CN108358951B - The method of Amoxicillin is recycled from the mother liquor of enzymatic clarification Amoxicillin - Google Patents
The method of Amoxicillin is recycled from the mother liquor of enzymatic clarification Amoxicillin Download PDFInfo
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- CN108358951B CN108358951B CN201810136796.1A CN201810136796A CN108358951B CN 108358951 B CN108358951 B CN 108358951B CN 201810136796 A CN201810136796 A CN 201810136796A CN 108358951 B CN108358951 B CN 108358951B
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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
- C07D499/44—Compounds with an amino radical acylated by carboxylic acids, attached in position 6
- C07D499/48—Compounds with an amino radical acylated by carboxylic acids, attached in position 6 with a carbon chain, substituted by hetero atoms or by carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, attached to the carboxamido radical
- C07D499/58—Compounds with an amino radical acylated by carboxylic acids, attached in position 6 with a carbon chain, substituted by hetero atoms or by carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, attached to the carboxamido radical substituted in alpha-position to the carboxamido radical
- C07D499/64—Compounds with an amino radical acylated by carboxylic acids, attached in position 6 with a carbon chain, substituted by hetero atoms or by carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, attached to the carboxamido radical substituted in alpha-position to the carboxamido radical by nitrogen atoms
- C07D499/68—Compounds with an amino radical acylated by carboxylic acids, attached in position 6 with a carbon chain, substituted by hetero atoms or by carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, attached to the carboxamido radical substituted in alpha-position to the carboxamido radical by nitrogen atoms with aromatic rings as additional substituents on the carbon chain
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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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- Organic Chemistry (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to Amoxicillin recycling fields, and in particular to the method that Amoxicillin is recycled from the mother liquor of enzymatic clarification Amoxicillin obtains the concentrate of Amoxicillin this method comprises: the Amoxicillin mother liquor of acidification is carried out UF membrane by (1)；(2) concentrate for the Amoxicillin that step (1) obtains is contacted with alkaline conditioner, is crystallized, obtain the magma of Amoxicillin.Have the characteristics that purity is high and the rate of recovery are high using the Amoxicillin that the method for the present invention obtains, and preparation process is simple, cost is relatively low, it is more environmentally friendly.In addition, for example, carrying out the precipitation of crystal under stirring conditions, and setting 2 stages or 3 stages for stirring under conditions of the present invention is more highly preferred to, enable to the granularity of gained Amoxicillin crystal more uniform.
Description
Technical field
The present invention relates to Amoxicillin recycling fields, and in particular to one kind recycled from the mother liquor of enzymatic clarification Amoxicillin Ah
The method of Amdinocillin.
Background technique
Amoxicillin belongs to penicillin antibiotics.It is a kind of biggish antibiotic drug of current usage amount.
At present the mother liquid disposal of Amoxicillin mainly by the way that crystalline mother solution is concentrated after, using PA ase by its
In Amoxicillin be hydrolyzed to 6-APA and D-pHPG after, pH value is adjusted respectively, in the isoelectric point of both substances
It crystallizes out, recycles solid.Or after hydrolysis finishes, using macroporous absorbent resin to 6-APA and D-pHPG into
Row separation and recovery.The separating effect of macroreticular resin is preferable compared to method for crystallising.
Methods the problem of being primarily present of both separation at present be by two kinds of raw materials of Amoxicillin recovery, recycling
Although raw material can be reused again and be produced, more have an economic benefit not as good as recycling Amoxicillin.Using macropore
The process cycle for adsorbing resin is longer, and treating capacity is limited, while plant maintenance is complex.
Summary of the invention
It is of the existing technology as above the purpose of the invention is to overcome the problems, such as, it provides a kind of from enzymatic clarification Ah Moses
The method that Amoxicillin is recycled in woods mother liquor has purity is high, activity high and the rate of recovery using the Amoxicillin that this method obtains
High feature, and preparation process is simple, cost is relatively low, energy conservation and environmental protection.
To achieve the goals above, the present invention provides one kind recycles Amoxicillin from the mother liquor of enzymatic clarification Amoxicillin
Method, this method comprises:
(1) the Amoxicillin mother liquor of acidification is subjected to UF membrane, obtains the concentrate of Amoxicillin；
(2) concentrate for the Amoxicillin that step (1) obtains is contacted with alkaline conditioner, is crystallized, obtains Ah not
The magma in XiLin.
