CN115414921A - Surface modification method of ion exchange filler - Google Patents
Surface modification method of ion exchange filler Download PDFInfo
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- CN115414921A CN115414921A CN202211046467.0A CN202211046467A CN115414921A CN 115414921 A CN115414921 A CN 115414921A CN 202211046467 A CN202211046467 A CN 202211046467A CN 115414921 A CN115414921 A CN 115414921A
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- 238000005342 ion exchange Methods 0.000 title claims abstract description 47
- 239000000945 filler Substances 0.000 title claims abstract description 34
- 238000002715 modification method Methods 0.000 title claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 90
- 238000006243 chemical reaction Methods 0.000 claims abstract description 58
- 238000003756 stirring Methods 0.000 claims abstract description 50
- 239000008213 purified water Substances 0.000 claims abstract description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000001914 filtration Methods 0.000 claims abstract description 40
- RCXHRHWRRACBTK-UHFFFAOYSA-N 3-(oxiran-2-ylmethoxy)propane-1,2-diol Chemical compound OCC(O)COCC1CO1 RCXHRHWRRACBTK-UHFFFAOYSA-N 0.000 claims abstract description 34
- 230000004048 modification Effects 0.000 claims abstract description 33
- 238000012986 modification Methods 0.000 claims abstract description 33
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- 229920000058 polyacrylate Polymers 0.000 claims abstract description 22
- 239000007864 aqueous solution Substances 0.000 claims abstract description 17
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 claims abstract description 16
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 claims abstract description 9
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims abstract description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims description 59
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
- 238000012856 packing Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 11
- 230000035484 reaction time Effects 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 238000005086 pumping Methods 0.000 claims description 5
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 4
- 238000004062 sedimentation Methods 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims 1
- 238000011068 loading method Methods 0.000 abstract description 22
- 235000019441 ethanol Nutrition 0.000 description 5
- 102000004169 proteins and genes Human genes 0.000 description 5
- 108090000623 proteins and genes Proteins 0.000 description 5
- 238000004811 liquid chromatography Methods 0.000 description 4
- 230000004913 activation Effects 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 125000000524 functional group Chemical group 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000012501 chromatography medium Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009509 drug development Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000006011 modification reaction Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000001742 protein purification Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/281—Sorbents specially adapted for preparative, analytical or investigative chromatography
- B01J20/282—Porous sorbents
- B01J20/285—Porous sorbents based on polymers
-
- 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
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a surface modification method of an ion exchange filler, which is characterized by comprising the following steps: base sphere modification: adding purified water and sodium hydroxide solid into a modification kettle, and uniformly stirring; adding polyacrylate-based balls into the modification kettle, and uniformly stirring; dropwise adding glycerol glycidyl ether into the modification kettle, and stirring for reaction for at least 3 hours; after the reaction is finished, transferring the materials into a centrifugal machine, and performing throwing filtration; bonding reaction: adding purified water and nitric acid into a bonding kettle, and uniformly stirring; adding the modified material obtained after the base ball modification, glycidyl methacrylate and 1,4-dioxane into the bonding kettle, and carrying out a first stirring reaction; after the reaction is finished, adding a trimethylamine aqueous solution into the bonding kettle, and carrying out a second stirring reaction; after the reaction is finished, transferring the materials into a centrifugal machine, and filtering by throwing. The invention can increase the dynamic loading capacity of the ion exchange material.
Description
Technical Field
The invention relates to the field of ion exchange packing, in particular to a surface modification method of ion exchange packing.
Background
At present, the liquid chromatography packing material is widely applied to the technical fields of drug development, substance analysis and separation and the like, wherein a High Performance Liquid Chromatography (HPLC) is the most common analysis and separation means. The packing material (i.e. liquid chromatography medium) of liquid chromatography is the key basis for the establishment and development of high performance liquid chromatography technology. The ion exchange packing is a common liquid chromatography packing. With the development of cell technology and bioengineering, there are a lot of purification and analysis works of biomolecules such as proteins and enzymes, and the ion exchange filler needs to have higher Dynamic loading (DBC) so as to separate and purify more target proteins with the same or even less amount of DBC.
The dynamic loading capacity of the existing ion exchange filler is generally not more than 60mg/mL, and the existing ion exchange filler can not meet the industrial requirements gradually along with the improvement of the requirements of protein separation and purification, so that the fast and high-loading ion exchange filler is urgently needed to meet the requirements of protein purification.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a surface modification method of an ion exchange filler, which can increase the dynamic loading capacity of an ion exchange material.
