Preparation method of anion chromatographic column
By introducing epoxy groups and modifying the chromatographic fillers of the anion column, the shortcomings of the anion column in the prior art in the polyacid and high-valent ion separation tests were solved, and the effect of rapid separation of seven anions in the hydroxide system was achieved.
Patent Information
- Application Number
- CN202411633424.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-15
- Publication Date
- 2025-03-28
AI Technical Summary
The existing anion columns lack fast separation and efficient chromatography columns in the polyacid and high-valent ion separation tests. Especially in the hydroxide system, the separation time is long, and the ionization degree of phosphate is high, making it difficult to elute and retain in strong alkali leachate.
By preparing matrix microspheres with epoxy groups and undergoing quaternization modification, a chromatographic filler with multiple β-hydroxy groups was obtained. The chromatographic filler aggregates functional groups on the surface of the matrix microspheres, but does not enter the internal pores of the matrix microspheres, improving the hydrophilicity and ion separation efficiency of the chromatographic filler.
The rapid separation and detection of seven anions in the hydroxide system was achieved, which improved the column efficiency and capacity of the chromatographic column, shortened the peak time, and enhanced the stability and reproducibility of the chromatographic filler.
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Abstract
Description
Technical Field
[0001] The invention relates to an ion chromatography technology, in particular to a preparation method of an anion chromatography column. Background Art
[0002] Ion chromatography (IC), a branch of liquid chromatography, is an irreplaceable analytical method that has become an indispensable means of separation and detection of various ionizable chemical substances in scientific research, industrial fields and quality monitoring.
[0003] The core component of ion chromatography separation is the chromatographic column, and its separation performance depends on the characteristics of the chromatographic stationary phase. The chromatographic stationary phase mainly consists of two parts: matrix microspheres and functional layers. Anion chromatography stationary phases commonly use polymer matrix microspheres, such as PS-DVB, EVB-DVB, etc.; functional layer modification methods include hyperbranching, surface grafting, and latex agglomeration.
[0004] At present, for anion chromatographic columns, there is a lack of fast separation and high efficiency chromatographic columns for the separation and testing of polyacids and high-valent ions. The separation time of chromatographic fillers used to separate seven anions in the hydroxide system is usually long. Since phosphate has a high degree of ionization, it is difficult to elute it in a strong alkaline eluent and has a long retention time. Therefore, it is difficult to test phosphate with a single injection of conventional chromatographic fillers. Therefore, it is of great significance to prepare a chromatographic column that can quickly separate and detect seven anions in the hydroxide system while having high column efficiency, high capacity, and stable reproducibility. Summary of the invention
[0005] In order to solve the above-mentioned deficiencies in the prior art, the object of the present invention is to provide a method for preparing an anion chromatography column.
[0006] The technical solution adopted by the present invention to solve the technical problem is: a method for preparing an anion chromatographic column, comprising the following steps:
[0007] S1, preparing chromatographic filler;
[0008] Wherein, the steps of preparing the chromatographic filler are:
[0009] S11, introducing functional groups into the matrix microspheres and causing polymerization reaction to obtain matrix microspheres having epoxy groups;
[0010] S12, quaternizing the obtained matrix microspheres having epoxy groups to obtain a chromatographic filler having multiple β-hydroxyl groups;
[0011] S13, the functional group introduced into the matrix microspheres is an amino group or an epoxy group;
[0012] S2, loading the chromatographic filler into an empty column to obtain a chromatographic column;
[0013] The prepared chromatographic filler is cleaned and dried at a drying temperature of 30°C to 80°C, for example, 50°C to 60°C, and a homogenization method is used to pack the column, the KOH solution is used for homogenization, the concentration of the KOH solution is 0.05 to 0.5 mol / L, for example, 0.1 to 0.2 mol / L, the chromatographic filler is loaded on a column packing machine, the column loading pressure is 10 to 40 MPa, for example, 20 to 30 MPa, and the loading time is 0.5 to 3 h, for example, 1 to 2 h, to obtain a chromatographic column;
[0014] S3, testing the prepared chromatographic column;
[0015] After the chromatographic column is prepared, it is rinsed with the above-mentioned KOH solution and tested. The test sample is F - , Cl - 、NO 2 - Br - 、NO 3 - 、SO 4 2- ,PO 4 3- .
