Preparation method of Pd-Fe/SiO2 hydrogenation catalyst

A technology of hydrogenation catalysts and additives, which is applied in the field of preparation of highly active and stable Pd-Fe/SiO2 hydrogenation catalysts, can solve the problems of poor selectivity, waste of noble metal Pd, and easy corrosion, and achieve enhanced shape-selective catalysis, inhibition of Effects of grain growth and high catalytic stability

Inactive Publication Date: 2016-07-27
WUHAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The carrier of the existing anthraquinone hydrogenation Pd catalyst is mainly γ-Al 2 o 3 , the Pd- content is generally high, and some Pd metal particles are dissolved in the carrier body and cannot play a catalytic role, resulting in a great waste of precious metal Pd; this type of catalyst also has low activity, poor selectivity, easy corrosion, pulverization, Problems such as inactivation and easy shedding of active ingredients

Method used

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  • Preparation method of Pd-Fe/SiO2 hydrogenation catalyst
  • Preparation method of Pd-Fe/SiO2 hydrogenation catalyst
  • Preparation method of Pd-Fe/SiO2 hydrogenation catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] First, 2.3mLTEOS, 1gP123 and 0.1853g (Fe(NO 3 ) 3 ﹒ 9H 2 O) Mix and dissolve in 70 mL of HNO at pH=1 at room temperature with magnetic stirring 3 solution (0.1mol / L), and then transfer this solution to a 100ml hydrothermal kettle for hydrothermal reaction at 110°C for 24h. The resulting precipitate was transferred to a beaker and washed with HNO 3 Adjust the pH of the solution to 3.0-3.5, and after aging for 4 hours at room temperature, the aged precipitate was centrifuged and washed to neutrality at a speed of 6000r / min, then dried overnight at 110°C, and roasted at 500°C for 4h (starting from room temperature, heating Fe-modified SiO was obtained after a rate of 4°C / min) 2 carrier.

[0031] Take the above 1g carrier and use 0.005g PdCl at 60°C 2 (0.3wt%) dissolved in HNO corresponding to saturated water absorption3 Solution (pH=3.5, 3.16×10 -4 mol / L) solution obtained by impregnating with equal volume for 2 h, then impregnating with 4 mL, 0.1 mol / L NaOH soluti...

Embodiment 2

[0034] First, 2.3 mL of LTEOS and 1 g of P123 were mixed and dissolved in 70 mL of HNO at pH=1 at room temperature with magnetic stirring 3 solution (0.1mol / L), and then transfer this solution to a 100ml hydrothermal kettle for hydrothermal reaction at 110°C for 24h. The resulting precipitate was transferred to a beaker and washed with HNO 3 Adjust the pH of the solution to 3.0-3.5, and after aging for 4 hours at room temperature, the aged precipitate was centrifuged and washed to neutrality at a speed of 6000r / min, then dried overnight at 110°C, and roasted at 500°C for 4h (starting from room temperature, heating The carrier was obtained after a rate of 4 °C / min).

[0035] Take the above 1g carrier and use 0.005g PdCl at 60°C 2 (0.3wt%) dissolved in HNO corresponding to saturated water absorption 3 Solution (pH=3.5, 3.16×10 -4 mol / L) of the obtained solution was impregnated in equal volume for 2 h, and then was impregnated with 4 mL of 0.1 mol / L NaOH solution at 60° C. fo...

Embodiment 3

[0038] First, 2.3mLTEOS, 3.3mLTPAOH and 0.1853g (Fe(NO 3 ) 3 ﹒ 9H 2 O) Mix and dissolve in 70 mL of HNO at pH=1 at room temperature with magnetic stirring 3 solution (0.1mol / L), and then transfer the solution to a 100ml hydrothermal kettle for hydrothermal reaction at 170°C for 24h. The resulting precipitate was transferred to a beaker and washed with HNO 3 Adjust the pH of the solution to 3.0-3.5, and after aging for 4 hours at room temperature, the aged precipitate was centrifuged and washed to neutrality at a speed of 6000r / min, then dried overnight at 110°C, and roasted at 500°C for 4h (starting from room temperature, heating The carrier was obtained after a rate of 4 °C / min).

[0039] Take the above 1g carrier and use 0.005g PdCl at 60°C 2 (0.3wt%) dissolved in HNO corresponding to saturated water absorption 3 Solution (pH=3.5, 3.16×10 -4 mol / L) of the obtained solution was impregnated in equal volume for 2 h, and then was impregnated with 4 mL of 0.1 mol / L NaOH s...

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Abstract

The invention provides a preparation method of a Pd-Fe / SiO2 hydrogenation catalyst. The method comprises the following steps that 1, tetraethyl orthosilicate, ferric nitrate and one of P123 or tetrapropyl ammonium hydroxide (TPAOH) are mixed, the mixture is dissolved with a HNO3 solution under magnetic stirring at room temperature, and then a hydrothermal reaction is conducted; 2, obtained precipitates are adjusted to be certain pH with the HNO3 solution and aged at room temperature, centrifugal washing, drying and roasting are sequentially conducted, and a carrier is obtained; 3, the carrier is subjected to equivalent-volume impregnation with a palladium nitrate solution, excessive impregnation is conducted with a NaOH solution, washing, drying and roasting are sequentially conducted, and the efficient loaded-type palladium catalyst is obtained. The preparation method of the Pd-Fe / SiO2 hydrogenation catalyst has the advantages that the preparation conditions are mild, and the Fe-additive is introduced in one step in the process of preparing the carrier precursor through a hydrothermal method; the prepared catalyst has good activity, selectivity and stability to an anthraquinone hydrogenation reaction, and the highest catalytic activity of the catalyst is increased by 143% compared with an industrial catalyst.

Description

technical field [0001] The invention belongs to the field of preparation and application of hydrogenation catalysts, in particular to an anthraquinone method for producing hydrogen 2 o 2 High activity and stability of Pd-Fe / SiO in hydrogenation process 2 Process for the preparation of hydrogenation catalysts. Background technique [0002] h 2 o 2 As a clean chemical product, it is widely used in medicine, papermaking and environmental protection. The anthraquinone method is the most widely used method at home and abroad to produce H 2 o 2 method, accounting for H 2 o 2 More than 95% of the total production, the key step is the hydrogenation reaction of anthraquinone, and the hydrogenation catalyst is the key factor to determine the quality and efficiency of the hydrogenation process. Therefore, the development of high-performance anthraquinone hydrogenation catalysts is of great significance. [0003] The carrier of the existing anthraquinone hydrogenation Pd catal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89C01B15/023
CPCB01J23/8906C01B15/023
Inventor 蔡卫权卓俊琳罗晓雷
Owner WUHAN UNIV OF TECH
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