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Method of desorbing zinc of waste catalyst for vinyl acetate synthesis

A waste catalyst and vinyl acetate technology, which is applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of narrow application range, difficult handling, and large amount of washing liquid and other problems, to achieve the effect of easy follow-up treatment, fast heating speed and high desorption rate

Inactive Publication Date: 2007-08-01
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 1. Using hydrochloric acid as a desorbent, there is a washing process in the process, the amount of washing liquid is large and the concentration of zinc is low, which makes it extremely difficult to handle, thus generating a large amount of industrial wastewater;
[0006] 2. Dilute hydrochloric acid is added during the leaching process, and the pH is generally maintained at 4-6. Under this condition, the spent catalyst has been pretreated by microwave and desorbed, and has a certain adsorption capacity, and its iodine adsorption value is 850-950 mg / g, which is suitable for The adsorption performance of zinc ions is excellent, although the ZnCl adsorbed in activated carbon 2 It can be used as an activator for activated carbon regeneration, but the activated carbon produced by this method has heavy metal residues, resulting in a very narrow application range

Method used

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  • Method of desorbing zinc of waste catalyst for vinyl acetate synthesis

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The chemical composition (weight percentage) of raw material spent catalyst: C 80.71%, Zn 8.16%, Fe 0.51%, Si0.15%, Mg 0.007%, Ca 0.015%;

[0029] Weigh 500g of spent catalyst, pretreat it in a microwave oven at 2450MHz, microwave power 850W, control the temperature at 910±10°C for 40min; add 150g of ammonium bicarbonate, 400ml of 18wt% ammonia water and 600ml of water, a total of 1L of desorbent, at room temperature Desorb under normal pressure for 3 hours, wash the filter residue twice and filter, and return the filtered washing liquid to prepare a desorbent; keep the tower temperature at 90-96°C during ammonia distillation, distill ammonia for 2 hours, filter after ammonia distillation, and use the obtained ammonia distillation waste liquid The ammonia gas obtained by absorbing ammonia distillation is returned to prepare a desorbent, and the obtained basic zinc carbonate is precipitated. After washing and filtering, the obtained washing liquid is directly returned to ...

Embodiment 2

[0031] The main chemical composition (weight percentage) of raw material spent catalyst: C 84.55%, Zn 8.7 1%, Fe 0.54%, Si 0.19%, Mg 0.010%, Ca 0.013%;

[0032] Weigh 1000g of spent catalyst, pretreat it in a microwave oven at 2450MHz, microwave power 2.25kW, control the temperature at 950±10°C for 45min; add 582g of ammonium bicarbonate, 1350ml of ammonia with a concentration of 26wt% and 1650ml of water, a total of 3L of desorbent, at room temperature Desorb under normal pressure for 4 hours, wash the filter residue 3 times and filter, and return the filtered washing liquid to prepare a desorbent; keep the temperature at the top of the tower at 90-96°C during the ammonia distillation process, distill ammonia for 3 hours, filter after ammonia distillation, and obtain ammonia distillation waste liquid It is used to absorb the ammonia gas obtained by distilling ammonia and return it to prepare a desorbent. The resulting basic zinc carbonate precipitates. After washing and filter...

Embodiment 3

[0034] The main chemical composition (weight percentage) of raw material spent catalyst: C 87.13%, Zn 8.94%, Fe 0.57%, Si 0.17%, Mg 0.009%, Ca 0.017%.

[0035] Weigh 1000g of spent catalyst, pretreat it in a microwave oven at 2450MHz, power 2.25kW, control the temperature at 990±10°C for 60min, add 920g of ammonium bicarbonate, 2000ml of ammonia with a concentration of 32wt% and 2000ml of water, a total of 4L of desorbent, at room temperature Desorb under pressure for 5 hours, wash the filter residue 5 times and filter, and return the filtered washing liquid to prepare a desorbent. During the ammonia distillation process, keep the tower temperature at 90-96°C, distill ammonia for 4 hours, filter after ammonia distillation, and return the obtained ammonia distillation waste liquid directly to Prepare a desorbent, the obtained basic zinc carbonate precipitates, wash and filter, and the washing liquid is used to absorb the ammonia gas obtained by distilling ammonia and then return...

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Abstract

The invention discloses a synthesizing method of zinc desorbent of waste catalyst through vinyl acetate, which comprises the following steps: adopting waste catalyst as raw material irradiated by microwave under 900-1000 deg.c; desorbing through solution of ammonia and ammonium bicarbonate under normal temperature and pressure for 3-5h; obtaining complex solution of zinc ammonia; evaporating ammonia; sintering; obtaining active zinc oxide; washing desorbed filtered slag and waste active charcoal; returning abluent to allocating course of desorbent.

Description

[0001] (1) Technical field: the present invention relates to a method for desorbing zinc from a waste catalyst used in vinyl acetate synthesis, which belongs to the technical field of metallurgy and chemical industry (2) Technical background [0002] Vinyl acetate is one of the organic chemical raw materials with the largest output in the world. The acetylene synthesis method is mainly used for the production of vinyl acetate. The catalyst used in the synthesis of vinyl acetate by this method is activated carbon loaded with zinc acetate. The synthesis of vinyl acetate by the acetylene method is simple and the catalyst is cheap. The activity is good and the selectivity is good, but the activity of the catalyst decreases rapidly and the life is short, so that a large amount of waste zinc acetate / activated carbon catalysts are produced, which puts great pressure on industrial reproduction and the environment. Therefore, the comprehensive utilization of these waste catalysts has imp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G9/02B01J23/94
CPCY02P20/584
Inventor 彭金辉李雷张泽彪张正勇张世敏张利波郭胜惠
Owner KUNMING UNIV OF SCI & TECH
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