The invention is realized by the following technical scheme:
a surface modification method of an ion exchange filler is characterized by comprising the following steps:
base sphere modification: adding purified water and sodium hydroxide solid into a modification kettle, and uniformly stirring; adding polyacrylate-based balls into the modification kettle, and uniformly stirring; dropwise adding glycerol glycidyl ether into the modification kettle, and stirring for reaction for at least 3 hours; after the reaction is finished, transferring the material into a centrifuge for spin-filtering to obtain a modified material;
bonding reaction: adding purified water and nitric acid into a bonding kettle, and uniformly stirring; adding the modified material obtained after base ball modification, glycidyl methacrylate and 1,4-dioxane into a bonding kettle, and carrying out primary stirring reaction; after the reaction is finished, adding a trimethylamine aqueous solution into the bonding kettle, and carrying out a second stirring reaction; and after the reaction is finished, transferring the materials into a centrifugal machine for filtering in a throwing way.
Further, the weight ratio of the polyacrylate ball, the sodium hydroxide solid and the glycerol glycidyl ether in the ball modification step is 1: 2.8-3.1.
Further, the weight ratio of the polyacrylate ball to the glycerol glycidyl ether is 1.
Further, the weight ratio of the modified material, nitric acid, glycidyl methacrylate, 1,4-dioxane and trimethylamine in the bonding reaction step is 1:0.09 to 0.11: 0.23-0.25.
Further, the dropping mode of the glycerol glycidyl ether is dropping the glycerol glycidyl ether at a constant speed at the temperature of 30-35 ℃, and the dropping time is 2.5-3.0 hours.
Furthermore, the stirring reaction time of the first stirring reaction in the bonding reaction is at least 1 hour, and the stirring reaction temperature is 20-30 ℃.
Furthermore, the stirring reaction time of the second stirring reaction in the bonding reaction is at least 18 hours, and the stirring reaction temperature is 20-30 ℃.
Further, the base ball modification further comprises the following steps:
rinsing: washing the material obtained after centrifugal filtration by using purified water, and draining after washing; washing the filtered and dried material by using absolute ethyl alcohol, and filtering to dry after washing; washing the filtered and dried material by using purified water, and filtering to be dried after washing is finished;
washing: washing the rinsed material with 0.5M sulfuric acid aqueous solution; washing again by using purified water, and filtering to dry after washing; and (5) filling the filtered and dried material into a material barrel for later use.
Further, the bonding reaction further comprises the following steps:
rinsing with purified water: washing the centrifugally filtered and dried material by using purified water, and filtering to dry after washing is finished;
sulfuric acid washing: washing the rinsed material with 0.5M sulfuric acid aqueous solution, then washing with purified water, and filtering to dry after washing;
and (3) settling: transferring the filtered and dried material to a deposition barrel, adding 20% ethanol water solution, stirring uniformly, settling, layering the filler, and then pumping out supernatant; repeatedly settling for multiple times;
centrifugal filtration: transferring the settled material to a centrifuge for centrifugal filtration.
Further, the number of times of sedimentation in the bonding reaction is 2.
Compared with the prior art, the invention has the advantages that:
1. the invention provides a surface modification method of an ion exchange filler, which realizes the increase of the dynamic loading capacity of an ion exchange material by carrying out surface activation and bonding reaction after modifying a polyacrylate-based sphere, and further has the characteristics of high ion exchange capacity, high protein binding loading capacity, high operation flow rate and the like.
2. By controlling the weight ratio of the polyacrylate-based spheres to the glycerol glycidyl ether to be 1.3-9.5 and selecting a mode of dropwise adding the glycidyl methacrylate at a constant speed, the glycerol glycidyl ether does not cover holes on the surface of the polyacrylate-based spheres due to excessive use amount or uneven dispersion in the adding process, and further, the situation that functional groups in internal holes cannot contact with the glycerol glycidyl ether and modified functional groups are reduced to influence the product loading capacity is avoided; and the functional groups in the polyacrylate-based sphere cannot be completely modified due to too little glycerol glycidyl ether; further increasing the dynamic loading of the ion-exchanged material.
