CN105732662B - A kind of technique that 6 APA and salt are reclaimed from 6 APA mother liquors - Google Patents
A kind of technique that 6 APA and salt are reclaimed from 6 APA mother liquors Download PDFInfo
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- CN105732662B CN105732662B CN201610129123.4A CN201610129123A CN105732662B CN 105732662 B CN105732662 B CN 105732662B CN 201610129123 A CN201610129123 A CN 201610129123A CN 105732662 B CN105732662 B CN 105732662B
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- apa
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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
-
- 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
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- 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 present invention relates to a kind of method that 6 APA and salt are reclaimed from 6 APA mother liquors, belong to pharmaceutical technology field.The technique includes concentrating 6 APA mother liquors with NF membrane, and 6 APA are reclaimed from nanofiltration concentrate, and ammonium chloride or sodium chloride are reclaimed from 6 APA nanofiltration dislysates, while in evaporation and crystal process the step of recovery condensed water.Compared with prior art, the advantage of the invention is that：While 6 APA, sodium chloride or ammonium chloride have been reclaimed from 6 APA mother liquors, while salt is reclaimed by evaporating, the steam condensation water of feed liquid is obtained, the condensate can be back to use workshop, realize the recycling of 6 APA mother liquors.
Description
Technical field
The present invention relates to a kind of recovery 6-APA and salt method, more particularly to one kind to reclaim 6-APA from 6-APA mother liquors
With the method for salt, belong to pharmaceutical technology field.
Background technology
The method for preparing 6-APA has chemical cleavage method and catalyzed by biological enzyme.The process route of chemical cracking is：Extremely low
Temperature conditionss under, the carboxyl of penicillin be first transformed into estersil and protected, then activate the acid amides on side chain, pass through to be formed
Penicillin substituted imine ether derivant, then under conditions of extremely gently, selective hydrolysis obtains 6-APA.Biological enzyme
Method is using penicillin as raw material, and in the presence of PA ase, penicillin is cracked into 6-APA and phenylacetic acid.Pass through solvent
Extraction separates 6-APA and phenylacetic acid, then by crystallizing, washing and be dried to obtain 6-APA.Chemical method severe reaction conditions,
The intractable organic wastewater with high concentration of environmental protection is produced simultaneously, and therefore, chemical method is substituted by enzyme process substantially.
Contain a certain amount of 6-APA in 6-APA mother liquors, if by the direct discharging of waste water, on the one hand cause waste discharge
COD it is higher, on the other hand cause the waste of resource.Patent CN101041663A reports to be reclaimed in crystalline mother solution with nanofiltration
6-APA method, the pH for adjusting 6-APA crystalline mother solutions first are 5.0-8.5, then coarse filtration, carry out nanofiltration, concentration times afterwards
Number is 5-20 times, obtains nanofiltration concentrate and nanofiltration dislysate.Concentrate is extracted through methyl iso-butyl ketone (MIBK), crystallizes, filters and done
Dry obtained 6-APA finished products.Although the patent has been reported for work the 6-APA reclaimed with NF membrane in mother liquor, but to the salt in dialyzate
Recovery is not reported.
The content of the invention
On the basis of the present invention studies more than, 6-APA, salt and condensed water are reclaimed from 6-APA mother liquors, without 6-
The discharge of APA crystalline mother solutions, alleviates environmental protection pressure.In order to realize the object of the invention, the technical scheme is that using nanofiltration
Film is concentrated to 6-APA mother liquors, and 6-APA is reclaimed from nanofiltration concentrate, and ammonium chloride is reclaimed from 6-APA nanofiltration dislysates
(or sodium chloride), while condensed water is reclaimed in evaporation and crystal process.