[0016] Optionally, the functional group introduced into the matrix microsphere is an amino group;
[0017] The step of introducing functional groups into the matrix microspheres is:
[0018] Dissolve the matrix microspheres in a set ratio of alcohol-water mixed solution, and stir thoroughly to make the matrix microspheres dispersed evenly;
[0019] Among them, the volume ratio of alcohol to water is 4:1~1:4, for example, 2:1~1:2; the alcohol in the alcohol-water mixed solution is a mixture of one or more of methanol, ethanol, isopropanol, and n-butanol; the mass ratio of the matrix microspheres to the alcohol-water mixed solution is 1:5~1:20, for example, 1:10~1:15.
[0020] A set amount of water-soluble initiator and mercaptoamine compound are added under nitrogen atmosphere, and then residual double bonds on the surface of microspheres react with the mercapto groups of the mercaptoamine compound at a set temperature to obtain matrix microspheres with epoxy groups on the surface;
[0021] Wherein, the water-soluble initiator is any one of azobisisobutylamidine hydrochloride, potassium persulfate, and ammonium persulfate; the amount of the water-soluble initiator added is 0.05wt%~2wt%, for example, 0.2wt%~1wt%;
[0022] The thiolamine compound is any one of β-mercaptoethylamine, mercaptopropylamine, cysteamine hydrochloride, and cysteine; the amount of the thiolamine compound added is 0.05 mol / L to 0.8 molmol / L, for example, 0.1 mol / L to 0.4 mol / L; the reaction temperature is 50°C to 90°C, for example, 60°C to 70°C; the reaction time is 0.5h to 8h, for example, 2h to 4h;
[0023] Optionally, the functional group introduced into the matrix microsphere is an epoxy group;
[0024] The step of introducing functional groups into the matrix microspheres is:
[0025] Dissolve the matrix microspheres in a set ratio of alcohol-water mixed solution, and stir thoroughly to make the matrix microspheres dispersed evenly;
[0026] The volume ratio of alcohol to water is 4:1 to 1:4, for example, 2:1 to 1:2; the alcohol in the alcohol-water mixed solution is a mixture of one or more of methanol, ethanol, isopropanol, and n-butanol; the mass ratio of the matrix microspheres to the alcohol-water mixed solution is 1:5 to 1:20, for example, 1:10 to 1:15;
[0027] Adding a set amount of water-soluble initiator and olefin epoxy compound under nitrogen atmosphere, and then polymerizing the residual double bonds on the surface of microspheres with the double bonds of olefin epoxy compound at a set temperature to obtain matrix microspheres with epoxy groups on the surface;
[0028] Wherein, the water-soluble initiator is any one of azobisisobutylamidine hydrochloride, potassium persulfate, and ammonium persulfate; the amount of the water-soluble initiator added is 0.05wt%~2wt%, for example, 0.2wt%~1wt%;
[0029] The olefin epoxide is any one of 3,4-epoxy-1-butene, allyl glycidyl ether, and glycidyl methacrylate; the amount of the olefin epoxide added is 0.05 mol / L~0.8 molmol / L, for example, 0.1 mol / L~0.4 mol / L; the reaction temperature is 50°C~90°C, for example, 60°C~70°C; the reaction time is 0.5h~8h, for example, 2h~4h.
[0030] Optionally, the step of quaternizing the matrix microspheres is:
[0031] The matrix microspheres having epoxy groups on the surface are reacted with a multifunctional diglycidyl ether compound in a set ratio, and an alkaline amine reagent is used or catalyzed under acidic conditions to hydrolyze the epoxy groups in the set ratio into hydroxyl groups;
[0032] Wherein, the diglycidyl ether compound is any one of ethylene glycol diglycidyl ether, 1,4-butanediol diglycidyl ether, bisphenol A diglycidyl ether, 1,6-hexanediol diglycidyl ether, and resorcinol diglycidyl ether; the addition amount of the diglycidyl ether compound is 2wt%~20wt%, for example, 5wt%~10wt%; the reaction temperature of the diglycidyl ether compound is 50℃~90℃, for example, 60℃~70℃; the reaction time is 0.5h~5h, for example, 2h~4h; the catalytic hydrolysis time is 0.5h~6h, for example, 1~3h.