Preferably, the pH value of the Amoxicillin mother liquor of the acidification is 0.5-3, preferably 1-2, more preferably 1.3-1.8.
Preferably, the UF membrane pressure 1-4MPa, preferably 2-3MPa.
Preferably, the temperature of the UF membrane is 5-20 DEG C, preferably 8-16 DEG C.
Preferably, the contact carries out under stirring conditions, and the stirring is divided into following 2 stages:
First stage, the revolving speed of the stirring are 120-350rpm, pH value 2.5-3.5；
Second stage, the revolving speed of the stirring are 200-350rpm, pH value 4.5-5.5.
Preferably, the contact carries out under stirring conditions, and the stirring is divided into following 3 stages:
First stage, the revolving speed of the stirring are 200-350rpm, pH value 2.5-3.5；
Second stage, the revolving speed of the stirring are 120-170rpm, pH value 2.5-3.5；
Phase III, the revolving speed of the stirring are 200-350rpm, pH value 4.5-5.5.
Through the above technical solutions, the present invention achieves following technical effect:
1, the Amoxicillin mother liquor generated to enzyme process is concentrated, and the filter liquor after being concentrated can enter the set of next group
With in the middle, 50% of quantity of wastewater effluent or more can be reduced.
2, the Amoxicillin mother liquor after being concentrated can recycle to obtain the Amoxicillin of solid by carrying out crystallization processes, can be with
Recycle 50% or more Amoxicillin in crystalline mother solution.
3, compared to the raw material after the hydrolysis of recycling Amoxicillin, recycling Amoxicillin more has economic benefit.
4, compared to a whole set of film device, reduce the relevant device and material of hydrolysis Amoxicillin and recycling, reduce
The cost of recycling.And film device is easy to maintain, maintains and replaces.
5, under conditions of the present invention is more highly preferred to, for example, carrying out the precipitation of crystal under stirring conditions, and will stirring
2 stages or 3 stages are set as, enable to the granularity of gained Amoxicillin crystal more uniform, and the grain of Amoxicillin crystal
Diameter integrated distribution is at 20-50 μm.
Specific embodiment
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
The method that the present invention provides a kind of to recycle Amoxicillin from the mother liquor of enzymatic clarification Amoxicillin, this method packet
It includes:
(1) the Amoxicillin mother liquor of acidification is subjected to UF membrane, obtains the concentrate of Amoxicillin；
(2) concentrate for the Amoxicillin that step (1) obtains is contacted with alkaline conditioner, is crystallized, obtains Ah not
The magma in XiLin.
In the present invention, " the enzymatic clarification Amoxicillin mother liquor " can be obtained according to the method for this field routine, wherein
The concentration of Amoxicillin is generally 2-5mg/ml in the mother liquor.
In the present invention, using the Amoxicillin mother liquor of acidification, the analysis of the Amoxicillin crystal in membrane separating process is avoided
Out, meanwhile, it ensure that the yield that crystal is precipitated in the follow-up process.Wherein, the acid for being acidified to Amoxicillin mother liquor
Property regulator can be selected in a wider scope, as long as will not react with Amoxicillin and influence its stability i.e.
Can, for example, the acid regulator can be at least one of hydrochloric acid, sulfuric acid and nitric acid, the concentration of the acid regulator
It can be 1-6mol/L.More preferably, the acid regulator is hydrochloric acid.
In the present invention, the pH value of the Amoxicillin mother liquor of the acidification preferably so that Amoxicillin in membrane separating process not
The precipitation of Amoxicillin crystal is had, for example, can be 0.5-3.But it was found by the inventors of the present invention that being 1-2 in pH value, more preferably
In the case where for 1.3-1.8, the stability of Amoxicillin can be further promoted, to improve the purity and yield of finished product.
In the present invention, the acid regulator can be added by following mode, and enzyme process reactive crystallization is terminated
Amoxicillin mother liquor afterwards is placed in the reactor with stirring, opens stirring, while opening temperature control device and temperature control exists
In following range, then by the way that acid regulator is slowly added dropwise into Amoxicillin mother liquor until reaching required pH.
