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Production technique for extracting ammonium thiosulfate and ammonium thiocyanate from desulfurization waste liquor

A technology of ammonium thiosulfate and desulfurization waste liquid, which is applied in the direction of thiosulfate/dithionite/polythionate, thiocyanate, etc., which can solve the problems that the products are difficult to meet the industrial requirements and reduce emissions And environmental pollution, improve the effect of economic benefits

Inactive Publication Date: 2010-10-06
QINGDAO CHUTIAN ENERGY SAVING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

USP5276189 reacts calcium hydroxide with desulfurization waste liquid to produce calcium thiocyanate, but the resulting product is difficult to meet industrial requirements

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take 500ml of desulfurization waste liquid in the HPF desulfurization production process of the coking plant, settle for 12 hours, filter to obtain 1.2g of sulfur, add 2g of activated carbon to the filtrate, heat and stir for 3 hours, filter to remove the activated carbon. Filtrate is added in the 1000ml three-necked flask that has stirrer, thermometer, under 5mmHg pressure, when underpressure distillation to temperature 80 ℃, filter while hot, filter cake oven dry, obtain ammonium thiosulfate 23.1g, content is 98.3%. Continue vacuum distillation until the filtrate is evaporated to dryness, add 400ml of methanol and 50ml of ethylenediamine mixture, reflux for 30 minutes, heat filter, and dry the filter cake to obtain 35.3g of ammonium thiosulfate with a content of 98.1%. The filtrate was pressurized to 7mmHg, and when 250ml of mixed solvent was steamed out by vacuum distillation, the heating was stopped, and the steamed mixed solvent was recovered and recycled, and the f...

Embodiment 2

[0022] Take 500ml of desulfurization waste liquid in the HPF desulfurization production process of the coking plant, settle for 12 hours, filter to obtain 1.1g of sulfur, add 3g of activated clay to the filtrate, heat and stir for 3 hours, filter to remove the activated clay. The filtrate was added in a 1000ml three-necked flask with a stirrer and a thermometer. Under 5mmHg pressure, when the pressure was distilled to a temperature of 80°C, it was filtered while it was hot, and the filter cake was dried to obtain 23.8g of ammonium thiosulfate, with a content of 98.4%. Continue vacuum distillation until the filtrate is evaporated to dryness, add 570ml of ethanol and 30ml of ethylenediamine mixture, reflux for 30 minutes, heat filter, and dry the filter cake to obtain 34.9g of ammonium thiosulfate with a content of 98.2%. The filtrate is pressurized to 7mmHg, and when decompression distillation steams 250ml mixed solvent, stop heating, steams mixed solvent and recycles, and filtr...

Embodiment 3

[0024] Take 500ml of desulfurization waste liquid in the HPF desulfurization production process of the coking plant, settle for 12 hours, filter to obtain 1.1g of sulfur, add 5g of activated clay to the filtrate, heat and stir for 3 hours, filter to remove the activated clay. Filtrate is added in the 1000ml three-necked flask that has stirrer, thermometer, under 5mmHg pressure, when underpressure distillation to temperature 80 ℃, filter while hot, filter cake oven dry, obtain ammonium thiosulfate 24.3g, content is 98.5%. Continue vacuum distillation until the filtrate is evaporated to dryness, add 450ml of acetonitrile and 50ml of ethylenediamine mixture, reflux for 30 minutes, heat filter, and dry the filter cake to obtain 34.9g of ammonium thiosulfate with a content of 98.4%. The filtrate is pressurized to 7mmHg, and when decompression distillation steams 250ml mixed solvent, stop heating, steams mixed solvent and recycles, and filtrate is cooled to room temperature, crystall...

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PUM

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Abstract

The invention discloses a production technique for extracting ammonium thiosulfate and ammonium thiocyanate from a desulfurization waste liquor, which comprises the following steps: settling, filtering, decoloring, concentrating, crystallizing, separating, drying a sulfur-containing waste liquor generated in a desulfurization production process of HPF in a coke-oven plant, and finally, recovering ammonium thiocyanate and ammonium thiosulfate by using a mixed organic solvent. The invention is a production technique for comprehensively treating waste water generated in the prior HPF desulfurization technique, and the mixed organic solvent is used for separating ammonium thiocyanate and ammonium thiosulfate. The invention effectively solves the problem of waste water recovery in the desulfurization process, reduces discharge and environmental pollution of waste water, recovers important chemical raw materials (ammonium thiocyanate and ammonium thiosulfate), and can increase the economic benefit.

Description

technical field [0001] The invention relates to a comprehensive treatment process for HPF desulfurization waste liquid in a coking plant, in particular to a production process for extracting ammonium thiosulfate and ammonium thiocyanate from the desulfurization waste liquid produced in the HPF desulfurization production process of a coking plant. The invention belongs to the technical field of chemical waste liquid treatment. Background technique [0002] Domestic coking plants mostly adopt HPF desulfurization production process. HPF desulfurization process has the advantages of high desulfurization efficiency, low cost and simple operation. However, when the content of the two salts (ammonium thiocyanate and ammonium thiosulfate) in the desulfurization liquid produced in the production process reaches 300g / L, the desulfurization system cannot operate normally, and a part of the desulfurization waste liquid needs to be discharged outside, at a rate of 2 million tons / year Ta...

Claims

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Application Information

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IPC IPC(8): C01B17/64C01C3/20
Inventor 李传碧楚振绪陈平
Owner QINGDAO CHUTIAN ENERGY SAVING TECH
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