CN107029807A - A kind of preparation method of quick anion chromatographic column packing - Google Patents
A kind of preparation method of quick anion chromatographic column packing Download PDFInfo
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- CN107029807A CN107029807A CN201710286924.6A CN201710286924A CN107029807A CN 107029807 A CN107029807 A CN 107029807A CN 201710286924 A CN201710286924 A CN 201710286924A CN 107029807 A CN107029807 A CN 107029807A
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- 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
- B01J41/00—Anion exchange; Use of material as anion exchangers; Treatment of material for improving the anion exchange properties
- B01J41/20—Anion exchangers for chromatographic processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/26—Selective adsorption, e.g. chromatography characterised by the separation mechanism
- B01D15/36—Selective adsorption, e.g. chromatography characterised by the separation mechanism involving ionic interaction
- B01D15/361—Ion-exchange
- B01D15/363—Anion-exchange
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- 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
- B01J41/00—Anion exchange; Use of material as anion exchangers; Treatment of material for improving the anion exchange properties
- B01J41/08—Use of material as anion exchangers; Treatment of material for improving the anion exchange properties
- B01J41/12—Macromolecular compounds
- B01J41/14—Macromolecular compounds obtained by reactions only involving unsaturated carbon-to-carbon bonds
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Abstract
The present invention is a kind of preparation method for the quick anion chromatographic column packing for being related to ion chromatographic column filler, applied to the quick anion chromatographic column of making.The present invention takes supported matrix to be the high crosslinking hydrophilic ethyl styrene divinylbenzene filler that sulfonic acid group is contained on surface, functional matrix is the Nano-grade latex that monomer 1-chloro-4-methyl-benzene and divinylbenzene use microemulsion polymerization method copolymerization with monomer vinyl acetate or GMA, through hydrolysis, demulsification cleaning, quaternized generation quatemized copolymer Nano-grade latex, supported matrix and functional matrix agglomeration are made to the technical scheme of quick anion exchange resin, solve existing latex agglomeration type anion chromatographic filling material, supported matrix sulfonation hardly possible control, it is inconsistent between batch, sulfonic acid surfactant radix amount is excessive, exchange capacity is relatively large, surfactant- free emulsion polymerization synthetic latex size distribution is uneven and particle is big, the anion chromatographic column column capacity being made is of a relatively high, the slower technical problem of separating rate.
Description
Technical field
Concretely it is a kind of preparation side of quick anion chromatographic column packing the present invention relates to ion chromatographic column filler
Method.
Background technology
Zeng Xueling,《The preparation and evaluation of latex agglomeration type anion chromatographic filling material》, Zhejiang University, master's opinion in 2016
Text discloses a kind of supported matrix of sulfonating surface and carries out surface agglomeration with quaternized Nano-grade latex particle, and latex agglomeration is made
The preparation method of type anion chromatographic filling material.In above-mentioned paper, supported matrix is utilized in styrene-divinylbenzene EVA
It is the method preparation of sulfonating surface, it has the disadvantage that sulfonation degree is difficult to control to, and is difficult between batch unanimously, is easily caused table
Face sulfonic group quantity is excessive, causes exchange capacity relatively large；Latex is that the resin system of styrene-t epoxy third is used
Surfactant- free emulsion polymerization is synthesized, particle diameter 300nm or more, and latex particle is big and size distribution is uneven；Surfactant- free emulsion polymerization
The reactivity of the epoxide group of the fat of monomer methacrylic acid epoxy third used is high, easily reacts, causes attached with tertiary amine
Chromatographic column column capacity after poly- is of a relatively high, and separating rate is slower.
The content of the invention
The invention solves the problems that in prepared by existing latex agglomeration type anion chromatographic filling material, supported matrix sulfonation degree is difficult to control
It is difficult between system, batch unanimously, is easily caused sulfonic acid surfactant radix amount excessively, causes exchange capacity relatively large；Without soap
Emulsion polymerization synthetic latex size distribution is uneven and particle is big；The anion chromatographic column column capacity being made is of a relatively high, separation
Slow technical problem is easily controlled there is provided a kind of supported matrix sulfonation process, sulfonic acid surfactant base moderate number, nano-emulsion
Glue exchange capacity is suitable, and granularity is small and relatively uniform, and the anion chromatographic column column capacity being made is moderate, fast quick of separating rate
The preparation method of anion chromatographic column packing.
