CN105597716A - Preparation method of anion exchange chromatography stationary phase - Google Patents
Preparation method of anion exchange chromatography stationary phase Download PDFInfo
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- CN105597716A CN105597716A CN201610024724.9A CN201610024724A CN105597716A CN 105597716 A CN105597716 A CN 105597716A CN 201610024724 A CN201610024724 A CN 201610024724A CN 105597716 A CN105597716 A CN 105597716A
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Abstract
The invention discloses a preparation method of an anion exchange chromatography stationary phase using highly-crosslinked glycidyl methacrylate-divinyl benzene microspheres as a matrix. The preparation method includes: adopting a dispersion polymerization method to prepare monodispersed linear polystyrene seed microspheres; adopting a two-step seed swelling method to prepare highly-crosslinked glycidyl methacrylate-divinyl benzene copolymer microspheres; using methylamine, dimethylamine, trimethylamine, diethylamine, triethylamine and 1, 4-butane dioldiglycidyl ether as reaction raw materials to modify the highly-crosslinked glycidyl methacrylate-divinyl benzene copolymer microspheres to prepare the anion exchange chromatography stationary phase.
Description
Technical field
The present invention relates to a kind of chemical preparation process, specifically, is that a kind of anion-exchange chromatography is fixed phasePreparation method.
Background technology
Silica gel, as a kind of fixing phase matrix that everybody knows, has stronger mechanical strength and is easy to chemical modificationEtc. feature, be widely used in the fixing phase system of reverse-phase chromatography; But silica matrix tolerance pH value is limited in scope (logicalNormal is 2-8), flow phase Acidity of Aikalinity is restricted, has hindered it and has further applied. And Polymer-based Chiral stationary phase is as heightCross-linked styrene-divinylbenzene organic polymer, can tolerate wider pH value scope, has relatively goodMechanical strength, be widely used in the fixing phase system of chromatography of ions; Meanwhile, monodispersed micrograde polymer is micro-Ball, as chromatograph packing material, not only can reduce post and press, and can also significantly improve post effect, is especially suitable for use as ionThe matrix of chromatographic stationary phases; Therefore, tolerate wider pH value scope and the organic polymer of good mechanical strengthMicroballoon will become the trend of chromatograph packing material matrix development.
At present, high cross-linked styrene-divinylbenzene copolymerization microsphere is more as the research report of fixing phase matrix,But the research of high crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization microsphere report is less. But,High cross-linked styrene-divinylbenzene copolymerization microsphere is not easy to carry out derivative reaction, limits it and further applies;And high crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization microsphere contains a large amount of epoxy radicals, be easy toFurther derivative reaction, has good development and application prospect.
The present invention has prepared a kind of novel high crosslinked methacrylic acid glycidyl ester-bis-by two step swelling methodsVinyl benzene copolymerization microsphere, microballoon has good monodispersity, good mechanical strength and is easy to chemical modificationEtc. characteristic, be suitable as very much chromatograph stationary-phase stuffing matrix; Meanwhile, the present invention, taking this microballoon as matrix, makesFor the fixing phase of a series of anion exchange.
Summary of the invention
Acid and alkali-resistance, poor chemical stability and existing height are not crosslinked to the present invention is directed to chromatograph packing material matrix inorganic silica gelStyrene-divinylbenzene copolymerization microsphere is difficult for carrying out the shortcoming of chemical modification, has prepared a kind of novel toleranceSoda acid, there is good mechanical strength and be easy to the high crosslinked methacrylic acid glycidyl ester-diethyl of chemical modificationAlkenyl benzene copolymerization microsphere, as chromatograph packing material matrix, has been prepared the anion exchange look taking this microballoon as matrix simultaneouslyThe fixing phase of spectrum.