[0033] The remaining epoxy groups are polymerized with alcohol amine compounds, and then connected with multifunctional compounds for polycondensation and repeated for multiple times to obtain a chromatographic filler with ion exchange capacity and multiple β-hydroxyl groups on the surface.
[0034] The alcoholamine compound is any one of ethanolamine, diethanolamine, triethanolamine, N-methyldiethanolamine and N,N-dimethylethanol; the polymerization reaction temperature is 50°C to 90°C, for example, 60°C to 80°C; and the reaction time is 0.5h to 6h, for example, 2h to 4h.
[0035] Optionally, the step of quaternizing the matrix microspheres is:
[0036] The matrix microspheres having epoxy groups on the surface are added to an aqueous solution of a basic amine compound in a set proportion or catalyzed under acidic conditions to hydrolyze the epoxy groups in a set proportion into hydroxyl groups;
[0037] Among them, the alkaline amine reagent is any one of triethylamine, N-ethylmorpholine, triethanolamine, and N,N'-dimethylpyridine; the addition ratio of the alkaline amine compound is 2wt%~20wt%, for example, 5wt%~15wt%; the reaction temperature of the alkaline amine compound is 50℃~90℃, for example, 60℃~70℃; the reaction time is 0.5h~5h, for example, 2h~4h.
[0038] The remaining epoxy groups are polymerized with alcohol amine reagents, connected with multifunctional compounds and polycondensed for multiple cycles to obtain a chromatographic filler with ion exchange capacity and multiple β-hydroxyl groups on the surface;
[0039] The alcoholamine compound is any one of ethanolamine, diethanolamine, triethanolamine, N-methyldiethanolamine and N,N-dimethylethanol; the polymerization reaction temperature is 50°C to 90°C, for example, 60°C to 80°C; and the reaction time is 0.5h to 6h, for example, 2h to 4h.
[0040] Optionally, when the chromatographic filler is loaded into an empty column, a homogenization method is used for loading the column.
[0041] Optionally, the matrix microspheres have a particle size of 3 μm to 10 μm, a cross-linking degree of 30% to 80%, and a pore size of 10 nm to 100 nm, for example, a particle size of 5 μm to 8 μm, a cross-linking degree of 50% to 80%, and a pore size of 10 to 50 nm.
[0042] The advantages of the present invention are that the prepared chromatographic filler has good stability and can be used for a long time. The surface of the matrix microspheres is modified by multi-step grafting to contain quaternary ammonium salts carrying multiple β-hydroxyls, so that a hydration zone can be formed near the surface of the matrix microspheres, which greatly improves the hydrophilicity of the chromatographic filler, and at the same time improves the ion separation efficiency, weakens the retention of polyacids, and shortens the peak time. The chromatographic column prepared by the method of the present invention has a chromatographic filler with functional groups attached to the surface of the matrix microspheres, but does not enter the internal pores of the matrix microspheres, which is conducive to improving the mass transfer efficiency, and the functional groups connected by the long carbon chains of the matrix microspheres are far away from the base of the matrix microspheres, which can reduce the interaction between non-ions. BRIEF DESCRIPTION OF THE DRAWINGS
[0043] Figure 1 This is a scanning electron micrograph of the matrix microspheres at a magnification of 5000 times.
[0044] Figure 2 is a chromatogram of the ion chromatography column prepared in Example 1 detecting seven kinds of anions;
[0045] Among them, 1 is F-; 2 is Cl-; 3 is NO2-; 4 is Br-; 5 is NO3-.
[0046] Figure 3 is a chromatogram of seven anions detected by the ion chromatography column prepared in Example 4;
[0047] Among them, 1 is F - ; 2 is Cl - ; 3 is SO4 2- ; 4 is NO2 - ; 5 is Br - ; 6 is PO 4 3- ; 7 is NO3-.
[0048] Figure 4 is a chromatogram of the ion chromatography column prepared in Example 5 for detecting seven kinds of anions;
[0049] Among them, 1 is F - ; 2 is Cl - ; 3 is SO4 2- +NO2 - ; 4 is Br - ; 5 is NO3 - ; 6 is PO 4 3- .
