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Catalyst for use in preparation of hydrogen peroxide by anthraquinone method and preparation method thereof

A technology of hydrogen peroxide and catalyst, which is applied in the field of palladium-loaded catalyst for the production of hydrogen peroxide by anthraquinone method and its preparation field, which can solve the problems of large particle size of catalyst active components, loss of metal active components, decline of catalyst activity, etc., and achieve Effects of improving electronic properties and geometric properties, increasing catalyst life, and increasing reaction activity

Active Publication Date: 2011-02-09
浙江泰德新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The particle size of the catalyst active component prepared by this method is large, and it is not easy to control, and the catalytic activity is general
In addition, due to the loss of metal active components during use, the catalyst activity continues to decline

Method used

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  • Catalyst for use in preparation of hydrogen peroxide by anthraquinone method and preparation method thereof
  • Catalyst for use in preparation of hydrogen peroxide by anthraquinone method and preparation method thereof
  • Catalyst for use in preparation of hydrogen peroxide by anthraquinone method and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Pipette 12.0mL concentration to be the Pd(Ac) of 0.0178mol / L 2 The solution was placed in a 250mL three-necked flask, and 80mL of aqueous ethanol (V 乙醇 :V 水 =1) For dilution, add 0.36 g of stabilizer PVP according to the molar ratio PVP:Pd=15:1 (PVP is calculated as monomer). Heating to 85° C. in a water bath, and refluxing for 2-3 hours under magnetic stirring to obtain a brown palladium sol, and adjusting the pH of the palladium colloid solution to 7 with ammonia water (5%) for later use. (the palladium nanoparticle average particle size that this method prepares is 10nm, the electron micrograph of gained palladium nanoparticle sees figure 1 .

[0027] After mixing 2.0 g of pseudo-boehmite and 20 mL of deionized water, heat to 85° C. under stirring to form pseudo-boehmite slurry.

[0028] According to the proportions of different mass ratios in Table 1, the metal palladium sol was added dropwise to the pseudo-boehmite slurry according to the formula ratio under st...

Embodiment 2

[0034] The preparation of metal palladium sol is the same as in the examples.

[0035] After mixing 2.0 g of pseudo-boehmite and 20 mL of deionized water, heat to 85° C. under stirring to form pseudo-boehmite slurry. Under stirring, metal palladium sol and lanthanum nitrate solution with a concentration of 9.2mmol / L were mixed and added dropwise to the pseudo-boehmite slurry (see the table below for the ratio of palladium, lanthanum oxide, and pseudo-boehmite), and the stirring reaction 4 Hour. Remove the solvent by rotary evaporation, dry the solid at 120°C, grind it, and bake it at 450°C for 4 hours to obtain a series of Pt-La / γ-Al 2 o 3 Catalyst, and carry out ICP elemental analysis to a series of catalysts, analyze the mass percentage content of palladium and dilanthanum trioxide in the catalyst.

[0036] m (palladium): m (lanthanum nitrate): m (pseudoboehmite)

[0037] Get 0.5g gained catalyst (Pd content 0.7%, La 2 o 3 content 1.5%), after mixing with 1g t...

Embodiment 3

[0039] The PVP in Example 1 was replaced with PVA, and the metal palladium sol was prepared according to the molar ratio PVA:Pd=30:1 (PVA is calculated as monomer), and the preparation method was as in Example 1. The palladium nanoparticles prepared by the method have an average diameter of 8nm. Use ammonia water (5%) to adjust the pH of the palladium colloid solution to 7 before use.

[0040] After mixing 2.0 g of pseudo-boehmite and 20 mL of deionized water, heat to 85° C. under stirring to form pseudo-boehmite slurry. Under stirring, metal palladium sol was mixed with lanthanum nitrate and cerium nitrate solutions with a concentration of 9.2mmol / L, and then added dropwise to the pseudo-boehmite slurry (see below for the ratio of palladium, rare earth metal oxides, and pseudo-boehmite) Table), stirred reaction 4 hours. Remove the solvent by rotary evaporation, dry the solid at 120°C, grind it, and bake it at 450°C for 4 hours to obtain a series of Pt-LaCe / γ-Al 2 o 3 Cata...

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Abstract

The invention belongs to the field of load catalysts, in particular relates to a palladium load catalyst for use in preparation of hydrogen peroxide by an anthraquinone method and a preparation method thereof. The method comprises the following steps of: (1) preparing metal palladium sol from palladium acetate serving as a raw material and mixed solution of ethanol and water serving as solvent in the presence of a stabilizing agent; and (2) preparing serous fluid of pseudo-boehmite, dripping solution containing the metal palladium sol obtained by the step (1) and rare-earth metal nitrate into the serous fluid of the pseudo-boehmite, stirring, reacting at the temperature of between 60 and 100 DEG C for 2 to 6 hours, removing the solvent through rotary evaporation, drying, grinding and roasting to obtain a load palladium catalyst serving aluminum oxide as a carrier. The catalyst has the advantages of low load capacity of noble metals, uniform size distribution of active ingredients, high catalytic activity and the like. In addition, polymer is decomposed into porous carbon and distributed on interfaces of the catalyst carrier and metal active particles, so the catalyst has excellent stability and long service period.

Description

technical field [0001] The invention belongs to the field of supported catalysts, and in particular relates to a palladium-supported catalyst used for the anthraquinone method to prepare hydrogen peroxide and a preparation method thereof. Background technique [0002] Hydrogen peroxide is an important chemical product, which is widely used in papermaking, chemical industry, food, environmental protection and other fields. Many valuable chemical products can be prepared from hydrogen peroxide, such as inorganic peroxyacids and their salts, epoxides, organic peroxides, and meaningful chemical reaction intermediates. As a weak oxidizing agent, hydrogen peroxide has much higher selectivity than other oxidizing agents in organic synthesis. Hydrogen peroxide is used as a bleaching agent in the textile industry and papermaking industry, as an oxidizing agent in chemical synthesis, as a disinfectant and bactericide in the food and pharmaceutical industries, and can be used to treat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B15/023B01J23/44B01J37/00
Inventor 杨平李青董玉培杜玉扣
Owner 浙江泰德新材料有限公司
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