The present invention is achieved through the following technical solutions:
The invention discloses a kind of taking high crosslinked methacrylic acid glycidyl ester-divinylbenzene microspheres as matrixThe preparation method of the fixing phase of anion-exchange chromatography, adopt dispersion copolymerization method to prepare monodispersed linear polyphenyl secondAlkene seed microballoon; Adopt two-step seed swelling method, prepare high crosslinked methacrylic acid glycidyl ester-divinylBase benzene copolymerization microsphere; Shrink with methylamine, dimethylamine, trimethylamine, diethylamine, triethylamine and BDO twoGlycerin ether is reaction raw materials, modifies high crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization microsphere,The anion exchange of preparation taking high crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization microsphere as matrixChromatographic stationary phases.
As further improve, the present invention in monodispersed linear polystyrene seed microballoon preparation process,Reaction medium is ethanol water, and volumetric concentration is 75～100%, and the mass concentration of monomer styrene is total amount5～40%, the quality of stabilizing agent polyvinylpyrrolidone is 0.5～4% of reaction medium quality, and initator is evenNitrogen bis-isobutyronitrile quality is monomer mass 1～5%, and reaction temperature is 40～85 DEG C, and mixing speed is 100～400R/min, the reaction time is 12～24h.
As further improve, the present invention in two-step seed swelling legal system for high crosslinked methacrylic acid glycidyl esterIn the process of-divinylbenzene copolymerization microsphere, monomer GMA mass concentration is for always organic5～40% of phase, the quality of crosslinking agent divinylbenzene is 15～40% of total organic phase quality, emulsifying agent 12Sodium alkyl sulfate quality is 2～4% of total organic phase quality, and stabilizing agent polyvinyl alcohol quality is gross mass0.5～5%, initator benzoyl peroxide quality is monomer mass 0.4～1.5%, and pore-foaming agent toluene quality is40～70% of total organic phase quality, swelling ratio is 25～70 times, emulsifying temperature is 20～35 DEG C, reaction temperatureBe 60～85 DEG C, mixing speed is 100～300r/min, and the reaction time is 12～24h, the crosslinked first of height of preparationBase glycidyl acrylate-divinylbenzene copolymerization microsphere particle diameter is between 6-8 μ m.
Do to improve further the friendship of described poly (glycidyl methacrylate)-divinylbenzene copolymerization microsphereConnection degree span is between 10-75%, by regulating poly (glycidyl methacrylate) and divinylbenzeneRatio control.
As improving further, high crosslinked methacrylic acid glycidyl ester-divinyl of the present inventionThe granularity of benzene copolymerization microsphere can be passed through pore-foaming agent, crosslinking agent, dispersion stabilizer solubility, emulsifying temperature, reactionThe selection of temperature, initiator concentration and swelling ratio is controlled.
As improving further, the present invention is modifying high crosslinked methacrylic acid glycidyl ester-divinylIn the process of benzene copolymerization microsphere, with methylamine, dimethylamine, trimethylamine, diethylamine, triethylamine and BDODiglycidyl ether is reaction raw materials, and water is solvent, heats 60 DEG C, stirs 50rpm reaction, preparesAnion-exchange chromatography is fixed phase.
As optimizing further, the anion-exchange chromatography of described preparation is fixing mutually with homogenate method dress post, and rightIts chromatographic performance characterizes by chromatographic performance to be evaluated, and shows higher ion exchange capacity, can be steady for a long timeSurely use.
Tool of the present invention has the following advantages:
High crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization microsphere monodispersity provided by the inventionGood, mechanical strength is high, can tolerate wider pH value scope, is easy to chemical modification, is suitable as chromatogram solidThe matrix of phasing.
High crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization microsphere preparation method provided by the inventionSimple and reliable; The granularity of microballoon can pass through pore-foaming agent, crosslinking agent, dispersion stabilizer solubility, emulsifying temperature,The selection of reaction temperature, initiator concentration and swelling ratio is controlled.