In order to solve above-mentioned technical problem, the present invention is adopted the technical scheme that：A kind of quick anion chromatographic column is filled out
The preparation method of material, including supported matrix carry out agglomeration with modified copolymer nano latex, and described supported matrix is monomer
The mixture of ethyl styrene and divinylbenzene is reacted with ion monomer styrene sulfonic acid potassium on surface, and generation surface is contained
High crosslinking hydrophilic ethyl styrene-divinylbenzene filler of sulfonic acid group；The copolymer nano latex of described modification is by monomer
1-chloro-4-methyl-benzene and divinylbenzene use micro-emulsion polymerization with monomer vinyl acetate or GMA
Method copolymerization is formed, the copolymer nano latex is hydrolyzed, the cleaning that is demulsified, quaterisation generation quatemized copolymer nano-emulsion
Glue；Quatemized copolymer Nano-grade latex and described surface are contained to high crosslinking hydrophilic ethyl styrene-diethyl of sulfonic acid group
Alkene benzene filler carries out agglomeration, and quick anion exchange resin is made.
Quickly analysis is the effective means for improving chromatography of ions operating efficiency to anion.For conventional seven kinds of anion analysis
Anion chromatographic column analysis time it is general more than ten minutes, hydrophilic anions chromatograph packing material, due to being often used to separation
Oxygen-containing halate, while fluorine ion requires to efficiently separate with water negative peak, therefore its analysis time is generally more than 20 minutes, fits
Together in the lab analysis to anion.And portable chromatography of ions scene or Emergent detection, then often because time, battery supply
The limitation of electricity or reagent is, it is necessary to which quick analyze, therefore quick anion analysis just shows to portable instrument or emergent Site Detection
It must be even more important.The analyze speed for improving anion is technical problem urgently to be resolved hurrily, anion chromatographic column prepared by the present invention
The chromatographic column that filler is loaded is shortened within six minutes to the analysis time of seven kinds of anion, realizes quick point to anion
Analysis.The present invention uses Chinese invention patent application, the A of application publication number CN 104788603,《A kind of hydrophilic ionic is to chromatogram
The synthetic method of filler》Contain the high crosslinking hydrophilic ethyl of sulfonic acid group in disclosed chromatograph packing material synthetic method, the surface of preparation
Styrene-divinylbenzene filler is as supported matrix, and it is micron order high molecular polymer, and sulfonation process is easily controlled, only
There is the slight moderate potassium sulfonate function base for being capable of Liquidity limit on its surface, compared with traditional sulfate resin, exchange and hold
Amount is small, and capacity is suitably easily-controllable, and resin uniformity is good.The copolymer nano latex of synthesis is by monomer 1-chloro-4-methyl-benzene and two
Vinyl benzene is with monomer vinyl acetate or GMA using the method copolymerization of micro-emulsion polymerization
Binary polymerization system.The copolymer nano latex particle size of the method copolymerization of micro-emulsion polymerization is evenly distributed on 50nm or so.
The reason for adding the third monomer hydrophilic olefin class material, monomer vinyl acetate or GMA copolymerization
Be, one, the density that copolymer nano latex chloromethyl can be reduced, so reduce it is quaternized after exchange capacity, secondly
It is after the third hydrophilic olefin class Substance P hydrolysis added that hydroxyl can be generated, increases the hydrophily of copolymer nano latex,
Filler can be effectively improved to hydrophobic and polarizable anions（Such as Br-And NO3 -）Absorption and separation.Copolymer after copolymerization is received
Rice milk glue is first passed through after hydrolysis, demulsification cleaning, then carries out quatemized copolymer nanometer of the quaterisation generation with positive charge
Latex, with anion exchange function.Reaction is hydrolyzed in copolymer nano latex, make hydrophilic olefin class vinyl acetate or
GMA monomer carries hydroxyl, increases the hydrophily of copolymer nano latex；And copolymer nano latex
In 1-chloro-4-methyl-benzene do not influenceed by hydrolysis.The introducing of vinyl acetate or GMA, not only
The effective content of cation exchange groups in copolymer nano latex is reduced, the hydrophily of latex is also add, reaches that separating rate is fast
Purpose.Quatemized copolymer Nano-grade latex carries out agglomeration as functional matrix and supported matrix, and obtained quick anion is handed over
The capacity for changing the chromatographic column that resin is made is suitable, controllability very well, the characteristics of with quick separating, it is adaptable to portable instrument or
The demand of emergent Site Detection.