In the present invention, the temperature of the Amoxicillin mother liquor of the acidification is preferably 5-30 DEG C, and more preferably 10-16 DEG C, example
Such as, 10 DEG C, 11 DEG C, 12 DEG C, 13 DEG C, 14 DEG C, 15 DEG C and 16 DEG C.
In the present invention, the UF membrane can be at least one of micro-filtration, nanofiltration and ultrafiltration, preferably 2 kinds of combination.
The molecular cut off of film is preferably 100-500Da in the UF membrane.
In the present invention, the pressure of the UF membrane is preferably 1-4MPa, more preferably 2-3MPa.The present inventor's hair
It is existing, when the pressure of UF membrane is excessive, it will lead to the rate of recovery decline of Amoxicillin, and when the pressure of UF membrane is too small, film
Disengaging time extends.
In the present invention, the temperature of the UF membrane is preferably 5-20 DEG C, and more preferably 8-16 DEG C.The present inventor's hair
It is existing, when the temperature is excessively high, it is unstable to will cause Amoxicillin, so that the rate of recovery declines, separation purity is also reduced, and when temperature
When spending low, separative efficiency reduction will also result in, to influence final product recovery rate and purity.
In the present invention, the UF membrane is carried out in a manner of recycling the Amoxicillin mother liquor of concentration acidification, that is, will acidification
Amoxicillin mother liquor from mother liquor storage tank lead to film separation unit, the concentrate after UF membrane be back to mother liquor storage
Tank obtains first circulation concentrate, and filter liquor leads to the processing for filtering out tank to carry out next step, then draws again from mother liquor storage tank
First circulation concentrate is to film separation unit, such multi-cycle separation out.When the mother liquor is stored in tank in the concentrate of Amoxicillin
The concentration of Amoxicillin can be with stopper film point when being 5-10 times, preferably 6-9 times of the concentration of Amoxicillin in the mother liquor of Amoxicillin
From.It was found by the inventors of the present invention that terminating UF membrane under the degree, separation costs and separative efficiency can be made to reach fine
Equilibrium.
In the present invention, preferably make Amoxicillin from the Amoxicillin after UF membrane by the method for adding alkaline conditioner
Concentrate be precipitated, the dosage of the alkaline conditioner can be selected specifically according to the actual situation.According to the present invention, institute
The dosage of alkaline conditioner is stated preferably so that the pH value of system is 2-6, more preferably 2.5-5.5.
Wherein, the alkaline conditioner can be selected in a wider scope, for example, sodium hydroxide and/or ammonium hydroxide,
More preferably sodium hydroxide.Wherein, the concentration of the alkaline conditioner can be 1-6mol/L.
In the present invention, the crystallization preferably carries out under stirring conditions, and the revolving speed of the stirring is 100-400rpm, example
Such as, 100rpm, 150rpm, 200rpm, 250rpm, 300rpm, 350rpm, 400rpm, temperature are 20-27 DEG C, for example, 20 DEG C,
21℃、22℃、23℃、24℃、25℃、26℃、27℃。
The present inventor is in the course of the study it has furthermore been found that when the stirred crystallization is divided into the 2 following stages
It carrying out, when the 3 more preferably following stages carry out, the particle diameter distribution of obtained Amoxicillin crystal is more uniform, and product
Yield and purity can also be further enhanced.
The stirring in 2 stage includes:
First stage, the revolving speed of the stirring are 120-350rpm, pH value 2.5-3.5；Wherein, stage it is lasting when
Between premised on crystal can sufficiently be precipitated, can specifically adjust according to the actual situation.
Second stage, the revolving speed of the stirring are 200-350rpm, pH value 4.5-5.5；Wherein, stage it is lasting when
Between can be 20-40min.
The stirring in 3 stage includes:
First stage, the revolving speed of the stirring are 200-350rpm, pH value 2.5-3.5；Wherein, stage it is lasting when
Between premised on crystal can sufficiently be precipitated, can specifically adjust according to the actual situation；
Second stage, the revolving speed of the stirring are 120-170rpm, pH value 2.5-3.5；Wherein, stage it is lasting when
Between can be 10-30min；
Phase III, the revolving speed of the stirring are 200-350rpm, pH value 4.5-5.5；Wherein, stage it is lasting when
Between can be 20-40min.
