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Preparation and chemical modification method of polymer graphene composite chromatographic filling material

A graphene composite and chromatographic packing technology is applied in the field of preparation and chemical modification of polymer graphene composite high-performance liquid chromatography columns, and can solve the problems of poor mechanical strength of stationary phase, low column efficiency of chromatographic columns, low exchange capacity, etc. , to achieve the effect of wide acid-base range, good chemical stability and simple process

Inactive Publication Date: 2017-03-22
ZHEJIANG UNIV
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the most widely used suppressed conductivity ion chromatography usually uses strong acid and strong base as mobile phase (pH12), which is far beyond the tolerance range of silica gel matrix, making silica gel matrix column excellent in ion chromatography. The application of polystyrene-divinylbenzene is greatly limited; the polymer matrix represented by polystyrene-divinylbenzene has a large pH tolerance range, so it is considered to be the best choice for ion chromatography column matrix
However, this type of polymer stationary phase has poor mechanical strength, stable chemical properties, and is difficult to chemically modify, which leads to the disadvantages of low column efficiency and low exchange capacity of the chromatographic column prepared with it.

Method used

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  • Preparation and chemical modification method of polymer graphene composite chromatographic filling material
  • Preparation and chemical modification method of polymer graphene composite chromatographic filling material
  • Preparation and chemical modification method of polymer graphene composite chromatographic filling material

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preparation example Construction

[0028] The preparation method of the polymer graphene composite chromatographic filler provided by the present invention is to reduce and agglomerate graphene oxide to polystyrene-divinylbenzene (PS-DVB) or On the surface of polyvinylbenzene-divinylbenzene (PEVB-DVB) microspheres, a wrinkled graphene shell is formed to obtain a polymer-graphene composite chromatographic filler, and the surface of a polymer-graphene composite chromatographic filler is prepared. The surface of graphene can undergo epoxy-amine, diazotization, and Diels-Alder reactions respectively, so that functional groups such as quaternary ammonium groups or carboxyl groups can be introduced into the surface of microspheres, and corresponding anion and cation exchange chromatography packings can be prepared. The chemically modified polymer carbon nanotube composite chromatographic filler is packed by homogenate method. The specific implementation steps of the above process are:

[0029] a. Synthesis of polyme...

Embodiment 1

[0043] Embodiment 1: This embodiment shows the process that in-situ reduction method prepares polymer graphene composite chromatographic filler. First, fully disperse 2.5g polystyrene-divinylbenzene (55% degree of cross-linking) resin in 80mL aqueous solution containing 6% (m / v) Triton X-100, then mix this solution with another 100mL 1mg / L of graphene oxide solution (containing 2 mL of ammonia water) was mixed, the solution was stirred at room temperature for 2 h, the temperature was raised to 95 degrees, and 20 mL of solution containing 90 mg of hydrazine hydrate was slowly added dropwise. After the above reaction was carried out at 95 degrees for 3 hours, the resin was filtered and washed with deionized water and ethanol to obtain a composite chromatographic filler with a graphene layer agglomerated on the surface.

Embodiment 2

[0044] Embodiment 2: This embodiment shows the process that distribution reduction method prepares polymer graphene composite chromatographic filler. First, heat 100mL of 1mg / L graphene oxide solution (containing 2mL of ammonia water) to 95°C, and slowly add dropwise to 20mL solution containing 90mg of hydrazine hydrate. After the above reaction was carried out at 95 degrees for 3 h, the above solution was filtered. The filtrate is collected and heated to 70 degrees, and 80 mL of 6% (m / v) triton X-100 aqueous solution dispersed with 2.5 g of polystyrene-divinylbenzene (55% degree of cross-linking) resin is slowly added dropwise , and stirred for 3h. Then the resin was filtered and washed with deionized water and ethanol to obtain a composite chromatographic filler with a graphene layer agglomerated on the surface with properties similar to that of Example 2.

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Abstract

The invention discloses a preparation and chemical modification method of a polymer graphene composite chromatographic filling material. According to the preparation and chemical modification method, polystyrene-divinyl benzene (PS-DVB) or poly(ethyl vinyl benzene)-divinyl benzene (PEVB-DVB), and oxidized graphene are used for preparing a substrate material, hydrazine hydrate in-situ reduction or fractional reduction is adopted to realize reduction of oxidized graphene and realize agglomeration of reduced oxidized graphene onto the surface of the substrate material so as to form a wrinkled graphene shell layer and obtain the polymer graphene composite chromatographic filling material. The polymer graphene composite chromatographic filling material is high in stability, is capable of tolerating a wide pH range, and possesses organic solvent compatibility; modification with a plurality of ion exchange groups can be realized based on different reaction characteristics of surface combined graphene so as to prepare anion and cation exchange chromatography filling materials at the same time; separation of common anions and cations is realized preferably; and the polymer graphene composite chromatographic filling material is especially suitable to be used in inhibiting conductive type ion chromatography.

Description

technical field [0001] The invention relates to a high performance liquid chromatography column and a preparation method thereof, in particular to a preparation and chemical modification method of a polymer graphene composite high performance liquid chromatography column. Background technique [0002] Ion chromatography is one of the branches of high performance liquid chromatography. It is mainly used for the separation of anions and cations, organic acids, organic amines and sugars. Separation and identification of ions composed of elements. The packing of ion chromatography is mainly composed of uncharged neutral matrix and ionizable functional groups, and the neutral matrix mainly includes silica gel and polymer. The silica gel matrix has high mechanical strength and is rich in silanol on the surface, which is conducive to chemical modification. Silica gel-based chromatographic columns are widely used in high-performance liquid chromatography, and have the characteristi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/30B01J20/285B01J20/26B01D15/08B01J13/02
CPCB01J20/285B01D15/08B01J13/02B01J20/264B01J20/267B01J2220/46B01J2220/4806B01J2220/4812
Inventor 张恺朱岩
Owner ZHEJIANG UNIV
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