Preparation method of hybrid silicon film with hydrophilically modified surface

A hybrid silicon membrane and hydrophilic modification technology, which is applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc., can solve the problems of weak surface hydrophilicity, achieve convenient post-processing, and avoid pollution Effect

Active Publication Date: 2018-01-16
CHANGZHOU UNIV
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  • Abstract
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  • Claims
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Problems solved by technology

[0003] In view of the fact that the surface of organic-inorganic hybrid silicon membrane materials is not very hydrophilic, and the current hydrophilic modification methods are all focused on the functionalization of sulfonic acid groups, it is necessary to use highly oxidizing or explosive hazardous chemicals (concentrated sulfuric acid, tert butyl hydroperoxide, etc.), the present invention provides a simple, mild and efficient hydrophilic modification method, by placing the hybrid silicon membrane material in bromine vapor for electrophilic addition reaction to obtain brominated hetero Then the brominated hybrid silicon membrane is placed in ammonia vapor to replace the bromine atoms with ammonia molecules to prepare the amino-functionalized hybrid silicon membrane, which improves the hydrophilicity of the membrane surface, and the water treatment process increased water permeability,

Method used

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  • Preparation method of hybrid silicon film with hydrophilically modified surface
  • Preparation method of hybrid silicon film with hydrophilically modified surface
  • Preparation method of hybrid silicon film with hydrophilically modified surface

Examples

Experimental program
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Effect test

Embodiment 1

[0026] (1) Put a beaker and a watch glass in the vacuum drying dish, put excess liquid bromine in the beaker, put into the watch glass by 1,2-bis(triethoxysilyl) ethylene sol to prepare the separation layer Hybrid silicon membrane, the hybrid silicon membrane is not in direct contact with liquid bromine,

[0027] Exhaust the vacuum drying dish, and control the pressure down to 3kPa at room temperature (25°C, the same below) to allow the bromine vapor to react with the hybrid silicon film;

[0028] (2) Evacuation step (1) The liquid bromine vapor in the vacuum drying dish, take out the hybrid silicon film, and carry out vacuum heating and drying at 100° C. for 12 hours at 0.0133 Pa;

[0029] (3) Put the hybrid silicon film dried in step (2) into a vacuum drying dish containing excess ammonia water in the same non-contact manner, and then also exhaust the vacuum drying dish at room temperature (25°C, the same below). Control the pressure down to 80kPa to fully react the hybrid ...

Embodiment 2

[0031] (1) with embodiment 1;

[0032] (2) with embodiment 1;

[0033] (3) Immerse the hybrid silicon membrane dried in step (2) into excess ethylenediamine solution, take out the hybrid silicon membrane after fully reacting, wash it with absolute ethanol for 3 times, and then put it into a 60°C vacuum drying oven save in .

Embodiment 3

[0035] (1) First, immerse the raw material hybrid silicon membrane consistent with step (1) of Example 1 into anhydrous acetonitrile containing excess sodium hydroxide solution, and after cooling to -5°C in an ice-water bath, add excess tert-butyl peroxide Oxidize the hydrogen solution and stir it sufficiently to cause an epoxidation reaction;

[0036] (2) Wash the membrane prepared in step (1) fully with absolute ethanol, dry it and put in excess NaHSO 3 / Na 2 SO 3 solution, fully stirred at 40°C for ring-opening sulfonation reaction, then washed with a large amount of distilled water, and then stored in a 60°C drying oven.

[0037] Table 1 is before hybrid silicon membrane treatment in embodiment 1 and with bromine vapor / ammonia vapor (embodiment 1), bromine vapor / ethylenediamine solution (embodiment 2) and tert-butyl hydroperoxide / NaHSO 3 / Na 2 SO 3 After the solution (embodiment 3) was processed, in the reverse osmosis experiment, the contrast of permeability and NaCl...

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Abstract

The invention belongs to the field of film material preparation, and particularly relates to a preparation method of a hybrid silicon film with a hydrophilically modified surface. One simple, mild andefficient hydrophilic modification method is provided, a hybrid silicon film material is left to stand in bromine vapor to be subjected to an electrophilic addition reaction, a brominated hybrid silicon film is obtained, then the brominated hybrid silicon film is left to stand in ammonia vapor, bromine atoms are enabled to be replaced with ammonia molecules, the amino-group functionalized hybridsilicon film is prepared accordingly, surface hydrophilicity of the film is improved, and water permeability in a water treatment process is increased.

Description

technical field [0001] The invention belongs to the field of membrane material preparation, in particular to a method for preparing a surface hydrophilic modified hybrid silicon membrane. Background technique [0002] Bridge structure [(R'O) 3 -Si-R-Si-(OR') 3 ] and side group structure [(R'O) 3 R in Si-R] hybrid silicon materials is usually a hydrophobic organic group, such as methyl, ethyl, vinyl, phenyl, thiophene, etc. The introduction of these organic groups makes this type of organic-inorganic hybrid material have good structural stability in water, but at the same time, these hydrophobic organic functional groups make the water permeability of the final hybrid silicon membrane relatively low during water treatment. Low. Contents of the invention [0003] In view of the fact that the surface of organic-inorganic hybrid silicon membrane materials is not very hydrophilic, and the current hydrophilic modification methods are all focused on the functionalization of s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D67/00B01D69/02C02F1/44
Inventor 徐荣程旭钟璟张琪戚律
Owner CHANGZHOU UNIV
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