Drawings
FIG. 1 is a flow chart illustrating a base sphere modification step in a surface modification method of an ion exchange packing according to the present invention;
FIG. 2 is a flow chart of the bonding reaction step in the surface modification method of an ion exchange packing of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples, so that those skilled in the art can fully understand the technical contents of the present invention. It should be understood that the following examples are intended to further illustrate the present invention and should not be construed as limiting the scope of the present invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art based on the foregoing description are intended to be covered by the present invention. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Referring to fig. 1 to 2, the present invention provides a surface modification method of an ion exchange filler, comprising the following main steps:
s1 base ball modification:
modification: adding purified water and sodium hydroxide solid into a modification kettle, and uniformly stirring; adding polyacrylate-based balls into the modification kettle, and uniformly stirring; and adding glycerol glycidyl ether into the modification kettle, and stirring for reaction for at least 3 hours. Wherein the weight ratio of the sodium hydroxide solid to the polyacrylate-based spheres to the glycerol glycidyl ether is (2.8-3.1). Further, the weight ratio of the polyacrylate ball to the glycerol glycidyl ether is preferably 1. Preferably, the dropping mode of the glycerol glycidyl ether is dropping the glycerol glycidyl ether at a constant speed at the temperature of 30-35 ℃, and the dropping time is 2.5-3.0 hours.
Centrifugal filtration: and transferring the modified material obtained after the reaction into a centrifugal machine for filtering in a throwing way.
Rinsing with purified water: washing the material obtained after centrifugal filtration by using purified water, wherein the weight ratio of the purified water to the polyacrylate-based spheres is 6-7:1, and draining the material after washing.
Ethanol rinsing: washing the drained material by using absolute ethyl alcohol, wherein the weight ratio of the absolute ethyl alcohol to the polyacrylate-based spheres is 5-6:1, and draining the material after washing.
Rinsing with purified water: washing the material obtained after centrifugal filtration by using purified water, wherein the weight ratio of the purified water to the polyacrylate-based spheres is 6-7:1, and draining the material after washing.
Sulfuric acid washing: and (3) washing the rinsed materials by using a 0.5M sulfuric acid aqueous solution, wherein the weight ratio of the 0.5M sulfuric acid aqueous solution to the polyacrylate-based balls is 10-11.
Washing with purified water: and (3) washing again by using purified water, wherein the weight ratio of the purified water to the polyacrylate-based spheres is 6-7:1, and filtering the materials to be dried after washing.
Loading into a material barrel: and (5) filling the filtered and dried material into a material barrel for later use.
S2, bonding reaction:
surface activation: adding purified water and nitric acid into the bonding kettle, and uniformly stirring; adding the modified material obtained after the base ball modification, glycidyl methacrylate and 1,4-dioxane into the bonding kettle, and carrying out a first stirring reaction. Wherein the weight ratio of the nitric acid to the modification material to the glycidyl methacrylate to the 1,4-dioxane is 0.09-0.11: 1: 0.23-0.25. The stirring reaction time of the first stirring reaction is at least 1 hour, and the stirring reaction temperature is 20-30 ℃.
Bonding: and after the surface activation reaction is finished, adding a trimethylamine aqueous solution into the bonding kettle, stirring for the second time and carrying out bonding reaction. Wherein the weight ratio of the modified material to the trimethylamine is 1:1.8 to 2.2. The stirring reaction time of the second stirring reaction is at least 18 hours, and the stirring reaction temperature is 20-30 ℃.
Centrifugal filtration: transferring the material obtained after the bonding reaction into a centrifuge for filtering.
Rinsing with purified water: washing the centrifugally filtered and dried material by using purified water, wherein the weight ratio of the purified water to the modified material is 5-7:1, and filtering the material to be dried after washing.
Sulfuric acid washing: and washing the rinsed material by using a 0.5M sulfuric acid aqueous solution, wherein the weight ratio of the 0.5M sulfuric acid aqueous solution to the modified material is 10-11.
Rinsing with purified water: and (3) continuously washing by using purified water, wherein the weight ratio of the purified water to the modified material is 5-7:1, and filtering the material to be dried after washing.
And (3) settling: transferring the filtered and dried material to a deposition barrel, adding 20% ethanol water solution, wherein the weight ratio of the 20% ethanol water solution to the modified material is 12-14; repeated sedimentation for 2 times;
centrifugal filtration: transferring the settled material to a centrifuge for centrifugal filtration.
Packaging: and (3) uniformly dispersing the centrifuged material by using a 20% ethanol aqueous solution, wherein the weight ratio of the 20% ethanol aqueous solution to the modified material is 15-17, filling the material into a material barrel, sampling and inspecting, sealing the material barrel, attaching a finished product label to a to-be-inspected area, and warehousing the material after the material is qualified.