The degree of cross linking of copolymer nano latex of microemulsion polymerization method copolymerization is used for 2-10%.
The degree of cross linking of copolymer nano latex of microemulsion polymerization method copolymerization is used for 4-8%.4-8% is preferred number
According to.
Copolymer nano latex is in 0.2-1.5mol/L sulfuric acid solution, 40-80 DEG C of temperature, time 4.0-20.0h bar
It is hydrolyzed under part.Reaction is hydrolyzed in copolymer nano latex in acid condition.
Copolymer nano latex is in 0.5-1.2mol/L sulfuric acid solution, 55-65 DEG C of temperature, time 5.5-16h condition
Under be hydrolyzed.0.5-1.2mol/L sulfuric acid solution, 55-65 DEG C of temperature, time 5.5-16.0h is preferred data.
The reagent of quaterisation is the short carbon chain tertiary amine of 1-4 carbon atom after the hydrolysis of copolymer nano latex.
The quality of vinyl acetate or GMA is the 4.0- of monomer 1-chloro-4-methyl-benzene quality
10.5%.Monomer 1-chloro-4-methyl-benzene and divinylbenzene and the third monomer hydrophilic olefin class material, monomer acetic acid of addition
Vinyl acetate or GMA use microemulsion polymerization method copolymerization, reduce the functional group of copolymer nano latex
Density.The ratio of vinyl acetate or GMA and monomer 1-chloro-4-methyl-benzene quality is adjusted, control is reached
The function radix amount of copolymer nano latex processed.Less than 4.0%, column capacities are too high, it is impossible to realize quick separating, are more than
10.5%, column capacities are too low, and side reaction causes performance not good during polymerization, it is impossible to separate conventional anion well.
The quality of vinyl acetate or GMA is the 6.0- of monomer 1-chloro-4-methyl-benzene quality
8.5%.6.0-8.5% is preference data.
It is an advantage of the invention that：Monomer 1-chloro-4-methyl-benzene and divinylbenzene and monomer vinyl acetate or metering system
Acid glycidyl ester using microemulsion polymerization method copolymerization form copolymer nano latex, be hydrolyzed, the cleaning that be demulsified, it is quaternized instead
High crosslinking hydrophilic ethyl styrene-divinylbenzene that the quatemized copolymer Nano-grade latex that should be generated contains sulfonic acid group with surface
Filler carries out agglomeration, obtained quick anion exchange resin.High crosslinking hydrophilic ethyl styrene-divinylbenzene filler sulfonation
Journey is easily controlled, and sulfonic acid surfactant base moderate number, copolymer nano latex exchange capacity is relatively suitable, latex epigranular, system
Into anion chromatographic column column capacity it is suitable, very well, separating rate is fast for controllability, is particularly suitable for use in portable instrument or emergent existing
The demand of field detection.
Brief description of the drawings
Fig. 1 is quick anion chromatographic column made from embodiment 1 to F-、Cl-、NO2 -、H2PO4 -、Br-、NO3 -And S04 2-Seven
Plant the chromatogram of mixed sample detection.
Embodiment
Embodiment 1
（1）Using Chinese invention patent application, 5g crosslinkings are made in synthetic method disclosed in the A of application notification number CN 104788603
Contain high crosslinking hydrophilic ethyl styrene-divinylbenzene filler of sulfonic acid group in the surface of degree 70%.It is cleaned multiple times with deionized water
40 DEG C of dry for standby afterwards.
（2）0.5g dodecyl sodium sulfates are dissolved in 100ml deionizations, are then added in 250ml three-neck flasks,
100r/min is stirred, 60 DEG C of heating.10ml 1-chloro-4-methyl-benzenes, 0.2ml divinylbenzenes and 0.4ml vinyl acetates are added
Into three-neck flask, nitrogen atmosphere 30min is kept.By 0.1g potassium peroxydisulfates 20ml deionized water dissolvings, it is then added to
State in three-neck flask, keep 100r/min stirrings, 60 DEG C of heating react 20.0h, obtain the copolymer of the particle diameter 50nm degrees of cross linking 2%
Nano-grade latex.
