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Spherical ordered mesoporous silicon oxide substrate chromatograph stationary phase and preparation

A technology of mesoporous silica and chromatographic stationary phase, which is applied in chemical instruments and methods, and other chemical processes, can solve the problems of narrow particle size distribution, increased mass transfer resistance, disordered arrangement, etc., and achieve uniform particle size distribution, high The effect of specific surface area and orderly arrangement

Inactive Publication Date: 2008-11-05
SHANGHAI SECOND POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention proposes a spherical ordered mesoporous silica matrix chromatographic stationary phase and its preparation method, the purpose of which is to overcome the sol-gel method used in the existing chromatographic analysis field to prepare silica gel particles, resulting in that the particle shape is not spherical and the diameter range Wider, so as to increase the mass transfer resistance and the final separation effect; although the spherical porous colloidal silica is prepared by the spray method, it needs to be graded, and the structure and size of the internal pores of the particles are inconsistent, and the arrangement is disorderly, which is not conducive to the bond of the stationary phase. Merging will cause mass transfer resistance to increase; adopt the method of the present invention to prepare, so that the chromatographic matrix particles have a spherical shape, the particle size distribution is narrow, and the structure and size of the internal pores are also arranged in an orderly manner, and the particle size distribution is uniform, so that the lack of general silica gel can be overcome.

Method used

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  • Spherical ordered mesoporous silicon oxide substrate chromatograph stationary phase and preparation
  • Spherical ordered mesoporous silicon oxide substrate chromatograph stationary phase and preparation
  • Spherical ordered mesoporous silicon oxide substrate chromatograph stationary phase and preparation

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Experimental program
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Effect test

Embodiment 1

[0029] 1) Synthesis of spherical mesoporous silica matrix

[0030] Dissolve 5.0g of P123 and 4.51g of KCl in 120ml of water, then add 13.3ml of sulfuric acid, stir the solution for 30min, add 4.32g of TMB, stir vigorously for 30min, add 8.90g of TEOS dropwise, stir vigorously for 30min, then turn to Put it into a polytetrafluoroethylene bottle and let it stand at 308K for 24h, then transfer to 373K for aging for 48h. The solid product was filtered and washed successively with deionized water, methanol, acetone, and water, and air-dried at room temperature. After air-drying, the product was heated at 873K (the heating rate was 1Kmin -1 ) calcined for 8 hours (cooling rate 10Kmin -1 ) to obtain a mesoporous silica matrix.

[0031] The specific surface area of ​​the obtained sample measured by the ASAP2020 specific surface pore size measuring instrument is 582.99m 2 / g, the X-ray diffraction pattern of the obtained sample is shown in figure 1 .

[0032] 2) Synthesis of bond...

Embodiment 2

[0035] 1) Synthesis of spherical mesoporous silica matrix

[0036] Dissolve 4.0g of P123 and 3.04g of KCl in 120ml of water, then add 20ml of hydrochloric acid, stir the solution for 30min, add 3.0g of TMB, stir vigorously for 30min, add 8.5g of TEOS dropwise, stir vigorously for 30min, then turn to Put it into a polytetrafluoroethylene bottle and let it stand at 308K for 24h, then transfer to 373K for aging for 24h. The solid product was filtered and washed successively with deionized water, methanol, acetone, and water, and air-dried at room temperature. After air-drying, the product was heated at 823K (the heating rate was 1Kmin -1 ) calcined for 6 hours (cooling rate 10Kmin -1 ) to obtain a mesoporous silica matrix.

[0037] The scanning electron microscope and pore size distribution diagram of the obtained sample are shown in figure 2 and image 3 .

[0038] 2) Synthesis of bonded stationary phase

[0039]Weigh 3.0 g of β-cyclodextrin, recrystallize three times wi...

Embodiment 3

[0041] 1) Synthesis of spherical mesoporous silica matrix

[0042] Dissolve 10g of P123 and 6.02g of KCl in 150ml of water, add 20ml of hydrochloric acid, when the solution is stirred and clarified, add 5.5g of 1,3,5-trimethylbenzene (TMB), stir vigorously for 30 minutes, then add dropwise Tetraethyl orthosilicate 8.5g, then vigorously stirred for 30 minutes, then transferred to a polytetrafluoroethylene bottle at 308K for 24 to 48 hours, and then transferred to 373K for aging for 24 hours. The solid product was filtered and washed successively with deionized water, methanol, acetone, and water, and air-dried at room temperature. After air-drying, the product was calcined at 873K for 8 hours to obtain a spherical mesoporous silica matrix product.

[0043] The specific surface area of ​​the obtained sample measured by the ASAP2020 specific surface pore size tester is 815.82m 2 / g, the pore size distribution diagram of the obtained sample is shown in Figure 4

[0044] 2) Sy...

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Abstract

The invention relates to a stationary phase material for the chromatogram of a spherical ordered mesoporous silica substance. Polyoxyethylene ether-polyoxyallyl ether-polyoxyethylene ether is adopted as a template, ethyl silicate is adopted as a silicon source, and the spherical ordered mesoporous silica synthesized by still-setting method serves as a substance in acid media; in a waterless condition, gamma-(2,3-epoxypropoxy) propyltrimethoxysilane is used for linking beta-cyclodextrin or a derivative thereof with chiral separation ability to the surface and the interior of the porous channel of the synthesized substance to prepare the filling of a chromatogram column. A test is carried out after homogenate is filled into the chromatogram column, thus successfully separating chiral medicine ibuprofen enantiomers with a separation degree of 2.03. The spherical ordered mesoporous silica prepared by the stationary phase material has relatively high specific surface area, does not need grinding classification, has simple technique, convenient preparation, evenly distributed particle diameter and pores with ordered structure and size arrangement and is beneficial to the linking of separation factors and the design of chromatogram stationary phase.

Description

technical field [0001] The invention relates to a chromatographic stationary phase material, in particular to a chromatographic stationary phase material and a preparation method of a spherical ordered mesoporous silicon oxide matrix with an adjustable pore diameter, and belongs to the technical field of porous material preparation and analytical chemistry. Background technique [0002] Inorganic mesoporous silica materials have an ordered internal structure, large specific surface area and pore volume, adjustable pore structure, adjustable pore size, modifiable surface properties, and controllable morphology. It has great applications in catalysis, sensing, and as a template for synthetic materials. [0003] The use of inorganic mesoporous silica materials as liquid chromatography matrix fillers is a new application of this material in the field of chromatographic analysis. The most widely used column packing matrix in liquid chromatography is silica gel, and its specific ...

Claims

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Application Information

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IPC IPC(8): B01J20/283
Inventor 陈胜文邴乃慈李庆华
Owner SHANGHAI SECOND POLYTECHNIC UNIVERSITY
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