Example 1
Modification reaction: pumping 16.62kg of purified water into a 100L modification kettle, adding 1.00kg of sodium hydroxide solid, and stirring for dissolving; adding 6.00kg of polyacrylate-based balls into the kettle, and uniformly stirring; and uniformly dropwise adding 56.42kg of glycerol glycidyl ether into the modification kettle, maintaining the temperature at 30-35 ℃, keeping the temperature for 2.5-3.0 hours, finishing dropwise adding, keeping the temperature at 30-35 ℃, and stirring for reaction for 3 hours. And after the reaction is finished, transferring the materials into a centrifugal machine for filtering in a throwing way.
Washing the obtained material after centrifugal filtration with purified water for three times, using 40.00kg of purified water each time, and filtering to dryness after washing is finished;
continuously washing the filtered and dried materials with absolute ethyl alcohol for three times, using 32.00kg of absolute ethyl alcohol each time, and filtering to dry after washing is finished;
continuously washing the filtered and dried material with purified water for three times, using 40.00kg of purified water each time, and filtering to dry after washing is finished;
the drained material was washed with 63.00kg of 0.5M aqueous sulfuric acid, then 10 times with 40.00kg of purified water each time, and drained for use after washing.
Bonding reaction: pumping 36.00kg of purified water into a 100L bonding kettle, adding 0.60kg of nitric acid, and uniformly stirring; adding 1.44kg of modified material obtained after base ball modification, 1.44kg of glycidyl methacrylate and 9.00kg of 1,4-dioxane, and stirring and reacting for 1 hour at the temperature of 20-30 ℃. After the reaction, 18.48L of 30% trimethylamine aqueous solution was continuously added into the bonding kettle, and the reaction was stirred at 20 to 30 ℃ for 18 hours. And after the reaction is finished, transferring the materials into a centrifugal machine for filtering in a throwing way.
Washing the centrifugally filtered and dried material with purified water for 10 times, wherein 40.00kg of purified water is used each time, and filtering to dry after washing is finished;
then, the drained material was washed with 63.00kg of 0.5M aqueous sulfuric acid solution, and then washed with 10 times of purified water, 40.00kg of purified water was used each time, and after the washing, the material was drained for use.
Transferring the filtered dry material to a settling tank, adding 76.00kg of 20% ethanol aqueous solution, stirring uniformly, settling, layering a filler, and then pumping out a supernatant. The settling operation was repeated 2 times.
The material was transferred to a grade D clean zone and the material was transferred to a centrifuge, centrifuged and held. And uniformly dispersing the drained materials by using 96.00kg of 20% ethanol aqueous solution, loading the materials into a material barrel, sampling and inspecting, sealing the material barrel, attaching a finished product label to a detection area, and warehousing the materials after the materials are qualified.
The dynamic loading capacity of the ion exchange filler prepared by the surface modification method of the ion exchange filler can reach 87.1mg/mL.
Example 2
The only difference from example 1 is: the addition amount of glycerol glycidyl ether was 62.06kg by dividing glycerol glycidyl ether into six equal parts and adding one part of glycerol glycidyl ether every half an hour. The rest steps and the usage amount are the same as those in the embodiment 1, and are not described herein.
The dynamic loading capacity of the ion exchange filler prepared by the surface modification method of the ion exchange filler can reach 63mg/mL.
Example 3
The only difference from example 1 is: the addition amount of glycerol glycidyl ether was 50.78kg, and the addition was carried out by dividing glycerol glycidyl ether into six equal parts and adding one part of glycerol glycidyl ether every half an hour. The rest steps and the usage amount are the same as those in the embodiment 1, and are not described herein.
The dynamic loading capacity of the ion exchange filler prepared by the surface modification method of the ion exchange filler can reach 59.6mg/mL.
Example 4
The only difference from example 1 is: the glycerol glycidyl ether is added in a mode that the glycerol glycidyl ether is divided into six equal parts, and one part of the glycerol glycidyl ether is added every half hour. The rest steps and the usage amount are the same as those in the embodiment 1, and are not described herein.
The dynamic loading capacity of the ion exchange filler prepared by the surface modification method of the ion exchange filler can reach 76mg/mL.
Example 5
The only difference from example 1 is: the glycerol glycidyl ether is added at one time in an adding mode. The rest steps and the usage amount are the same as those in the embodiment 1, and are not described herein.
