CN108707247A - The preparation method of resin for antibiotic purification - Google Patents
The preparation method of resin for antibiotic purification Download PDFInfo
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- CN108707247A CN108707247A CN201810241390.XA CN201810241390A CN108707247A CN 108707247 A CN108707247 A CN 108707247A CN 201810241390 A CN201810241390 A CN 201810241390A CN 108707247 A CN108707247 A CN 108707247A
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- resin
- antibiotic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
-
- 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
- B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/02—Chemical treatment or coating of shaped articles made of macromolecular substances with solvents, e.g. swelling agents
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/05—Elimination by evaporation or heat degradation of a liquid phase
- C08J2201/0502—Elimination by evaporation or heat degradation of a liquid phase the liquid phase being organic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
Abstract
The invention discloses a kind of preparation methods of the resin for antibiotic purification, include the following steps：1) oil phase is prepared；2) water phase is prepared；3) oil phase and aqueous phase reactions, make mixed liquor gradually be solidified into milky white granules, obtain Archon；4) by the Archon of gained chloromethylation solvent expansion, 6H is reacted under the action of catalyst iron chloride, chlorine ball is obtained after washing is dry；5) remaining pore-foaming agent in chlorine ball is eluted, macropore cation resin semi-finished product are made.6) above-mentioned wet resin 100ml is taken, the liquid caustic soda of a concentration of 20-25% of 300ml is added, 75-80 DEG C of reaction 8-12H, column is filled after reaction, it is washed with isometric deionized water, column 4-5H is crossed by hydrochloric acid, is then washed with deionized water to neutrality, Macroporous weak acid cation exchange resin is made, the purification rate for being used for purifying antibiotic using resin made from this method significantly improves.
Description
Technical field
The present invention relates to antibiotic to purify field, and in particular to a kind of preparation method of resin for antibiotic purification.
Background technology
The common isolation and purification method of antibiotic mainly has solvent extraction, absorption method, ion-exchange, precipitation and knot
Crystalline substance, chromatographic isolation etc., solvent extraction are the differences using solute distribution coefficient between immiscible two-phase, and solute is made to select
A kind of being transferred in another solvent from solvent for selecting property and the method for being purified or being concentrated, this method is easy to operate, but purifies
Rate is not very high；Absorption method is to be adsorbed antibiotic on the sorbent using the molecular attraction between adsorbent and antibiotic,
The active charcoal of common adsorbent, aluminium oxide, macroporous absorbent resin etc..Macroporous absorbent resin is present microorganism natural products point
Develop one of most rapid, most active branch from technical field, it has gradually replaced the adsorbents such as activated carbon and aluminium oxide at present,
Increasingly consequence is shown in antibiotic industry.Macroporous absorbent resin is suitable for adsorbing various antibiotic, it is not only
Adsorbable fat-soluble compound, and water soluble compound can be adsorbed.In recent years, domestic application macroporous absorbent resin is divided
From, extraction, concentration, purifying antibiotic cover the resin purification rate phase for being currently known all types of antibiotic, but using
For traditional solvent extraction without too big raising.
Invention content
The present invention provides a kind of preparation method of the resin for antibiotic purification, is used for using resin made from this method
The purification rate of purification antibiotic significantly improves.
To achieve the goals above, the present invention uses following technical scheme：A kind of system of resin for antibiotic purification
Preparation Method includes the following steps：
1) take 100-200 parts and 10-20 parts 5-10 parts of styrene, acrylic acid divinylbenzenes as monomer by weight,
The pore-foaming agent isooctane of the 10-15% of monomer mass is added, the oxygen benzoyl of monomer mass 1-2% is added as initiator,
It is sufficiently mixed stirring 10-12H in reaction kettle and obtains oil phase；
2) it takes 50-100 parts of polyethylene of dispersing agent alcohol to be added in 700 parts of deionized waters, forms water phase；
3) oil phase of step 1) is mixed with the water phase of step 2), is thoroughly mixed in a kettle, and 40-50 is heated to
DEG C, 2H is reacted, is gradually heated up to 70-80 DEG C, reacts 4H, then be heated up to 90-100 DEG C, 8H is reacted, mixed liquor is made gradually to be solidified into
Milky white granules obtain Archon；
4) by the Archon of gained chloromethylation solvent expansion, 6H is reacted under the action of catalyst iron chloride, washing is dry
Chlorine ball is obtained after dry；
5) by gained chlorine ball move into elution column in, be passed through temperature be 140-160 DEG C vapor be used as eluant, eluent, elute
4H elutes remaining pore-foaming agent in chlorine ball, and macropore cation resin semi-finished product are made.
6) above-mentioned wet resin 100ml is taken, the liquid caustic soda of a concentration of 20-25% of 300ml is added, 75-80 DEG C is reacted 8-12H, instead
Column is filled after answering, is washed with isometric deionized water, column 4-5H is crossed by hydrochloric acid, is then washed with deionized water to neutrality, system
Obtain Macroporous weak acid cation exchange resin.
