Method for preparing epoxy resin base polyalcohol integral pole and special mold thereof

Abstract

The invention relates to a preparation method of epoxy resin-based polymer monolithic column; a given quantity of the epoxy resin and firming agents and a low molecular weight polymer mixture with a good compatibility used as pore-forming agents are added in an empty tube column; solidification temperature is controlled so as to regulate the speed of polymerization reaction; after the solidification is finished, the pore-forming agents are removed by washing so as to get the polymer monolithic column. The preparation process of the invention is simple and environmental friendly. The inventionalso discloses a dedicated mould. The monolithic column can be made into various specifications and forms as required and has the advantages of evenly distributed aperture, adjustable size, strong hydrophilic property, acid and alkali resistance, solvent resistance and good thermostabilization; and a large number of reactive functional groups are contained in the chemical constitution of the material of the monolithic column, which is suitable for performing a plurality of chemical modifications to an inner surface of a pore canal so as to further functionalize. The preparation method of the epoxy resin-based polymer monolithic column can be applied extensively to the fields such as the extraction and recovery of solid phase, the preparation of chromatogram, the separation of biological medicines, the environmental protection and the catalysis etc.

Description

technical field [0001] The invention relates to a preparation method of a polymer monolithic column, in particular to a preparation method of an epoxy resin-based polymer monolithic column, and also relates to a special mold used in the above preparation method. Background technique [0002] In recent years, the monolithic column (monoliyhiv volume), also known as the monolithic stationary phase (monolithic statiomary phase), rod column or continuous bed, is a continuous bed stationary phase that uses inorganic or organic polymerization methods to perform in-situ polymerization in the chromatographic column. It has become the fourth generation of separation media following biogel materials, cross-linked and modified porous microspheres, and monodisperse porous microsphere materials, and is especially suitable for complex sample systems (especially biomacromolecular samples and environmental samples) It is a new type of separation material for rapid, efficient, high-throughpu...

AI Technical Summary

Problems solved by technology

[0006] 1. The preparation method and process are relatively complicated, and the follow-up processing is cumbersome;

[0007] 2. It is often necessary to add a variety of toxic organic mixtures (such as toluene, chloroform, etc.), which is costly and polluting;

[0008] 3. Radical polymerization releases a lot of heat. When preparing a large-sized monolithic column, due to internal heat accumulation, it will eventually cause serious pore defects and lose the characteristics that the monolithic column should have. Currently, it can only be used for microcolumns with a diameter of less than a few millimeters. Liquid chromatography columns and capillary electrophoresis;

[0009] 4. The polymerization reaction speed is fast, the growth of the macromolecular chain is almost instantaneous, and the molecular weight is difficult to control. Although the prepared monolithic column appears to be a large piece, the internal microstructure is often formed by the accumulation of small balls, not a real large piece. gel, resulting in lower mechanical strength;

[0010] 5. It is very difficult to use this method to prepare molecular / ion imprinted columns, especially for molecularly imprinted monolithic columns with poor stability, or it is extremely cumbersome to further prepare adsorption and separation resins with chelating functions;

[0011] 6. These three series of polymer monolithic columns have poor bonding force with glass tubes and stainless steel tubes, and have different swelling ratios under the action of different polar solvents, which may easily cause the separation of the matrix material and the tube wall to form leakage and changes in pore size, resulting in a sharp drop in column performance and reduced lifetime

[0012] At the same time, the existing monolithic column preparation is usually completed in a cylindrical empty column. When the size of the monolithic column to be prepared is very large, it takes too long to remove the porogen, and a temperature gradient is easily formed inside the monolithic column, which affects The pore size and the uniformity of distribution inside the monolithic column affect its use effect

[0013] There are also literatures that use concentric sleeve ring molds to prepare large-sized monolithic columns to overcome the influence of temperature unevenness, and finally assemble them together to prepare them, but the shrinkage rates of rings of different sizes are often different , which can easily lead to defects in the final assembly

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