyl acetate and methyl iso-butyl ketone (MIBK) be respectively 30,85,
96 and 5ppm.
(2) regulation of 6-APA mother solution pH
6-APA mother solution after above-mentioned removing solvent is lowered the temperature, when temperature reduces to 10 DEG C, adds or 20% ammonia in this mother solution
Water, the pH of regulation feed liquid is 6.8.
(3) nanofiltration of 6-APA mother solution concentrates
6-APA mother solution after above-mentioned regulation pH is processed through cartridge filter, is then the nanofiltration of 200 with molecular cut off
Film concentrates, and feed temperature is 9 DEG C, and entering film pressure is 2.2MPa, and cycles of concentration is 10 times, 6-APA in 6-APA mother solution
Concentration is 2.8g/L, and phenylacetic acid concentration is 1.1g/L, and in final concentrated solution, 6-APA concentration is 26.9g/L, and phenylacetic acid concentration is
11.2g/L。
(4) from concentrated solution, 6-APA is reclaimed
Take above-mentioned 6-APA mother solution nanofiltration concentrated solution 1L, lower the temperature in ice-water bath, when temperature is less than 8 DEG C, be added thereto to
500mL methyl iso-butyl ketone (MIBK), under stirring, is added thereto to 30% hydrochloric acid, and the pH making feed liquid is 1.0, this feed liquid is poured into
Standing split-phase in separatory funnel, separate lower floor's aqueous phase, aqueous phase volume is 1100mL.This aqueous phase is placed in ice-water bath, then
Add 3.3g activated carbon, stir 30min, sucking filtration.This filtrate is placed in ice-water bath, under stirring, adds 20% ammonia,
The pH of feed liquid is adjusted to 4.0, growing the grain 90min, sucking filtration, washs with purified water and acetone, respectively by gained 6-APA
Wet-milling is vacuum dried, and baking temperature is 60 DEG C, and vacuum is 0.089MPa, obtains 6-APA dry powder 16.7g, yield
It is 62%.The product quality of gained 6-APA is shown in Table 1.
Table 1 reclaims the product quality of 6-APA from 6-APA mother solution
From data in table 1, the 6-APA reclaimed from 6-APA mother solution by above-mentioned technique, its product quality meets
Top grade product standard, can reclaim the 6-APA of qualified product from 6-APA mother solution by this technique.
(5) salt is reclaimed in the evaporation of dialysis solution
Taking 6-APA mother solution nanofiltration dialysis solution 1.5L, carry out decompression distillation, control feed temperature and be 40-70 DEG C, vacuum is
0.090MPa, stops distillation, obtains feed liquid and coagulate water 1330mL, be placed in ice-water bath by concentrated solution when occurring crystal in feed liquid
Cooling 60min, sucking filtration, obtain solid ammonium chloride, content is 99.6%.Feed liquid is coagulated the water quality data of water and is shown in Table 2.
Table 2 6-APA mother solution nanofiltration dialysis solution distillation feed liquid coagulates water water quality data
From data in table 2, after the distillation of 6-APA mother solution nanofiltration dialysis solution, the feed liquid of gained coagulates water, its electrical conductivity, chlorine from
Son is relatively low, can use to workshop as a Water circulation.
Embodiment 2
RBA (the butyl acetate phase containing penicillin after activated carbon decolorizing and washing), splits alkalization, the cracking of penicillin
Used in the process of the regulation of the solution extraction of liquid, the crystallization of 6-APA and 6-APA mother solution pH, alkali is sodium hydroxide, and acid used is
Hydrochloric acid.
(1) removing of solvent in 6-APA mother solution
By the solvent in decompression distillation removing 6-APA mother solution, feed temperature is 48 DEG C, and vacuum is 0.088MPa, de-
After solvent, in 6-APA mother solution the content of acetone, n-butyl alcohol, n-butyl acetate and methyl iso-butyl ketone (MIBK) be respectively 32,87,
85 and 5ppm.
(2) regulation of 6-APA mother solution pH
6-APA mother solution after above-mentioned removing solvent is lowered the temperature, when temperature reduces to 10 DEG C, in this mother solution, adds 30% hydrogen-oxygen
Changing sodium solution, the pH of regulation feed liquid is 6.5.