Exchanger resin water content 50-58% made from this method, rate of small round spheres >=90% after mill, average pore size 27-28nm are used
Exchanger resin made from this law purifies antibiotic, and antibiotic purification rate is 95-99%, full exchange capacity 4.8-4.9mmlo
(dry)/g, compared with the existing technology for, made from this law exchanger resin purification antibiotic purification rate significantly improve.
Specific implementation mode
In order to make the technical means, the creative features, the aims and the efficiencies achieved by the present invention be easy to understand, tie below
It closes specifically, the present invention is furture elucidated.
Embodiment 1
It takes 100 parts and 10 parts 5 parts of styrene, acrylic acid divinylbenzenes as monomer by weight, monomer mass is added
10-% pore-foaming agent isooctane, be added monomer mass 1% oxygen benzoyl as initiator, be sufficiently mixed in a kettle
Stirring 10H obtains oil phase；Take 50 parts of polyethylene of dispersing agent alcohol to be added in 700 parts of deionized waters, form water phase, by water phase and
Oil phase is thoroughly mixed in a kettle, is heated to 40 DEG C, reacts 2H, is gradually heated up to 70 DEG C, reacts 4H, then be heated up to 90
DEG C, 8H is reacted, so that mixed liquor is gradually solidified into milky white granules, obtains Archon；The Archon of gained is swollen with chloromethylation solvent
It is swollen, 6H is reacted under the action of catalyst iron chloride, and chlorine ball is obtained after washing is dry；Gained chlorine ball is moved into elution column, is led to
Enter the vapor that temperature is 140 DEG C and be used as eluant, eluent, elute 4H, elute remaining pore-foaming agent in chlorine ball, obtained macropore sun from
Subtree fat semi-finished product.
Above-mentioned wet resin 100ml is taken, the liquid caustic soda of a concentration of 20-25% of 300ml is added, 75 DEG C are reacted 8H, after reaction
Column is filled, is washed with isometric deionized water, column 4-5H is crossed by hydrochloric acid, is then washed with deionized water to neutrality, it is weak that macropore is made
Acid cation exchange resin.
Exchanger resin water content 50% obtained, rate of small round spheres 95% after mill, average pore size 27.5nm is using made from this law
Exchanger resin purifies antibiotic, and antibiotic purification rate is 99%, full exchange capacity 4.8mmlo (dry)/g.
Embodiment 2
It takes 200 parts and 20 parts 10 parts of styrene, acrylic acid divinylbenzenes as monomer by weight, monomer mass is added
10-15% pore-foaming agent isooctane, be added monomer mass 2% oxygen benzoyl as initiator, in a kettle fully mix
It closes stirring 12H and obtains oil phase；It takes 100 parts of polyethylene of dispersing agent alcohol to be added in 700 parts of deionized waters, water phase is formed, by water phase
It is thoroughly mixed in a kettle with oil phase, is heated to 50 DEG C, react 2H, be gradually heated up to 80 DEG C, react 4H, then be heated up to
100 DEG C, 8H is reacted, so that mixed liquor is gradually solidified into milky white granules, obtains Archon；By the Archon of gained chloromethylation solvent
Expansion reacts 6H under the action of catalyst iron chloride, chlorine ball is obtained after washing is dry；Gained chlorine ball is moved into elution column,
It is passed through the vapor that temperature is 160 DEG C and is used as eluant, eluent, elute 4H, elute remaining pore-foaming agent in chlorine ball, it is positive that macropore is made
Ion exchange resin semi-finished product.
Above-mentioned wet resin 100ml is taken, the liquid caustic soda of 300ml a concentration of 25% is added, 80 DEG C of reaction 12H are filled after reaction
Column is washed with isometric deionized water, crosses column 5H by hydrochloric acid, be then washed with deionized water to neutrality, and macropore faintly acid is made
Cation exchange resin.
Exchanger resin water content 58% obtained, rate of small round spheres 97% after mill, average pore size 28nm are handed over using this law is obtained
Resin purification antibiotic is changed, antibiotic purification rate is 99%, full exchange capacity 4.85mmlo (dry)/g.
Reference examples
Resin finished product made from any mode in the prior art is taken to carry out purification antibiotic, antibiotic purification rate is
88%, exchange capacity 4.28mmlo (dry)/g.
The basic principles and main features and the features of the present invention of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement is both fallen in the range of claimed invention.The scope of protection of present invention is by appended claims
And its equivalent thereof.
Claims (3)
1. a kind of preparation method of resin for antibiotic purification, it is characterised in that：Include the following steps：
1) it takes 100-200 parts and 10-20 parts 5-10 parts of styrene, acrylic acid divinylbenzenes as monomer by weight, is added
The pore-foaming agent isooctane of the 10-15% of monomer mass is added the oxygen benzoyl of monomer mass 1-2% as initiator, is reacting
It is sufficiently mixed stirring 10-12H in kettle and obtains oil phase；
2) it takes 50-100 parts of polyethylene of dispersing agent alcohol to be added in 700 parts of deionized waters, forms water phase；
3) oil phase of step 1) is mixed with the water phase of step 2), is thoroughly mixed in a kettle, is heated to 40-50 DEG C, instead
2H is answered, is gradually heated up to 70-80 DEG C, reacts 4H, then be heated up to 90-100 DEG C, 8H is reacted, so that mixed liquor is gradually solidified into milky white
Coloured particles obtain Archon；
4) by the Archon of gained chloromethylation solvent expansion, 6H is reacted under the action of catalyst iron chloride, after washing is dry
Obtain chlorine ball；
5) by gained chlorine ball move into elution column in, be passed through temperature be 140-160 DEG C vapor be used as eluant, eluent, elution 4H, wash
Deviate from remaining pore-foaming agent in chlorine ball, macropore cation resin semi-finished product are made.