（3）By step（2）The 100ml copolymer nano latexes of preparation are poured into clean 250ml three-neck flasks, are added
The concentration H of 1.1ml 98%2SO4Hydrolysis, hydrolysis time 20h are stirred under 40 DEG C, 120r/min speed conditions.
（4）By step（3）Copolymer nano latex after hydrolysis is demulsified with saturation KCL, low temperature drying.Use deionization
Screen filtration is used after water cleaning, then is dried.This operation 5 times is repeated, until unnecessary KCL is cleaned up, white dry powder is obtained
Shape material.
（5）Triethylamine is configured to 1% amine aqueous solution.Step（4）5g copolymer nano latexes after the demulsification cleaning of preparation
Ultrasonic disperse is transferred in 250ml three-neck flasks in 100ml 1% amine aqueous solution, stirring reaction 6h at 60 DEG C, obtains quaternized
Copolymer nano latex.
（6）By step（5）The quatemized copolymer Nano-grade latex and step of preparation（1）The table of the 5g degrees of cross linking 70% of preparation
High crosslinking hydrophilic ethyl styrene-divinylbenzene filler that sulfonic acid group is contained in face carries out agglomeration, and quick anion chromatographic is made
Column packing.
（7）By step（6）Quick anion color is made using homogenate method dress post in obtained quick anion chromatographic column packing
Compose post.Use 3.6mM Na2CO3With 4.5mM NaHCO3Leacheate, SHD-2 electric conductivity detectors, SHY-A-5 suppressors, F-
(2mg/L)、Cl-(3mg/L)、NO2 -(5mg/L)、H2PO4 -(10mg/L)、Br-(10mg/L)、NO3 -(10mg/L) and S04 2-
(10mg/L) seven kinds of mixed samples.5.5 minutes analysis times, Fig. 1 is the spectrogram that detection is obtained, and the detection of standard specimen reflects this hair
Filler dress post detection has the significant advantages such as analyze speed is fast, peak type is good made from bright preparation method.
Embodiment 2
（1）Using Chinese invention patent application, 5g crosslinkings are made in synthetic method disclosed in the A of application notification number CN 104788603
Contain high crosslinking hydrophilic ethyl styrene-divinylbenzene filler of sulfonic acid group in the surface of degree 85%.It is cleaned multiple times with deionized water
40 DEG C of dry for standby afterwards.
（2）0.5g dodecyl sodium sulfates are dissolved in 100ml deionizations, are then added in 250ml three-neck flasks,
100r/min is stirred, 60 DEG C of heating.10ml 1-chloro-4-methyl-benzenes, 1ml divinylbenzenes and 1.05ml vinyl acetates are added
Into three-neck flask, nitrogen atmosphere 30min is kept.By 0.1g potassium peroxydisulfates 20ml deionized water dissolvings, it is then added to
State in three-neck flask, keep 100r/min stirrings, 60 DEG C of heating react 20.0h, obtain the copolymerization of the particle diameter 50nm degrees of cross linking 10%
Thing Nano-grade latex.
（3）100ml copolymer nano latexes prepared by step (2) are poured into clean 250ml three-neck flasks, are added
The concentration H of 8.15ml 98%2SO4Hydrolysis, hydrolysis time 4.0h are stirred under 80 DEG C, 120r/min speed conditions.
（4）Copolymer nano latex after step (3) is hydrolyzed is demulsified with saturation KCL, low temperature drying.Use deionization
Screen filtration is used after water cleaning, then is dried.This operation 5 times is repeated, until unnecessary KCL is cleaned up, white dry powder is obtained
Shape material.
（5）By N, N- dimethylethanolamines are configured to 1% amine aqueous solution.Step（4）5g copolymerization after the demulsification cleaning of preparation
Thing Nano-grade latex ultrasonic disperse is transferred in 250ml three-neck flasks in 100ml 1% amine aqueous solution, stirring reaction 6h at 60 DEG C,
Obtain quatemized copolymer Nano-grade latex.