The dynamic loading capacity of the ion exchange filler prepared by the surface modification method of the ion exchange filler can reach 75.5mg/mL
The dynamic loadings of the ion exchange packing prepared in examples 1-5 are shown in table 1 below:
as can be seen from the data in Table 1, the dynamic loading capacity of the ion exchange filler prepared by the surface modification method can reach 59-88 mg/mL, and is more excellent compared with the loading capacity of the existing ion exchange filler, and the ion exchange filler has the characteristics of high ion exchange capacity, high protein binding capacity, high operation flow rate and the like. Furthermore, the dynamic loading of the ion exchange filler can be controlled to be 75 to 88mg/mL by controlling the weight ratio of the polyacrylate sphere to the glycerol glycidyl ether to be 1.3 to 9.5. Further adopts a feeding mode of dropping glycerol glycidyl ether at a constant speed, so that the dynamic loading capacity of the ion exchange filler can reach 87.1mg/mL. Therefore, the dynamic loading capacity of the ion exchange filler can be further improved by controlling the weight ratio of the polyacrylate-based spheres to the glycerol glycidyl ether to be 1.3-9.5 and by controlling the feeding mode of dropwise adding the glycerol glycidyl ether at a constant speed, so that the performance of the ion exchange filler is further improved.
It should be noted that the above-mentioned preferred embodiments are merely illustrative of the technical concepts and features of the present invention, and are intended to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (10)
1. A surface modification method of an ion exchange filler is characterized by comprising the following steps:
base sphere modification: adding purified water and sodium hydroxide solid into a modification kettle, and uniformly stirring; adding polyacrylate-based balls into the modification kettle, and uniformly stirring; dropwise adding glycerol glycidyl ether into the modification kettle, and stirring for reaction for at least 3 hours; after the reaction is finished, transferring the material into a centrifuge for spin-filtering to obtain a modified material;
bonding reaction: adding purified water and nitric acid into a bonding kettle, and uniformly stirring; adding the modified material obtained after base ball modification, glycidyl methacrylate and 1,4-dioxane into a bonding kettle, and carrying out primary stirring reaction; after the reaction is finished, adding a trimethylamine aqueous solution into the bonding kettle, and carrying out a second stirring reaction; and after the reaction is finished, transferring the materials into a centrifugal machine for filtration.
2. The method for modifying the surface of an ion exchange packing according to claim 1, wherein the weight ratio of polyacrylate balls, solid sodium hydroxide and glycerol glycidyl ether in the ball modification step is 1: 2.8-3.1.
3. The method of claim 2, wherein the weight ratio of the polyacrylate spheres to the glycerol glycidyl ether is 1.
4. The method for modifying the surface of an ion exchange packing according to claim 1, wherein the weight ratio of the modifying material, nitric acid, glycidyl methacrylate, 1,4-dioxane and trimethylamine in the bonding reaction step is 1:0.09 to 0.11: 0.23-0.25.
5. The method for modifying the surface of an ion exchange filler according to claim 2, wherein the glycerol glycidyl ether is added dropwise at a constant rate at a temperature of 30 to 35 ℃ for 2.5 to 3.0 hours.
6. The method for modifying the surface of an ion exchange filler according to any one of claims 1 to 4, wherein the stirring reaction time of the first stirring reaction in the bonding reaction is at least 1 hour, and the stirring reaction temperature is 20 to 30 ℃.
7. The method for modifying the surface of an ion exchange filler according to any one of claims 1 to 4, wherein the stirring reaction time of the second stirring reaction in the bonding reaction is at least 18 hours, and the stirring reaction temperature is 20 to 30 ℃.
8. The method for surface modification of ion exchange packing according to any one of claims 1 to 4, wherein the base sphere modification further comprises the steps of:
rinsing: washing the material obtained after centrifugal filtration by using purified water, and filtering to dry after washing is finished; washing the drained materials by using absolute ethyl alcohol, and draining after washing is finished; washing the filtered and dried material by using purified water, and filtering and drying after washing is finished;
washing: washing the rinsed material with 0.5M sulfuric acid aqueous solution; and washing again by using purified water, and filtering to dry after washing.
9. The method for modifying the surface of an ion exchange packing according to any one of claims 1 to 4, wherein the bonding reaction further comprises the steps of:
rinsing with purified water: washing the centrifugally filtered and dried material by using purified water, and filtering to dry after washing is finished;
sulfuric acid washing: washing the rinsed material with 0.5M sulfuric acid aqueous solution, then washing with purified water, and filtering to dry after washing;
and (3) settling: transferring the filtered and dried material to a sedimentation barrel, adding 20% ethanol water solution, stirring uniformly, settling, layering filling materials, and then pumping out supernatant; repeatedly settling for multiple times;
centrifugal filtration: transferring the settled material to a centrifuge for centrifugal filtration.