[0050] Figure 5 is a chromatogram of the ion chromatography column prepared in Example 7 for detecting seven kinds of anions;
[0051] Among them, 1 is F - ; 2 is Cl - ; 3 is SO4 2- ; 4 is NO2 - ; 5 is Br - 6 is PO 4 3- ; 7 is NO3 - . DETAILED DESCRIPTION
[0052] The present application is further described in detail below in conjunction with the accompanying drawings and embodiments. It is to be understood that the specific embodiments described herein are only used to explain the relevant invention, rather than to limit the invention. It is also necessary to explain that, for ease of description, only the parts related to the invention are shown in the accompanying drawings.
[0053] It should be noted that, in the absence of conflict, the embodiments and features in the embodiments of the present application can be combined with each other. The present application will be described in detail below with reference to the accompanying drawings and in combination with the embodiments.
[0054] Embodiment 1:
[0055] Step (1): Weigh 5 g of PS-DVB microspheres with a particle size of 5 μm, a cross-linking degree of 80%, and a surface pore size of 10 nm, add 50 mL of a mixed solution of methanol and water (volume ratio of 1:4) and ultrasonically disperse for 5 min to ensure that the matrix microspheres are evenly dispersed. Nitrogen is introduced at a flow rate of 5 mL / min to keep the reaction system in a nitrogen atmosphere, and 1.13 g of cysteamine hydrochloride and 0.1 g of azobisisobutylamidine hydrochloride are added thereto. After mixing, add to a three-necked flask, heat to 70°C, react for 3 h, and wash.
[0056] Step (2): add 45 g of pure water to the filler of step (1) and disperse it evenly by ultrasonication, then add 5 g of 1,4-butanediol diglycidyl ether, react at 70°C for 2 h, and wash; add 47.5 g of pure water to disperse it evenly by ultrasonication, then add 2.5 g of 2-(methylamino)ethanol to react for 2 h, and wash; add 30 mL of 5% diglycidyl ether aqueous solution to react at 60°C for 2 h.
[0057] Step (3): The surface-grafted filler was washed and dried, and loaded into the column using the homogenization method. The column tube specification was 4.0*250 mm. After loading, the column was flushed at a flow rate of 1.0 mL / min for 30 min and tested. The chromatograph model was IC6600 produced by Wanyi, equipped with a suppressed conductivity detector, and the test conditions were 1.0 mL / min, 20 mM kOH.
[0058] Embodiment 2:
[0059] The difference between this embodiment and embodiment 1 is that an amine catalyst is used to hydrolyze part of the epoxy groups into hydroxyl groups, and the steps are as follows:
[0060] Step (1): Weigh 5 g of PS-DVB microspheres with a particle size of 5 μm, a cross-linking degree of 80%, and a surface pore size of 10 nm, add 50 mL of a mixed solution of methanol and water (volume ratio of 1:4) and ultrasonically disperse for 5 min to ensure that the matrix microspheres are evenly dispersed. Nitrogen is introduced at a flow rate of 5 mL / min to keep the reaction system in a nitrogen atmosphere, and 1.13 g of cysteamine hydrochloride and 0.1 g of azobisisobutylamidine hydrochloride are added thereto. After mixing, add to a three-necked flask, heat to 70°C, react for 3 h, and wash.
[0061] Step (2): add 45 g of pure water to the filler in step (1) and disperse it evenly, then add 5 g of 1,4-butanediol diglycidyl ether, react at 70°C for 2 h, and wash; add 50 mL of 3% triethanolamine aqueous solution, react at 90°C for 2 h, then add 2.5 g of 2-(methylamino)ethanol, react for 2 h, and wash; add 30 mL of 5% diglycidyl ether aqueous solution at 60°C and react for 2 h.
[0062] Step (3): Same as step (3) of Example 1.
[0063] There are no drawings for this embodiment.
[0064] Embodiment 3:
[0065] The difference between this embodiment and embodiment 1 is that the alkaline condition causes partial hydrolysis of epoxy to hydroxyl groups, and the steps are as follows:
[0066] Step (1): Weigh 5 g of PS-DVB microspheres with a particle size of 5 μm, a cross-linking degree of 80%, and a surface pore size of 10 nm, add 50 mL of a mixed solution of methanol and water (volume ratio of 1:4) and ultrasonically disperse for 5 min to ensure that the matrix microspheres are evenly dispersed. Nitrogen is introduced at a flow rate of 5 mL / min to keep the reaction system in a nitrogen atmosphere, and 1.13 g of cysteamine hydrochloride and 0.1 g of azobisisobutylamidine hydrochloride are added thereto. After mixing, add to a three-necked flask, heat to 70°C, react for 3 h, and wash.