Methylamine provided by the invention, dimethylamine, trimethylamine, diethylamine, triethylamine and BDO two shrinkGlycerin ether method of modifying is simple and reliable, and cost is low, repeatable strong;
High crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization microsphere that patent system of the present invention is standby, singleGood dispersion, wider with respect to existing silica matrix tolerance pH value scope, than high cross-linked styrene-divinylThe easily further derivatization of benzene copolymerization microsphere, and there is good mechanical strength, be suitable as chromatographic stationary phasesMatrix; The phenyl ring cavity knot of high crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization microsphere porousStructure, can provide the similar spatial selectivities of supermolecule such as picture crown ether, cyclodextrin, calixarenes; High crosslinked methylGlycidyl acrylate-divinylbenzene copolymerization microsphere provides a large amount of epoxide groups, and this radical reaction is strong,Reaction condition gentleness, can react with multiple group single steps such as hydroxyl, amino, acid anhydrides, derivatization objectVery extensive, these class methods have higher feasibility and repeatability; The present invention is by methylamine and BDOHigh crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization microsphere after diglycidyl ether is modified, thisInvention shows that this high crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization microsphere has extensively as matrixWealthy application prospect and practical application meaning.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of high crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization microsphere;
Fig. 2 is methylamine, dimethylamine, trimethylamine, diethylamine, triethylamine and BDDEThe preparation process of the fixing phase of high crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization microsphere of modifyingFigure;
Fig. 3, Fig. 4 are that 7 kinds of anion are at the fixing separate colors spectrogram of going up mutually of preparation.
Detailed description of the invention
The invention provides the preparation method of the fixing phase of a kind of anion-exchange chromatography, comprise single seed-dispersed microballoonPreparation, preparation and the anion exchange of high crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization microsphereThe preparation of chromatographic stationary phases. Concrete technical scheme is as follows:
The present invention adopts dispersion copolymerization method to prepare monodispersed linear polystyrene seed microballoon; Adopt two step seedsSwelling method, prepares high crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization microsphere; With methylamine, twoMethylamine, trimethylamine, diethylamine, triethylamine and BDDE are that raw material is modified high crosslinked firstBase glycidyl acrylate-divinylbenzene copolymerization microsphere, high crosslinked methacrylic acid glycidyl ester-bis-Quaternary ammonium functional group is introduced on vinyl benzene copolymerization microsphere surface; With homogenate method dress post, and its chromatographic performance is carried outCharacterize; Concrete preparation process is:
A. adopt dispersion copolymerization method to prepare monodispersed linear polystyrene seed microballoon
Taking styrene as monomer, polyvinylpyrrolidone is stabilizing agent, and azodiisobutyronitrile is initator, ethanolWith water mixed solution be reaction medium; By dispersion copolymerization method, prepare particle diameter controlled, the linearity that monodispersity is goodPolystyrene seed microballoon;
B. adopt two-step seed swelling legal system for the copolymerization of high crosslinked methacrylic acid glycidyl ester-divinylbenzeneMicroballoon
Single Decentralized Linear polystyrene seed microballoon is activated in dibutyl phthalate emulsion; After activationAdd and contain monomer GMA, crosslinking agent divinylbenzene, emulsifying agent dodecyl sulphateSodium, stabilizing agent polyvinyl alcohol, the emulsion of initator benzoyl peroxide and pore-foaming agent toluene carries out swelling; SoAfter add thermal-initiated polymerization, prepare high crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization microsphere;
C. methylamine, dimethylamine, trimethylamine, diethylamine, triethylamine and BDDE are modifiedHigh crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization microsphere
Respectively by methylamine, dimethylamine, trimethylamine, diethylamine, triethylamine and BDDEBe scattered in water with high crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization microsphere successively, heating is stirredMix reaction; Reaction finishes, and water, ethanol wash successively;
D. homogenate method dress post
Get 2.0g filler in 50mL beaker, add and high crosslinked methacrylic acid glycidyl ester-diethylThe isopycnic homogenate of alkenyl benzene copolymerization microsphere (water/acetonitrile mixed liquor), ultrasonic dispersion ten minutes; Then addIn packing column machine homogenate tank, taking water as displacement fluid, under 35MPa pressure, fill post, displacement fluid at least flows out 300mL.
