CN110841608A - Preparation method of penicillin fermentation liquor refined adsorbent - Google Patents
Preparation method of penicillin fermentation liquor refined adsorbent Download PDFInfo
- Publication number
- CN110841608A CN110841608A CN201911193659.2A CN201911193659A CN110841608A CN 110841608 A CN110841608 A CN 110841608A CN 201911193659 A CN201911193659 A CN 201911193659A CN 110841608 A CN110841608 A CN 110841608A
- Authority
- CN
- China
- Prior art keywords
- penicillin
- parts
- adsorbent
- penicillin fermentation
- mass
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
- B01J20/28019—Spherical, ellipsoidal or cylindrical
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
-
- 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
-
- 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
- C07D499/46—Compounds with an amino radical acylated by carboxylic acids, attached in position 6 with acyclic hydrocarbon radicals or such radicals substituted by carbocyclic or heterocyclic rings, attached to the carboxamido radical
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
The invention relates to the field of preparation of microbial fermentation products, in particular to a preparation method of a penicillin fermentation liquor refining adsorbent, which is characterized in that a porous melamine resin microsphere is prepared, and a microporous surface modifier is used for carrying out surface modification on the porous melamine resin microsphere to prepare the porous penicillin fermentation liquor refining adsorbent, the adsorbent can enrich effective component penicillin in low-valence filtrate generated in the penicillin production process and then desorb the penicillin in an acidic solution to achieve the aim of refining penicillin, and the microporous surface modifier contains a large number of lactam groups, has good nucleophilicity on β -lactam antibiotic penicillin high efficiency, and has the advantages of good adsorption performance, good enrichment effect and good recycling effect.
Description
Technical Field
The invention relates to the field of preparation of microbial fermentation products, in particular to a preparation method of a penicillin fermentation liquor refining adsorbent.
Background
Penicillin, the first antibiotic found in humans, is synthesized by penicillium chrysogenum through secondary metabolism during fermentation. The discovery of penicillin opens the door to antibiotics for humans.
201810720504.9 provides a continuous culture method of penicillin fermentation liquor, which comprises the following steps: (a) setting a first-stage fermentation tank, a second-stage fermentation tank, a third-stage fermentation tank and a fourth-stage fermentation tank; (b) placing the redundant 2-5 ten thousand mu/mL fermentation liquid sterile belt in the normal fermentation tank into a primary fermentation tank for culture; (c) placing the redundant fermentation liquor sterile zones in the normal fermentation tank and 5-8 ten thousand mu/mL fermentation liquor sterile zones in the primary fermentation tank into a secondary fermentation tank for culture; (d) placing the residual fermentation liquid in the normal fermentation tank and 8-11 ten thousand mu/mL fermentation liquid sterile zones in the secondary fermentation tank into a third fermentation tank for culture; (e) placing the residual fermentation liquid sterile zones in the normal fermentation tank and the fermentation liquid sterile zones more than 11 ten thousand mu/mL in the third-stage fermentation tank into a fourth-stage fermentation tank for culture; (f) and culturing the fermentation liquor in the four-stage fermentation tank and filtering. The invention greatly improves the fermentation unit of the penicillins with the fermentation liquor, obviously reduces the COD concentration in the fermentation wastewater and reduces the environmental protection cost.
201711131932.X relates to a method for improving the biological fermentation yield of penicillin. The invention discloses a new regulation and control strategy in the penicillin fermentation process, mainly relates to the regulation and control of the middle and later stages in the optimized fermentation process, and can remarkably improve the biological fermentation yield of penicillin.