In the present invention, it is described from the mother liquor of enzymatic clarification Amoxicillin recycle Amoxicillin method still further comprise by
Obtained magma is separated by solid-liquid separation and is dried, and Amoxicillin dry powder is obtained.Wherein, the method for the separation of solid and liquid can be with
It is operated according to the method for this field routine, for example, passing through the method for filtering.The drying can also be according to this field routine
Method carry out, for example, 30-40 DEG C at a temperature of it is 1-3 hours dry.
The present invention will be described in detail by way of examples below.
Embodiment 1
The present embodiment is used to illustrate the side provided by the invention that Amoxicillin is recycled from the mother liquor of enzymatic clarification Amoxicillin
Method
1) Amoxicillin 30L crystalline mother solution is measured, wherein amoxicillin content is 3.78mg/ml for liquid phase detection, and control is female
Liquid temperature is 10.5-11.5 DEG C.
2) stirring is opened, setting speed 300rpm starts to be added dropwise 3M salt slow acid adjusting material liquid pH to 1.5.
3) feed liquid is pressed into 230 molecular weight nanofiltration membranes using pump, adjusting concentration pressure is 3MPa.
4) temperature controlling instruments is opened, the temperature of film is controlled at 14.5-15.5 DEG C.
5) concentrate is back in storage tank, filtrate collection is concentrated into Amoxicillin knot into filtrate collection tank
The concentration of 8 times of brilliant mother liquor.
6) concentrate is transferred in crystallizing tank, adjusts speed of agitator 200rpm, 3M sodium hydroxide solution is slowly added dropwise, adjusted
PH to 2.97 is saved, controlled at 20.5-21.0 DEG C, goes out crystalline substance at this time.
7) speed of agitator is down to 150rpm, stirred growing the grain 20 minutes, during which control temperature between 20.5-21.0 DEG C,
PH is controlled 2.97.
8) revolving speed is adjusted after growing the grain to 200rpm, is added dropwise and is adjusted pH=5.0.It adjusts and finishes, growing the grain 30min.
9) filtration drying obtains finished product 74g, sample detection finished product, moisture 14.7%, purity 98.4%.Withdraw mother liquor
The amount of middle Amoxicillin is 55%.It is measured using particles distribution instrument, obtained Amoxicillin crystal particle diameter integrated distribution is in 20-50
Between μm, ratio is about 52%.
Embodiment 2
The present embodiment is used to illustrate the side provided by the invention that Amoxicillin is recycled from the mother liquor of enzymatic clarification Amoxicillin
Method
1) Amoxicillin crystalline mother solution same as Example 1 is taken, control mother liquor temperature is 15.5-16 DEG C.
2) stirring is opened, setting speed 250rpm starts to be added dropwise 3M salt slow acid adjusting material liquid pH to 1.3.
3) feed liquid is pressed into 160 molecular weight nanofiltration membranes using pump, adjusting concentration pressure is 2.5MPa.
4) temperature controlling instruments is opened, the temperature of film is controlled at 10.5-11.5 DEG C.
5) concentrate is back in storage tank, filtrate collection is concentrated into Amoxicillin knot into filtrate collection tank
The concentration of 6 times of brilliant mother liquor.
6) concentrate is transferred in crystallizing tank, adjusts speed of agitator 250rpm, 3M sodium hydroxide solution is slowly added dropwise, adjusted
PH to 3.5 is saved, controlled at 22.5-23.0 DEG C, goes out crystalline substance at this time.
7) speed of agitator is down to 120rpm, stirred growing the grain 20 minutes, during which control temperature between 22.5-23.0 DEG C,
PH is controlled 3.5.
9) revolving speed is adjusted after growing the grain to 250rpm, is added dropwise and is adjusted pH=5.5.It adjusts and finishes, growing the grain 30min.
10) filtration drying obtains finished product 94g, sample detection finished product, moisture 15.2%, purity 97.9%.It withdraws female
The amount of Amoxicillin is 58% in liquid.It is measured using particles distribution instrument, obtained Amoxicillin crystal particle diameter integrated distribution is in 20-
Between 50 μm, ratio is about 48%.