Anion exchange Stationary phase preparation method provided by the invention is with high crosslinked methacrylic acid glycidylEster-divinylbenzene copolymerization microsphere is matrix, with methylamine, dimethylamine, trimethylamine, diethylamine, triethylamine andBDDE is functional group, and water is solvent, high crosslinked methacrylic acid glycidyl ester-Divinylbenzene copolymerization microsphere surface covalent bonding quaternary ammonium type functional group.
Below by detailed description of the invention, technical scheme of the present invention is described in further detail:
Embodiment 1: high crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization microsphere weak-type cationThe making step of fixing phase is:
1, first prepare single Decentralized Linear polystyrene seed of particle diameter 1.8 about μ m by dispersion copolymerization method micro-Ball, reaction medium is ethanol water mixed solution, ethanol consumption is 75% (v/v); Monomer styrene consumption is5% (m/m) of reaction medium consumption, stabilizing agent polyvinylpyrrolidone consumption is 0.5% of reaction medium consumption(m/m), initator azodiisobutyronitrile consumption is 1% (m/m) of monomer consumption, and reaction temperature is 40 DEG C,Mixing speed is 100r/min, and the reaction time is 12h;
2, the high crosslinked methacrylic acid of the single dispersion that is 75% by two-step seed swelling legal system for the degree of cross linking is shunkGlyceride-divinylbenzene copolymerization microsphere. Seed microballoon 0.6g, monomer GMA consumptionFor 5% (m/m) of total organic phase consumption, crosslinking agent divinylbenzene consumption is 25% of total organic phase consumption(m/m), emulsifier sodium lauryl sulfate consumption is 4% (m/m) of total organic phase consumption, and stabilizing agent gathers secondEnol consumption is 5% (m/m) of total amount, and initator benzoyl peroxide consumption is 1.5% of monomer consumption(m/m), pore-foaming agent toluene consumption is 60% (m/m) of total organic phase consumption, and swelling ratio is 70 times, emulsification temperatureDegree is 35 DEG C, and reaction temperature is 85 DEG C, and mixing speed is 300r/min, and the reaction time is 24h, preparationHigh crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization microsphere particle size range between 6-8 μ m,Monodispersity is good, without carrying out classification and screening; Polymer microballoon is removed to pore-foaming agent with toluene extracting, thenWater, ethanol washing; Copolymerization microsphere particle diameter is about 6 μ m.
3, with methylamine, dimethylamine, trimethylamine, diethylamine, triethylamine and BDDEFor functional group is modified high crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization microsphere;
4, by homogenate method, methylamine, dimethylamine, trimethylamine, diethylamine, triethylamine and BDO two are contractedHigh crosslinked methacrylic acid glycidyl ester-divinylbenzene filler dress post after water glycerin ether is modified;
5, use aqueous sodium carbonate as mobile phase, suppress electric conductivity detector 7 kinds of cations are detected.
Embodiment 2: with reference to method and the step of embodiment 1
1, first synthesize particle diameter 1.8 μ m monodisperse polystyrene seed microballoons, reaction medium by dispersion copolymerization methodFor ethanol water mixed solution, ethanol consumption is 100% (v/v); The concentration of monomer styrene is 30% of total amount(m/m), 4% (m/v) that stabilizing agent polyvinylpyrrolidone consumption is reaction medium, initator azo two is differentButyronitrile consumption is 5% (m/m) of monomer consumption, 85 DEG C of reaction temperatures, and mixing speed is at 400r/min, anti-Between seasonable 16 hours;
2, the high crosslinked methacrylic acid of the single dispersion that is 40% by two-step seed swelling legal system for the degree of cross linking is shunkGlyceride-divinylbenzene copolymerization microsphere. Seed microballoon 0.6g, the use of monomer GMAAmount is 10% (m/m) of total organic phase consumption, and crosslinking agent divinylbenzene consumption is total organic phase consumption40% (m/m), emulsifier sodium lauryl sulfate consumption is 2.7% (m/m) of total organic phase consumption, stable1.5% (m/m) that agent polyvinyl alcohol consumption is total amount, initator benzoyl peroxide consumption is monomer consumption0.7% (m/m), pore-foaming agent toluene consumption is 45% (m/m) of total organic phase consumption, swelling ratio is 55 times,Emulsifying temperature is 20 DEG C, 70 DEG C of reaction temperatures, and mixing speed 250r/min, reaction time 24h, will gatherCompound microballoon is removed pore-foaming agent with toluene extracting, then water, ethanol washing; Copolymerization microsphere particle diameter is about 6 μ m.
