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High-dispersion particle catalyst applied to synthesis of hydrogen peroxide as well as preparation method and application thereof

A particle catalyst, catalyst technology, applied in catalyst activation/preparation, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of reducing precious metal content, poor selectivity, low hydrogenation efficiency, etc.

Inactive Publication Date: 2017-08-04
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

[0011] Aiming at the disadvantages of low hydrogenation efficiency and poor selectivity in the prior art, the object of the present invention is to provide a highly dispersed supported catalyst for hydrogenation of anthraquinone to produce hydrogen peroxide and a preparation method thereof, so as to improve single-pass hydrogenation efficiency and Effective anthraquinone selectivity and further reduction of noble metal content

Method used

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  • High-dispersion particle catalyst applied to synthesis of hydrogen peroxide as well as preparation method and application thereof
  • High-dispersion particle catalyst applied to synthesis of hydrogen peroxide as well as preparation method and application thereof
  • High-dispersion particle catalyst applied to synthesis of hydrogen peroxide as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0069] a) Weigh 0.2g AlPO-11, 0.8g Al 2 o 3 , after mixing evenly, tableting and granulation, the tableting pressure is 5MPa, and the particle size is 20-30 mesh.

[0070] b) Take 3mg La(NO 3 ) 3 ·6H 2 O dissolved in 5ml of water forms La(NO 3 ) 3 solution, immerse the particles obtained in step 1) in the solution for 2 hours, and then dry at 80° C. for 12 hours to obtain a carrier.

[0071] c) Take 0.5g carrier and impregnate it in 1ml of H2O with a concentration of 0.6mg / ml 2 PtCl 6 solution (calculated as Pt), the immersion time is 2h.

[0072] d) Dry at 80°C for 12h and then calcinate at 400°C for 2h to obtain the catalyst in oxidation state.

[0073] e) Put the oxidized catalyst in 20ml of formaldehyde solution (0.1M) for reduction, the reduction temperature is controlled at 60°C, the reduction time is 1h, and then rinsed with deionized water and dried at room temperature to obtain catalyst A.

[0074] TEM photo see figure 1 , and the evaluation results of cata...

Embodiment 2

[0076] a) Weigh 0.4g SAPO-34, 0.6g SiO 2 , 0.1g of silica sol (40wt%) and 20ml of deionized water, mixed evenly, dried at 80°C, and granulated, with a particle size of 10-20 mesh.

[0077] b) Take 0.64g Mg(NO 3 ) 2 ·6H 2 O dissolved in 5ml of water to form Mg(NO 3 ) 2 solution, immerse the particles obtained in step 1) in the solution for 2 hours, and then dry at 80° C. for 12 hours to obtain a carrier.

[0078] c) Take 0.5g carrier and impregnate it in 1ml of H2O with a concentration of 3mg / ml 2 PdCl 4 solution (calculated as Pd), the immersion time is 2h.

[0079] d) After drying at 80°C for 12h, calcining at 300°C for 2h to obtain the catalyst in the oxidized state.

[0080] e) Place the oxidation state catalyst in H 2 Reduction in the atmosphere, the reduction temperature is 60 ° C, and the reduction time is 24 hours to obtain catalyst B.

[0081] The evaluation results of catalyst hydrogenation performance are shown in Table 2.

Embodiment 3

[0083] a) Weigh 0.6g VPI-5, 0.4g CeO 2 , 0.1g cerium sol (10wt.%), 0.52g Nd(NO 3 ) 3 ·6H 2 O and 20ml of deionized water were evenly mixed, dried at 120°C, and granulated to obtain a carrier with a particle size of 10-20 mesh.

[0084] b) Take 0.5g carrier and impregnate it in 1ml Pd(NO 3 ) 2 solution (calculated as Pd), the immersion time is 2h.

[0085] c) Vacuum drying at 60°C for 12 hours and then calcining at 250°C for 2 hours to obtain the catalyst in an oxidized state.

[0086] d) Put the oxidation state catalyst in NaBH 4 Reduction in a solution (10wt%), the reduction time is 1 h, the reduction temperature is 30 degrees, and then washed with deionized water and dried at room temperature to obtain catalyst C.

[0087] The evaluation results of catalyst hydrogenation performance are shown in Table 2.

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Abstract

The invention provides a high-dispersion particle catalyst applied to synthesis of hydrogen peroxide as well as a preparation method and application thereof. The preparation method of the catalyst is characterized by taking one or combination of two of noble metals Pd and Pt as a main active component, loading the main active component on a composite carrier prepared from AlPO series, SAPO series, silicon zincate molecular sieves, phosphates and oxides to prepare the catalyst. The catalyst carrier has a micropore-mesopore compounded hierarchical porous structure; through micropores, the dispersity of active metals and the spillover of hydrogen atoms can be improved, so that the hydrogenation activity of the catalyst, and the consumption of the noble metals is reduced; through mesopores, diffusion channels are provided for reactants and products, so that the mass transfer in the pores is facilitated, the mass production of byproducts is effectively avoided, and then the selectivity of the catalyst is improved; in addition, the composite carrier is easy to modify; acidity and alkalinity can be regulated; the performance of the catalyst can be further improved.

Description

[0001] Technical field: [0002] The invention belongs to the field of petrochemical industry, and in particular relates to an anthraquinone hydrogenation integral catalyst and a preparation method thereof. [0003] Background technique: [0004] Hydrogen peroxide is an excellent chemical product. Because it only produces water and oxygen after use and does not cause secondary pollution, it is called a "green chemical product". It can be used as oxidizing agent, bleaching agent, disinfectant, deoxidizer, etc., and is widely used in papermaking, chemical industry, environmental protection, electronics, aerospace and other industries. 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. As of the end of 2014, there were more than 50 domestic hydrogen peroxide produ...

Claims

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Application Information

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IPC IPC(8): B01J29/83B01J29/85B01J29/89B01J29/82C01B15/023
CPCB01J29/74B01J37/02B01J37/04B01J37/16C01B15/023B01J29/83B01J29/82B01J29/85B01J29/89
Inventor 王树东李晓彤苏宏久陈海军杨晓野李大卫
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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