Embodiment 3
The present embodiment is used to illustrate the side provided by the invention that Amoxicillin is recycled from the mother liquor of enzymatic clarification Amoxicillin
Method
1) Amoxicillin crystalline mother solution same as Example 1 is taken, control mother liquor temperature is 12.5-13.5 DEG C.
2) stirring is opened, setting speed 300rpm starts to be added dropwise 3M salt slow acid adjusting material liquid pH to 1.8.
3) feed liquid is pressed into 130 molecular weight nanofiltration membranes using pump, adjusting concentration pressure is 2MPa.
4) temperature controlling instruments is opened, the temperature of film is controlled at 8.5-9.5 DEG C.
5) concentrate is back in storage tank, filtrate collection is concentrated into Amoxicillin knot into filtrate collection tank
The concentration of 9 times of brilliant mother liquor.
6) concentrate is transferred in crystallizing tank, adjusts speed of agitator 300rpm, 3M sodium hydroxide solution is slowly added dropwise, adjusted
PH to 2.5 is saved, controlled at 25.5-27.0 DEG C, goes out crystalline substance at this time.
8) speed of agitator is down to 170rpm, stirred growing the grain 20 minutes, during which control temperature between 25.5-27.0 DEG C,
PH is controlled 2.5.
9) revolving speed is adjusted after growing the grain to 300rpm, is added dropwise and is adjusted pH=4.5.It adjusts and finishes, growing the grain 30min.
10) filtration drying obtains finished product 72g, sample detection finished product, moisture 13.4%, purity 98.2%.It withdraws female
The amount of Amoxicillin is 58% in liquid.It is measured using particles distribution instrument, obtained Amoxicillin crystal particle diameter integrated distribution is in 20-
Between 50 μm, ratio is about 45%.
Embodiment 4
Embodiment 4 (including embodiment 4-1~4-3) is used to illustrate the shadow of different acid regulator and alkaline conditioner
It rings.
Embodiment 4 is the procedure of Example 1 was followed except that replace with other acid for the hydrochloric acid in step 2)
Property regulator and step 6) in sodium hydroxide replace with ammonium hydroxide, it is specific as shown in table 1.
Table 1
As it can be seen from table 1 can be further improved final products by using currently preferred acid-base modifier
Purity and the rate of recovery, and the crystal form of obtained product is more regular, granularity is more uniform.
Embodiment 5
Embodiment 5 (including embodiment 5-1~5-4) is used to illustrate the influence of crystalline mother solution pH in step 2).
The procedure of Example 1 was followed except that the dosage for changing hydrochloric acid makes pH value different, specific pH value
And resulting the results are shown in Table 2.
Table 2
From table 2 it can be seen that can be further improved most when the pH value of crystalline mother solution is in preferred scope of the invention
The purity and the rate of recovery of finished product, and the crystal form of obtained product is more regular, granularity is more uniform.
Embodiment 6
Embodiment 6 (including embodiment 6-1~6-3) is used to illustrate the influence of the temperature and pressure of UF membrane.
The procedure of Example 1 was followed except that by UF membrane temperature and separating pressure control shown in the table 3
Range, it is resulting that the results are shown in Table 3.
Table 3
From table 3 it can be seen that can be further improved most when the pH value of crystalline mother solution is in preferred scope of the invention
The purity and the rate of recovery of finished product, and the crystal form of obtained product is more regular, granularity is more uniform.
Embodiment 7
The present embodiment is used to illustrate the influence of 2 stage crystallization provided by the invention
The procedure of Example 1 was followed except that by step 6) -9) crystallisation step replace with following 2 stage
The step of crystallization
6) concentrate is transferred in crystallizing tank, adjusts speed of agitator 200rpm, 3M sodium hydroxide solution is slowly added dropwise, adjusted
PH to 2.97 is saved, controlled at 20.5-21.0 DEG C, goes out crystalline substance at this time.
7) revolving speed 200rpm is kept, is added dropwise and adjusts pH=5.0.It adjusts and finishes, growing the grain 50min.