（6）By step（5）The quatemized copolymer Nano-grade latex and step of preparation（1）The table of the 5g degrees of cross linking 85% of preparation
High crosslinking hydrophilic ethyl styrene-divinylbenzene filler that sulfonic acid group is contained in face carries out agglomeration, and quick anion chromatographic is made
Column packing.
Identical standard specimen is detected under the same conditions as example 1, by the present embodiment filler system
Compared to Figure 1, difference is less than 4 percent to the collection of illustrative plates obtained into chromatogram post detection.The present embodiment does not have accompanying drawing.
Embodiment 3
（1）Using Chinese invention patent application, the A of application notification number CN 104788603 disclose synthetic method and the 5g degrees of cross linking are made
Contain high crosslinking hydrophilic ethyl styrene-divinylbenzene filler of sulfonic acid group in 75% surface.After being cleaned multiple times with deionized water
40 DEG C of dry for standby.
（2）0.5g dodecyl sodium sulfates are dissolved in 100ml deionizations, are then added in 250ml three-neck flasks,
100r/min is stirred, 60 DEG C of heating.10ml 1-chloro-4-methyl-benzenes, 0.4ml divinylbenzenes and 0.60ml vinyl acetates are added
Enter into three-neck flask, keep nitrogen atmosphere 30min.By 0.1g potassium peroxydisulfates 20ml deionized water dissolvings, it is then added to
In above-mentioned three-neck flask, 100r/min stirrings are kept, 60 DEG C of heating react 20.0h, the copolymer for obtaining the 50nm degrees of cross linking 4% is received
Rice milk glue.
（3）100ml copolymer nano latexes prepared by step (2) are poured into clean 250ml three-neck flasks, are added
The concentration H of 2.7ml 98%2SO4, hydrolysis, hydrolysis time 16h are stirred under 55 DEG C, 120r/min speed conditions.
（4）Copolymer nano latex after step (3) is hydrolyzed is demulsified with saturation KCL, low temperature drying.Use deionization
Screen filtration is used after water cleaning, then is dried.This operation 5 times is repeated, until unnecessary KCL is cleaned up, white dry powder is obtained
Shape material.
（5）Trimethylamine is configured to 1% amine aqueous solution.Step（4）5g copolymer nano latexes after the demulsification cleaning of preparation
Ultrasonic disperse is transferred in 250ml three-neck flasks in 100ml 1% amine aqueous solution, stirring reaction 6h at 60 DEG C, obtains quaternized
Copolymer nano latex.
（6）By step（5）The quatemized copolymer Nano-grade latex and step of preparation（1）The table of the 5g degrees of cross linking 75% of preparation
High crosslinking hydrophilic ethyl styrene-divinylbenzene filler that sulfonic acid group is contained in face carries out agglomeration, and quick anion chromatographic is made
Column packing.
Identical standard specimen is detected under the same conditions as example 1, and chromatogram post detection is made by the present embodiment filler and obtained
Compared to Figure 1, difference is less than 2 percent to the collection of illustrative plates arrived.The present embodiment does not have accompanying drawing.
Embodiment 4
（1）Using Chinese invention patent application, the A of application notification number CN 104788603 disclose synthetic method and the 5g degrees of cross linking are made
Contain high crosslinking hydrophilic ethyl styrene-divinylbenzene filler of sulfonic acid group in 80% surface.After being cleaned multiple times with deionized water
40 DEG C of dry for standby.
（2）0.5g dodecyl sodium sulfates are dissolved in 100ml deionizations, are then added in 250ml three-neck flasks,
100r/min is stirred, 60 DEG C of heating.10ml 1-chloro-4-methyl-benzenes, 0.8ml divinylbenzenes and 0.85ml vinyl acetates are added
Enter into three-neck flask, keep nitrogen atmosphere 30min.By 0.1g potassium peroxydisulfates 20ml deionized water dissolvings, it is then added to
In above-mentioned three-neck flask, 100r/min stirrings are kept, 60 DEG C of heating react 20.0h, the copolymer for obtaining the 50nm degrees of cross linking 8% is received
Rice milk glue.