201310138205.1 discloses a penicillin fermentation broth treatment process, which comprises the following steps: cooling the original penicillin fermentation liquor, feeding the penicillin fermentation liquor into a closed ceramic membrane cross-flow filtration system for filtration, and collecting high-titer ceramic membrane filtrate; in the filtering process, when the wet-solid content of the penicillin fermentation liquor is increased to 1.8-2 times of the original wet-solid content, adding water with the weight 2 times of the weight of the original fermentation liquor for dialysis, and collecting and storing the obtained low-titer ceramic membrane filtrate, and performing nanofiltration, concentration and dehydration for later use; continuously adding water with the weight 2 times of the weight of the original fermentation liquor for dialysis, and collecting and storing the obtained extra-low titer ceramic membrane filtrate; stopping filtering until the titer of the penicillin in the penicillin fermentation liquid is as low as 800U of 500-; the bacterial slag intercepted by the ceramic membrane filtration system is collected and stored; the obtained high-valence ceramic membrane filtrate enters the steps of 6APA conversion or oxidation, ring expansion and cracking to prepare 7-ADCA; collecting the obtained bacterial dregs, and adding engineering bacteria to decompose the bacterial dregs.
The penicillin fermentation liquor is treated by adopting a plate frame, a ceramic membrane or a rotary drum, and the produced low-titer filtrate is dialyzed and then concentrated.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a penicillin fermentation liquor refining adsorbent.
A preparation method of an adsorbent refined by penicillin fermentation liquor comprises the following specific scheme:
adding 50-80 parts of melamine formaldehyde resin prepolymer, 2-7 parts of surfactant dodecyl triphenyl phosphonium bromide, 5-10 parts of ethyl acetate, 14-22 parts of curing agent imido disulfonic acid propyl amine salt and 3-8 parts of pore-foaming agent into a reaction kettle, controlling the temperature to be 40-60 ℃, stirring and mixing uniformly, then adding 80-100 parts of water and 0.1-3 parts of glucan hydroxypropyl trimethyl ammonium chloride, stirring and mixing uniformly to form suspended emulsion, controlling the temperature to be 80-105 ℃, reacting for 12-24 hours, washing the microspheres clean after the reaction is finished, removing the pore-foaming agent, and obtaining melamine resin porous microspheres; adding the obtained microspheres into 500 parts of 300-parts of isopropanol, adding 10-15% of microporous surface modifier into 300 parts of 100-300-parts of isopropanol, uniformly stirring and mixing, controlling the temperature to be 50-70 ℃, then dropwise adding 50-80 parts of 5-10% azodiisobutyronitrile solution into a reaction kettle, stirring and reacting for 3-5h after dropwise adding is finished, taking out the microspheres after the reaction is finished, and washing and drying to obtain the penicillin fermentation liquor refining adsorbent.
The preparation method of the microporous surface modifier comprises the following steps:
adding 50-80 parts by mass of isopropanol, 40-60 parts by mass of vinyl caprolactam, 5-10 parts by mass of diallyl tetramethyl disiloxane, 10-20 parts by mass of diacetone acrylamide and 1-5 parts by mass of allylamine hydrochloride into a reaction kettle, uniformly stirring and mixing, then dissolving 0.01-0.5 part by mass of azobisisobutyronitrile into 10-15 parts by mass of isopropanol, dropwise adding into the reaction kettle, controlling the temperature to be 40-50 ℃, carrying out prepolymerization for 10-30min, cooling to room temperature, adding isopropanol to dilute to 10-15%, and thus obtaining the microporous surface modifier.
The melamine-formaldehyde resin is a precondensate of melamine and formaldehyde, and the molar ratio of the melamine to the formaldehyde during synthesis is 0.8-2.4: 1.
The pore-foaming agent is 1, 4-butanediol or polyethylene glycol 400 or polyethylene glycol 1000.
The using method of the penicillin fermentation liquor refining adsorbent comprises the following steps: and (2) passing the low-titer filtrate generated in the penicillin production process through a column with the penicillin fermentation broth refined adsorbent as a filler, adsorbing and concentrating the penicillin in the column, taking out the penicillin fermentation broth refined adsorbent, and soaking the penicillin fermentation broth refined adsorbent in an acidic aqueous solution with the pH value of 1-4 for 5-10 hours to complete the desorption of the penicillin.
After the penicillin fermentation liquor refining adsorbent is used, the adsorbent is soaked in alkali liquor with the concentration of 0.1-0.5mol/L for 3-8 hours, and then is washed by hydrophilic for 5-10min, so that the recovery can be completed.