The technique that 6-APA and salt are reclaimed in a kind of mother liquor from 6-APA provided by the invention, comprises the following steps：
(1) in 6-APA mother liquors solvent removing
By being evaporated under reduced pressure the solvent removed in 6-APA mother liquors, feed temperature control at 30-50 DEG C, vacuum >=
0.085MPa, solvent residual is measured by sampling in subtractive process, as content of acetone≤50ppm in 6-APA mother liquors, levels of n-butanol≤
200ppm, n-butyl acetate content≤200ppm, during content≤10ppm of methyl iso-butyl ketone (MIBK), stop being evaporated under reduced pressure；
(2) 6-APA mother liquors pH regulation
6-APA mother liquors after above-mentioned removing solvent are cooled, when temperature is reduced to 10 DEG C, 30% hydrogen is added into the mother liquor
Sodium hydroxide solution (or 20% ammoniacal liquor), the pH for adjusting feed liquid are 6.5-7.0；
(3) the nanofiltration concentration of 6-APA mother liquors
Above-mentioned 6-APA mother liquors pass through 5 μm of cartridge filter, are handled subsequently into one-level nanofiltration, one-level nanofiltration dislysate
Nanofiltration dislysate storage tank is entered, one-level nanofiltration concentrate enters two level nanofiltration processing, and two level nanofiltration dislysate, which enters, to be received
Filter dialysis liquid storage tank, two level nanofiltration concentrate, which is entered to three-level nanofiltration, to be handled, and three-level nanofiltration dislysate enters dialyzate storage
Tank, three-level nanofiltration concentrate carry out follow-up 6-APA recovery；Controlled during being concentrated with NF membrane to 6-APA mother liquors
Feed temperature processed 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) 6-APA is reclaimed from concentrate
Above-mentioned three-level nanofiltration concentrate is taken, is cooled in ice-water bath, makes its temperature≤8 DEG C, then adds methyl-isobutyl
Ketone, dosage is the 1/3-1/2 of nanofiltration concentrate volume, and under stirring, 20-30% hydrochloric acid is added into the feed liquid, controls feed liquid
PH be 0.8-1.5；Then the feed liquid is poured into and split-phase is stood in separatory funnel, separate lower floor's aqueous phase；The aqueous phase is placed in ice
In water-bath, feed temperature≤8 DEG C are controlled, activated carbon is then added and is decolourized, activated carbon dosage is 1-5 ‰, stirs 15-
30min, filter；Filtrate is placed in ice-water bath, under stirring, adds 15-30% sodium hydroxide solutions (or 10- thereto
20% ammoniacal liquor), the pH of feed liquid is adjusted to 3.8-4.2, growing the grain 90min, filters, is washed respectively with purified water and acetone；Will
Gained 6-APA wet-millings, which are placed in vacuum drying chamber, to be dried, and drying temperature is 40-60 DEG C, vacuum >=0.085MPa, is dried
End obtains 6-APA dry powder.
(5) the evaporation recovery salt of dialyzate
6-APA mother liquor nanofiltration dislysates are evaporated under reduced pressure, it is 40-80 DEG C to control feed temperature, vacuum >=
0.085MPa, stop distillation when occurring crystal in feed liquid, concentrate is cooled down into 60-90min in ice-water bath, filter, obtain
Solid ammonium chloride (or sodium chloride).
The method of a kind of effectively processing 6-APA mother liquors of the present invention, due to containing on a small quantity in 6-APA crystalline mother solutions
Solvent, in order to reduce infringement of the solvent to NF membrane, before with nanofiltration membrane treatment 6-APA mother liquors, the mother liquor must first remove solvent；
Due to the less stables of 6-APA at high temperature, in order to reduce 6-APA degraded, the quality of recovery 6-APA products, institute are improved
To select removed under reduced pressure solvent at a lower temperature；In order to prevent the precipitation of the 6-APA in nanofiltration concentration process, so will material
The pH of liquid is adjusted to 6.5-7.0, solubility of the increase 6-APA in water；It is 5-10 that feed temperature is controlled in nanofiltration concentration process
DEG C, prevent under higher temperature conditions, 6-APA degraded；With the progress of concentration, 6-APA and phenylacetic acid in nanofiltration concentrate
Concentration increase, so the phenylacetic acid in concentrate and 6-APA are separated by solvent extraction；To the aqueous phase after extraction
With activated carbon decolorizing, further go the removal of impurity, then crystallize, filter, wash and be dried to obtain 6-APA dry powder, gained it is secondary
Mother liquor returns to front end circular treatment；In order to be recovered to the single salt of composition from 6-APA nanofiltration dislysates, from filtrate to 6-
Single bronsted lowry acids and bases bronsted lowry is used in APA preparation process.Alkali used is ammonia when being alkalized to the butyl acetate containing penicillin
Water, lysate extraction process used in acid be hydrochloric acid, alkali is ammoniacal liquor used in 6-APA crystallization process, alkali used in regulation mother liquor pH is
Ammoniacal liquor, the then salt reclaimed to 6-APA nanofiltration dislysates by evaporative crystallization are ammonium chloride；If by it is above-mentioned it is used during
Alkali replaces with sodium hydroxide, then the salt reclaimed to 6-APA nanofiltration dislysates by evaporative crystallization is sodium chloride.In evaporation process
In caused condensed water can be back to use workshop.