10. The method of claim 9, wherein the number of settlings in the bonding reaction is 2.
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020099104A1 (en) * | 2001-01-24 | 2002-07-25 | Tosoh Corporation | Anion exchanger, process for producing same, and its use |
| CN104945637A (en) * | 2015-06-24 | 2015-09-30 | 浙江大学 | Method for preparing grafting type strong preservation anion chromatographic packing |
| CN105396628A (en) * | 2015-12-06 | 2016-03-16 | 杭州飞山浩科技有限公司 | Preparation method of polyethylene polyamine graft-modified polystyrene-divinyl benzene ion chromatographic packing |
| CN105478094A (en) * | 2015-12-25 | 2016-04-13 | 四川大学 | Aminated poly-glycidyl methacrylate crosslinked composite microsphere and preparation method as well as application thereof |
| CN105727911A (en) * | 2016-03-10 | 2016-07-06 | 天津大学 | Glycidyl-methacrylate-grafted and diethylamine-modified agarose gel chromatographic medium, method for preparing same and application of glycidyl-methacrylate-grafted and diethylamine-modified agarose gel chromatographic medium |
| CN108467481A (en) * | 2018-03-13 | 2018-08-31 | 常州大学 | A kind of synthetic method of the degradable polymer of the double bond containing pendency |
| WO2021238315A1 (en) * | 2020-05-25 | 2021-12-02 | 浙江大学 | Grafted quaternary ammonium group cation resin and preparation method therefor |
| 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 |
| CN114262465A (en) * | 2021-11-03 | 2022-04-01 | 赛分科技扬州有限公司 | Polyacrylate-based sphere and amine salt modification method thereof |
| WO2022083799A1 (en) * | 2021-06-15 | 2022-04-28 | 广东省农业科学院农业生物基因研究中心 | Immobilized metal ion affinity chromatographic packing, chromatographic column, and preparation method therefor |
-
2022
- 2022-08-30 CN CN202211046467.0A patent/CN115414921B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020099104A1 (en) * | 2001-01-24 | 2002-07-25 | Tosoh Corporation | Anion exchanger, process for producing same, and its use |
| CN104945637A (en) * | 2015-06-24 | 2015-09-30 | 浙江大学 | Method for preparing grafting type strong preservation anion chromatographic packing |
| CN105396628A (en) * | 2015-12-06 | 2016-03-16 | 杭州飞山浩科技有限公司 | Preparation method of polyethylene polyamine graft-modified polystyrene-divinyl benzene ion chromatographic packing |
| CN105478094A (en) * | 2015-12-25 | 2016-04-13 | 四川大学 | Aminated poly-glycidyl methacrylate crosslinked composite microsphere and preparation method as well as application thereof |
| CN105727911A (en) * | 2016-03-10 | 2016-07-06 | 天津大学 | Glycidyl-methacrylate-grafted and diethylamine-modified agarose gel chromatographic medium, method for preparing same and application of glycidyl-methacrylate-grafted and diethylamine-modified agarose gel chromatographic medium |
| CN108467481A (en) * | 2018-03-13 | 2018-08-31 | 常州大学 | A kind of synthetic method of the degradable polymer of the double bond containing pendency |
| WO2021238315A1 (en) * | 2020-05-25 | 2021-12-02 | 浙江大学 | Grafted quaternary ammonium group cation resin and preparation method therefor |
| WO2022083799A1 (en) * | 2021-06-15 | 2022-04-28 | 广东省农业科学院农业生物基因研究中心 | Immobilized metal ion affinity chromatographic packing, chromatographic column, and preparation method therefor |
| 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 |
| CN114262465A (en) * | 2021-11-03 | 2022-04-01 | 赛分科技扬州有限公司 | Polyacrylate-based sphere and amine salt modification method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 卜春苗;龚波林;: "两种无孔强阳离子交换色谱固定相的制备及色谱性能比较", 石油化工应用, no. 06, 25 June 2017 (2017-06-25) * |
| 王宇成 主编: "《最新色谱分析检测方法及应用技术实用手册 第四卷》", 31 December 2004, 银声音像出版社, pages: 1944 - 1949 * |
| 陈培榕 邓勃 主编: "《现代仪器分析实验与技术》", 31 December 1999, 清华大学出版社, pages: 225 - 227 * |
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