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Ruthenium catalyst for anthraquinone hydrogenation to prepare hydrogen peroxide, and preparation method thereof

A ruthenium catalyst and catalyst technology, applied in the direction of metal/metal oxide/metal hydroxide catalyst, chemical instrument and method, physical/chemical process catalyst, etc., can solve the problems of poor practicability and achieve good stability and high yield Less, reduce the effect of anthraquinone consumption

Inactive Publication Date: 2018-05-22
贵研工业催化剂(云南)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Catalysts with Mo and Co as active components need to go through high temperature and high pressure during activation treatment, so the practicability is poor

Method used

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  • Ruthenium catalyst for anthraquinone hydrogenation to prepare hydrogen peroxide, and preparation method thereof
  • Ruthenium catalyst for anthraquinone hydrogenation to prepare hydrogen peroxide, and preparation method thereof
  • Ruthenium catalyst for anthraquinone hydrogenation to prepare hydrogen peroxide, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] (1) Dissolving 0.4g ruthenium trichloride (Ru content 37.7%) in 100ml 1,3-propanediol and stirring to obtain a ruthenium trichloride mixed solution;

[0042] (2) Add 15g of 3.0mm spherical activated alumina carrier formed by rolling balls into the mixed solution obtained in step (1), and further stir for 0.5h;

[0043] (3) Stir and heat the mixed solution obtained in (2) to 180°C, and keep it for 0.5h, filter to obtain the catalyst, then wash off chloride ions with deionized water, and obtain 1% Ru / Al after vacuum drying 2 o 3 Catalyst, and keep it sealed.

[0044] Add 3g of the above catalyst and 50mL of working solution into a 100mL autoclave, and react at 55°C and 0.3MPa for 1h. The hydrogenation efficiency of the reaction is 8.5g / L, and the selectivity is 95.2%.

Embodiment 2

[0046] (1) 0.2g ruthenium trichloride (Ru content 37.7%) is dissolved in 100ml ethylene glycol and stirred to obtain a ruthenium trichloride mixed solution;

[0047] (2) 15g extruded 3.0mm toothed spherical SiO 2 -Al 2 o 3 The carrier is added to the mixed solution obtained in step (1), and further stirred for 0.5h;

[0048] (3) Stir and heat the mixed solution obtained in (2) to 180°C, and keep it for 0.5h, filter to obtain the catalyst, then wash off the chloride ions with deionized water, and obtain 0.5% Ru / Al after vacuum drying 2 o 3 Catalyst, and keep it sealed.

[0049] Add 3 g of the above catalyst and 50 mL of working solution into a 100 mL autoclave, and react at 55° C. and 0.3 MPa for 1 hour. The hydrogenation efficiency of the reaction is 7.7 g / L, and the selectivity is 97.2%.

Embodiment 3

[0051] (1) 0.5g ruthenium nitrate (Ru content 30%) is dissolved in 100ml glycerol and stirred to obtain ruthenium nitrate mixed solution;

[0052] (2) Add 15 g of extruded 3.0 mm spherical activated alumina carrier into the mixed solution obtained in step (1), and further stir for 0.5 h;

[0053] (3) Stir and heat the mixed solution obtained in (2) to 180°C, and keep it for 0.5h, filter to obtain the catalyst, then wash off chloride ions with deionized water, and obtain 1% Ru / Al after vacuum drying 2 o 3 Catalyst, and keep it sealed.

[0054] Add 3 g of the above catalyst and 50 mL of working solution into a 100 mL autoclave, and react at 55° C. and 0.6 MPa for 1 hour. The hydrogenation efficiency of the reaction is 9.6 g / L, and the selectivity is 93.2%.

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Abstract

The invention discloses a ruthenium catalyst for anthraquinone hydrogenation to prepare hydrogen peroxide, and a preparation method thereof. The catalyst is represented by Ru / Al2O3 or Ru / Al2O3-MOx, wherein M represents Si, Mg or Ti, and the ruthenium content is 0.3-2.0 wt%. The catalyst is prepared through a polyol reduction technology, and is prepared through reduction, washing and vacuum drying.2-vinylanthraquinone hydrogenation activity and selectivity test is carried out under a hydrogen pressure of 0.1-0.7 MPa at a reaction temperature of 40-70 DEG C. The catalyst has the advantages of low cost, simple preparation process, good stability, small generation amount of tetrahydroanthraquinone, and high reaction selectivity, can be widely used in anthraquinone process hydrogenation to prepare hydrogen peroxide, and has excellent economic benefits.

Description

technical field [0001] The invention relates to a ruthenium catalyst used for hydrogenation of anthraquinone to prepare hydrogen peroxide and the preparation thereof, belonging to the fields of industrial catalysts and fine chemicals. Background technique [0002] Hydrogen peroxide is an important inorganic chemical raw material, which is widely used in the synthesis of inorganic and organic intermediates and other chemicals, textiles, medicine, electronics, food and metallurgical industries. The anthraquinone method is currently the most mature and mainstream process for producing hydrogen peroxide. The technological process of the anthraquinone method mainly includes four processes of hydrogenation, oxidation, extraction and post-treatment, among which the hydrogenation process is one of the cores of the whole process. Commercial hydrogenation catalysts use 0.3% Pd / Al 2 o 3 , there are disadvantages such as large investment in catalyst at one time, poor hydrogenation se...

Claims

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Application Information

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IPC IPC(8): B01J23/46C01B15/023
CPCB01J23/002B01J23/462C01B15/023
Inventor 戴云生谢继阳吴美岩安霓虹张梦旭魏建伟沈亚峰
Owner 贵研工业催化剂(云南)有限公司
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