Compared with prior art, the advantage of the invention is that：6-APA, sodium chloride or chlorine have been reclaimed from 6-APA mother liquors
While changing ammonium, while salt is reclaimed by evaporating, the steam condensation water of feed liquid is obtained, the condensate can be back to use workshop, realize
The recyclings of 6-APA mother liquors.
Brief description of the drawings
Fig. 1 is the technological process that 6-APA and salt are reclaimed from 6-APA mother liquors.
Embodiment
The present invention is described in further detail with reference to embodiment.
Embodiment 1
RBA (the butyl acetate phase containing penicillin after activated carbon decolorizing and washing) alkalization, cracking of penicillin, split
Alkali is ammoniacal liquor used in the process of solving extraction, 6-APA crystallization and the 6-APA mother liquors pH regulation of liquid, and acid used is hydrochloric acid.
(1) in 6-APA mother liquors solvent removing
By being evaporated under reduced pressure the solvent removed in 6-APA mother liquors, feed temperature is 45 DEG C, vacuum 0.087MPa, is taken off
After solvent, acetone in 6-APA mother liquors, n-butanol, the content of n-butyl acetate and methyl iso-butyl ketone (MIBK) are respectively 30,85,96
And 5ppm.
(2) 6-APA mother liquors pH regulation
6-APA mother liquors after above-mentioned removing solvent are cooled, when temperature is reduced to 10 DEG C, the addition or 20% into the mother liquor
Ammoniacal liquor, the pH for adjusting feed liquid are 6.8.
(3) the nanofiltration concentration of 6-APA mother liquors
6-APA mother liquors after above-mentioned regulation pH are handled through cartridge filter, then with the nanofiltration that molecular cut off is 200
Film is concentrated, and feed temperature is 9 DEG C, and it is 2.2MPa to enter film pressure, and cycles of concentration is 10 times, 6-APA concentration in 6-APA mother liquors
For 2.8g/L, phenylacetic acid concentration is 1.1g/L, and 6-APA concentration is 26.9g/L in final concentrate, and phenylacetic acid concentration is 11.2g/
L。
(4) 6-APA is reclaimed from concentrate
Above-mentioned 6-APA mother liquors nanofiltration concentrate 1L is taken, is cooled in ice-water bath, when temperature is less than 8 DEG C, is added thereto
500mL methyl iso-butyl ketone (MIBK)s, under stirring, 30% hydrochloric acid is added thereto, the pH for making feed liquid is 1.0, and the feed liquid is poured into liquid separation
Split-phase is stood in funnel, separates lower floor's aqueous phase, aqueous phase volume is 1100mL.The aqueous phase is placed in ice-water bath, then added
3.3g activated carbons, 30min is stirred, filtered.The filtrate is placed in ice-water bath, under stirring, 20% ammoniacal liquor is added, by the pH of feed liquid
4.0, growing the grain 90min are adjusted to, filters, is washed respectively with purified water and acetone, gained 6-APA wet-millings progress vacuum is done
Dry, drying temperature is 60 DEG C, vacuum 0.089MPa, obtains 6-APA dry powder 16.7g, yield 62%.Gained 6-APA's
Product quality is shown in Table 1.
Table 1 reclaims 6-APA product quality from 6-APA mother liquors
From data in table 1, the 6-APA reclaimed by above-mentioned technique from 6-APA mother liquors, its product quality meets
Top grade product standard, the 6-APA of qualified product can be reclaimed from 6-APA mother liquors with the technique.
(5) the evaporation recovery salt of dialyzate
6-APA mother liquor nanofiltration dislysate 1.5L are taken, are evaporated under reduced pressure, it is 40-70 DEG C to control feed temperature, and vacuum is
0.090MPa, stop distillation when occurring crystal in feed liquid, obtain feed liquid condensate 1330mL, concentrate is placed in cold in ice-water bath
But 60min, filter, obtain solid ammonium chloride, content 99.6%.The water quality data of feed liquid condensate is shown in Table 2.