（3）100ml copolymer nano latexes prepared by step (2) are poured into clean 250ml three-neck flasks, are added
The concentration H of 6.5ml 98%2SO4, hydrolysis, hydrolysis time 5.5h are stirred under 65 DEG C, 120r/min speed conditions.
（4）Copolymer nano latex after step (3) is hydrolyzed is demulsified with saturation KCL, low temperature drying.Use deionization
Screen filtration is used after water cleaning, then is dried.This operation 5 times is repeated, until unnecessary KCL is cleaned up, white dry powder is obtained
Shape material.
（5）Triethylamine is configured to 1% amine aqueous solution.5g copolymer nano latexes after demulsification cleaning prepared by step (4)
Ultrasonic disperse is transferred in 250ml three-neck flasks in 100ml 1% amine aqueous solution, stirring reaction 6h at 60 DEG C, obtains quaternized
Copolymer nano latex.
（6）By step（5）The quatemized copolymer Nano-grade latex and step of preparation（1）The table of the 5g degrees of cross linking 80% of preparation
High crosslinking hydrophilic ethyl styrene-divinylbenzene filler that sulfonic acid group is contained in face carries out agglomeration, and quick anion chromatographic is made
Column packing.
Identical standard specimen is detected under the same conditions as example 1, and chromatogram post detection is made by the present embodiment filler and obtained
Compared to Figure 1, difference is less than 6 percent to the collection of illustrative plates arrived.The present embodiment
There is no accompanying drawing.
Embodiment 5
（1）Using Chinese invention patent application, the A of application notification number CN 104788603 disclose synthetic method and the 5g degrees of cross linking are made
Contain high crosslinking hydrophilic ethyl styrene-divinylbenzene filler of sulfonic acid group in 77% surface.After being cleaned multiple times with deionized water
40 DEG C of dry for standby.
（2）0.5g dodecyl sodium sulfates are dissolved in 100ml deionizations, are then added in 250ml three-neck flasks,
100r/min is stirred, 60 DEG C of heating.10ml 1-chloro-4-methyl-benzenes, 0.6ml divinylbenzenes and 0.73ml vinyl acetates are added
Enter into three-neck flask, keep nitrogen atmosphere 30min.By 0.1g potassium peroxydisulfates 20ml deionized water dissolvings, it is then added to
In above-mentioned three-neck flask, 100r/min stirrings are kept, 60 DEG C of heating react 20.0h, the copolymer for obtaining the 50nm degrees of cross linking 6% is received
Rice milk glue.
（3）100ml copolymer nano latexes prepared by step (2) are poured into clean 250ml three-neck flasks, are added
The concentration H of 4.35ml 98%2SO4, hydrolysis, hydrolysis time 11h are stirred under 60 DEG C, 120r/min speed conditions.
（4）Copolymer nano latex after step (3) is hydrolyzed is demulsified with saturation KCL, low temperature drying.Use deionization
Screen filtration is used after water cleaning, then is dried.This operation 5 times is repeated, until unnecessary KCL is cleaned up, white dry powder is obtained
Shape material.
（5）Triethylamine is configured to 1% amine aqueous solution.5g copolymer nano latexes after demulsification cleaning prepared by step (4)
Ultrasonic disperse is transferred in 250ml three-neck flasks in 100ml 1% amine aqueous solution, stirring reaction 6h at 60 DEG C, obtains quaternized
Copolymer nano latex.
（6）By step（5）The quatemized copolymer Nano-grade latex and step of preparation（1）The table of the 5g degrees of cross linking 77% of preparation
High crosslinking hydrophilic ethyl styrene-divinylbenzene filler that sulfonic acid group is contained in face carries out agglomeration, and quick anion chromatographic is made
Column packing.
Identical standard specimen is detected under the same conditions as example 1, and chromatogram post detection is made by the present embodiment filler and obtained
Compared to Figure 1, difference is less than 8 percent to the collection of illustrative plates arrived.The present embodiment does not have accompanying drawing.
Embodiment 6
Difference with embodiment 1 is：Step（2）It is middle by 10ml 1-chloro-4-methyl-benzenes, 0.2ml divinylbenzenes and 0.4ml methyl
Glycidyl acrylate is added in three-neck flask.