The invention relates to a process for preparing penicillin fermentation liquor refining adsorbent, which comprises preparing a porous melamine resin microsphere, surface modifying with a microporous surface modifier, preparing a porous penicillin fermentation liquor refining adsorbent, enriching penicillin in low-valence filtrate generated in penicillin production process, desorbing in acid solution to obtain refined penicillin, wherein the microporous surface modifier contains a large amount of lactam groups, has good nucleophilicity to β -lactam antibiotics penicillin, high-efficiency adsorption performance, good enriching effect and good recycling effect
Detailed Description
The invention is further illustrated by the following specific examples:
the specific surface area of the prepared adsorbent is determined by adopting a GB T19587-2017 gas adsorption BET method; preparing 100g of prepared adsorbent into an adsorption column, then enriching with filtrate with the titer of 500U at the flow rate of 5ml/min, detecting the titer of the effluent of the adsorption column, stopping enrichment when the titer of the effluent is 480U, recording the mass of the passing filtrate, wherein the more the mass of the passing filtrate, the better the adsorption effect of the adsorbent.
Example 1
A preparation method of an adsorbent refined by penicillin fermentation liquor comprises the following specific scheme:
adding 50g of melamine formaldehyde resin prepolymer, 2g of surfactant dodecyl triphenyl phosphonium bromide, 5g of ethyl acetate, 14g of curing agent imido disulfonic acid propyl amine salt and 3g of pore-foaming agent into a reaction kettle according to the mass parts, controlling the temperature to be 40 ℃, uniformly stirring and mixing, then adding 80g of water and 0.1g of glucan hydroxypropyl trimethyl ammonium chloride, uniformly stirring and mixing to form suspended emulsion, controlling the temperature to be 80 ℃, reacting for 24 hours, washing the microspheres clean after the reaction is finished, and removing the pore-foaming agent to obtain melamine resin porous microspheres; adding the obtained microspheres into 300g of isopropanol, adding 100g of 10% microporous surface modifier, stirring and mixing uniformly, controlling the temperature to be 50 ℃, then dropwise adding 50g of 5% azodiisobutyronitrile solution into a reaction kettle, stirring and reacting for 3 hours after the dropwise adding is finished, taking out the microspheres after the reaction is finished, washing with water, and drying to obtain the penicillin fermentation liquor refining adsorbent.
The preparation method of the microporous surface modifier comprises the following steps:
adding 50g of isopropanol, 40g of vinyl caprolactam, 5g of diallyl tetramethyl disiloxane, 10g of diacetone acrylamide and 1g of allylamine hydrochloride into a reaction kettle according to the mass parts, uniformly stirring and mixing, then dissolving 0.01g of azobisisobutyronitrile into 10g of isopropanol, dropwise adding into the reaction kettle, controlling the temperature to be 40 ℃, pre-polymerizing for 10min, cooling to room temperature, adding isopropanol, diluting to 10%, and thus obtaining the microporous surface modifier.
The melamine-formaldehyde resin is a precondensate of melamine and formaldehyde, and the molar ratio of the melamine to the formaldehyde during synthesis is 0.8: 1.
The pore-foaming agent is 1, 4-butanediol.
The using method of the penicillin fermentation liquor refining adsorbent comprises the following steps: and (2) passing the low-titer filtrate generated in the penicillin production process through a column with the penicillin fermentation broth refined adsorbent as a filler, adsorbing and concentrating penicillin in the column, taking out the penicillin fermentation broth refined adsorbent, and soaking the penicillin fermentation broth refined adsorbent in an acidic aqueous solution with the pH value of 1 for 5 hours to complete the desorption of penicillin.
After the penicillin fermentation liquor refining adsorbent is used, the adsorbent is soaked in alkali liquor with the concentration of 0.1mol/L for 8 hours, and then the adsorbent is washed by hydrophilic water for 5 minutes, so that the recovery can be completed.
The adsorbent prepared in the experiment has the specific surface area of 1542.3m2The mass of the filtrate passing through the adsorption experiment was 12.34 kg/g.