The 6-APA mother liquors nanofiltration dislysate of table 2 distills feed liquid condensate water quality data
From data in table 2, the feed liquid condensate of gained after the distillation of 6-APA mother liquors nanofiltration dislysate, its electrical conductivity, chlorine from
Son is relatively low, can be used as a Water circulation to workshop.
Embodiment 2
RBA (the butyl acetate phase containing penicillin after activated carbon decolorizing and washing) alkalization, cracking of penicillin, split
Alkali is sodium hydroxide used in the process of solving extraction, 6-APA crystallization and the 6-APA mother liquors pH regulation of liquid, and acid used is hydrochloric acid.
(1) in 6-APA mother liquors solvent removing
By being evaporated under reduced pressure the solvent removed in 6-APA mother liquors, feed temperature is 48 DEG C, vacuum 0.088MPa, is taken off
After solvent, acetone in 6-APA mother liquors, n-butanol, the content of n-butyl acetate and methyl iso-butyl ketone (MIBK) are respectively 32,87,85
And 5ppm.
(2) 6-APA mother liquors pH regulation
6-APA mother liquors after above-mentioned removing solvent are cooled, when temperature is reduced to 10 DEG C, 30% hydrogen is added into the mother liquor
Sodium hydroxide solution, the pH for adjusting feed liquid are 6.5.
(3) the nanofiltration concentration of 6-APA mother liquors
6-APA mother liquors after above-mentioned regulation pH are handled through cartridge filter, then with the nanofiltration that molecular cut off is 200
Film is concentrated, and feed temperature is 9 DEG C, and it is 2.2MPa to enter film pressure, and cycles of concentration is 10 times, 6-APA concentration in 6-APA mother liquors
For 2.5g/L, phenylacetic acid concentration is 1.3g/L, and 6-APA concentration is 24.2g/L in final concentrate, and phenylacetic acid concentration is 13.2g/
L。
(4) 6-APA is reclaimed from concentrate
Above-mentioned 6-APA mother liquors nanofiltration concentrate 1L is taken, is cooled in ice-water bath, when temperature is less than 8 DEG C, is added thereto
500mL methyl iso-butyl ketone (MIBK)s, under stirring, 30% hydrochloric acid is added thereto, the pH for making feed liquid is 0.9, and the feed liquid is poured into liquid separation
Split-phase is stood in funnel, separates lower floor's aqueous phase, aqueous phase volume is 1050mL.The aqueous phase is placed in ice-water bath, then added
3.5g activated carbons, 30min is stirred, filtered.The filtrate is placed in ice-water bath, under stirring, adds 30% sodium hydroxide solution, will
The pH of feed liquid is adjusted to 4.0, growing the grain 90min, filters, is washed respectively with purified water and acetone, and gained 6-APA wet-millings are carried out
Vacuum drying, drying temperature are 60 DEG C, vacuum 0.089MPa, obtain 6-APA dry powder 14.5g, yield 60%.Gained 6-
APA product quality is shown in Table 3.
Table 3 reclaims 6-APA product quality from 6-APA mother liquors
From data in table 3, the 6-APA reclaimed by above-mentioned technique from 6-APA mother liquors, specific rotation, moisture, suction
Luminosity and acidity meet top grade product standard, and content meets inner quality standard.Product can be reclaimed with the technique from 6-APA mother liquors
Up-to-standard 6-APA.
(5) the evaporation recovery salt of dialyzate
6-APA mother liquor nanofiltration dislysate 1.5L are taken, are evaporated under reduced pressure, it is 40-70 DEG C to control feed temperature, and vacuum is
0.087MPa, stop distillation when occurring crystal in feed liquid, obtain feed liquid condensate 1320mL, concentrate is placed in cold in ice-water bath
But 60min, filter, obtain solid sodium chloride, content 99.6%.The water quality data of feed liquid condensate is shown in Table 4.
The 6-APA mother liquors nanofiltration dislysate of table 4 distills feed liquid condensate water quality data
From data in table 4, the feed liquid condensate of gained after the distillation of 6-APA mother liquors nanofiltration dislysate, its electrical conductivity, chlorine from
Son is relatively low, can be used as a Water circulation to workshop.