[0067] Step (2): add 45 g of pure water to the filler in step (1) and disperse it evenly, then add 5 g of 1,4-butanediol diglycidyl ether and react at 70°C for 2 h; prepare 100 mL of 0.1 M NaOH solution, disperse the filler in the NaOH solution, stir at room temperature for 2 h, and wash; add 47.5 g of pure water to disperse it evenly by ultrasonic, then add 2.5 g of 2-(methylamino)ethanol to react for 2 h, and wash; and add 30 mL of 5% diglycidyl ether aqueous solution at 60°C and react for 2 h.
[0068] Step (3): Same as step (3) of Example 1.
[0069] There are no drawings for this embodiment.
[0070] Embodiment 4:
[0071] The difference between this embodiment and embodiment 2 is that the polyhydroxyamine compound is grafted gradually, and the steps are as follows:
[0072] Step (1): Weigh 5 g of PS-DVB microspheres with a particle size of 5 μm, a cross-linking degree of 80%, and a surface pore size of 10 nm, add 50 mL of a mixed solution of methanol and water (volume ratio of 1:4) and ultrasonically disperse for 5 min to ensure that the matrix microspheres are evenly dispersed. Nitrogen is introduced at a flow rate of 5 mL / min to keep the reaction system in a nitrogen atmosphere, and 1.13 g of cysteamine hydrochloride and 0.1 g of azobisisobutylamidine hydrochloride are added thereto. After mixing, add to a three-necked flask, heat to 70°C, react for 3 h, and wash.
[0073] Step (2): add 45g of pure water to the filler of step (1) and disperse it evenly, then add 5g of 1,4-butanediol diglycidyl ether, react at 70°C for 2h, and wash; add 50mL of 3% triethanolamine aqueous solution, react at 90°C for 2h, then add 2.5g of 2-(methylamino)ethanol to react for 2h, and wash; add 45g of pure water to disperse it evenly by ultrasonic, then add 5g of 1,4-butanediol diglycidyl ether, react at 70°C for 2h, and wash; add 47.5g of pure water to disperse it evenly, then add 2.5g of N-methyldiethanolamine to react for 2h;
[0074] Step (3): The same as step (3) of Example 1, the test conditions were 1.0 mL / min, 38 mM kOH.
[0075] Embodiment 5:
[0076] The difference between this embodiment and embodiment 4 is that the surface of the base ball is modified with hydroxyl groups, and the steps are as follows:
[0077] Step (1): Weigh 5 g of PS-DVB microspheres with a particle size of 5 μm, a crosslinking degree of 80%, and a surface pore size of 10 nm, add 100 mL of a mixed solution of methanol and water (volume ratio of 3:2) and ultrasonically disperse for 5 min to ensure that the matrix microspheres are evenly dispersed. Nitrogen is introduced at a flow rate of 5 mL / min to keep the reaction system in a nitrogen atmosphere, and 1.13 g of cysteamine hydrochloride, 1.73 g of vinyl acetate, and 0.1 g of azobisisobutylamidine hydrochloride are added thereto. After mixing, add to a three-necked flask, heat to 70°C, react for 4 h, and wash.
[0078] Step (2): add 45 g of pure water to step (1) and disperse evenly, then add 5 g of 1,4-butanediol diglycidyl ether, react at 70°C for 2 h, and wash; add 47.5 g of pure water to disperse evenly by ultrasonic, then add 2.5 g of 2-(methylamino)ethanol to react for 2 h, and wash; add 5 g of 1,4-butanediol diglycidyl ether to disperse evenly, then add 47.5 g of pure water to disperse evenly, then add 2.5 g of N-methyldiethanolamine to react for 2 h, and wash; prepare 100 mL of 0.5 M methanesulfonic acid aqueous solution, and place the prepared filler in the solution and stir for 2 h.
[0079] Step (3): The same as step (3) of Example 1, the test conditions were 1.0 mL / min, 20 mM kOH.
