CN112028218A - Device and method for synchronous catalytic oxidation and decoloration of coking desulfurization waste liquid - Google Patents
Device and method for synchronous catalytic oxidation and decoloration of coking desulfurization waste liquid Download PDFInfo
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- CN112028218A CN112028218A CN202010866006.2A CN202010866006A CN112028218A CN 112028218 A CN112028218 A CN 112028218A CN 202010866006 A CN202010866006 A CN 202010866006A CN 112028218 A CN112028218 A CN 112028218A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/74—Treatment of water, waste water, or sewage by oxidation with air
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/18—Nature of the water, waste water, sewage or sludge to be treated from the purification of gaseous effluents
Abstract
The device comprises a device shell, wherein the upper part of the device shell is a columnar area, the lower part of the device shell is a conical area, the columnar area is of a jacket type structure, a heating spiral pipe is arranged in the jacket type structure, a compressed air injection pipeline is arranged at the lower part of the columnar area, a desulfurization waste liquid inlet, a catalyst feeding port and a tail gas outlet are arranged at the upper part of the device shell, a desulfurization waste liquid outlet is arranged on the device shell below the heating spiral pipe, and a solid discharge port is arranged at the bottom of the conical area. The method adopts the catalyst with dual functions of catalysis and decoloration to synchronously realize two processes of thiosulfate oxidation and decoloration in the coking desulfurization waste liquid in one device, replaces the stirring effect of a traditional motor through the spraying or swirling effect of the desulfurization waste liquid and the turbulent effect of compressed air, reduces the consumption of steam or heating medium, and obviously improves the heat utilization rate; the utilization rate of the device is improved, the occupied area is reduced, and continuous production can be realized.
Description
Technical Field
The invention belongs to the field of coal chemical wastewater treatment and resource recycling, and particularly relates to a device and a method for synchronous catalytic oxidation and decoloration of coking desulfurization waste liquid.
Background
The scientific and reasonable treatment or the comprehensive utilization of the coking desulfurization waste liquid is an environmental protection problem which needs to be solved urgently by coking enterprises. At present, most of domestic coking enterprises adopt HPF catalytic wet oxidation method and few coking enterprises adopt tannin extract paint method and other technologies to remove H in coke oven gas2S and HCN, the process has low cost and high desulfurization and decyanation efficiency, but a large amount of desulfurization waste liquid is inevitably generated in the operation process. The desulfurization waste liquid contains a large amount of inorganic secondary salts such as thiocyanate, thiosulfate and sulfate, and organic matters such as phenols and PAHs, the specific secondary salts are related to the desulfurization method and the alkali source thereof, for example, the secondary salts in the desulfurization waste liquid of the HPF method are mainly NH4SCN、(NH4)2S2O3、(NH4)2SO4. According to the report, the traditional treatment mode of desulfurization waste liquid of various coking enterprises is coke quenching or coking coal spraying for re-coking, and the extensive treatment mode not only influences the coke quality and increases the coking energy consumption, but also severely restricts the sustainable development and even the long-term survival of the enterprises under the increasingly strict environment protection policy environment of the country. However, from the aspect of resource recycling, the secondary salt in the desulfurization waste liquid is a potential valuable chemical raw material and a strategic rare earth preparation raw material with great market demands, so that the extraction of the secondary salt is beneficial to fundamentally solving the treatment problem of the desulfurization waste liquid and creating economic benefits, environmental benefits and social benefits for coking enterprises.
At present, a fractional crystallization method is dominant in the research and engineering application of a coking desulfurization waste liquid salt extraction technology, and before fractional crystallization, colored substances and other impurities in the desulfurization waste liquid are removed under the adsorption effect of activated carbon so as to ensure the subsequent extraction of high-quality secondary salt products. Because the solubility of thiocyanate and thiosulfate is similar and the market demand of the latter is smaller, and the solubility of sulfate is different from the solubility of the former two, the separation difficulty of thiocyanate, thiosulfate and sulfate in the desulfurization waste liquid needs to be reduced, and the thiosulfate needs to be converted into sulfate through oxidation before decolorization. However, both the decoloring and the oxidation sections need steam heating and filter pressing operation, so that the problems of low steam utilization rate, repeated filter pressing, complex operation, large floor area, low device utilization rate and the like are caused; meanwhile, the oxidation and decoloration processes need stirring, and the desulfurized waste liquid has strong corrosion and is easy to corrode and the stirring paddle causes frequent maintenance. In addition, the desulfurization waste liquid oxidation section mainly adopts concentrated H2SO4Oxidation which is critical to the equipment material and produces SO or air oxidation2The recovery rate of the secondary salt is reduced, secondary pollution is easily caused, and the oxidation efficiency of the secondary salt is lower.
