Supported noble-metal hydrogenation catalyst, and preparation method and application of catalyst

A hydrogenation catalyst and precious metal technology, applied in the fields of hydrogenation catalyst and its preparation and application, can solve problems such as retention, and achieve the effects of fast filtration, simplified process flow and good stability

Active Publication Date: 2017-12-15
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the nitrophenyl ether catalytic hydrogenation technology mentioned in the above-mentioned existing literature only stays in the process exploration and development of the alternative catalytic hydroge...

Method used

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  • Supported noble-metal hydrogenation catalyst, and preparation method and application of catalyst
  • Supported noble-metal hydrogenation catalyst, and preparation method and application of catalyst
  • Supported noble-metal hydrogenation catalyst, and preparation method and application of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Weigh 10g of activated carbon, the specific surface area of ​​activated carbon is 1000m 2 / g, the proportion of mesopores is 50%, and the pore volume is 0.8mL / g. Weigh 1g of water, 8g of ethanol, and 0.1g of ethyl orthosilicate in a beaker, and stir well until completely dissolved. Activated carbon was poured into the mixture and stirred at 25°C for 2 hours. Then chloroplatinic acid containing 0.2 g of platinum was added, followed by adjusting the pH of the activated carbon slurry to 1.0 with hydrochloric acid, and aging at 25° C. for 20 hours. Then adjust the pH of the activated carbon slurry to 9.0 with 5 wt% potassium hydroxide solution, continue aging at constant temperature for 5 hours, filter, wash with ethanol until the pH of the filtrate reaches neutral, and obtain a catalyst precursor. Finally, in a hydrogen atmosphere, the room temperature was raised from room temperature at 0.1°C / min (heating rate 1) to 150°C (final temperature 1), and then at 0.5°C / min (he...

Embodiment 14

[0060]Add 100g of p-nitrophenethyl ether and 0.8g of the catalyst of Example 1 into a 500mL autoclave, close the autoclave, replace the air in the reactor with nitrogen, then replace the nitrogen with hydrogen, start stirring, and the stirring speed is 1400r / min. The reaction was carried out by maintaining the reaction temperature at 50° C. and the hydrogen pressure at 1.0 MPa. During the reaction, the pH value of the hydrogenation solution is monitored online in real time, and the cesium hydroxide lye is adjusted in real time to keep the pH value of the hydrogenation solution in the kettle at 6.0-7.5, and control the concentration of cesium ions in the hydrogenation solution to 0.5g / L. When the content of p-nitrophenethyl ether 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 c...

Embodiment 27

[0068] Embodiment 27 is the catalyst application experiment of Embodiment 14, and the results are shown in Table 3.

[0069]

[0070]

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Abstract

The invention discloses a supported noble-metal hydrogenation catalyst, and a preparation method and an application of the catalyst. The catalyst is prepared according to the following steps: (1) preparing a mixed solution consisting of water, an alcohol and tetraethyl orthosilicate; (2) pouring activated carbon into the mixed solution obtained in the step (1) and performing stirring, then adding a soluble noble metal salt, regulating the pH value of the slurry to a range of 0.5-2.5, and performing stirring aging to obtain a reaction slurry; (3) adding a base liquor into the reaction slurry to regulate the pH value to a range of 7.5-14, wherein the basic substance in the base liquor is one or a combination of more selected from a group consisting of potassium hydroxide, cesium hydroxide, potassium acetate, cesium acetate, potassium carbonate and cesium carbonate, continuing to perform stir, and finally performing filtering and washing to obtain a catalyst precursor; and (4) performing reduction on the catalyst precursor to obtain the supported noble-metal hydrogenation catalyst. The invention provides an application of the catalyst in catalyzing hydrogenation synthesis of amino phenyl ether compounds which are represented as a formula II by using compounds which are represented as a formula II, the conversion rate reaches 100%, the selectivity can reach 99.5% or more, and the catalyst can be used for 50 times or more.

Description

(1) Technical field [0001] The invention relates to a hydrogenation catalyst and its preparation and application, in particular to a supported noble metal hydrogenation catalyst, its preparation method and its application in catalytic hydrogenation reduction synthesis of aminophenyl ether compounds. (2) Technical background [0002] Aminophenyl ether compounds are an important class of fine chemical intermediates, widely used in medicine, dyes, feed, spices, rubber and other fields. Its synthesis method mainly uses nitrophenyl ether compounds as raw materials through chemical reduction or catalytic hydrogenation reduction. The chemical reduction method is to use the reducing properties of chemical reagents such as iron powder, sodium sulfide, and hydrazine hydrate to undergo a stoichiometric redox reaction with the raw materials. Therefore, this method has many wastes, high labor intensity, and poor product quality, and has been forcibly eliminated by the current environmen...

Claims

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Application Information

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IPC IPC(8): B01J23/42B01J23/44B01J37/03B01J37/18C07C213/02C07C215/80C07C215/76
CPCB01J23/42B01J23/44B01J37/035B01J37/18C07C213/02C07C215/80C07C215/76
Inventor 李小年卢春山丰枫马磊张群峰许孝良
Owner ZHEJIANG UNIV OF TECH
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