[0080] Embodiment 6:
[0081] The difference between this embodiment and embodiment 4 is that matrix microspheres of different specifications are used, and the steps are as follows:
[0082] Step (1): Weigh 5 g of PS-DVB microspheres with a particle size of 5 μm, a cross-linking degree of 80%, and a surface pore size of 30 nm, add 50 mL of a mixed solution of methanol and water (volume ratio of 1:4) and ultrasonically disperse for 5 min to ensure that the matrix microspheres are evenly dispersed. Nitrogen is introduced at a flow rate of 5 mL / min to keep the reaction system in a nitrogen atmosphere, and 1.13 g of cysteamine hydrochloride and 0.1 g of azobisisobutylamidine hydrochloride are added thereto. After mixing, add to a three-necked flask, heat to 70°C, react for 3 h, and wash.
[0083] Step (2): add 45g of pure water to the filler of step (1) and disperse it evenly, then add 5g of 1,4-butanediol diglycidyl ether, react at 70°C for 2h, and wash; add 50mL of 3% triethanolamine aqueous solution, react at 90°C for 2h, then add 2.5g of 2-(methylamino)ethanol to react for 2h, and wash; add 45g of pure water to disperse it evenly by ultrasonic, then add 5g of 1,4-butanediol diglycidyl ether, react at 70°C for 2h, and wash; add 47.5g of pure water to disperse it evenly, then add 2.5g of N-methyldiethanolamine to react for 2h;
[0084] Step (3): Same as step (3) of Example 1.
[0085] There are no drawings for this embodiment.
[0086] Embodiment 7:
[0087] The difference between this embodiment and embodiment 4 is that the base ball is epoxy functionalized-quaternized, and the steps are as follows:
[0088] Step (1): Weigh 5 g of PS-DVB microspheres with a particle size of 5 μm, a crosslinking degree of 80%, and a surface pore size of 10 nm, add 50 mL of a mixed solution of methanol and water (volume ratio of 1:4) and ultrasonically disperse for 5 min to ensure that the matrix microspheres are evenly dispersed. Nitrogen is introduced at a flow rate of 5 mL / min to keep the reaction system in a nitrogen atmosphere, and 2.28 g of allyl glycidyl ether and 0.1 g of azobisisobutylamidine hydrochloride are added thereto. After mixing, add to a three-necked flask, heat to 70°C, react for 3 h, and wash.
[0089] Step (2): add 50 mL of 3% triethanolamine aqueous solution to the filler in step (1), react at 90°C for 2 h, then add 2.5 g of 2-(methylamino)ethanol to react for 2 h, and wash; add 45 g of pure water to disperse evenly by ultrasonic, then add 5 g of 1,4-butanediol diglycidyl ether, react at 70°C for 2 h, and wash; add 47.5 g of pure water to disperse evenly, then add 2.5 g of N-methyldiethanolamine to react for 2 h;
[0090] Step (3): The same as step (3) of Example 1, the test conditions were 1.0 mL / min, 38 mM kOH.
[0091] The above description is only a preferred embodiment of the present application and an explanation of the technical principles used. Those skilled in the art should understand that the scope of the invention involved in the present application is not limited to the technical solution formed by a specific combination of the above technical features, but should also cover other technical solutions formed by any combination of the above technical features or their equivalent features without departing from the inventive concept. For example, the above features are replaced with (but not limited to) technical features with similar functions disclosed in the present application.
[0092] Except for the technical features described in the specification, the remaining technical features are known technologies to those skilled in the art. In order to highlight the innovative features of the present invention, the remaining technical features will not be described here in detail.
Claims
1. A method for preparing an anion chromatography column, characterized in that: The following steps are involved: S1, preparing chromatographic filler; Wherein, the steps of preparing the chromatographic filler are: S11, introducing functional groups into the matrix microspheres and causing polymerization reaction to obtain matrix microspheres having epoxy groups; S12, quaternizing the obtained matrix microspheres having epoxy groups to obtain a chromatographic filler having multiple β-hydroxyl groups; S13, the functional group introduced into the matrix microspheres is an amino group or an epoxy group; S2, loading the chromatographic filler into an empty column to obtain a chromatographic column; The prepared chromatographic filler is cleaned and dried, and then loaded into a column by a homogenization method, wherein the chromatographic filler is homogenized with a KOH solution and loaded into a column packing machine to prepare a chromatographic column; S3, testing the prepared chromatographic column; After the chromatographic column was prepared, it was rinsed with KOH solution and tested. The test sample was F - , Cl - 、NO2 - Br - 、NO3 - 、SO4 2- PO4 3- .
