One-step microwave synthesis method of metalloporphyrin-titanium dioxide composite catalyst

A composite catalyst, metal porphyrin technology, applied in organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of time-consuming and cumbersome, and achieve easy process control. , the reaction conditions are mild, the effect of good photocatalytic performance

Inactive Publication Date: 2013-11-27
CHONGQING TIANYI HENGHUA TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a one-step microwave synthesis method of metalloporphyrin-titanium dioxide composite catalyst, which solves the time-consuming and cumbersome problems in the preparation of metalloporphyrin-titanium dioxide composite catalyst in the prior art

Method used

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  • One-step microwave synthesis method of metalloporphyrin-titanium dioxide composite catalyst
  • One-step microwave synthesis method of metalloporphyrin-titanium dioxide composite catalyst
  • One-step microwave synthesis method of metalloporphyrin-titanium dioxide composite catalyst

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Effect test

Embodiment 1

[0027] Step 1, take 9 ml of absolute ethanol in a beaker, drop 7 ml of tetra-n-butyl titanate (TBOT) to obtain liquid A;

[0028] Weigh 1.63 mg of CoTCPP, dissolve it in 19 ml of absolute ethanol, then add 2 ml of distilled water, and wait until it is completely dissolved to obtain liquid B;

[0029] Step 2, slowly pour liquid B into liquid A under magnetic stirring state, and stir for 30 minutes; after the stirring is completed, put the above mixed liquid into a 50 ml microwave reaction tank, use a high-pressure microwave synthesis workstation, and the reaction conditions are temperature-controlled method, the reaction temperature is 100°C, and the reaction time is 10 minutes; after the reaction, cool to room temperature, take out the reaction kettle, add 10 ml of absolute ethanol to the solid product for washing once, pour out the upper liquid after centrifugation, and then add 10 ml of deionized water, washed three times repeatedly, and dried in an oven (60°C), the final ca...

Embodiment 2

[0031] Step 1, 2 ml of n-butyl titanate was dissolved dropwise into 9 ml of absolute ethanol under magnetic stirring conditions to obtain liquid A;

[0032] Then 8 mg of metalloporphyrin was dissolved in 19 ml of absolute ethanol, and 1 ml of deionized water was slowly added dropwise to obtain liquid B.

[0033] Step 2, slowly pour liquid B into liquid A under magnetic stirring, and stir for 20 minutes to obtain a mixed liquid;

[0034] After the stirring is completed, put the mixed solution into a microwave reaction tank, and use a high-pressure microwave synthesis workstation. The reaction conditions are temperature control mode, the microwave reaction temperature is 150°C, and the reaction time is 30 minutes;

[0035] After the microwave reaction, cool to normal temperature, take out the solid product in the reactor, wash with absolute ethanol and deionized water respectively, and finally put the solid product in an oven (60°C) to dry.

Embodiment 3

[0037] Step 1, dissolve 9 ml of n-butyl titanate dropwise into 9 ml of absolute ethanol under magnetic stirring conditions to obtain liquid A;

[0038] Then 0.2 mg of metalloporphyrin was dissolved in 19 ml of absolute ethanol, and then 3 ml of deionized water was slowly added dropwise to obtain liquid B.

[0039] Step 2, slowly pour liquid B into liquid A under magnetic stirring, and stir for 25 minutes to obtain a mixed liquid;

[0040] After the stirring is completed, put the mixed solution into a microwave reaction tank, and use a high-pressure microwave synthesis workstation. The reaction conditions are temperature control mode, the microwave reaction temperature is 130°C, and the reaction time is 20 minutes;

[0041] After the microwave reaction, cool to normal temperature, take out the solid product in the reactor, wash with absolute ethanol and deionized water respectively, and finally put the solid product in an oven (60°C) to dry.

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Abstract

The invention discloses a one-step microwave synthesis method of a metalloporphyrin-titanium dioxide composite catalyst. The method comprises: step 1, blending titanium tetrabutoxide into ethanol absolute dropwisely under a magnetic stirring condition, keeping the volume ratio of titanium tetrabutoxide to ethanol absolute at 2-9ml:9ml, thus obtaining a solution A; dissolving metalloporphyrin in ethanol absolute, keeping the ingredient ratio of metalloporphyrin to titanium tetrabutoxide at 0.2-8mg:4.28ml, then adding deionized water slowly in a dropwise manner, keeping the volume ratio of deionized water to ethanol absolute at 1-3ml:19ml, thus obtaining a solution B; and step 2, pouring the solution B into the solution A under a magnetic stirring condition to obtain a mixed solution; subjecting the mixed solution to a microwave reaction; conducting cooling to room temperature, taking out the solid product, conducting washing respectively with ethanol absolute and deionized water, and finally placing the solid product in a drying oven to dry it. According to the preparation method disclosed in the invention, the product related performance is good, and the working efficiency is high.

Description

technical field [0001] The invention belongs to the technical field of photocatalyst preparation, and relates to a one-step microwave synthesis method of a metalloporphyrin-titanium dioxide composite catalyst. Background technique [0002] Using metalloporphyrin as a sensitizer to sensitize titanium dioxide is one of the effective ways to improve the visible light catalytic effect of titanium dioxide. However, the current traditional method for preparing metalloporphyrin-titanium dioxide composite catalysts is to first prepare TiO 2 Place the metalloporphyrin in an organic solvent and reflux for a certain period of time (tens of minutes to several hours), so that the metalloporphyrin can be physically adsorbed on TiO 2 surface, and then the solvent is spin-dried, and the final sample is dried to prepare the metalloporphyrin-titanium dioxide composite catalyst. Such a preparation method is time-consuming, cumbersome, and has low production efficiency. Contents of the inven...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/38
Inventor 钮金芬姚秉华宁和峰彭超
Owner CHONGQING TIANYI HENGHUA TECH CO LTD
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