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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: 2008-01-02
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 100 mg of rutin in 10 ml of pyridine, add 0.5 ml of aminopropyltriethoxysilane and 0.5 ml of N.N-dimethylformamide, and reflux at 65°C for 36 hours. After the reaction, Remove pyridine with a rotary evaporator to obtain a rutin precursor, dissolve 10ml of tetraethoxysilane in 50ml of ethanol solution, add 5ml of the rutin precursor prepared above, and then add 1ml of N, N-dimethyl formamide and 15ml of deionized water, then adjust the pH to 4.9 with HCL, and reflux at 60°C for 10 hours to carry out synergistic hydrolysis to prepare silica sol, followed by aging at room temperature for 2 hours. Al 2 o 3 The board is polished, then decocted with 0.05mol / L hydrochloric acid, sodium hydroxide, ethanol and ultrasonically immersed in the previously prepared sol, dip-coated repeatedly 7 times, and then placed in a muffle furnace for sintering, the highest temperature setting 170°C, heat up at 0.5°C / min, take it out after 6.5 hours, then use 90% ethanol so...

Embodiment 2

[0013] Example 2: Dissolve 100 mg of quercetin in 20 ml of ethanol, add 5 ml of chloropropyltriethoxysilane and 2.0 ml of N, N-dimethylformamide, reflux at 70 ° C for 24 hours, after the reaction, Remove tetrahydrofuran with a rotary evaporator to obtain a quercetin precursor. Dissolve 15ml of tetraethoxysilane in 30ml of ethanol solution, add 5ml of the quercetin precursor prepared above, and then add 3ml of N,N- Dimethylformamide and 20ml of deionized water were used to adjust the pH to 9.5 with sodium hydroxide, and then refluxed at 60°C for 10 hours for synergistic hydrolysis to prepare silica sol, followed by aging at room temperature for 2.5 hours. Al 2 o 3 The plate is polished, then decocted with 0.10mol / L hydrochloric acid, sodium hydroxide, ethanol and ultrasonically immersed in the previously prepared sol, dipped and coated 6 times, and then placed in a muffle furnace for sintering, the highest temperature setting 180°C, heat up at 1°C / min, take out the composite ...

Embodiment 3

[0014] Example 3: Dissolve 150 mg of morphine in 30 ml of tetrahydrofuran, add 10 ml of 3-propylisocyanatotriethoxysilane and 1.5 ml of N,N-dimethylacetamide, condense and reflux at 80°C for 12 hours, and the reaction ends Finally, the tetrahydrofuran was removed with a rotary evaporator to obtain a morphine precursor. Dissolve 15ml of tetraethoxysilane in 30ml of ethanol solution, add 5ml of the morphine precursor prepared above, and then add 3ml of N, N-dimethyl Formamide and 20ml of deionized water were used to adjust the pH to 6.5 with acetic acid, and then refluxed at 60°C for 8 hours for synergistic hydrolysis to prepare silica sol, followed by aging at room temperature for 4 hours. Al 2 o 3 The board is polished, then decocted with 0.15mol / L hydrochloric acid, sodium hydroxide, ethanol and ultrasonically immersed in the previously prepared sol, dipped and coated 6 times, and then placed in a muffle furnace for sintering, the highest temperature setting The temperature...

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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 preparation method of 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, 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 ...

Claims

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Application Information

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