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Preparation method for mesoporous silica coated gold nanorod doping integral column

A technology of mesoporous silica and gold nanorods, applied in chemical instruments and methods, alkali metal oxides/hydroxides, inorganic chemistry, etc., can solve the complex synthesis process of RTIL, accelerate the speed of polymerization reaction, and difficult to volatilize and other problems, to achieve the effect of good permeability, improved separation ability and compact structure

Inactive Publication Date: 2018-11-13
TIANJIN MEDICAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In recent years, room temperature ionic liquids (RTILs) have become a kind of green polymerization medium due to their low vapor pressure and high boiling point, and they can accelerate the polymerization reaction when used as porogens [Wang H, Gurau G, Rogers R D . Ionicliquid processing of cellulose. Chemical Society Reviews, 2012, 41: 1519-1537], however, RTIL synthesis process is complicated, purification is difficult, cost is high and it is difficult to volatilize and degrade

Method used

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  • Preparation method for mesoporous silica coated gold nanorod doping integral column
  • Preparation method for mesoporous silica coated gold nanorod doping integral column
  • Preparation method for mesoporous silica coated gold nanorod doping integral column

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Experimental program
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Effect test

Embodiment 1

[0025] To confirm GNRs@mSiO 2 In the synthesis of capillary monolithic columns, we prepared two kinds of capillary monolithic columns, one is doped GNRs@mSiO 2 capillary monolithic column, the other is undoped GNRs@mSiO 2 The capillary monolithic column, and scanning electron microscope analysis was carried out on the two monolithic columns to characterize the morphological characteristics of the particles. The specific operation steps are as follows:

[0026] Doped GNRs@mSiO 2 Preparation method of capillary monolithic column:

[0027] The porogen GNRs@mSiO 2 / choline chloride-ethanol and ionic liquid 30.61% (both mass percent), 1-hexyl-3-methylimidazolium tetrafluoroborate [HMIM]BF 4 49.88%, functional monomer methacrylic acid 1.86% and butyl methacrylate 9.21%, initiator ammonium persulfate 0.31% and tetramethylethylenediamine 3.98%, crosslinking agent ethylene glycol dimethacrylate 4.15% After mixing, the mixture was sonicated at low temperature for 15 min (300 W), an...

Embodiment 2

[0033] In order to investigate doped GNRs@mSiO 2 GNRs@mSiO in capillary monolithic column 2 The influence of the concentration dispersed in choline chloride-ethanol on the performance of capillary monolithic column, GNRs@mSiO with different concentrations were synthesized 2 -The monolithic column of choline chloride-ethanol uses acetone as a marker to separate alkylbenzene analogs (acetophenone, butyrophenone, toluene, ethylbenzene, propylbenzene, butylbenzene), and the electrochromatographic conditions are : 12 kV, 254 nm, ACN: 10 mmol / L acetate buffer (pH 6.0) (70 / 30, v / v), for the results of electrochromatographic experiments see figure 2 .

[0034] The results show that when no doping GNRs@mSiO 2 When (that is, blank), the capillary monolithic column has low separation efficiency for alkylbenzene analogs, and the peak eluting time is late, and the peak tailing is serious. Doped GNRs@mSiO 2 The capillary monolithic column with GNRs@mSiO in the polymerization system 2...

Embodiment 3

[0036] In order to investigate the effect of the ratio of ionic liquid and choline chloride-ethanol in the porogen on the separation performance of capillary monolithic columns, four monolithic columns with different ratios of ionic liquid and choline chloride-ethanol were synthesized and acetone was used as a marker , separation of alkylbenzene analogues (acetophenone, butyrophenone, toluene, ethylbenzene, propylbenzene, butylbenzene), electrochromatographic conditions: 12 kV, 254nm, ACN: 10 mmol / L acetate buffer solution (pH 6.0) (70 / 30, v / v), the results of electrochromatographic experiments are shown in image 3 .

[0037] The results show that with the decrease of the ionic liquid in the porogen system, the maximum column efficiency for the separation of p-alkylbenzene analogs increases first and then decreases. When the ratio of ionic liquid to deep eutectic solvent is 3:2 , the highest column efficiency and highest resolution are achieved. When the proportion of ionic...

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Abstract

The invention relates to a preparation method for a mesoporous silica coated gold nanorod doping integral column. The preparation method comprises the following steps: leading GNRs@mSiO2 into preparation of a capillary tube integral column which takes green solvent ionic liquid and a low eutectic system as a binary pore-foaming agent, regulating proportion of GNRs@mSiO2 to choline chloride-alcohol, the type of ionic liquid and the proportion of the ionic liquid to a low eutectic solvent to observe separating ability, on small molecular substances, of the capillary tube integral column. The preparation method is easy to operate, and is easy and easy to implement. The integral column is compact in material structure, and is good in permeability; the prepared capillary tube integral column iscompact in material structure; according to the electro-chromatographic experiment for alkylbenzene analogues, the column effect (168000 boards / meter) of the GNRs@mSiO2 doped integral column is obviously higher than that (87300 boards / meter) of a blank column, indicating that the column effect of the capillary tube integral column can be effectively improved by doping GNRs@mSiO2; and an organic-inorganic hybrid integral column prepared by a gold nanorod doping scheme has a potential application prospect.

Description

technical field [0001] The invention relates to a method for preparing a mesoporous silica-coated gold nanorod-doped monolithic column, in particular to a green preparation method for a mesoporous silica-coated gold nanorod-doped capillary monolithic column. Background technique [0002] A monolithic column is a chromatographic column obtained by in-situ polymerization of a mixture of monomers, initiators, porogens, etc. in a capillary column using organic or inorganic polymerization methods. It has the advantages of simple preparation and good reproducibility. , better porosity and permeability, can achieve fast and efficient separation and other advantages. Since the organic polymer monolithic column mainly contains macropores and mesopores in the polymer stationary phase, it is difficult to separate small molecular compounds efficiently. Nanomaterials have the characteristics of large specific surface area, diverse shapes, and strong plasticity. Therefore, doping nanomat...

Claims

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Application Information

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IPC IPC(8): B01J20/28B01J20/285B01J20/30
CPCB01J20/28B01J20/285
Inventor 黄艳萍李欣欣刘照胜
Owner TIANJIN MEDICAL UNIV
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