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Method for preparing ordered mesoporous Pd-TiO2 heterogeneous catalyst and application thereof

A heterogeneous catalyst, ordered mesoporous technology, applied in organic chemistry methods, chemical instruments and methods, physical/chemical process catalysts, etc. problem, to achieve the effect of strong bonding force, high mechanical strength and lower production cost

Inactive Publication Date: 2014-01-08
HUAIYIN TEACHERS COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to solubility limitations, most of the current Suzuki reactions use homogeneous Pd(II) organometallic catalysts.
Its disadvantage is repeated use and heavy metal pollution
The solution is to immobilize homogeneous catalysts, but the catalytic activity is low due to the decrease in the dispersion of catalytic active sites

Method used

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  • Method for preparing ordered mesoporous Pd-TiO2 heterogeneous catalyst and application thereof
  • Method for preparing ordered mesoporous Pd-TiO2 heterogeneous catalyst and application thereof
  • Method for preparing ordered mesoporous Pd-TiO2 heterogeneous catalyst and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1: Prepare ordered mesoporous Pd-TiO according to the following steps 2 catalyst

[0018] Step 1: First at 20 o C Dissolve 1.7 g of P123 in 38 mL of absolute ethanol, then add 5.0 mL of n-butyl titanate and stir for 25 min, then add 1.8 mL of titanium tetrachloride and stir for 10 min, and finally add 3.6 mL of 0.025 g / mL PdCl 2 Alcoholic solution, 20 o C was vigorously stirred for 3h to obtain solution A;

[0019] The second step: the solution A obtained in step 1 undergoes a solvent evaporation-induced self-assembly process, that is, at 20 o C. 35 o C.95 o C kept for 24 h to obtain solid powder A;

[0020] The third step: the solid powder A obtained in step 2 is placed in the muffle furnace, starting from 20 o C to 1 o C / min heating rate up to 100 o C, again with 0.5 o C / min heating rate up to 200 o C, final with 0.2 o C / min heating rate up to 350 o C, and at 350 o C was roasted for 220 min to obtain solid powder B;

[0021] The fourth step: t...

Embodiment 2

[0025] Example 2: Prepare ordered mesoporous Pd-TiO according to the following steps 2 catalyst

[0026] Step 1: First at 25 o C Dissolve 1.95 g P123 in 40 mL of absolute ethanol, then add 6.0 mL of n-butyl titanate and stir for 30 min, then add 2.0 mL of titanium tetrachloride and stir for 15 min, and finally add 4.0 mL of 0.025 g / mL PdCl 2 Alcoholic solution, 25 o C was vigorously stirred for 4h to obtain solution A;

[0027] The second step: the solution A obtained in step 1 undergoes a solvent evaporation-induced self-assembly process, that is, at 25 o C. 40 o C. 100 o C kept for 24 h to obtain solid powder A;

[0028] The third step: the solid powder A obtained in step 2 is placed in the muffle furnace, starting from 25 o C to 1 o C / min heating rate up to 100 o C, again with 0.5 o C / min heating rate up to 200 o C, final with 0.2 oC / min heating rate up to 350 o C, and at 350 o C was roasted for 240 min to obtain solid powder B;

[0029] The fourth step: the...

Embodiment 3

[0030] Example 3: Prepare ordered mesoporous Pd-TiO according to the following steps 2 catalyst

[0031] Step 1: First at 30 o C Dissolve 2.2 g of P123 in 42 mL of absolute ethanol, then add 7.0 mL of n-butyl titanate and stir for 35 min, then add 2.2 mL of titanium tetrachloride and stir for 20 min, and finally add 4.4 mL of 0.025 g / mL PdCl 2 Alcoholic solution, 30 o C was vigorously stirred for 5h to obtain solution A;

[0032] The second step: the solution A obtained in step 1 undergoes a solvent evaporation-induced self-assembly process, that is, at 30 o C. 45 o C. 105 o C kept for 24 h to obtain solid powder A;

[0033] The third step: the solid powder A obtained in step 2 is placed in the muffle furnace, starting from 30 o C to 1 o C / min heating rate up to 100 o C, again with 0.5 o C / min heating rate up to 200 o C, final with 0.2 o C / min heating rate up to 350 o C, and at 350 o C was roasted for 260 min to obtain solid powder B;

[0034] The fourth step:...

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Abstract

The invention discloses a method for preparing an ordered mesoporous Pd TiO2 heterogeneous catalyst and an application thereof. The method comprises the steps of: dissolving P123 in absolute ethyl alcohol, adding butyl titanate, titanium tetrachloride, and alcohol solution of PdCl2 and mixing to obtain solution A; processing the solution A by solvent evaporation-induced self-assembly to obtain solid powder A; putting the solid powder A into a muffle furnace and calcining to obtain solid powder B; and putting the solid powder B into a tube furnace and reducing it for 3-5 hours in N2 atmosphere containing 10% H2 and at a temperature of 260-300 DEG C to obtain the ordered mesoporous Pd-TiO2 heterogeneous catalyst. The heterogeneous catalyst provided by the invention has an ordered two-dimensional hexagonal mesoporous structure, a larger specific surface area, high catalytic activity, fast reaction rate, and low production cost. Moreover, the heterogeneous catalyst is recyclable and has little pollution to environment.

Description

technical field [0001] The invention relates to a preparation method of a catalyst, in particular to a method for preparing ordered mesoporous Pd-TiO 2 Methods of heterogeneous catalysts and their applications. Background technique [0002] In recent years, the use of water instead of organic solvents for organic synthesis has become an important branch of green chemistry. Suzuki and Sonogashira reactions are an important class of organic reactions for C-C bond formation. Traditionally, the catalyst used for Suzuki reaction is mainly noble metal Pd, and the reaction medium is organic solvent. In order to overcome the solubility limitation of reaction substrates in aqueous media, a variety of immobilized organic Pd catalyst heterogeneous catalysts have been developed in recent years for the Suzuki and Sonogashira reactions in aqueous media, but the steps in the immobilized Pd process are cumbersome and It requires organic ligands and a large amount of organic matter, which...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/44C07B37/00C07C15/54C07C15/14C07C2/86
CPCY02P20/584
Inventor 朱凤霞周建峰朱惠琴李和兴
Owner HUAIYIN TEACHERS COLLEGE