Embodiment 7
Difference with embodiment 2 is：Step（2）It is middle by 10ml 1-chloro-4-methyl-benzenes, 1ml divinylbenzenes and 1.05ml methyl-props
Olefin(e) acid ethylene oxidic ester is added in three-neck flask.
Embodiment 8
Difference with embodiment 3 is：Step（2）It is middle by 10ml 1-chloro-4-methyl-benzenes, 0.4ml divinylbenzenes and 0.60ml methyl
Glycidyl acrylate is added in three-neck flask.
Claims (7)
1. a kind of preparation method of quick anion chromatographic column packing, including supported matrix enter with modified copolymer nano latex
Row agglomeration, it is characterised in that described supported matrix is the mixture and ion monomer benzene of monomer ethyl styrene and divinylbenzene
Vinyl sulfonic acid potassium is reacted on surface, and high crosslinking hydrophilic ethyl styrene-divinylbenzene of sulfonic acid group is contained on generation surface
Filler；The copolymer nano latex of described modification is by monomer 1-chloro-4-methyl-benzene and divinylbenzene and monomer vinyl acetate
Or GMA is formed using microemulsion polymerization method copolymerization, the copolymer nano latex is hydrolyzed, is demulsified
Cleaning, quaterisation generation quatemized copolymer Nano-grade latex；Quatemized copolymer Nano-grade latex is contained with described surface
High crosslinking hydrophilic ethyl styrene-divinylbenzene the filler for having sulfonic acid group carries out agglomeration, and quick anion exchange resin is made.
2. the preparation method of a kind of quick anion chromatographic column packing according to claim 1, it is characterised in that using micro-
The degree of cross linking of the copolymer nano latex of emulsion polymerization copolymerization is 2-10%.
3. the preparation method of a kind of quick anion chromatographic column packing according to claim 1, it is characterised in that using micro-
The degree of cross linking of the copolymer nano latex of emulsion polymerization copolymerization is 4-8%.
4. a kind of preparation method of quick anion chromatographic column packing according to claim 1, it is characterised in that copolymer
Nano-grade latex is in 0.2-1.5mol/L sulfuric acid solution, 40-80 DEG C of temperature, is hydrolyzed under the conditions of time 4.0-20.0h.
5. a kind of preparation method of quick anion chromatographic column packing according to claim 1, it is characterised in that copolymer
Nano-grade latex is in 0.5-1.2mol/L sulfuric acid solution, 55-65 DEG C of temperature, is hydrolyzed under the conditions of time 5.5-16h.
6. a kind of preparation method of quick anion chromatographic column packing according to claim 1, it is characterised in that acetic acid second
The quality of alkene ester or GMA is the 4.0-10.5% of monomer 1-chloro-4-methyl-benzene quality.
7. a kind of preparation method of quick anion chromatographic column packing according to claim 1, it is characterised in that acetic acid second
The quality of alkene ester or GMA is the 6.0-8.5% of monomer 1-chloro-4-methyl-benzene quality.
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| CN110327990A (en) * | 2019-07-30 | 2019-10-15 | 王金平 | A kind of preparation method of latex agglomeration type anion chromatographic column packing |
| CN111812266A (en) * | 2020-08-04 | 2020-10-23 | 江西华赣瑞林稀贵金属科技有限公司 | Method for detecting chlorine content in smelting smoke dust by using organic grease as raw material |
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| CN112742359A (en) * | 2019-10-31 | 2021-05-04 | 昭和电工株式会社 | Method for producing column packing for glycated hemoglobin analysis |
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| CN111812266A (en) * | 2020-08-04 | 2020-10-23 | 江西华赣瑞林稀贵金属科技有限公司 | Method for detecting chlorine content in smelting smoke dust by using organic grease as raw material |
| CN115850589A (en) * | 2023-02-24 | 2023-03-28 | 北京中科康仑环境科技研究院有限公司 | Resin containing active metal group and preparation method and application thereof |
| CN115850589B (en) * | 2023-02-24 | 2023-05-16 | 北京中科康仑环境科技研究院有限公司 | Resin containing active metal groups, and preparation method and application thereof |
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