Example 2
A preparation method of an adsorbent refined by penicillin fermentation liquor comprises the following specific scheme:
adding 60g of melamine formaldehyde resin prepolymer, 4g of surfactant dodecyl triphenyl phosphonium bromide, 8g of ethyl acetate, 18g of curing agent imido disulfonic acid propyl amine salt and 5g of pore-foaming agent into a reaction kettle, controlling the temperature to be 40-60 ℃, uniformly stirring and mixing, then adding 90g of water and 2g of glucan hydroxypropyl trimethyl ammonium chloride, uniformly stirring and mixing to form suspended emulsion, controlling the temperature to be 95 ℃, reacting for 18 hours, washing the microspheres clean after the reaction is finished, and removing the pore-foaming agent to obtain melamine resin porous microspheres; adding the obtained microspheres into 400g of isopropanol, adding 200g of 13% of microporous surface modifier, stirring and mixing uniformly, controlling the temperature to be 60 ℃, then dropwise adding 70g of 8% azodiisobutyronitrile solution into a reaction kettle, stirring and reacting for 4 hours after the dropwise adding is finished, taking out the microspheres after the reaction is finished, washing with water, and drying to obtain the penicillin fermentation liquor refining adsorbent.
The preparation method of the microporous surface modifier comprises the following steps:
adding 60g of isopropanol, 50g of vinyl caprolactam, 7g of diallyl tetramethyl disiloxane, 15g of diacetone acrylamide and 3g of allylamine hydrochloride into a reaction kettle according to the mass parts, uniformly stirring and mixing, then dissolving 0.25g of azobisisobutyronitrile into 15g of isopropanol, dropwise adding into the reaction kettle, controlling the temperature to 45 ℃, pre-polymerizing for 20min, cooling to room temperature, adding isopropanol, diluting to 13%, and thus obtaining the microporous surface modifier.
The melamine-formaldehyde resin is a precondensate of melamine and formaldehyde, and the molar ratio of the melamine to the formaldehyde during synthesis is 0.8-2.4: 1.
The pore-foaming agent is polyethylene glycol 400.
The using method of the penicillin fermentation liquor refining adsorbent comprises the following steps: and (2) passing the low-titer filtrate generated in the penicillin production process through a column with the penicillin fermentation broth refined adsorbent as a filler, adsorbing and concentrating penicillin in the column, taking out the penicillin fermentation broth refined adsorbent, and soaking the penicillin fermentation broth refined adsorbent in an acidic aqueous solution with the pH value of 3 for 8 hours to complete the desorption of penicillin.
After the penicillin fermentation liquor refining adsorbent is used, the adsorbent is soaked in alkali liquor with the concentration of 0.3mol/L for 5 hours, and then is washed by hydrophilic water for 8 minutes, so that the recovery can be completed.
The adsorbent prepared in the experiment has the specific surface area of 1587.6m2The mass of the filtrate passing through the adsorption test was 13.27 kg/g.
Example 3
A preparation method of an adsorbent refined by penicillin fermentation liquor comprises the following specific scheme:
adding 80g of melamine formaldehyde resin prepolymer, 7g of surfactant dodecyl triphenyl phosphonium bromide, 10g of ethyl acetate, 122g of curing agent imido disulfonic acid propyl amine salt and 8g of pore-foaming agent into a reaction kettle, controlling the temperature to be 60 ℃, uniformly stirring and mixing, then adding 100g of water and 3g of glucan hydroxypropyl trimethyl ammonium chloride, uniformly stirring and mixing to form suspended emulsion, controlling the temperature to be 105 ℃, reacting for 24 hours, washing the microspheres clean after the reaction is finished, removing the pore-foaming agent, and obtaining the porous melamine resin microspheres; adding the obtained microspheres into 500g of isopropanol, adding 300g of 15% microporous surface modifier, stirring and mixing uniformly, controlling the temperature at 70 ℃, then dropwise adding 80g of 10% azodiisobutyronitrile solution into a reaction kettle, stirring and reacting for 5 hours after the dropwise adding is finished, taking out the microspheres after the reaction is finished, washing with water, and drying to obtain the penicillin fermentation liquor refining adsorbent.