Disclosure of Invention
The invention provides a device and a method for synchronous catalytic oxidation and decoloration of coking desulfurization waste liquid, and aims to improve or optimize an oxidation and decoloration technology and a device in a salt extraction process of coking desulfurization waste liquid.
In order to achieve the purpose, the invention adopts the following technical scheme:
the utility model provides a synchronous catalytic oxidation of coking desulfurization waste liquid and decoloration device, includes the device shell, the upper portion of device shell is the column district, and the lower part is the toper district, the column district is the jacket formula structure, is equipped with the heating spiral pipe in the jacket formula structure column district lower part is equipped with compressed air and sprays the pipeline the upper portion of device shell is equipped with desulfurization waste liquid import, catalyst and throws with mouth, tail gas outlet be equipped with desulfurization waste liquid outlet on the device shell of heating spiral pipe below the bottom in toper district is equipped with the solid discharge port.
The heating medium introduced into the heating spiral pipe is steam or hot oil.
The upper part of the device shell is also provided with a window, a thermometer, a pH meter and a liquid level meter.
The direction of the desulfurization waste liquid inlet comprises a tangential mode or a radial mode, wherein when the desulfurization waste liquid enters in the tangential mode, the desulfurization waste liquid forms rotational flow by utilizing a columnar structure of the device; the desulfurization waste liquid inlet is provided with a spray head when entering in the radial direction.
The compressed air injection pipeline comprises a compressed air inlet pipe, a compressed air distribution header pipe and compressed air distribution branch pipes, the compressed air inlet pipe is outwards communicated with the compressed air pipeline and inwards communicated with the compressed air distribution header pipe, the compressed air distribution branch pipes are connected above the compressed air distribution header pipe, and compressed air injection outlets are upwards arranged on the compressed air distribution branch pipes.
A synchronous catalytic oxidation and decoloration method for coking desulfurization waste liquid is characterized in that a synchronous catalytic oxidation and decoloration device for coking desulfurization waste liquid is adopted, thiosulfate in the coking desulfurization waste liquid is catalytically oxidized into sulfate and sulfur in an integrated device, colored substances and impurities in the desulfurization waste liquid are removed in an adsorption mode in an oxidation process, and the desulfurization waste liquid is separated from the sulfur and solid such as a waste catalyst by gravity settling, and the specific method comprises the following steps:
1) the catalytic oxidation and decoloration conditions of the coking desulfurization waste liquid are as follows: reacting for 5-8 h at normal pressure and 90-100 ℃ and pH 4-9;
2) the catalyst used for catalytic oxidation is powdered activated carbon loaded with Fe, Mn and Co active components prepared by an impregnation method, a deposition precipitation method and the like, has dual functions of catalysis and decoloration, and has the dosage of 2.5-5 kg of catalyst per m3Desulfurization waste liquid;
3) when the desulfurization waste liquid enters, the desulfurization waste liquid and the added catalyst are stirred and mixed comprehensively through the rotational flow effect or the spraying effect and the turbulent flow effect formed by the compressed air at the lower part.
The conversion rate of the thiosulfate oxidized into the sulfate in the desulfurization waste liquid is 95-98%, and the byproduct sulfur is very little, so that the recovery rate of the secondary salt in the desulfurization waste liquid is improved.
Compared with the prior art, the invention has the beneficial effects that:
1) the method adopts a catalyst with dual functions of catalysis and decoloration to synchronously realize two processes of thiosulfate oxidation and decoloration in the coking desulfurization waste liquid in one device, and simultaneously separates the desulfurization waste liquid from sulfur particles and the waste catalyst through gravity settling effect, thereby reducing filter pressing times and even avoiding the tedious twice filter pressing in the traditional 'oxidation-filter pressing-decoloration-filter pressing';
2) the traditional motor stirring effect is replaced by the spraying or swirling effect of the desulfurization waste liquid and the turbulent effect of compressed air, so that mass transfer and mixing among solid-liquid-gas three phases (catalyst, desulfurization waste liquid and compressed air) are facilitated, and the problem of maintenance caused by corrosion of a stirring paddle in motor stirring is solved;
3) because the two processes of oxidation and decoloration are integrated in one device, the traditional oxidation device and the traditional decoloration device are prevented from being heated independently, so that the consumption of steam or heating medium is reduced, and the heat utilization rate is obviously improved;
4) because the two processes of oxidation and decoloration are integrated in one device, the occupied area of the device is reduced, the construction cost and the operation cost are saved, and meanwhile, the integrated device can realize continuous production.
