Process for preparing silicon separating films with specialized selectivity to natural products

A natural product and selective technology, applied in the direction of semi-permeable membrane separation, chemical instruments and methods, membrane technology, etc., can solve the problems of low mechanical strength, deterioration, large separation coefficient, etc., and achieve wide application temperature range and pollution resistance Strong, easy-to-prepare effect

Inactive Publication Date: 2006-12-27
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Membrane separation technology has many advantages, such as no phase change in the separation process, low energy consumption; large separation coefficient, continuous operation, high efficiency, and no secondary pollution; low operating temperature, suitable for heat-sensitive substances (juice, enzymes, medicines) separation, purification and enrichment; the device is simple, easy to operate, etc., but there are still many problems in practical applications, such as serious membrane fouling and degradation; most organic membrane materials, especially hydrophilic materials, have poor thermal stability, Low mechanical strength, poor resistance to chemicals, etc.; at present, the selectivity of membrane technology separation is achieved by molecular weight cut-off, but natural products, drugs or some chemical products have relatively close molecular weights, and it is difficult to use existing membrane technology to accurately Separation, so improving the selectivity of the membrane and making the membrane separation achieve accurate separation is one of the difficult problems faced by the current membrane technology.
Molecular imprinting is a technology developed in the past 20 years to prepare highly selective adsorption materials. It imitates the principle of keys and locks in the biological world. It can selectively separate the components to be separated from the molecular level. However, the molecular imprinting technology used Most of the functional monomers and cross-linking agents are organic compounds, and the molecular imprinting and molecular recognition processes cannot be realized in polar solvents, while many natural products, drugs or some chemical products are water-soluble substances, which exist in the application. with difficulty

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Example 1: Dissolve 100mg of rutin in 10ml of pyridine, add 0.5ml of aminopropyltriethoxysilane and 0.5ml of N,N-dimethylformamide, condense and reflux at 65°C for 36 hours, the reaction is complete Afterwards, the pyridine was removed with a rotary evaporator to obtain a rutin precursor. 10ml of tetraethoxysilane was dissolved in 50ml of ethanol solution, and 5ml of the rutin precursor prepared above was added, and then 1ml of N, N- Dimethylformamide and 15ml of deionized water, then adjusted pH=4.9 with HCL, refluxed at 60°C for 10 hours for synergistic hydrolysis to prepare silica sol, and then aged for 2 hours at room temperature. Al 2 O 3 The board is polished, then decocted with 0.05 mol / L hydrochloric acid, sodium hydroxide, and ultrasonicated with ethanol, and then immersed in the previously prepared sol. Repeated dip coating 7 times, and then placed in a muffle furnace for sintering. The highest temperature is set The temperature is 170°C, the temperature is increa...

Embodiment 2

[0013] Example 2: Dissolve 100mg of quercetin in 20ml of ethanol, add 5ml of chloropropyltriethoxysilane and 2.0ml of N,N-dimethylformamide, and reflux at 70°C for 24 hours. After the reaction, The tetrahydrofuran was removed with a rotary evaporator to obtain the quercetin precursor. 15ml of tetraethoxysilane was dissolved in 30ml of ethanol solution, and 5ml of the quercetin precursor prepared above was added, and then 3ml of N, N- Dimethylformamide and 20ml of deionized water were used to adjust pH=9.5 with sodium hydroxide, and then refluxed at 60°C for 10 hours for synergistic hydrolysis to prepare silica sol, and then aged for 2.5 hours at room temperature. Al 2 O 3 The plate is polished, then decocted with 0.10mol / L hydrochloric acid, sodium hydroxide, and sonicated with ethanol, and then immersed in the previously prepared sol, repeated dip coating 6 times, and then placed in a muffle furnace for sintering, and the highest temperature is set The temperature is 180°C, the t...

Embodiment 3

[0014] Example 3: Dissolve 150mg of morphine in 30ml of tetrahydrofuran, add 10ml of 3-propisocyanatotriethoxysilane and 1.5ml of N,N-dimethylacetamide, condense and reflux at 80°C for 12 hours, the reaction is complete Then, the tetrahydrofuran was removed by a rotary evaporator to obtain a morphine precursor. 15ml of tetraethoxysilane was dissolved in 30ml ethanol solution, and 5ml of the morphine precursor prepared above was added, and then 3ml of N,N-dimethyl was added. Carboxamide and 20ml of deionized water were used to adjust pH=6.5 with acetic acid, and then refluxed at 60°C for 8 hours for synergistic hydrolysis to prepare silica sol, and then aged at room temperature for 4 hours. Al 2 O 3 The board is polished, decocted with 0.15 mol / L hydrochloric acid, sodium hydroxide, and sonicated with ethanol, and then immersed in the previously prepared sol. Repeated dip coating 6 times, and then placed in a muffle furnace for sintering. The highest temperature is set The temperat...

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PUM

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Abstract

Disclosed is a preparation method of silicon separation membrane, having specific selectivity to natural products, which belongs to a membrane preparation technique. The method comprises: dissolving a template agent into an alcohol solution to produce template agent solution, then, adding functional monomers into said produced solution, adding in stabilizer, condensing and refluxing to remove the solvent and produce a silane precursor, dissolving tetraethoxysilane into the alcohol solution, adding in the silane precursor followed by condensing and refluxing to prepare a sol, next, aging at room temperature and dipping treated Al2O3 plate into the sol, finally, sintering in a muffle, eluting the template agent and drying to produce silicon separation membrane. The present invention is characterized in simple preparation, the produced separation membrane realizing selectively separation of a certain substance in molecular scale, water-phase molecule recognition, particularly fit for natural products separation and extensive general uses.

Description

Technical field [0001] The invention relates to a method for preparing a siliceous separation membrane with specific selectivity for natural products. It belongs to the preparation technology of separation membrane. Background technique [0002] Membrane separation technology is one of the unit operations with the most development potential in the 21st century and has broad application prospects. Membrane separation technology has many advantages, such as no phase change in the separation process, low energy consumption; large separation coefficient, continuous operation, high efficiency, no secondary pollution; low operating temperature, suitable for heat-sensitive substances (juices, enzymes, medicines) Separation, purification and enrichment; simple equipment, easy to operate, etc., but there are still many problems in practical applications, such as serious membrane pollution and degradation; most organic membrane materials, especially hydrophil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/02B01D69/10
Inventor 张裕卿张红柳
Owner TIANJIN UNIV
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