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Palladium/alkali metal compound supported catalyst and preparation method and application thereof

A technology of alkali metal compounds and supported catalysts, which is applied in the direction of metal/metal oxide/metal hydroxide catalysts, amino compound preparation, organic compound preparation, etc., and can solve the difficulty of separation in the process of increasing the recovery and reuse of precious metal active components , Aggravate the environmental pollution of recycled waste liquid rich in heavy metals, weaken the catalytic hydrogenation activity of catalysts, etc., and achieve the effects of stable properties of alkali metal compounds, more times of application, and high metal utilization

Active Publication Date: 2015-12-30
ZHEJIANG UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In summary, there are two major disadvantages in the existing catalysts: (1) Adding other metal promoters or using oxide supports, the selectivity of halogenated aromatic amines is low, and the effect of inhibiting dehalogenation is not good.
At the same time, the addition of metal additives and oxide carriers increases the difficulty of separation during the recovery and reuse of precious metal active components, reduces the metal recovery rate, and aggravates the environmental pollution of heavy metal-rich recycling waste liquid; (2) Adding inhibitors , increasing the particle size of the active component, etc. to strengthen the effect of inhibiting dehalogenation will inevitably weaken the catalytic hydrogenation activity of the catalyst, reduce the hydrogenation reaction rate, and the conditions of the recycling process are harsh

Method used

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  • Palladium/alkali metal compound supported catalyst and preparation method and application thereof
  • Palladium/alkali metal compound supported catalyst and preparation method and application thereof
  • Palladium/alkali metal compound supported catalyst and preparation method and application thereof

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Effect test

Embodiment 1～ Embodiment 18

[0046] The content, proportion and preparation conditions of the catalyst active components are provided (as shown in Table 1).

[0047] Catalyst concrete preparation process is as follows (taking embodiment 1 as example):

[0048] (a) Set the specific surface area to 1400m 2 / g, 0.85mL / g pore volume, 3.2% ash content coconut shell activated carbon was vacuum-dried and dehydrated at 120°C for 3h; L) in 50mL deionized water, adjust the pH value to 0.8 with hydrochloric acid;

[0049] (b) then immerse 10 g of activated carbon that has been vacuum-dried and dehydrated in palladium liquid, fully stir and impregnate at 80° C. for 5 hours, and adjust the pH value to 9.5 with ammonia water;

[0050] (c) After half an hour, 1.5 mL of formaldehyde solution (GB-T685-1993) was added dropwise, and reduced at 80° C. for 2 h. After cooling down to room temperature, the reaction system was filtered, the filter cake was washed with deionized water until neutral, and dried and dehydrated at...

Embodiment 19

[0066]Add 200g of 6-chloro-2-nitrotoluene and 1.0g of the palladium / alkali metal compound supported catalyst prepared in Example 1 into a 500mL autoclave, close the autoclave, replace the air in the reactor with nitrogen, and then replace it with hydrogen Nitrogen, start stirring, stirring rotation speed 1000r / min, maintain reaction temperature 50°C, hydrogen pressure 0.5MPa to carry out the reaction. When the content of 6-chloro-2-nitrotoluene was detected to be 0 by chromatography, the reaction was stopped and the catalyst was filtered. The filtrate is the product after phase separation, water separation and dehydration by vacuum distillation. Quantitative analysis (molar percentage) by chromatography shows that the conversion rate of hydrogenation reaction is 100%, and the selectivity is 99.96%.

[0067] The operating condition of embodiment 20~embodiment 39 is the same as embodiment 19, is respectively the hydrogenation catalyst that the embodiment 2~embodiment 18 and comp...

Embodiment 58

[0076] Example 58 is the experimental situation of using the catalyst prepared in Example 2 in the catalytic hydrogenation reaction of 3,4-dichloronitrobenzene under the operating conditions of Example 19. The results are shown in Table 4.

[0077] Catalyst prepared in the embodiment 2 of table 4 synthesizes 3, the mechanically applied experimental result of 4-dichloroaniline reaction

[0078]

[0079]

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Abstract

The invention provides a palladium / alkali metal compound supported catalyst and a preparation method and application thereof. The catalyst is composed of a supporter and an active component supported on the supporter. The supporter is active carbon. The active component comprises elemental palladium and an alkali metal compound. Based on the mass of the supporter active carbon, the supporting amount of the elemental palladium is 0.25-15.0wt%, and the theoretical supporting amount of alkali metal elements in the alkali metal compound is 0.01-5.0wt%. The catalyst can be applied to a catalytic hydrogenation reaction of a haloaromatic nitrocompound and / or an aromatic nitro compound. The catalyst is high in catalytic activity and easy to recycle and use indiscriminately, no dehalogenation inhibitor needs to be added when the catalyst is applied to the catalytic hydrogenation reaction of the haloaromatic nitrocompound, and the reaction conversion rate and the product selectivity are still excellent on the premise of keeping the high reaction speed.

Description

(1) Technical field [0001] The invention relates to a palladium / alkali metal compound supported catalyst and a preparation method thereof. The catalyst can be applied to the catalytic hydrogenation reaction of a single halogenated aromatic nitro compound or a single aromatic nitro compound, and can also be applied to a halogenated aromatic nitro compound Catalytic hydrogenation reaction of nitro compound and aromatic nitro compound blend system. (2) Technical background [0002] Halogenated aromatic amines are an important class of organic synthesis intermediates, widely used in dyes, medicines, pesticides, plasticizers, textiles, spices, synthetic fibers, printing and dyeing auxiliaries, liquid crystal materials, chelating agents, polymers, and flame retardants Synthesis of organic fine chemicals. The production method of the halogenated aromatic amine is mainly prepared by reduction of the corresponding halogenated aromatic nitro compound. The catalytic hydrogenation red...

Claims

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Application Information

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IPC IPC(8): B01J23/58C07C211/52C07C209/36
Inventor 卢春山丰枫张群峰马磊李小年
Owner ZHEJIANG UNIV OF TECH
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