Drawings
FIG. 1 is a schematic diagram of the integrated device for synchronous catalytic oxidation and decolorization of coking desulfurization waste liquid.
Figure 2 is a top view of the compressed air inlet tube and compressed air distribution tube in the apparatus of the present invention.
In the figure: 1-a device housing; 2-desulfurization waste liquid inlet; 3-a catalyst feeding port; 4-a compressed air inlet pipe; 5-compressed air distribution branch pipes; 6-desulfurization waste liquid outlet; 7-solid discharge; 8-a tail gas outlet; 9-a window; 10-a thermometer; 11-a pH meter; 12-a spray head; 13-heating chamber; 14-heating the spiral tube; 15-a liquid level meter; 16-compressed air distribution manifold.
Detailed Description
The following embodiments are further illustrated by reference to the following specific examples:
as shown in fig. 1 and 2, a device for synchronous catalytic oxidation and decoloration of coking desulfurization waste liquid comprises a device shell 1, the upper portion of the device shell 1 is a column area, the lower portion is a cone area, the column area is of a jacket type structure, a heating spiral pipe 14 is arranged in a heating cavity 13 of the jacket type structure, a compressed air injection pipeline is arranged on the lower portion of the column area, a desulfurization waste liquid inlet 2, a catalyst feeding port 3 and a tail gas outlet 8 are arranged on the upper portion of the device shell 1, a desulfurization waste liquid outlet 6 is arranged on the device shell 1 below the heating spiral pipe 14, and a solid discharge port 7 is arranged at the bottom of the cone area.
The column area mainly realizes the catalytic oxidation and the decoloration of the desulfurization waste liquid, and the cone area mainly realizes the separation of solid precipitates such as sulfur particles, waste catalysts and the like generated after the catalytic oxidation and the decoloration of the desulfurization waste liquid.
The conical zone mainly realizes the solid-liquid separation of the desulfurization waste liquid, the sulfur particles and the waste catalyst through the gravity settling effect, and the subsequent secondary separation can be carried out through a filter press because the separation is only primary separation, the filter press filtrate enters a subsequent working section (usually evaporation concentration), the solid mixture of the sulfur particles and the waste catalyst can recover high-quality sulfur through steam heating and condensation processes, and the catalyst can also be regenerated.
The heating medium introduced into the heating spiral pipe 14 is steam or hot oil.
The upper part of the device shell 1 is also provided with a window 9, a thermometer 10, a pH meter 11 and a liquid level meter 15.
The window 9 is used for observing the material reaction condition in the device, the temperature of the desulfurization waste liquid is monitored by the thermometer 10, the acidity and alkalinity of the desulfurization waste liquid is monitored by the pH meter 11, and the liquid level of the desulfurization waste liquid is observed by the liquid level meter 15.
The direction of the desulfurization waste liquid inlet 2 comprises a tangential mode or a radial mode, wherein the desulfurization waste liquid forms rotational flow by utilizing a columnar structure of the device when entering tangentially; the desulfurization waste liquid inlet 2 is provided with a spray head 12 when entering in the radial direction.
The compressed air injection pipeline comprises a compressed air inlet pipe 4, a compressed air distribution header pipe 16 and compressed air distribution branch pipes 5, the compressed air inlet pipe 4 is communicated with the compressed air pipeline outwards and communicated with the compressed air distribution header pipe 16 inwards, the compressed air distribution branch pipes 5 are connected above the compressed air header pipe 16, and compressed air injection outlets are formed in the compressed air distribution pipes 5 upwards.
The internal compressed air distribution branch pipes 5 are radially distributed, the radial distribution is favorable for fully mixing three phases of the desulfurization waste liquid, the catalyst and the compressed air, and the length of the compressed air distribution header pipe 16 and the number of the compressed air distribution branch pipes 5 can be adjusted according to the inlet direction of the desulfurization waste liquid. When the inlet direction of the desulfurization waste liquid is tangential, the rotational flow stirring effect mainly occurs around the device, and the central area is relatively weak, and at the moment, the length of the distribution pipe main pipe 16 is preferably shortened to enhance the turbulent flow stirring effect of the compressed air. When the inlet direction of the desulfurization waste liquid is radial, the spraying effect mainly occurs in the central area of the device, and the peripheral area is relatively weak, so that the length of the distribution pipe main pipe 16 is preferably prolonged, and the number of the compressed air distribution branch pipes 5 is increased to enhance the turbulent stirring effect of the compressed air.
