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Pd loaded attapulgite catalyst and method for reducing para-nitrobenzyl cyanide by using same

A technology of p-nitrophenylacetonitrile and attapulgite, applied in chemical instruments and methods, organic chemistry, carboxylic acid nitrile preparation, etc., can solve the problems of flammability and high cost, and achieve low production cost, less side reactions, and easy The effect of preparation

Inactive Publication Date: 2013-06-12
HUAIYIN TEACHERS COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The metal palladium catalyst used in catalytic hydrogenation uses activated carbon as a carrier. Activated carbon has good performance as a carrier and is widely used, but it also has the disadvantages of high cost and flammability. Therefore, it is necessary to find a material with good performance, low cost and non-flammability to replace activated carbon. Carriers for metal palladium

Method used

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  • Pd loaded attapulgite catalyst and method for reducing para-nitrobenzyl cyanide by using same
  • Pd loaded attapulgite catalyst and method for reducing para-nitrobenzyl cyanide by using same
  • Pd loaded attapulgite catalyst and method for reducing para-nitrobenzyl cyanide by using same

Examples

Experimental program
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Embodiment 1

[0014] Embodiment 1: 16.7mg PdCl 2 Add it into 2 mL of 5 mol / L hydrochloric acid solution, stir to dissolve; then add 1.0 g of attapulgite, stir and soak for 1 hour; Reduce until no hydrogen chloride gas is released; cool to room temperature under the protection of hydrogen to obtain a Pd-supported attapulgite catalyst (Pd / attapulgite) with a Pd content of 1%.

Embodiment 2

[0015] Embodiment 2: 83.6mg PdCl 2 Add to 2 mL of 5 mol / L hydrochloric acid solution, stir to dissolve; then add 1.0 g of attapulgite, stir and impregnate for 2 hours; Reduce until no hydrogen chloride gas is released; cool to room temperature under the protection of hydrogen to obtain a Pd-supported attapulgite catalyst (Pd / attapulgite) with a Pd content of 5%.

Embodiment 3

[0016] Embodiment 3: 167mg PdCl 2 Add to 2 mL of 5 mol / L hydrochloric acid solution, stir to dissolve; then add 1.0 g of attapulgite, stir and impregnate for 3 hours; Reduce until no hydrogen chloride gas is released; cool to room temperature under the protection of hydrogen to obtain a Pd-supported attapulgite catalyst (Pd / attapulgite) with a Pd content of 10%.

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Abstract

The invention discloses a Pd loaded attapulgite catalyst and a method for reducing para-nitrobenzyl cyanide by using the catalyst. The method comprises the following steps of: adding PdCl2 into hydrochloric acid liquid and stirring and dissolving; then adding attapulgite, and stirring and dipping; drying, grinding and placing in a quartz tube of a resistance furnace, and reducing by hydrogen till no hydrogen chloride is released; cooling to room temperature under protection of hydrogen to obtain the Pd loaded attapulgite catalyst; adding para-nitrobenzyl cyanide, ethanol and a catalyst to a pressure reaction kettle, replacing air in the reaction kettle with argon and introducing hydrogen, standing after reaction and opening the pressure reaction kettle, evaporating part of ethanol, placing and crystallizing, filtering and drying to obtain a coarse product; and recrystallizing the coarse product by ethanol and decoloring by active carbon to obtain brown crystals. The catalyst provided by the invention is easy to prepare, low in production cost, difficult to combust, mild in reduction reaction condition, good in selectivity, less in side effect, easy to purify and high in yield.

Description

technical field [0001] The invention relates to a Pd loaded attapulgite catalyst and a method for reducing p-nitrophenylacetonitrile. Background technique [0002] Attapulgite clay, referred to as "attapulgite" or "attapulgite", is a porous chain-layered hydrous magnesium-rich aluminum silicate clay mineral with attapulgite as the main component. The unique chain layer crystal structure of attapulgite makes it have many special physical and chemical properties, mainly including adsorption, ion exchange, rheology, catalysis and plasticity. Due to these characteristics of attapulgite, it is widely used in many fields such as petroleum, chemical industry, building materials, medicine, agriculture, environmental protection, and daily necessities. [0003] The reduction of aromatic nitro compounds to corresponding aromatic amines has become a common method for fine chemical production to prepare aromatic amines because of its simple operation and readily available raw materials....

Claims

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Application Information

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IPC IPC(8): B01J23/44C07C255/42C07C253/30
Inventor 韦长梅支三军王素青夏敏刘炳华
Owner HUAIYIN TEACHERS COLLEGE