Moisture is 16.1% in final products obtained therefrom, purity 97.0%.The amount for withdrawing Amoxicillin in mother liquor is 53%.
It is measured using particles distribution instrument, for obtained Amoxicillin crystal particle diameter integrated distribution between 20-50 μm, ratio is about 48%.
The preferred embodiment of the present invention has been described above in detail, and still, the present invention is not limited thereto.In skill of the invention
In art conception range, can with various simple variants of the technical solution of the present invention are made, including each technical characteristic with it is any its
Its suitable method is combined, and it should also be regarded as the disclosure of the present invention for these simple variants and combination, is belonged to
Protection scope of the present invention.
Claims (16)
1. a kind of method for recycling Amoxicillin from the mother liquor of enzymatic clarification Amoxicillin, which is characterized in that this method comprises:
(1) the Amoxicillin mother liquor of acidification is subjected to UF membrane, obtains the concentrate of Amoxicillin；
(2) concentrate for the Amoxicillin that step (1) obtains is contacted with alkaline conditioner, is crystallized, obtains Amoxicillin
Magma,
The concentration of Amoxicillin is 2-5mg/ml in the mother liquor,
Wherein, in step (2), the contact carries out under stirring conditions, and the stirring is divided into following 3 stages:
First stage, the revolving speed of the stirring are 200-350rpm, pH value 2.5-3.5；
Second stage, the revolving speed of the stirring are 120-170rpm, pH value 2.5-3.5；
Phase III, the revolving speed of the stirring are 200-350rpm, pH value 4.5-5.5.
2. according to the method described in claim 1, wherein, the pH value of the Amoxicillin mother liquor of the acidification is 0.5-3；The acid
The temperature of the Amoxicillin mother liquor of change is 5-30 DEG C.
3. according to the method described in claim 2, wherein, the pH value of the Amoxicillin mother liquor of the acidification is 1-2.
4. according to the method described in claim 3, wherein, the pH value of the Amoxicillin mother liquor of the acidification is 1.3-1.8.
5. according to the method described in claim 2, wherein, the temperature of the Amoxicillin mother liquor of the acidification is 10-16 DEG C.
6. according to right want 1 described in method, wherein be adjusted using pH value of the acid regulator to Amoxicillin mother liquor,
The acid regulator is selected from least one of hydrochloric acid, sulfuric acid and nitric acid.
7. according to the method described in claim 6, wherein, being adjusted using pH value of the acid regulator to Amoxicillin mother liquor
Section, the acid regulator are hydrochloric acid.
8. method according to any one of claims 1-7, wherein the UF membrane is in micro-filtration, nanofiltration and ultrafiltration
At least one；The molecular cut off of the film is 100-500Da.
9. method according to any one of claims 1-7, wherein the UF membrane pressure is 1-4MPa；The film
Isolated temperature is 5-20 DEG C.
10. according to the method described in claim 9, wherein, the UF membrane pressure is 2-3MPa.
11. according to the method described in claim 9, wherein, the temperature of the UF membrane is 8-16 DEG C.
12. method described in any one of -7 and 10-11 according to claim 1, wherein the alkaline conditioner is hydroxide
Sodium and/or ammonium hydroxide.
13. according to the method for claim 12, wherein the alkaline conditioner is sodium hydroxide.
14. according to claim 1-7, method described in any one of 10-11 and 13, wherein in step (2), the stirring
Temperature is 20-27 DEG C.
15. according to the method described in claim 1, wherein, in step (1), Amoxicillin in the concentrate of the Amoxicillin
Concentration be 5-10 times of concentration of Amoxicillin in the mother liquor of Amoxicillin.
16. being obtained according to the method described in claim 1, wherein, this method further includes being separated by solid-liquid separation the magma
Amoxicillin crystal.
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| CN104762359A (en) * | 2015-04-15 | 2015-07-08 | 内蒙古常盛制药有限公司 | Recycling process of amoxicillin in enzymatically synthesized amoxicillin mother liquor |
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| CN104762359A (en) * | 2015-04-15 | 2015-07-08 | 内蒙古常盛制药有限公司 | Recycling process of amoxicillin in enzymatically synthesized amoxicillin mother liquor |
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