3, with methylamine, dimethylamine, trimethylamine, diethylamine, triethylamine and BDDEFor functional group is modified high crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization microsphere;
4, by homogenate method, methylamine, dimethylamine, trimethylamine, diethylamine, triethylamine and BDO two are contractedHigh crosslinked methacrylic acid glycidyl ester-divinylbenzene filler dress post after water glycerin ether is modified;
5, by embodiment 1 (5) method, chromatogram column chromatography performance is measured, result is consistent with 1 (5).
Embodiment 3: with reference to method and the step of embodiment 1
1, prepare particle diameter approximately 1.8 μ m monodisperse polystyrene seed microballoons, reaction medium by dispersion copolymerization methodBe 95% ethanol water, 10% (m/m) that the consumption of monomer styrene is total amount, stabilizing agent polyethylene pyrrolePyrrolidone consumption is 1.6% (m/m) of reaction medium, and initator azodiisobutyronitrile consumption is monomer consumption2.2% (m/m), 60 DEG C of reaction temperatures, mixing speed is 200r/min, the reaction time is 20h;
2, the high crosslinked methacrylic acid of the single dispersion that is 15% by two-step seed swelling legal system for the degree of cross linking is shunkGlyceride-divinylbenzene copolymerization microsphere. Seed microballoon 0.6g, the use of monomer GMAAmount is 40% (m/m) of total organic phase consumption, and crosslinking agent divinylbenzene consumption is total organic phase consumption15% (m/m), emulsifier sodium lauryl sulfate consumption is 2% (m/m) of total organic phase consumption, stabilizing agentPolyvinyl alcohol consumption is 0.5% (m/m) of total amount, and initator benzoyl peroxide consumption is monomer consumption0.4% (m/m), pore-foaming agent toluene consumption is 40% (m/m) of total organic phase consumption, swelling ratio is 25 times,Emulsifying temperature is 28 DEG C, 60 DEG C of reaction temperatures, and mixing speed 100r/min, reaction time 12h, will gatherCompound microballoon is removed pore-foaming agent with toluene extracting, then water, ethanol washing; Copolymerization microsphere particle diameter is about 6 μ m.
3, with methylamine, dimethylamine, trimethylamine, diethylamine, triethylamine and BDDEFor functional group is modified high crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization microsphere;
4, by homogenate method, methylamine, dimethylamine, trimethylamine, diethylamine, triethylamine and BDO two are contractedHigh crosslinked methacrylic acid glycidyl ester-divinylbenzene filler dress post after water glycerin ether is modified;
5, by embodiment 1 (5) method, chromatogram column chromatography performance is measured, result is consistent with 1 (5).
