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Modified silica gel material, and preparation method and application thereof

A silica gel and modified technology, applied in the field of materials, can solve the problem that it is difficult to adjust the ratio of polar groups and non-polar groups, the position and number of polar groups are not fixed, and the reproducibility of fillers is difficult to ensure. problems, to achieve the effect of superior water resistance, increased hydrophilicity, and long service life

Active Publication Date: 2021-12-14
浙江月旭材料科技有限公司 +2
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these two ways of introducing polar groups also have certain problems
The weakness of the polar embedding technology lies in: (1) Although the polar group embedding into the C18 stationary phase solves the problem of poor peak shape of basic substances, the shape selectivity is poor due to the short carbon chain in the functional group. When separating substances with similar structures, the ideal separation effect cannot be achieved; (2) the polar embedding method is to insert a polar group between each non-polar group and silica gel, that is, a polar group and a non-polar group The ratio between groups is 1:1, it is difficult to adjust the ratio of polar groups and non-polar groups, in addition, the spatial position of polar groups and non-polar groups is relatively fixed, it is difficult to control , resulting in separation selectivity
The method of polar tailing is to bond polar small molecular groups on the surface of silica gel. Although this method can greatly increase the hydrophilicity of the filler, it also has the problem that the position and number of polar groups are not fixed. , making it difficult to guarantee the reproducibility of the filler
[0006] CN111001188A discloses a reversed-phase separation medium and a preparation method thereof, including coating a neutral hydrophilic layer on the stationary phase and the surface of the stationary phase, and the reversed-phase separation medium provided has good water resistance, high ion selectivity, and ion Exchange interaction interferes with low characteristics, but not durable enough
CN101987293B discloses a preparation process of a silica gel surface copolymerization chromatographic separation material. The separation material has a novel bonded phase structure, has both non-polar groups and polar groups, and can simultaneously provide non-polar forces and various The polar force of the form can improve the selectivity of reversed phase chromatography, but the water resistance is not enough

Method used

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  • Modified silica gel material, and preparation method and application thereof
  • Modified silica gel material, and preparation method and application thereof
  • Modified silica gel material, and preparation method and application thereof

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preparation example Construction

[0098] The present application provides a preparation method of a modified silica gel material to solve the problems of poor water resistance, poor selectivity and short life when the silica gel material in the prior art is used as a chromatographic column. The preparation method of modified silica gel material comprises the steps:

[0099] 1) Silane coupling agent modified silica gel and hydrophilic polymer carry out cross-linking reaction to obtain hydrophilic modified silica gel;

[0100] 2) Substituting the hydrophilic modified silica gel with a non-polar silane reagent to obtain hydrophobic modified silica gel;

[0101] 3) Substituting the hydrophobically modified silica gel with a polar silane reagent to obtain the modified silica gel material.

[0102] The concrete route of the preparation method of modified silicon material in the present application is as follows:

[0103]

[0104] In this application, the active silanol on the surface of the silica gel reacts wi...

Embodiment 1

[0107] In this embodiment, the modified silica gel material and its preparation method include the following:

[0108] 1) 50g of spherical silica gel and 100g of γ-(2,3-glycidoxy)propyltrimethoxysilane were dispersed in 250mL of toluene solution, and reacted at 80°C for 2h to obtain 53g of silane coupling agent modified silica gel.

[0109] 2) Add 100g of soluble starch to the above 53g of silane coupling agent-modified silica gel, and reflux at 97°C for cross-linking reaction for 20h; after the reaction, cool and reflux for 12h; wash with 200mL distilled water, 200mL tetrahydrofuran and 200mL acetonitrile, and filter , to obtain hydrophilic modified silica gel.

[0110] 3) Add 250mL of toluene, 50g of octadecyltrichlorosilane, and 2g of triethylamine in sequence to the above-mentioned hydrophilic modified silica gel, and reflux and stir at 105°C for 1 hour; Wash with methanol, filter, and repeat this step once; dry in the air, and vacuum dry at 105° C. for 2 hours to obtain ...

Embodiment 2

[0113] In this embodiment, the modified silica gel material and its preparation method include the following:

[0114] 1) 50g of spherical silica gel and 100g of γ-(2,3-glycidoxy)propyltrimethoxysilane were dispersed in 250mL of toluene solution, and reacted at 80°C for 2h to obtain 53g of silane coupling agent modified silica gel.

[0115] 2) Add 100g of soluble starch to the above 53g of silane coupling agent-modified silica gel, and reflux at 97°C for cross-linking reaction for 20h; after the reaction, cool and reflux for 12h; wash with 200mL distilled water, 200mL tetrahydrofuran and 200mL acetonitrile, and filter , to obtain hydrophilic modified silica gel.

[0116] 3) Add 250mL of toluene, 50g of octyltrichlorosilane, and 2g of triethylamine in sequence to the above-mentioned hydrophilic modified silica gel, and reflux and stir at 105°C for 1 hour; after the reaction, add 400mL of distilled water and 400mL of methanol Wash, filter, and repeat this step once; dry in the ...

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Abstract

The invention belongs to the technical field of materials, and particularly relates to a modified silica gel material, and a preparation method and application thereof. The preparation method of the modified silica gel material comprises the following steps: 1) carrying out cross-linking reaction on silane coupling agent modified silica gel and a hydrophilic polymer to obtain hydrophilic modified silica gel; 2) carrying out substitution reaction on the hydrophilic modified silica gel and a non-polar silane reagent to obtain hydrophobic modified silica gel; and 3) carrying out substitution reaction on the hydrophobic modified silica gel and a polar silane reagent to obtain the modified silica gel material. The hydrophilic modified silica gel is formed by introducing a compact hydrophilic polymer coating layer on the surface of the silica gel, so the hydrophilicity of the silica gel is increased; and the hydrophilic modified silica gel is modified by adopting a non-polar silane reagent, and further modification is performed by adopting a polar silane reagent, so that residual silicon hydroxyl on the surface of the silica gel is shielded to a great extent, the tolerance of the material to a high-proportion water phase is widened, the hydrolytic stability of the material is improved, the peak pattern of an alkaline compound is improved, and the service life of the material is prolonged.

Description

technical field [0001] The invention belongs to the technical field of materials, and in particular relates to a modified silica gel material and its preparation method and application. Background technique [0002] High performance liquid chromatography (HPLC) has always played an important role in the field of separation and analysis, and has become one of the most widely used tools in analytical chemistry due to its advantages of high separation characteristics, good selectivity and excellent reproducibility. . Chromatographic column is the "heart" of liquid chromatography in colleges and universities, and its condition directly affects the accuracy and reliability of the results. At present, chromatographic separation materials in reversed phase chromatography, hydrophilic interaction chromatography, ion exchange chromatography, size exclusion chromatography and chiral chromatography have been widely used in pharmaceutical analysis, environmental monitoring, food testin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/28B01J20/30B01D15/30B01D15/32C08G83/00
CPCB01J20/267B01J20/28002B01D15/305B01D15/327C08G83/001
Inventor 薛昆鹏任兴发屠炳芳李良翔王健王睿李崟
Owner 浙江月旭材料科技有限公司
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