The preparation method of the microporous surface modifier comprises the following steps:
adding 80g of isopropanol, 60g of vinyl caprolactam, 10g of diallyl tetramethyl disiloxane, 20g of diacetone acrylamide and 5g of allylamine hydrochloride into a reaction kettle according to the mass parts, uniformly stirring and mixing, then dissolving 0.5g of azobisisobutyronitrile into 10-15g of isopropanol, dropwise adding into the reaction kettle, controlling the temperature at 50 ℃, carrying out prepolymerization for 30min, cooling to room temperature, adding isopropanol, diluting to 15%, and thus obtaining the microporous surface modifier.
The melamine-formaldehyde resin is a precondensate of melamine and formaldehyde, and the molar ratio of the melamine to the formaldehyde during synthesis is 2.4: 1.
The pore-foaming agent is polyethylene glycol 1000.
The using method of the penicillin fermentation liquor refining adsorbent comprises the following steps: and (2) passing the low-titer filtrate generated in the penicillin production process through a column with the penicillin fermentation broth refined adsorbent as a filler, adsorbing and concentrating penicillin in the column, taking out the penicillin fermentation broth refined adsorbent, and soaking the penicillin fermentation broth refined adsorbent in an acidic aqueous solution with the pH value of 4 for 10 hours to complete the desorption of penicillin.
After the penicillin fermentation liquor refining adsorbent is used, the adsorbent is soaked in alkali liquor with the concentration of 0.5mol/L for 3 hours, and then is washed with hydrophilic water for 10 minutes, so that the recovery can be completed.
The adsorbent prepared in the experiment has the specific surface area of 1601.4m2The mass of the filtrate passing through the adsorption test was 13.97 kg/g.
Comparative example 1
A preparation method of an adsorbent refined by penicillin fermentation liquor comprises the following specific scheme:
adding 50g of melamine formaldehyde resin prepolymer, 2g of surfactant dodecyl triphenyl phosphonium bromide, 5g of ethyl acetate, 14g of curing agent imido disulfonic acid propyl amine salt and 3g of pore-foaming agent into a reaction kettle, controlling the temperature to be 40 ℃, uniformly stirring and mixing, then adding 80g of water and 0.1g of glucan hydroxypropyl trimethyl ammonium chloride, uniformly stirring and mixing to form suspended emulsion, controlling the temperature to be 80 ℃, reacting for 24 hours, washing the microspheres clean after the reaction is finished, removing the pore-foaming agent, obtaining melamine resin porous microspheres, and drying to obtain the penicillin fermentation liquor refining adsorbent.
The melamine-formaldehyde resin is a precondensate of melamine and formaldehyde, and the molar ratio of the melamine to the formaldehyde during synthesis is 0.8: 1.
The pore-foaming agent is 1, 4-butanediol.
The adsorbent prepared in the experiment has the specific surface area of 1548.9m2The mass of the filtrate passing through the adsorption experiment was 6.07 kg/g.
Comparative example 2
A preparation method of an adsorbent refined by penicillin fermentation liquor comprises the following specific scheme:
adding 50g of melamine formaldehyde resin prepolymer, 2g of surfactant dodecyl triphenyl phosphonium bromide, 5g of ethyl acetate, 14g of curing agent imido disulfonic acid propyl amine salt and 3g of pore-foaming agent into a reaction kettle according to the mass parts, controlling the temperature to be 40 ℃, uniformly stirring and mixing, then adding 80g of water and 0.1g of glucan hydroxypropyl trimethyl ammonium chloride, uniformly stirring and mixing to form suspended emulsion, controlling the temperature to be 80 ℃, reacting for 24 hours, washing the microspheres clean after the reaction is finished, and removing the pore-foaming agent to obtain melamine resin porous microspheres; adding the obtained microspheres into 300g of isopropanol, adding 100g of 10% microporous surface modifier, stirring and mixing uniformly, controlling the temperature to be 50 ℃, then dropwise adding 50g of 5% azodiisobutyronitrile solution into a reaction kettle, stirring and reacting for 3 hours after the dropwise adding is finished, taking out the microspheres after the reaction is finished, washing with water, and drying to obtain the penicillin fermentation liquor refining adsorbent.
