Nano-spherical mesoporous organic metal catalyst, preparation method and application thereof

An organometallic and catalyst technology, applied in the field of nano-spherical mesoporous organometallic catalysts, to achieve the effect of simple operation and preventing pollution

Inactive Publication Date: 2012-05-30
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there is no report on the preparation of mesoporous organometallic catalysts by spray drying

Method used

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  • Nano-spherical mesoporous organic metal catalyst, preparation method and application thereof
  • Nano-spherical mesoporous organic metal catalyst, preparation method and application thereof
  • Nano-spherical mesoporous organic metal catalyst, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Preparation of the catalyst: at room temperature, the mixed solution of 1.6g surfactant CTAB (0.0044mol), 33ml ethanol (0.57mol), 0.39g sodium chloride, 6.5ml water and 0.22ml hydrochloric acid aqueous solution (2M) was stirred for 1 After ~6 hours, 4.3 ml of inorganic silicon source TEOS (0.019 mol) was added, prehydrolyzed for 1 hour, and 0.27 g (0.00029 mol) of freshly prepared bis-(1-triethoxysilyl-2) dissolved in 2 ml of tetrahydrofuran was added - diphenylphosphine) ethane palladium dichloride (organometallic palladium silicon source), continue to stir for 1 to 3 hours until it becomes a uniform solution. Subsequently, after spray drying at 573K and 1Mpa pressure, extraction and washing with ethanol at 353K for 24 hours, and vacuum drying, the milky yellow solid powder obtained is a nano-spherical ordered mesoporous organometallic catalyst with a high specific surface area. MOC-AASA said. The content of Pd in ​​the product is 0.14mmol / g (2% by mass), and the acti...

Embodiment 2

[0032]Take 0.014ml iodobenzene (0.125mmol), 0.014ml phenylacetylene (0.125mmol), 0.030ml n-heptane (internal standard), 0.21ml DBU (1,8-diazacyclo[5,4,0]deca Monoene-7) (1.48mmol), 0.0050g cocatalyst cuprous iodide (0.0259mmol), 4.0ml deionized water, Pd(II)-MOC-AASA (Pd content is 0.005mmol) prepared in Example 1 , Reaction at 353K for 5h, the resulting product was extracted five times with 10ml toluene, and the reaction product was analyzed by gas chromatography (Agilent GC1790). The analysis results are shown in Table 1.

[0033] Catalytic performance of catalyst in table 1 embodiment 1 and 2

[0034]

Embodiment 3

[0036] Carry out the activity test of benzaldehyde homologue according to the Barbier reaction system of embodiment 1, take the substituent material of different benzaldehyde para-position of equimolar number as reaction substrate, reaction condition and detection means are the same as embodiment 1. The analysis results are shown in Table 2.

[0037] Catalytic performance of catalyst in table 2 embodiment 3

[0038]

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Abstract

The invention discloses a nano-spherical mesoporous organic metal catalyst. In the nano-spherical mesoporous organic metal catalyst, the grain diameter is between 100 and 600nm, the pore diameter is between 1.5 and 8.0nm, the pore volume is between 0.2 and 1.0cm<3> / g, the specific surface area is between 800 and 1,200m<2> / g, and the Pd element content is between 0.05 and 0.35mmol / g. The preparation method comprises the following steps: mixing organic metal silane, solution of inorganic silane, a template, water and ethanol; performing a hydrolytic polycondensation reaction by using a spray drying method; and extracting the template from an obtained solid by using alcohols to prepare the nano-spherical mesoporous organic metal catalyst. By using the method, an organic metallic catalyst with ordered mesopore arrangement can be quickly prepared, the active ingredients of the organic metallic catalyst are highly dispersed in pore passages, and the organic metallic catalyst serves as a catalyst for Barbier reaction or Sonogashira reaction in a water medium, and the organic metallic catalyst can have the catalytic performance similar to that of a homogenous organic metal catalyst.

Description

technical field [0001] The invention relates to a nano-spherical mesoporous organometallic catalyst, in particular to its preparation scheme and the application of the catalytic material in cleaning organic reactions in aqueous media. Background technique [0002] Water is the most harmless substance on earth and the safest solvent. As a green and non-polluting reaction medium, water has been widely concerned by people. In recent years, the use of water instead of organic solvents for organic synthesis has become an important branch of green chemistry. At present, homogeneous organometallic catalysts are mostly used in aqueous media because of their high activity and selectivity. However, due to their difficulty in separation and recycling from the reaction system, it is difficult to make breakthroughs in industrial applications. In addition, homogeneous catalysts It will also cause pollution of heavy metal ions. In order to solve the above problems, people generally choos...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/12B01J35/10B01J37/08C07C33/30C07C29/38C07C15/54C07C2/86
Inventor 张昉康春梅李和兴
Owner SHANGHAI NORMAL UNIVERSITY
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