A kind of activation regeneration method of CO synthesis dimethyl oxalate deactivation catalyst

A deactivated catalyst, dimethyl oxalate technology, applied in the direction of catalyst regeneration/reactivation, chemical instruments and methods, physical/chemical process catalysts, etc., to achieve the effect of simple process, easy operation, and promotion of clean and efficient utilization

Active Publication Date: 2018-11-27
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The activity of the catalyst sample after activation by this method can only recover to about 85% of that of the fresh catalyst.

Method used

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  • A kind of activation regeneration method of CO synthesis dimethyl oxalate deactivation catalyst
  • A kind of activation regeneration method of CO synthesis dimethyl oxalate deactivation catalyst

Examples

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Effect test

Embodiment 1

[0029] Put 10mL of deactivated catalyst and 20mL of 5mol / L sodium hydroxide solution in a 200mL reactor, and keep it in an oven at 180°C for 5 hours at a constant temperature. After the temperature drops to room temperature, the catalyst is suction-filtered and washed with water until the filtrate pH=7. The deactivated catalyst washed with alkali was soaked in 10 mL of polyethylene glycol solution with a concentration of 2 mol / L for 3 h, and after suction filtration, the catalyst was roasted in a muffle furnace at 600° C. for 4 h. Pack the calcined catalyst into a quartz tube with an inner diameter of 20mm with a heating jacket, control the heating temperature to 150°C, and feed 50mL / min N into the quartz tube through a rotameter. 2 and 50mL / min HCl, after ventilating for 5h, put the catalyst in 10mL of sodium hydroxide solution with a mass fraction of 20% and soak for 2h, suction filter, wash with distilled water until the filtrate pH=7, and then use 10mL of 30% sodium hydroxi...

Embodiment 2

[0031] Put 10mL of deactivated catalyst and 20mL of 4mol / L hexamethylenetetramine solution in a 200mL reactor, and keep it in an oven at 200°C for 6h at a constant temperature. After the temperature drops to room temperature, filter and wash the catalyst with water until the pH of the filtrate=7 . The deactivated catalyst washed with alkali was soaked in 10 mL of glucose solution with a concentration of 4 mol / L for 3 hours, and after suction filtration, the catalyst was roasted in a muffle furnace at 500°C for 6 hours. Pack the calcined catalyst into a quartz tube with an inner diameter of 20mm with a heating jacket, control the heating temperature to 180°C, and feed 30mL / min N into the quartz tube through a rotameter. 2 and 70mL / min HCl, after aeration treatment for 3h, then place the catalyst in a mixed solution of 10mL of 10% mass fraction of sodium hydroxide and sodium bicarbonate and soak for 3h, after soaking, wash the catalyst with distilled water until the filtrate pH=...

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Abstract

The invention discloses an activation and regeneration method of a deactivated catalyst in a process of synthesizing dimethyl oxalate by CO. The activation and regeneration method mainly comprises the following steps: washing the deactivated catalyst with alkali at high temperature and under high pressure and removing organic matters attached on the surface of the catalyst; immersing with a pore-expanding agent solution and roasting at 400 DEG C to 700 DEG C to remove deposited carbon attached on the surface of the catalyst and dredge a blocked pore channel of the catalyst; purging with mixed gas of nitrogen gas and hydrogen chloride to disperse an active Pd material which grow large by agglomeration again; immersing with alkali liquid and fixing the Pd material, which is dispersed again, on a carrier; finally, reducing with the catalyst through two steps including a wet process and a dry process, so as to reduce palladium oxide into palladium. The deactivated catalyst is subjected to activation treatment by the method and the agglomerated and sintered active Pd material is effectively dispersed; the activity of the catalyst can be recovered to be about 96 percent of original activity. The method provided by the invention is simple in process, easy to operate and low in cost, and circulating utilization of a noble metal catalyst is realized.

Description

technical field [0001] The invention provides a method for activating and regenerating a deactivated catalyst for CO coupling synthesis of dimethyl oxalate, belonging to the technical field of deactivated catalyst activation and regeneration. Background technique [0002] The gas-phase catalytic coupling of carbon monoxide to synthesize dimethyl oxalate is an important research topic of carbon-one chemistry. The successful implementation of its technology can change the traditional production mode of ethylene glycol in my country and effectively promote the development of my country's coal-to-ethylene glycol industry. The catalysts currently used in industrial devices all use Pd as the active component. Since the gas-phase catalytic coupling of carbon monoxide to synthesize dimethyl oxalate is a violent exothermic reaction, if the reaction operating conditions are not properly controlled in an industrial device, it is very easy to cause the catalyst bed to overheat. Under h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J38/64B01J38/66B01J38/02B01J38/48B01J38/04B01J23/96C07C67/36C07C69/36
CPCY02P20/584
Inventor 姚元根张鑫潘鹏斌黄园园覃业燕
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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