The preparation method of the microporous surface modifier comprises the following steps:
adding 50g of isopropanol, 40g of vinyl caprolactam, 5g of diallyl tetramethyl disiloxane and 1g of allylamine hydrochloride into a reaction kettle according to the mass parts, uniformly stirring and mixing, then dissolving 0.01g of azobisisobutyronitrile into 10g of isopropanol, dropwise adding into the reaction kettle, controlling the temperature at 40 ℃, carrying out prepolymerization for 10min, cooling to room temperature, adding isopropanol, diluting to 10%, and thus obtaining the microporous surface modifier.
The melamine-formaldehyde resin is a precondensate of melamine and formaldehyde, and the molar ratio of the melamine to the formaldehyde during synthesis is 0.8: 1.
The pore-foaming agent is 1, 4-butanediol.
The adsorbent prepared in the experiment has the specific surface area of 1534.1m2The mass of the filtrate passing through the adsorption experiment was 10.17 kg/g.
Comparative example 3
A preparation method of an adsorbent refined by penicillin fermentation liquor comprises the following specific scheme:
adding 50g of melamine formaldehyde resin prepolymer, 2g of surfactant dodecyl triphenyl phosphonium bromide, 5g of ethyl acetate and 14g of curing agent imido disulfonic acid propyl alcohol amine salt into a reaction kettle according to the mass parts, controlling the temperature to be 40 ℃, uniformly stirring and mixing, then adding 80g of water and 0.1g of glucan hydroxypropyl trimethyl ammonium chloride, uniformly stirring and mixing to form suspended emulsion, controlling the temperature to be 80 ℃, reacting for 24 hours, washing the microspheres clean after the reaction is finished, and removing a pore-forming agent to obtain the melamine resin porous microspheres; adding the obtained microspheres into 300g of isopropanol, adding 100g of 10% microporous surface modifier, stirring and mixing uniformly, controlling the temperature to be 50 ℃, then dropwise adding 50g of 5% azodiisobutyronitrile solution into a reaction kettle, stirring and reacting for 3 hours after the dropwise adding is finished, taking out the microspheres after the reaction is finished, washing with water, and drying to obtain the penicillin fermentation liquor refining adsorbent.
The preparation method of the microporous surface modifier comprises the following steps:
adding 50g of isopropanol, 40g of vinyl caprolactam, 5g of diallyl tetramethyl disiloxane, 10g of diacetone acrylamide and 1g of allylamine hydrochloride into a reaction kettle according to the mass parts, uniformly stirring and mixing, then dissolving 0.01g of azobisisobutyronitrile into 10g of isopropanol, dropwise adding into the reaction kettle, controlling the temperature to be 40 ℃, pre-polymerizing for 10min, cooling to room temperature, adding isopropanol, diluting to 10%, and thus obtaining the microporous surface modifier.
The melamine-formaldehyde resin is a precondensate of melamine and formaldehyde, and the molar ratio of the melamine to the formaldehyde during synthesis is 0.8: 1.
The adsorbent prepared in the experiment has the specific surface area of 874.5m2The mass of the filtrate passing through the adsorption experiment was 8.19 kg/g.
