Resource process method for coking sulfur-containing waste water

A treatment method and resource-based technology, applied in the field of resource-based treatment of sulfur-containing wastewater from membrane coking, can solve the problems of long removal time of insoluble matter, high content of mother liquor, and low separation efficiency, and achieve remarkable membrane separation effect and excellent operating conditions Easy to control, good separation effect

Active Publication Date: 2008-11-19
NANJING UNIV OF TECH
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Problems solved by technology

Patent CN101012065A provides a method for separating and recovering three kinds of ammonium salts from coke oven gas desulfurization and decyanation wastewater, but the method is cumbersome to operate, the separation efficiency is not high, and the yields of ammonium thiocyanate and ammonium thiosulfate are not high less than 50%, the resource recovery efficiency is low, and the treatment of elemental sulfur solids in coking sulfur-containing wastewater is not considered
It is worth mentioning that the treatment method of sulfur-containing wastewater provided by the patent CN1955120 uses membrane separation technology to successfully separate elemental sulfur and secondary salts. The requirements for conveying equipment and pipelines are relatively high. The latter consumes a lot of energy and is prone to generate sulfur foam to cause tower blockage, making continuous operation difficult; the salts ammonium thiocyanate and ammonium thiosulfate in the saline clear liquid are directly Evaporation and crystallization, the salt purity

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  • Resource process method for coking sulfur-containing waste water

Examples

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Example Embodiment

[0028] Example 1:

[0029] The SS of coking sulfur-containing wastewater is 1.6g·L -1 , use 0.8μm zirconia ceramic membrane pretreatment, control operating conditions, temperature 50 ℃, pressure 0.1MPa, membrane surface velocity 3m s -1 , the stable flux is maintained at 1600L m -2 h -1, the permeate liquid does not contain elemental sulfur, and the concentration factor is increased to 80 times. The concentrated elemental sulfur is washed three times and then centrifuged to obtain elemental sulfur with a particle size of 0.1-5 μm; the water washing liquid and the ceramic membrane microfiltration permeate enter together The membrane material is cellulose acetate nanofiltration membrane device for salt separation, the concentration of ammonium thiosulfate is 72.09g L -1 , ammonium thiocyanate concentration 109.05g L -1 , the control pressure is 2.5MPa, the temperature is 48°C, and the permeate volume is 60L·m -2 h -1 , the interception rate of ammonium thiosulfate is 95.6%...

Example Embodiment

[0030] Example 2:

[0031] The SS of coking sulfur-containing wastewater is 20g·L -1 , using 0.22μm organic polymer membrane for pretreatment, the membrane material is polyvinylidene fluoride, the operating conditions are controlled, the temperature is 30°C, the pressure is 0.3MPa, and the membrane surface flow rate is 4m s -1 , the stable flux is maintained at 2000L m -2 h -1 , the permeate supernatant does not contain elemental sulfur, the concentration factor is increased to 50 times, the concentrated elemental sulfur is washed with water three times and then centrifuged, and further purified with chloroform to obtain elemental sulfur with a particle size of 0.5-5 μm. Enter the nanofiltration device for salt separation, the nanofiltration membrane material is polypiperazine amide, and the concentration of ammonium thiosulfate at this time is 68.43g L -1 , ammonium thiocyanate concentration 106.96g L -1 , control pressure 2.0MPa, temperature 30°C, flow rate 650L m -2 h ...

Example Embodiment

[0032] Example 3:

[0033] The SS of coking sulfur-containing wastewater is 34g·L -1 , using 0.02μm stainless steel metal membrane for concentration treatment, controlled operating conditions, temperature 20°C, pressure 0.05MPa, membrane surface velocity 5m s -1 , the stable flux is maintained at 120L m -2 h -1 , use chloroform, dissolve and saturate, adjust the temperature to precipitate elemental sulfur in the water phase, the particle size is 0.1 ~ 5μm, after the washing liquid is centrifuged, it enters the nanofiltration device together with the permeate for salt separation, and the nanofiltration membrane material is alumina, thiosulfuric acid Ammonium concentration 75.51g·L -1 , ammonium thiocyanate concentration 109.78g L -1 , control pressure 1.0MPa, temperature 48°C, flow 600L m -2 h -1 , permeate volume 15L m -2 h -1 , the interception rate of ammonium thiosulfate is 97.5%, the concentration of ammonium thiosulfate in the concentrated solution is gradually in...

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Abstract

The invention relates to a method for resourceful treatment of coking sulfur-containing wastewater. The coking sulfur-containing wastewater is added into a microfiltration or ultrafiltration membrane separator, solid elemental sulfur contained in the wastewater is entrapped and condensed, and is subject to the washing purification to produce pure sulfur; penetrating fluid is led into a nanofiltration membrane separator, ammonium thiosulfate is entrapped and condensed, and is extracted to produce the ammonium thiosulfate; then the penetrating fluid is led into a reverse osmosis membrane separator, ammonium thiocyanate is trapped and condensed, and is extracted to produce the ammonium thiocyanate, wherein, the penetrating fluid is purified water and can be returned to the working section for repeated use. The method can separate and purify valuable sulfur and secondary salt in the coking sulfur-containing wastewater to create certain economic value, can also improve the circulating utilization rate of industrial water to realize zero draining of wastewater and achieve the requirement of cyclic economy, and is suitable for treating the coking sulfur-containing wastewater of desulfurization and decyanization processes using a HPF method of various coking gas.

Description

technical field [0001] The present invention relates to a resource treatment method of coking sulfur-containing wastewater by membrane method, in particular to the separation and recovery of elemental sulfur, the purification of two salts of ammonium thiosulfate and ammonium thiocyanate from coke oven gas HPF desulfurization and decyanation process wastewater, and Implement the method of recycling purified water. Background technique [0002] The coking plant is an important part of the iron and steel enterprises. It mainly produces metallurgical coke for blast furnace ironmaking, and also recovers ammonia, benzene and other chemical products from coke oven gas. Its water supply and drainage is an important link to ensure production, but the discharged wastewater contains a large amount of organic and inorganic substances. Due to the influence of various factors such as the nature of raw coal, coking temperature, coking product recovery process, etc., its composition is com...

Claims

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Application Information

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IPC IPC(8): C02F9/02C02F1/44C01B17/027C01B17/64C01C3/20C02F103/16
Inventor 邢卫红殷娜徐南平
Owner NANJING UNIV OF TECH
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