Treatment method of chromium-containing waste catalyst

A treatment method and catalyst technology, applied in chemical instruments and methods, catalyst activation/preparation, physical/chemical process catalysts, etc., can solve problems such as waste of resources, achieve pollution reduction, waste of resources, high environmental and economic value Effect

Inactive Publication Date: 2017-04-26
SHANDONG HUAAN NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a treatment method for spent chromium-containing catalysts, to solve the problem of treatment and recycling of spent chromium-based catalysts widely used in fluorination reactions, and to solve the problem of waste of resources caused by conventional methods

Method used

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  • Treatment method of chromium-containing waste catalyst

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Experimental program
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Effect test

Embodiment 1

[0017] (1) The industrially deactivated waste catalyst is calcined with oxygen in a rotary furnace to decompose and remove organic materials and carbon. The calcining temperature of the converter is 900°C and the residence time is 2 hours.

[0018] (2) After the solid is cooled to normal temperature after calcination, use a pulverizer to pulverize the remaining larger particles to a size above 100 mesh.

[0019] (3) Mix the powder with 23 wt% hydrochloric acid solution at a mass ratio of 1:10, and stir at a constant temperature of 50°C for 2 hours.

[0020] (4) Filtrate the solution while it is hot, add sodium hydroxide solution to the obtained filtrate to adjust its pH value to 4, and stir thoroughly.

[0021] (5) Use the mixture of aluminum oxide and activated carbon as the carrier to impregnate and impregnate for 6 hours.

[0022] (6) Filter the above solution to obtain a filter residue that is washed several times with deionized water, then dried, and pressed into tablets...

Embodiment 2

[0027] (1) The industrially deactivated waste catalyst is calcined with oxygen in a rotary furnace to decompose and remove organic materials and carbon. The calcining temperature of the converter is 800°C and the residence time is 8 hours.

[0028] (2) After the solid is cooled to normal temperature after calcination, use a pulverizer to pulverize the remaining larger particles to a size above 100 mesh.

[0029] (3) The powder was mixed with 23 wt% mass concentration hydrochloric acid solution at a mass ratio of 1:10, and stirred at a constant temperature of 40°C for 2 hours.

[0030] (4) Filtrate the solution while it is hot, add sodium hydroxide solution to the obtained filtrate to adjust its pH value to 4, and stir thoroughly.

[0031] (5) Use the mixture of aluminum oxide and activated carbon as the carrier for impregnation and adsorption for 6 hours.

[0032] (6) Filter the above solution to obtain a filter residue that is washed several times with deionized water, then ...

Embodiment 3

[0037] (1) The industrially deactivated spent catalyst is calcined with oxygen in a rotary furnace to decompose and remove organic materials and carbon. The calcining temperature of the converter is 500°C and the residence time is 5 hours.

[0038] (2) After the solid is cooled to normal temperature after calcination, use a pulverizer to pulverize the remaining larger particles to a size above 100 mesh.

[0039] (3) The powder was mixed with 23 wt% mass concentration hydrochloric acid solution at a mass ratio of 1:6, and stirred at a constant temperature of 30° C. for 3 hours.

[0040] (4) Filtrate the solution while it is hot, add sodium hydroxide solution to the obtained filtrate to adjust its pH value to 3, and fully stir.

[0041] (5) Use the mixture of aluminum oxide and activated carbon as the carrier for impregnation and adsorption for 6 hours.

[0042] (6) Filter the above solution to obtain a filter residue that is washed several times with deionized water, then drie...

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Abstract

The invention relates to a treatment method of a chromium-containing waste catalyst. The treatment method comprises the steps that oxygen-enriched calcination is conducted on the waste chromium-based fluorination catalyst, so that organic matter materials and carbon are decomposed and removed, a calcination product is cooled and then ground to be powder until the particle size of the powder is 100 mesh or above, excessive acid liquid is added according to the mass ratio of 1:(1-10), stirring is conducted, filtration is conducted while the liquid is hot, alkali liquid is added into the obtained filtrate and fully stirred to regulate the PH value of the filtrate, a catalyst carrier is taken as a carrier for soaking and adsorbing, separation is conducted after full mixing is conducted, the obtained insoluble substance is washed with deionized water multiple times and then subjected to drying and tabletting or extrusion moulding, and a target precursor is obtained; the target precursor is activated with anhydrous hydrogen fluoride, and a fluorination catalyst is obtained. According to the treatment method, the waste catalyst is treated and then used for preparing the original catalyst, the product hydrates chromium oxide at high purity, the waste materials are changed into things of value, the product can be directly sold, harmful substances are controlled in the whole process, pollution of chromium in the waste catalyst to the environment is reduced, and on the other hand, the catalyst using cost in production is reduced.

Description

technical field [0001] The invention relates to a treatment method for chromium-containing waste catalyst. Background technique [0002] Metal catalysts are widely used in various fluorination reactions, among which chromium-based fluorination catalysts are more typical metal catalysts. During the reaction process, its activity gradually decreased with the prolongation of use time. Part of the deactivation is due to coking of the catalyst due to carbon deposition on the surface. The catalyst can be reactivated or regenerated by contacting it with air and hydrogen fluoride; or by contacting the catalyst with air mixed with an inert gas such as nitrogen or a mixture thereof to burn off the carbon. However, these methods can only reactivate the catalyst in a short period of time, and finally the catalyst is deactivated so that it can no longer be used and becomes a spent catalyst. Such catalysts are usually sent to landfills or sent to hazardous waste treatment plants for di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/132B01J27/32B01J37/02B01J37/08C01G37/02
CPCY02P20/584B01J37/08B01J27/132B01J27/32B01J37/0009B01J37/0036B01J37/0201C01G37/02
Inventor 段琦王瑞英徐甲超王通周浩
Owner SHANDONG HUAAN NEW MATERIAL
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