Claims (6)
1. A preparation method of an adsorbent refined by penicillin fermentation liquor comprises the following specific scheme:
adding 50-80 parts of melamine formaldehyde resin prepolymer, 2-7 parts of surfactant dodecyl triphenyl phosphonium bromide, 5-10 parts of ethyl acetate, 14-22 parts of curing agent imido disulfonic acid propyl amine salt and 3-8 parts of pore-foaming agent into a reaction kettle, controlling the temperature to be 40-60 ℃, stirring and mixing uniformly, then adding 80-100 parts of water and 0.1-3 parts of glucan hydroxypropyl trimethyl ammonium chloride, stirring and mixing uniformly to form suspended emulsion, controlling the temperature to be 80-105 ℃, reacting for 12-24 hours, washing the microspheres clean after the reaction is finished, removing the pore-foaming agent, and obtaining melamine resin porous microspheres; adding the obtained microspheres into 500 parts of 300-parts of isopropanol, adding 10-15% of microporous surface modifier into 300 parts of 100-300-parts of isopropanol, uniformly stirring and mixing, controlling the temperature to be 50-70 ℃, then dropwise adding 50-80 parts of 5-10% azodiisobutyronitrile solution into a reaction kettle, stirring and reacting for 3-5h after dropwise adding is finished, taking out the microspheres after the reaction is finished, and washing and drying to obtain the penicillin fermentation liquor refining adsorbent.
2. The method for preparing penicillin fermentation broth refining adsorbent as claimed in claim 1, wherein: the preparation method of the microporous surface modifier comprises the following steps:
adding 50-80 parts by mass of isopropanol, 40-60 parts by mass of vinyl caprolactam, 5-10 parts by mass of diallyl tetramethyl disiloxane, 10-20 parts by mass of diacetone acrylamide and 1-5 parts by mass of allylamine hydrochloride into a reaction kettle, uniformly stirring and mixing, then dissolving 0.01-0.5 part by mass of azobisisobutyronitrile into 10-15 parts by mass of isopropanol, dropwise adding into the reaction kettle, controlling the temperature to be 40-50 ℃, carrying out prepolymerization for 10-30min, cooling to room temperature, adding isopropanol to dilute to 10-15%, and thus obtaining the microporous surface modifier.
3. The method for preparing penicillin fermentation broth refining adsorbent as claimed in claim 1, wherein: the melamine-formaldehyde resin is a precondensate of melamine and formaldehyde, and the molar ratio of the melamine to the formaldehyde during synthesis is 0.8-2.4: 1.
4. The method for preparing penicillin fermentation broth refining adsorbent as claimed in claim 1, wherein: the pore-foaming agent is 1, 4-butanediol or polyethylene glycol 400 or polyethylene glycol 1000.
5. The method for preparing penicillin fermentation broth refining adsorbent as claimed in claim 1, wherein: the using method of the penicillin fermentation liquor refining adsorbent comprises the following steps: and (2) passing the low-titer filtrate generated in the penicillin production process through a column with the penicillin fermentation broth refined adsorbent as a filler, adsorbing and concentrating the penicillin in the column, taking out the penicillin fermentation broth refined adsorbent, and soaking the penicillin fermentation broth refined adsorbent in an acidic aqueous solution with the pH value of 1-4 for 5-10 hours to complete the desorption of the penicillin.
6. The method for preparing penicillin fermentation broth refining adsorbent as claimed in claim 1, wherein: after the penicillin fermentation liquor refining adsorbent is used, the adsorbent is soaked in alkali liquor with the concentration of 0.1-0.5mol/L for 3-8 hours, and then is washed by hydrophilic for 5-10min, so that the recovery can be completed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911193659.2A CN110841608A (en) | 2019-11-28 | 2019-11-28 | Preparation method of penicillin fermentation liquor refined adsorbent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911193659.2A CN110841608A (en) | 2019-11-28 | 2019-11-28 | Preparation method of penicillin fermentation liquor refined adsorbent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110841608A true CN110841608A (en) | 2020-02-28 |
Family
ID=69605959
