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A supported Ru-based catalyst supported by molybdenum oxide-zinc oxide-zirconia composite oxide

A composite oxide, carrier-supported technology, applied in metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, catalyst activation/preparation, etc. The products are difficult to separate, and the amount of precious metal Ru is large, so as to achieve uniform loading and activation, improved selectivity and stability, and improved selectivity.

Active Publication Date: 2020-12-29
FUZHOU UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the non-supported RuZn catalyst produced by Asahi Kasei uses a large amount of precious metal Ru, and the manufacturing cost is high. During the reaction, due to particle collisions, it is easy to cause the growth of Ru crystallites, resulting in irreversible deactivation. In addition, the separation of nanoscale catalysts and products is relatively difficult. difficulty
For this reason, most domestic patents use ZrO 2 、Al 2 o 3 , SiO 2 , SBA-15, composite oxide and other carriers to load metal Ru (CN103785477A, ​​CN 100496728C, CN 1978053B, CN 101219391A, CN 1015492925B), aiming at solving the problem that the catalyst and the product are difficult to separate
But the consumption of above-mentioned catalyst supporting precious metal Ru is bigger, is unfavorable for reducing production cost

Method used

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  • A supported Ru-based catalyst supported by molybdenum oxide-zinc oxide-zirconia composite oxide
  • A supported Ru-based catalyst supported by molybdenum oxide-zinc oxide-zirconia composite oxide
  • A supported Ru-based catalyst supported by molybdenum oxide-zinc oxide-zirconia composite oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Preparation of zirconia

[0023] To 125 g 750 mL of ZrOCl 2 ·8H 2 Gradually add 12.5 wt% ammonia water to O aqueous solution until the pH of the solution reaches 10, and stir and reflux at 100 °C for 48 h to obtain a white precipitate, which is washed three times with deionized water and twice with absolute ethanol, and dried at 60 °C 24 h, and then calcined at 800 °C for 5 h to obtain zirconia powder. ZrO 2 Characterization shows: ZrO 2 The specific surface area is 83.7 m 2 / g, the pore volume is 0.38 cm 3 / g -1 , with an average pore diameter of 18.3 nm.

[0024] (2) Preparation of catalyst

[0025] Weigh 4.5 g of the above ZrO 2 Dispersed in 0.029 g (NH 4 ) 6 Mo 7 o 24 ∙4H 2 O and 0.174 g of Zn ( NO 3 ) 2 ∙6H 2O into 10 mL aqueous solution, stirred for 0.5 h, added 10 wt% ammonium bicarbonate solution to adjust the pH to 8, continued to stir for 1 h, and then dried in a drying oven at 100 °C for 2 h, and then dried in a muffle furnace at 300 °C ...

Embodiment 2

[0027] (1) Zirconia same as Example 1

[0028] (1) Preparation of catalyst

[0029] Weigh 4.5 g ZrO 2 Dissolved in 0.029 g (NH 4 ) 6 Mo 7 o 24 ∙4H 2 O and 0.348 g Zn( NO 3 ) 2 ∙6H 2 O into 10 mL aqueous solution, stirred for 0.5 h, added 10 wt% ammonium bicarbonate solution to adjust the pH to 8, continued to stir for 1 h, dried in a drying oven at 100 °C for 2 h, and baked in a muffle furnace at 300 °C 1 h. Weigh 4 g of the above-mentioned carrier and dissolve it in 50 mL of deionized water. Under stirring conditions, dissolve 0.602 g of 20 mL of RuCl 3 ·3H 2 O aqueous solution and 5 wt% NaOH solution were added together to adjust the pH to 9.5, stirred for 3.5 h, and 0.315 g of 10 mL of NaBH was slowly added 4 Aqueous solution, stirred for 1h. The obtained precipitate was centrifuged and washed with deionized water until neutral; the precipitate was vacuum-dried at 80 °C for 24 h.

Embodiment 3

[0031] (1) Zirconia same as Example 1

[0032] (2) Preparation of catalyst

[0033] Weigh 4.5 g ZrO 2 Dissolve in 0.015 g (NH 4 ) 6 Mo 7 o 24 ∙4H 2 O and 0.523 g Zn( NO 3 ) 2 ∙6H 2 In the 10 mL aqueous solution prepared by O, stir for 0.5 h, add 10wt% ammonium bicarbonate solution to adjust the pH to 8, continue stirring for 1 h, then dry in a drying oven at 100 °C for 2 h, and bake in a muffle furnace at 300 °C 1 h. Weigh 4 g of the above-mentioned carrier and dissolve it in 50 mL of deionized water. Under stirring conditions, dissolve 0.602 g of 20 mL of RuCl 3 ·3H 2 O aqueous solution and 5 wt% NaOH solution were added together to adjust the pH to 9.5, stirred for 3.5 h, and 0.315 g of 10 mL of NaBH was slowly added 4 aqueous solution, stirred for 1 h. The obtained precipitate was centrifuged and washed with deionized water until neutral; the precipitate was vacuum-dried at 80 °C for 24 h.

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Abstract

The present invention relates to MoO 3 ‑ZnO‑ZrO 2 Preparation method of supported Ru-based catalyst with composite oxide as carrier, said catalyst consists of active components Ru, MoO 3 ‑ZrO 2 ZnO composite oxide carrier is composed of 2 The carrier is added to the mixed aqueous solution of Mo salt and Zn salt, a precipitant is added, and MoO is obtained after drying and roasting. 3 ‑ZnO‑ZrO 2 carrier, and finally activate the active component Ru through chemical reduction to obtain MoO 3 ‑ZnO‑ZrO 2 Ru-based catalyst as a carrier. The catalyst prepared by the invention has a simple preparation process and a small amount of active component Ru, and has the advantages of higher activity, selectivity, stability and other advantages when used in the selective hydrogenation of benzene to produce cyclohexene.

Description

technical field [0001] The present invention relates to MoO 3 -ZnO-ZrO 2 The invention relates to a supported Ru-based catalyst with a composite oxide as a carrier and a preparation method thereof, belonging to the technical field of catalyst preparation. Background technique [0002] Before the last century, the production of cyclohexene was mainly through methods such as dehydration of cyclohexanol, dehydrohalogenation of halocyclohexane and Brich reduction. Due to the many disadvantages of traditional methods (for example, complex process, high energy consumption, low yield, high cost, large pollution, etc.), the scope of application of cyclohexene is limited. With the development of the synthetic industry, the demand for nylon-6 and nylon-66 is increasing day by day, and it is urgent to explore new processes for the large-scale production of cyclohexene. At present, the process commonly used at home and abroad is a new method of catalytic selective hydrogenation of cy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/652B01J35/10B01J37/03B01J37/02B01J37/16C07C5/11C07C13/20
CPCB01J23/6525B01J23/002B01J37/031B01J37/0207B01J37/16C07C5/11B01J2523/00C07C2601/16B01J35/647B01J2523/27B01J2523/48B01J2523/68C07C13/20
Inventor 詹瑛瑛金凡董森陈崇启周创郭学华刘树俊江莉龙王亚涛
Owner FUZHOU UNIV
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