2. The method for preparing an anion chromatography column according to claim 1, characterized in that: The functional groups introduced into the matrix microspheres are amino groups; The step of introducing functional groups into the matrix microspheres is: Dissolve the matrix microspheres in a set ratio of alcohol-water mixed solution, and stir thoroughly to make the matrix microspheres dispersed evenly; A set amount of water-soluble initiator and mercaptoamine compound are added under nitrogen atmosphere, and then at a set temperature, residual double bonds on the surface of microspheres react with the mercapto groups of the mercaptoamine compound to obtain matrix microspheres with epoxy groups on the surface.
3. The method for preparing an anion chromatography column according to claim 1, characterized in that: The functional groups introduced into the matrix microspheres are epoxy groups; The step of introducing functional groups into the matrix microspheres is: Dissolve the matrix microspheres in a set ratio of alcohol-water mixed solution, and stir thoroughly to make the matrix microspheres dispersed evenly; A set amount of water-soluble initiator and olefin epoxy compound are added under nitrogen atmosphere, and then the residual double bonds on the surface of microspheres are polymerized with the double bonds of olefin epoxy compound at a set temperature to obtain matrix microspheres with epoxy groups on the surface.
4. The method for preparing an anion chromatography column according to claim 2, characterized in that: The steps of quaternizing the matrix microspheres are as follows: The matrix microspheres having epoxy groups on the surface are reacted with a multifunctional diglycidyl ether compound in a set ratio, and an alkaline amine reagent is used or catalyzed under acidic conditions to hydrolyze the epoxy groups in the set ratio into hydroxyl groups; The remaining epoxy groups are polymerized with alcohol amine compounds, and then connected with multifunctional compounds for polycondensation and repeated for multiple times to obtain a chromatographic filler with ion exchange capacity and multiple β-hydroxyl groups on the surface.
5. The method for preparing anion chromatography column according to claim 3, characterized in that: The steps of quaternizing the matrix microspheres are as follows: The matrix microspheres having epoxy groups on the surface are added to an aqueous solution of a basic amine compound in a set proportion or catalyzed under acidic conditions to hydrolyze the epoxy groups in a set proportion into hydroxyl groups; The remaining epoxy groups are polymerized with alcohol amine reagents, connected with multifunctional compounds through condensation polymerization, and cycled for multiple times to obtain a chromatographic filler with ion exchange capacity and multiple β-hydroxyl groups on the surface.
6. The method for preparing anion chromatography column according to claim 1, characterized in that: When loading chromatographic packing into an empty column, the homogenization method is used.
7. The method for preparing anion chromatography column according to claim 1, characterized in that: The matrix microspheres have a particle size of 3 μm to 10 μm, a cross-linking degree of 30% to 80%, and a pore size of 10 nm to 100 nm.
8. The method for preparing anion chromatography column according to claim 2, characterized in that: The water-soluble initiator is any one of azobisisobutylamidine hydrochloride, potassium persulfate, and ammonium persulfate; The mercaptoamine compound is any one of β-mercaptoethylamine, mercaptopropylamine, cysteamine hydrochloride and cysteine.
9. The method for preparing anion chromatography column according to claim 3, characterized in that: The olefin epoxide is any one of 3,4-epoxy-1-butene, allyl glycidyl ether, and glycidyl methacrylate.
10. The method for preparing anion chromatography column according to claim 4, characterized in that: The diglycidyl ether compound is any one of ethylene glycol diglycidyl ether, 1,4-butanediol diglycidyl ether, bisphenol A diglycidyl ether, 1,6-hexanediol diglycidyl ether, and resorcinol diglycidyl ether; The alkaline amine reagent is any one of triethylamine, N-ethylmorpholine, triethanolamine, and N,N'-dimethylpyridine; The alcoholamine compound is any one of ethanolamine, diethanolamine, triethanolamine, N-methyldiethanolamine and N,N-dimethylethanol.