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911193659.2A Withdrawn CN110841608A (en) | 2019-11-28 | 2019-11-28 | Preparation method of penicillin fermentation liquor refined adsorbent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110841608A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101250247A (en) * | 2008-03-13 | 2008-08-27 | 华东理工大学 | Magnetic polymer microsphere for enzyme immobilization and preparation method thereof |
| CN101696210A (en) * | 2009-08-28 | 2010-04-21 | 海南美大制药有限公司 | High-purity antibiotic medicinal compound |
| CN108102119A (en) * | 2017-12-21 | 2018-06-01 | 贺州宝兴新材料有限公司 | A kind of preparation method of melamine resin hollow microsphere |
| CN108929416A (en) * | 2018-07-03 | 2018-12-04 | 南京林业大学 | A kind of synthetic method and its application of melamine resin nanosphere |
| CN109942768A (en) * | 2019-03-28 | 2019-06-28 | 太尔胶粘剂(广东)有限公司 | Spherical porous melamine-formaldehyde-thiocarbamide fluoropolymer resin and preparation method thereof |
-
2019
- 2019-11-28 CN CN201911193659.2A patent/CN110841608A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101250247A (en) * | 2008-03-13 | 2008-08-27 | 华东理工大学 | Magnetic polymer microsphere for enzyme immobilization and preparation method thereof |
| CN101696210A (en) * | 2009-08-28 | 2010-04-21 | 海南美大制药有限公司 | High-purity antibiotic medicinal compound |
| CN108102119A (en) * | 2017-12-21 | 2018-06-01 | 贺州宝兴新材料有限公司 | A kind of preparation method of melamine resin hollow microsphere |
| CN108929416A (en) * | 2018-07-03 | 2018-12-04 | 南京林业大学 | A kind of synthetic method and its application of melamine resin nanosphere |
| CN109942768A (en) * | 2019-03-28 | 2019-06-28 | 太尔胶粘剂(广东)有限公司 | Spherical porous melamine-formaldehyde-thiocarbamide fluoropolymer resin and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 姚文山: "《国家基本药物处方集》", 28 February 2019, 天津科学技术出版社 * |
| 黄金敏，方应权: "《全国高职高专药学类专业规划教材 第二轮 药物化学 第2版》", 31 August 2019 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US9139856B2 (en) | Process for production of galactooligosaccharides (GOS) | |
| CN104004002B (en) | A kind of method directly being prepared 6-amino-penicillanic acid by penicillin fermentation liquid | |
| CN107012138B (en) | Silicon/carbon-based composite immobilized enzyme environment-friendly material and preparation method thereof | |
| CN107574201A (en) | Using the method for fermentation method production β thymidines | |
| CN102154429A (en) | One-step enzymatic method for preparing 7-aminocephalosporanic acid | |
| CN103641895B (en) | Method for producing vancomycin hydrochloride by utilizing vancomycin fermentation broth | |
| US20100041124A1 (en) | Multi-stage cstr bioreactor system equipped with cell recycle unit | |
| CN201988375U (en) | Cyclohexanone ammonia oximation reaction catalyst separation device | |
| CN110841608A (en) | Preparation method of penicillin fermentation liquor refined adsorbent | |
| CN109553650B (en) | Water phase extraction method of erythromycin fermentation liquor | |
| CN103059105A (en) | Method for extraction of colistin sulphate | |
| CN110294726A (en) | The preparation method of ISOASCORBIC ACID potassium | |
| CN1986823A (en) | Cefradine preparing process | |
| CN1238514C (en) | Method for producing acrylamide using film technique microbiological transformation | |
| CN107345233B (en) | Method for preparing gamma-aminobutyric acid by 732 resin continuous circulation auxiliary immobilized cells | |
| CN105384151A (en) | Comprehensive utilization and treatment method of waste sulfuric acid | |
| CN101875889A (en) | Immobilizing method for yellow rice wine brewing yeast | |
| CN111545177A (en) | Preparation method of modified magnetic bamboo fiber composite adsorbent | |
| CN112359028B (en) | Biosynthesis method of tomoxetine intermediate and carbonyl reductase | |
| CN106554374A (en) | A kind of method that purification prepares vistamycin in fermentation liquid from ribostamycin | |
| CN102153605B (en) | Method for purifying Mizoribine | |
| CN100334221C (en) | Process for preparing acrylamide aqueous solution through direct method cell enzyme reaction | |
| CN106188376A (en) | A kind of preparation method of colistin sulfate purification adsorbent | |
| CN107651758B (en) | Method for preparing organic fertilizer by using starch wastewater | |
| CN114107114A (en) | Preparation method of immobilized neurospora |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20200228 |