Highly-dispersed catalyst for hydrogen peroxide synthesis and preparation method thereof

A technology of catalyst and hydrogen peroxide, applied in chemical instruments and methods, peroxide/peroxyhydrate/peroxyacid/superoxide/ozonide, inorganic chemistry, etc., can solve highly toxic organotin compounds, not applicable Production and other problems, to improve catalyst activity and overcome the effect of large crystal grains

Inactive Publication Date: 2016-01-27
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, highly toxic organotin compounds are used in the

Method used

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  • Highly-dispersed catalyst for hydrogen peroxide synthesis and preparation method thereof
  • Highly-dispersed catalyst for hydrogen peroxide synthesis and preparation method thereof
  • Highly-dispersed catalyst for hydrogen peroxide synthesis and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Catalyst preparation

[0037] 1) Weigh 2.0gAl 2 o 3 , 100ml ethylene glycol, 25ml isopropanol, 0.1gPVP, 0.24gNaOH in a three-necked flask, pass into N 2 , stirred for 1h.

[0038] 2) Add 0.043gPd(NO 3 ) 2 , heated to 110°C in an oil bath, and refluxed for 3h.

[0039] 3) After the mixture is cooled to room temperature, add 0.5M HNO 3 To pH = 3, stirred for 10h.

[0040] 4) suction filtration, the obtained solid was washed with ethanol and deionized water until neutral.

[0041] 5) dry. The obtained solid was dried at 110° C. for 12 h to obtain catalyst A.

[0042] The CO chemical adsorption pulse test shows that the Pd dispersion is 53.4%, and the particle size of Pd particles is 2.8nm according to TEM. The TEM photo is shown in figure 1 , The evaluation results of catalyst hydrogenation performance are shown in Table 1.

Embodiment 2

[0044] Catalyst preparation

[0045] 1) Weigh 2.0gMg-Al hydrotalcite, 100ml methanol, 25ml isopropanol, 0.04gPVP, 0.12gNaOH in a flat-bottomed three-necked flask, and pass into N 2 , stirred for 1h.

[0046] 2) Add 0.0086gPd(NO 3 ) 2 , Stir evenly and heat in microwave for 1min with a power of 900W.

[0047] 3) After the mixture is cooled to room temperature, add 0.5M HNO 3 To pH = 3, stirred for 10h.

[0048] 4) suction filtration, the obtained solid was washed with ethanol and deionized water until neutral.

[0049] 5) dry. The obtained solid was dried at 70°C for 12 hours to obtain catalyst B.

[0050] The CO chemisorption pulse test shows that the Pd dispersion is 13.7%. The hydrogenation performance evaluation results of the catalyst are shown in Table 1.

Embodiment 3

[0052] Catalyst preparation

[0053] 1) Weigh 2.0g SiO2 2 , 100ml methanol, 0.3gCTAB, 0.24gNaOH in a three-necked flask, N 2 , stir.

[0054] 2) Add 0.033PdCl to the flask 2 , heated to 50°C in an oil bath, and refluxed for 12h.

[0055] 3) After the mixture is cooled to room temperature, add 0.5M HNO 3 To pH = 3, stirred for 10h.

[0056] 4) suction filtration, the obtained solid was washed with ethanol and deionized water until neutral.

[0057] 5) dry. The obtained solid was vacuum-dried at 50°C for 12 hours to obtain catalyst C.

[0058] The CO chemical adsorption pulse test shows that the Pd dispersion is 33.9%, and the particle size of Pd particles is 3.7nm according to TEM. The TEM photo is shown in figure 2 , Catalyst hydrogenation evaluation results are shown in Table 1.

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Abstract

A highly-dispersed catalyst for hydrogen peroxide synthesis and a preparation method thereof belong to the field of petrochemical engineering. The catalyst mainly comprises catalyst active ingredients and a catalyst carrier. All the catalyst active ingredients are supported on the carrier to form a granular catalyst. The main catalyst active ingredient is a platinum-family precious metal active ingredient which accounts for 0.01-2wt% of the total weight of the catalyst weighed on the basis of the simple substance of precious metal. The catalyst carrier accounts for 98-99.00 wt% of the total weight of the catalyst. The preparation method comprises the following steps: carrying out heat treatment on the platinum-family precious metal active ingredient under the action of a reducing agent and a protective agent to prepare nano-particle sol, supporting the nano-particle sol onto the granular catalyst carrier, and drying to prepare the catalyst. In comparison with a traditional catalyst prepared by an immersion method, the highly-dispersed granular catalyst has advantages as follows: problems of large crystalline grain of the active ingredients and low dispersity are overcome, and catalyst activity is raised. In addition, use of toxic reagents such as organic tin and the like is avoided during the preparation process. The preparation method is green and environmentally friendly and is suitable for production.

Description

technical field [0001] The invention belongs to the field of petrochemical industry, and in particular relates to a highly dispersed catalyst for hydrogen peroxide synthesis and a preparation method thereof. Background technique [0002] Hydrogen peroxide is an important inorganic chemical, which can be used as an oxidant, bleach, disinfectant, deoxidizer, etc., and is widely used in papermaking, chemical industry, environmental protection, electronics, aerospace and other industries. The product of hydrogen peroxide after use is water and oxygen, which has no pollution to the environment and is a green chemical. In recent years, in the new green chemical industry, such as caprolactam, cyclohexanone, hydroquinone, propylene oxide and other products, hydrogen peroxide is used as the oxidant in the production process, further opening up new application fields of hydrogen peroxide. With the continuous deepening of the concept of developing green chemistry, the hydrogen peroxid...

Claims

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Application Information

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IPC IPC(8): B01J23/42B01J23/44B01J23/63C01B15/023
Inventor 王树东李晓彤苏宏久任高远
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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