Embodiment 4: with reference to method and the step of embodiment 1
1, prepare particle diameter approximately 1.8 μ m monodisperse polystyrene seed microballoons, reaction medium by dispersion copolymerization methodBe 90% ethanol water, 25% (m/m) that the consumption of monomer styrene is total amount, stabilizing agent polyethylene pyrrolePyrrolidone consumption is 1.6% (m/m) of reaction medium, and initator azodiisobutyronitrile consumption is monomer consumption2.2% (m/m), 70 DEG C of reaction temperatures, mixing speed is 250r/min, the reaction time is 24h;
2, the high crosslinked methacrylic acid of the single dispersion that is 55% by two-step seed swelling legal system for the degree of cross linking is shunkGlyceride-divinylbenzene copolymerization microsphere. Seed microballoon 0.6g, the use of monomer GMAAmount is 18% (m/m) of total organic phase consumption, and crosslinking agent divinylbenzene consumption is total organic phase consumption36% (m/m), emulsifier sodium lauryl sulfate consumption is 2.7% (m/m) of total organic phase consumption, stable1.5% (m/m) that agent polyvinyl alcohol consumption is total amount, initator benzoyl peroxide consumption is monomer consumption0.7% (m/m), pore-foaming agent toluene consumption is 47% (m/m) of total organic phase consumption, swelling ratio is 55 times,Emulsifying temperature is 25 DEG C, 70 DEG C of reaction temperatures, and mixing speed 250r/min, reaction time 24h, will gatherCompound microballoon is removed pore-foaming agent with toluene extracting, then water, ethanol washing; Copolymerization microsphere particle diameter is about 6 μ m(Fig. 1).
3, with methylamine, dimethylamine, trimethylamine, diethylamine, triethylamine and BDDEFor functional group is modified high crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization microsphere;
4, by homogenate method, methylamine, dimethylamine, trimethylamine, diethylamine, triethylamine and BDO two are contractedHigh crosslinked methacrylic acid glycidyl ester-divinylbenzene filler dress post after water glycerin ether is modified;
5, by embodiment 1 (5) method, chromatogram column chromatography performance is measured, result is consistent with 1 (5).
Embodiment 5: chromatographic performance test
By utilizing 7 kinds of anion fixing to carry out mutually chromatographic performance analysis to this, demonstrate superior chromatographic isolationCharacteristic.
Instrument: ICS3000 ion chromatograph
Splitter: 4.6 × 200mm stainless steel chromatogram post that self-made fill is loaded;
Leacheate: 25mmol/LNa2CO3；
Flow velocity: 1mL/min;
Sample: 7 kinds of anion (1, F-2,PO4 3-3,SO4 2-4,Cl-5,NO2 -6,Br-7,NO3 -)。
Fig. 1 is the scanning electron microscope (SEM) photograph of high crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization microsphere,By observing scanning electron microscope (SEM) photograph, high crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization of preparation is micro-Ball particle size range is between 6-8 μ m, and monodispersity is good, without carrying out classification and screening;
Fig. 2 is methylamine, dimethylamine, trimethylamine, diethylamine, triethylamine and BDDEPreparation process figure (a, the first of high crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization microsphere of modifyingAmine grafting one deck b, two layers of c of methylamine grafting, three layers of d of methylamine grafting, trimethylamine grafting one deck e, dimethylamine connectsBranch one deck f, triethylamine grafting one deck g, diethylamine grafting one deck);
Fig. 3 is that 7 kinds of anion are modified the fixing separate colors going up mutually at methylamine and BDDESpectrogram (a, methylamine grafting one deck b, two layers of c of methylamine grafting, three layers of methylamine grafting);
Fig. 4 is that 7 kinds of anion are in dimethylamine, trimethylamine, diethylamine, triethylamine and BDO two shrinksThe fixing separate colors spectrogram of going up mutually of glycerin ether modification (a, trimethylamine grafting one deck b, dimethylamine grafting one deck c,Triethylamine grafting one deck d, diethylamine grafting one deck);
What more than enumerate is only part specific embodiment of the present invention, obviously, the invention is not restricted to above embodiment,Can also have many distortion, those of ordinary skill in the art can directly derive or join from content disclosed by the inventionAll distortion of expecting, all should think protection scope of the present invention.