(3) nanofiltration of 6-APA mother solution concentrates
6-APA mother solution after above-mentioned regulation pH is processed through cartridge filter, is then the nanofiltration of 200 with molecular cut off
Film concentrates, and feed temperature is 9 DEG C, and entering film pressure is 2.2MPa, and cycles of concentration is 10 times, 6-APA in 6-APA mother solution
Concentration is 2.5g/L, and phenylacetic acid concentration is 1.3g/L, and in final concentrated solution, 6-APA concentration is 24.2g/L, and phenylacetic acid concentration is
13.2g/L。
(4) from concentrated solution, 6-APA is reclaimed
Take above-mentioned 6-APA mother solution nanofiltration concentrated solution 1L, lower the temperature in ice-water bath, when temperature is less than 8 DEG C, be added thereto to
500mL methyl iso-butyl ketone (MIBK), under stirring, is added thereto to 30% hydrochloric acid, and the pH making feed liquid is 0.9, this feed liquid is poured into
Standing split-phase in separatory funnel, separate lower floor's aqueous phase, aqueous phase volume is 1050mL.This aqueous phase is placed in ice-water bath, then
Add 3.5g activated carbon, stir 30min, sucking filtration.This filtrate is placed in ice-water bath, under stirring, adds 30% hydroxide
Sodium solution, is adjusted to 4.0 by the pH of feed liquid, growing the grain 90min, and sucking filtration washs with purified water and acetone, respectively by institute
Obtaining 6-APA wet-milling to be vacuum dried, baking temperature is 60 DEG C, and vacuum is 0.089MPa, obtains 6-APA dry powder 14.5g,
Yield is 60%.The product quality of gained 6-APA is shown in Table 3.
Table 3 reclaims the product quality of 6-APA from 6-APA mother solution
From data in table 3, the 6-APA reclaimed from 6-APA mother solution by above-mentioned technique, specific optical rotation, moisture,
Absorbance and acidity all meet top grade product standard, and content meets inner quality standard.Can reclaim from 6-APA mother solution by this technique
The 6-APA of qualified product.
(5) salt is reclaimed in the evaporation of dialysis solution
Taking 6-APA mother solution nanofiltration dialysis solution 1.5L, carry out decompression distillation, control feed temperature and be 40-70 DEG C, vacuum is
0.087MPa, stops distillation, obtains feed liquid and coagulate water 1320mL, be placed in ice-water bath by concentrated solution when occurring crystal in feed liquid
Cooling 60min, sucking filtration, obtain solid sodium chloride, content is 99.6%.Feed liquid is coagulated the water quality data of water and is shown in Table 4.
Table 4 6-APA mother solution nanofiltration dialysis solution distillation feed liquid coagulates water water quality data
From data in table 4, after the distillation of 6-APA mother solution nanofiltration dialysis solution, the feed liquid of gained coagulates water, its electrical conductivity, chlorine from
Son is relatively low, can use to workshop as a Water circulation.
Below it is only the preferred embodiment of the present invention, not in order to limit the present invention, to those skilled in the art,
Under the premise without departing from the principles of the invention, it is also possible to some improvement of making, retouching, equivalent, should be included in this
Within the protection domain of invention.
Claims (2)
1. reclaiming 6-APA and a technique for salt from 6-APA mother solution, it includes carrying out dense by NF membrane to 6-APA mother solution
Contracting, reclaims 6-APA from nanofiltration concentrated solution, reclaims ammonium chloride or sodium chloride, simultaneously in evaporation from 6-APA nanofiltration dialysis solution
Crystallization process reclaims the step of condensed water.
A kind of recovery 6-APA and technique of salt from 6-APA mother solution the most according to claim 1, it is characterised in that
Comprise the steps:
(1) removing of solvent in 6-APA mother solution
By the solvent in decompression distillation removing 6-APA mother solution, feed temperature controls at 30-50 DEG C, vacuum >=0.085MPa,
Sampling and measuring solvent residual in subtractive process, when content of acetone≤50ppm in 6-APA mother solution, levels of n-butanol≤200ppm, second
During acid N-butyl content≤200ppm, the content≤10ppm of methyl iso-butyl ketone (MIBK), stop decompression distillation；
(2) regulation of 6-APA mother solution pH
6-APA mother solution after above-mentioned removing solvent is lowered the temperature, when temperature reduces to 10 DEG C, in this mother solution, adds 30% hydroxide
Sodium solution (or 20% ammonia), the pH of regulation feed liquid is 6.5-7.0；
(3) nanofiltration of 6-APA mother solution concentrates
Above-mentioned 6-APA mother solution, through the cartridge filter of 5 μm, processes subsequently into one-level nanofiltration, and one-level nanofiltration dialysis solution enters