6) above-mentioned wet resin 100ml is taken, the liquid caustic soda of a concentration of 20-25% of 300ml, 75-80 DEG C of reaction 8-12H, reaction knot is added
Column is filled after beam, is washed with isometric deionized water, column 4-5H is crossed by hydrochloric acid, is then washed with deionized water to neutrality, is made big
Hole weak-acid cation-exchange resin.
2. the preparation method for the resin of antibiotic purification as described in claim 1, it is characterised in that：Described in step 1)
Pore-foaming agent be pentane.
3. the preparation method of the resin described in claim 1 for antibiotic purification, it is characterised in that：It is rinsed in step 6)
A concentration of 10-15% of hydrochloric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810241390.XA CN108707247A (en) | 2018-03-22 | 2018-03-22 | The preparation method of resin for antibiotic purification |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810241390.XA CN108707247A (en) | 2018-03-22 | 2018-03-22 | The preparation method of resin for antibiotic purification |
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| Publication Number | Publication Date |
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| CN108707247A true CN108707247A (en) | 2018-10-26 |
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| CN201810241390.XA Pending CN108707247A (en) | 2018-03-22 | 2018-03-22 | The preparation method of resin for antibiotic purification |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110314668A (en) * | 2019-07-08 | 2019-10-11 | 湖南城市学院 | A kind of D151 resin and its preparation method and application of salt tolerance ferric ion load |
| CN111019037A (en) * | 2019-12-05 | 2020-04-17 | 安徽皖东树脂科技有限公司 | Preparation method of special resin for magnesium sulfate mother liquor decolorization |
| CN111036180A (en) * | 2019-12-05 | 2020-04-21 | 安徽皖东树脂科技有限公司 | Preparation process of macroporous adsorption resin for extracting noble metal and rare metal |
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| CN101693750A (en) * | 2009-10-16 | 2010-04-14 | 崔建 | Preparation method of macroporous absorption resin |
| CN103951780A (en) * | 2014-05-13 | 2014-07-30 | 安徽三星树脂科技有限公司 | Preparation method of macroporous weak-acidity cation exchange resin |
| CN104844744A (en) * | 2015-03-30 | 2015-08-19 | 山东鲁抗立科药业有限公司 | Resin with specific adsorption for cephalosporin C and preparation method therefor |
| CN105504128A (en) * | 2015-12-16 | 2016-04-20 | 宁波争光树脂有限公司 | Adsorbent resin used for treating phenolic wastewater and preparing method and application thereof |
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2018
- 2018-03-22 CN CN201810241390.XA patent/CN108707247A/en active Pending
Patent Citations (6)
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|---|---|---|---|---|
| JPH07215901A (en) * | 1994-01-28 | 1995-08-15 | Mitsui Toatsu Chem Inc | Method for separating phenol |
| CN1923368A (en) * | 2005-08-27 | 2007-03-07 | 兰爱克谢斯德国有限责任公司 | Weakly acid cation exchange resin |
| CN101693750A (en) * | 2009-10-16 | 2010-04-14 | 崔建 | Preparation method of macroporous absorption resin |
| CN103951780A (en) * | 2014-05-13 | 2014-07-30 | 安徽三星树脂科技有限公司 | Preparation method of macroporous weak-acidity cation exchange resin |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110314668A (en) * | 2019-07-08 | 2019-10-11 | 湖南城市学院 | A kind of D151 resin and its preparation method and application of salt tolerance ferric ion load |
| CN110314668B (en) * | 2019-07-08 | 2022-02-01 | 湖南城市学院 | Salt-tolerant ferric ion loaded D151 resin and preparation method and application thereof |
| CN111019037A (en) * | 2019-12-05 | 2020-04-17 | 安徽皖东树脂科技有限公司 | Preparation method of special resin for magnesium sulfate mother liquor decolorization |
| CN111036180A (en) * | 2019-12-05 | 2020-04-21 | 安徽皖东树脂科技有限公司 | Preparation process of macroporous adsorption resin for extracting noble metal and rare metal |
| CN111019037B (en) * | 2019-12-05 | 2022-04-22 | 安徽皖东树脂科技有限公司 | Preparation method of special resin for magnesium sulfate mother liquor decolorization |
| CN111036180B (en) * | 2019-12-05 | 2022-07-12 | 安徽皖东树脂科技有限公司 | Preparation process of macroporous adsorption resin for extracting noble metal and rare metal |
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Application publication date: 20181026 |