It the above is only the preferred embodiment of the present invention, be not intended to limit the invention, come for those skilled in the art
Say, under the premise without departing from the principles of the invention, some improvement that can also make, retouching, equivalent substitution, should be included in this
Within the protection domain of invention.
Claims (1)
1. the technique of 6-APA and salt is reclaimed in a kind of mother liquor from 6-APA, it is characterised in that comprise the following steps：
(1) in 6-APA mother liquors solvent removing
By being evaporated under reduced pressure the solvent removed in 6-APA mother liquors, feed temperature is controlled at 30-50 DEG C, vacuum >=0.085MPa,
Solvent residual is measured by sampling in subtractive process, when content of acetone≤50ppm in 6-APA mother liquors, levels of n-butanol≤200ppm, second
When sour N-butyl content≤200ppm, content≤10ppm of methyl iso-butyl ketone (MIBK), stop being evaporated under reduced pressure；
(2) 6-APA mother liquors pH regulation
6-APA mother liquors after above-mentioned removing solvent are cooled, when temperature is reduced to 10 DEG C, 30% hydroxide is added into the mother liquor
Sodium solution or 20% ammoniacal liquor, the pH for adjusting feed liquid are 6.5-7.0；
(3) the nanofiltration concentration of 6-APA mother liquors
Above-mentioned 6-APA mother liquors pass through 5 μm of cartridge filter, are handled subsequently into one-level nanofiltration, and one-level nanofiltration dislysate enters
To nanofiltration dislysate storage tank, one-level nanofiltration concentrate enters two level nanofiltration processing, and it is saturating that two level nanofiltration dislysate enters nanofiltration
Liquid storage tank is analysed, two level nanofiltration concentrate, which is entered to three-level nanofiltration, to be handled, and three-level nanofiltration dislysate enters dialysis liquid storage tank, and three
Level nanofiltration concentrate carries out follow-up 6-APA recovery；Feed liquid is controlled during being concentrated with NF membrane to 6-APA mother liquors
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) 6-APA is reclaimed from concentrate
Above-mentioned three-level nanofiltration concentrate is taken, is cooled in ice-water bath, makes its temperature≤8 DEG C, then adds methyl iso-butyl ketone (MIBK), add
Measure as the 1/3-1/2 of nanofiltration concentrate volume, under stirring, 20-30% hydrochloric acid is added into the feed liquid, the pH for controlling feed liquid is
0.8-1.5；Then the feed liquid is poured into and split-phase is stood in separatory funnel, separate lower floor's aqueous phase；The aqueous phase is placed in ice-water bath,
Feed temperature≤8 DEG C are controlled, activated carbon is then added and is decolourized, activated carbon dosage is 1-5 ‰, stirs 15-30min, is filtered；
Filtrate is placed in ice-water bath, under stirring, 15-30% sodium hydroxide solutions or 10-20% ammoniacal liquor are added thereto, by feed liquid
PH be adjusted to 3.8-4.2, growing the grain 90min, filter, washed respectively with purified water and acetone；Gained 6-APA wet-millings are placed in
It is dried in vacuum drying chamber, drying temperature is 40-60 DEG C, vacuum >=0.085MPa, and dry end obtains 6-APA and done
Powder；
(5) the evaporation recovery salt of dialyzate
6-APA mother liquor nanofiltration dislysates are evaporated under reduced pressure, it is 40-80 DEG C to control feed temperature, vacuum >=0.085MPa,
Stop distillation when occurring crystal in feed liquid, concentrate is cooled down into 60-90min in ice-water bath, filter, obtain 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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| 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 |
| 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 |
| 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 |
| 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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| CA736918A (en) * | 1966-06-21 | Farbenfabriken Bayer, A.G. | Process for the production of 6-amino-penicillanic acid | |
| CN101041663A (en) * | 2006-03-24 | 2007-09-26 | 北京大井易通科技发展有限公司 | Method for recovering 6-amino penicillanic acid by employing membrane |
| CN101773786B (en) * | 2009-12-17 | 2013-07-10 | 杭州天创环境科技股份有限公司 | Method for desalination and concentration of medical intermediate |
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