To nanofiltration dialysis solution storage tank, one-level nanofiltration concentrated solution enters into two grades of nanofiltrations and processes, and two grades of nanofiltration dialysis solution enter into nanofiltration dialysis
Liquid storage tank, two grades of nanofiltration concentrated solutions carry out processing into three grades of nanofiltrations, and three grades of nanofiltration dialysis solution enter into dialysis solution storage tank, three grades
Nanofiltration concentrated solution carries out the recovery of follow-up 6-APA；Feed liquid temperature is controlled during 6-APA mother solution being concentrated by NF membrane
Degree, for 5-10 DEG C, enters film pressure≤2.5MPa, and cycles of concentration is 8-10 times, and the molecular cut off of NF membrane is 200；
(4) from concentrated solution, 6-APA is reclaimed
Take above-mentioned three grades of nanofiltration concentrated solutions, lower the temperature in ice-water bath so that it is temperature≤8 DEG C, be subsequently adding methyl iso-butyl ketone (MIBK), add
Amount is the 1/3-1/2 of nanofiltration concentrated solution volume, under stirring, adds the hydrochloric acid of 20-30% in this feed liquid, and the pH controlling feed liquid is
0.8-1.5；Then this feed liquid is poured into standing split-phase in separatory funnel, separates lower floor's aqueous phase；This aqueous phase is placed in ice-water bath,
Controlling feed temperature≤8 DEG C, be subsequently adding activated carbon and decolour, activated carbon dosage is 1-5 ‰, stirs 15-30min, sucking filtration；
Filtrate is placed in ice-water bath, under stirring, is added thereto to 15-30% sodium hydroxide solution (or 10-20% ammonia), will material
The pH of liquid is adjusted to 3.8-4.2, growing the grain 90min, sucking filtration, washs with purified water and acetone respectively；By wet for gained 6-APA
Powder is placed in vacuum drying oven and is dried, and baking temperature is 40-60 DEG C, vacuum >=0.085MPa, and dry end obtains 6-APA
Dry powder；
(5) salt is reclaimed in the evaporation of dialysis solution
6-APA mother solution nanofiltration dialysis solution is carried out decompression distillation, controls feed temperature and be 40-80 DEG C, vacuum >=0.085MPa,
Stop distillation when feed liquid occurs crystal, concentrated solution is cooled down in ice-water bath 60-90min, sucking filtration, obtains solid ammonium chloride
Or sodium chloride.
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| CN201610129123.4A CN105732662B (en) | 2016-03-07 | 2016-03-07 | A kind of technique that 6 APA and salt are reclaimed from 6 APA mother liquors |
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| CN201610129123.4A CN105732662B (en) | 2016-03-07 | 2016-03-07 | A kind of technique that 6 APA and salt are reclaimed from 6 APA mother liquors |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108218893A (en) * | 2017-12-18 | 2018-06-29 | 伊犁川宁生物技术有限公司 | A kind of method that 6-APA is recycled in the crystalline mother solution from 6-APA |
| CN108658757A (en) * | 2018-05-11 | 2018-10-16 | 国药集团大同威奇达中抗制药有限公司 | The recovery method of phenylacetic acid in 6-amino-penicillanic acid enzyme process aqueous solution |
| CN109553627A (en) * | 2017-09-25 | 2019-04-02 | 联邦制药(内蒙古)有限公司 | A kind of recovery method of improved 7-ACA crystalline mother solution |
| CN111662307A (en) * | 2019-03-08 | 2020-09-15 | 伊犁川宁生物技术有限公司 | Method for desalting and recycling 6-APA mother liquor dialysate |
| CN113072566A (en) * | 2021-03-03 | 2021-07-06 | 内蒙古常盛制药有限公司 | Process for recovering 6-APA and salt from 6-APA mother liquor by two-stage membrane method |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109553627A (en) * | 2017-09-25 | 2019-04-02 | 联邦制药(内蒙古)有限公司 | A kind of recovery method of improved 7-ACA crystalline mother solution |
| CN108218893A (en) * | 2017-12-18 | 2018-06-29 | 伊犁川宁生物技术有限公司 | A kind of method that 6-APA is recycled in the crystalline mother solution from 6-APA |
| CN108218893B (en) * | 2017-12-18 | 2021-02-23 | 伊犁川宁生物技术有限公司 | Method for recovering 6-APA from 6-APA crystallization mother liquor |
| CN108658757A (en) * | 2018-05-11 | 2018-10-16 | 国药集团大同威奇达中抗制药有限公司 | The recovery method of phenylacetic acid in 6-amino-penicillanic acid enzyme process aqueous solution |
| CN108658757B (en) * | 2018-05-11 | 2020-11-06 | 国药集团威奇达药业有限公司 | Method for recovering phenylacetic acid from 6-aminopenicillanic acid enzymatic aqueous solution |
| CN111662307A (en) * | 2019-03-08 | 2020-09-15 | 伊犁川宁生物技术有限公司 | Method for desalting and recycling 6-APA mother liquor dialysate |
| CN113072566A (en) * | 2021-03-03 | 2021-07-06 | 内蒙古常盛制药有限公司 | Process for recovering 6-APA and salt from 6-APA mother liquor by two-stage membrane method |
| CN113072566B (en) * | 2021-03-03 | 2023-08-01 | 内蒙古常盛制药有限公司 | Process for recovering 6-APA and salt from 6-APA mother liquor by two-stage membrane method |
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