Claims (7)
1. a preparation method for the fixing phase of anion-exchange chromatography, is characterized in that: adopt dispersion copolymerization method preparation singleThe linear polystyrene seed microballoon disperseing; Adopt two-step seed swelling method, prepare high crosslinked methacrylic acid contractingWater glyceride-divinylbenzene copolymerization microsphere; With methylamine, dimethylamine, trimethylamine, diethylamine, triethylamine andBDDE is reaction raw materials, modifies high crosslinked methacrylic acid glycidyl ester-divinylBase benzene copolymerization microsphere, preparation is taking high crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization microsphere as baseThe fixing phase of anion-exchange chromatography of matter.
2. the preparation method of the fixing phase of anion-exchange chromatography according to claim 1, is characterized in that: at listIn the linear polystyrene seed microballoon preparation process of disperseing, reaction medium is ethanol water, and volumetric concentration is75～100%, the mass concentration of monomer styrene is total amount 5～40%, stabilizing agent polyvinylpyrrolidoneQuality is 0.5～4% of reaction medium quality, and initator azodiisobutyronitrile quality is monomer mass1～5%, reaction temperature is 40～85 DEG C, and mixing speed is 100～400r/min, and the reaction time is 12～24h.
3. the preparation method of the fixing phase of anion-exchange chromatography according to claim 1, is characterized in that: twoIn the process of the synthetic poly (glycidyl methacrylate)-divinylbenzene copolymerization microsphere of step seed swelling method, singleBody GMA mass concentration is total organic phase 5～40%, crosslinking agent divinylbenzeneQuality is 15～40% of total organic phase quality, and emulsifier sodium lauryl sulfate quality is total organic phase quality2～4%, stabilizing agent polyvinyl alcohol quality is gross mass 0.5～5%, and initator benzoyl peroxide quality is single0.4～1.5% of weight, pore-foaming agent toluene quality is 40～70% of total organic phase quality, swelling ratio is25～70 times, emulsifying temperature is 20～35 DEG C, and reaction temperature is 60～85 DEG C, and mixing speed is 100～300R/min, the reaction time is 12～24h, poly (glycidyl methacrylate)-divinylbenzene copolymerization of preparationMicrospherulite diameter is between 6-8 μ m.
4. the preparation method of the fixing phase of anion-exchange chromatography according to claim 3, is characterized in that: described inThe degree of cross linking span of poly (glycidyl methacrylate)-divinylbenzene copolymerization microsphere 10-75% itBetween, control by the ratio that regulates poly (glycidyl methacrylate) and divinylbenzene.
5. the preparation method of the fixing phase of anion-exchange chromatography according to claim 3, is characterized in that: described inThe granularity of poly (glycidyl methacrylate)-divinylbenzene copolymerization microsphere can pass through pore-foaming agent, crosslinkedThe selection of agent, dispersion stabilizer solubility, emulsifying temperature, reaction temperature, initiator concentration and swelling ratio is controlledSystem.
6. the preparation method of the fixing phase of anion-exchange chromatography according to claim 1, is characterized in that: repairingAdorn in the process of high crosslinked methacrylic acid glycidyl ester-divinylbenzene copolymerization microsphere, successively with methylamine,Trimethylamine, dimethylamine, triethylamine and diethylamine and BDDE are reaction raw materials, and water isSolvent, heats 60 DEG C, stirs 50rpm reaction.
7. the preparation method of the fixing phase of anion exchange according to claim 1, is characterized in that: described preparationAnion-exchange chromatography is fixing mutually with homogenate method dress post, and its chromatographic performance is characterized, and passes through chromatographic performanceEvaluate, show higher ion exchange capacity, can use steadily in the long term.
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| CN113512152A (en) * | 2021-06-09 | 2021-10-19 | 深圳普门科技股份有限公司 | Vinyl monomer-polyvinyl cross-linking agent copolymer non-porous microsphere and preparation method and application thereof |
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| CN114149594A (en) * | 2021-11-03 | 2022-03-08 | 赛分科技扬州有限公司 | Amine salt type polyacrylate emulsion and preparation method thereof |
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