And valves are arranged on the desulfurization waste liquid inlet 2, the catalyst feeding port 3, the compressed air inlet pipe 4, the desulfurization waste liquid outlet 6, the solid discharge port 7 and the tail gas outlet 8. When the direction of the desulfurization waste liquid inlet 2 is radial, the tail end of the desulfurization waste liquid inlet is provided with the spray nozzle 12 so as to better mix the desulfurization waste liquid with the catalyst added by the catalyst adding port 3, and when the direction of the desulfurization waste liquid inlet 2 is tangential, the spray nozzle 12 is not arranged. The catalyst feeding port 3 is slightly higher than the desulfurization waste liquid inlet 2, and the compressed air distribution branch pipe 5 is higher than the desulfurization waste liquid outlet 6, so as to avoid influencing the effective separation of the desulfurization waste liquid, sulfur particles and the waste catalyst.
A synchronous catalytic oxidation and decoloration method for coking desulfurization waste liquid is characterized in that a synchronous catalytic oxidation and decoloration device for coking desulfurization waste liquid is adopted, thiosulfate in the coking desulfurization waste liquid is catalytically oxidized into sulfate and sulfur in an integrated device, colored substances and impurities in the desulfurization waste liquid are removed in an adsorption mode in an oxidation process, and the desulfurization waste liquid is separated from the sulfur and solid such as a waste catalyst by gravity settling, and the specific method comprises the following steps:
1) the catalytic oxidation and decoloration conditions of the coking desulfurization waste liquid are as follows: reacting for 5-8 h at normal pressure and 90-100 ℃ and pH 4-9;
NH is generated by the thermal decomposition of substances such as ammonium salt and the like in the catalytic oxidation and decoloration processes of the coking desulfurization waste liquid3The tail gas is the main tail gas, the tail gas can enter a condenser through a tail gas discharge port 8 to be liquefied into ammonia water, and the ammonia water can be used for desulfurization in a coal gas desulfurization working section.
2) The catalyst used for catalytic oxidation is powdered activated carbon loaded with Fe, Mn and Co active components prepared by an impregnation method, a deposition precipitation method and the like, has dual functions of catalysis and decoloration, and has the dosage of 2.5-5 kg of catalyst per m3Desulfurization waste liquid;
the powdered activated carbon used as raw material for preparing the catalyst can be commercial powdered coconut shell activated carbon, shell activated carbon (including apricot shell activated carbon, fruit core shell activated carbon, walnut shell activated carbon and the like), wood activated carbon and coal activated carbon.
3) When the desulfurization waste liquid enters, the desulfurization waste liquid and the added catalyst are stirred and mixed comprehensively through the rotational flow effect or the spraying effect and the turbulent flow effect formed by the compressed air at the lower part.
The conversion rate of the thiosulfate oxidized into the sulfate in the desulfurization waste liquid is 95-98%, and the byproduct sulfur is very little, so that the recovery rate of the secondary salt in the desulfurization waste liquid is improved.
Specifically, the synchronous catalytic oxidation and decoloration processes of the coking desulfurization waste liquid are as follows:
1) before the device is started, a desulfurization waste liquid inlet 2, a catalyst feeding port 3 and a tail gas discharge port 8 are opened, a compressed air inlet pipe 4, a desulfurization waste liquid outlet 6 and a solid discharge port 7 are closed, and normal work of a window 9, a temperature 10, a pH meter 11, a liquid level meter 15 and a heating spiral pipe 14 in a heating cavity 13 of the device is ensured.
2) Coking desulfurization waste liquid is sprayed into the device from a desulfurization waste liquid inlet 2 by using a sprayer, and a catalyst (2.5-5 kg of catalyst/m) with dual functions of catalysis and decolorization is added from a catalyst adding port 33Desulfurized waste liquid), compressed air is firstly introduced into the device from a compressed air inlet pipe 4 by utilizing a blower and then distributed in the device through a compressed air distribution header pipe 16 and a compressed air distribution branch pipe 5, so that the desulfurized waste liquid, a catalyst and the compressed air are enabled to pass through the rotational flow or spraying and turbulent flow effectsAnd (4) fully mixing.
3) And comprehensively judging the reaction condition of the desulfurization waste liquid, the catalyst and the compressed air in the device according to the window 9, the thermometer 10, the pH meter 11 and the liquid level meter 15. Especially observing the color change of the desulfurization waste liquid according to a window 9; according to the temperature of the desulfurization waste liquid measured by the thermometer 10, the temperature of a heating medium in a heating spiral tube 14 is properly adjusted, so that the temperature of the desulfurization waste liquid is 90-100 ℃; measuring the pH value of the desulfurization waste liquid in the device according to a pH meter to judge the optimal end point of catalytic oxidation and decolorization reaction of the desulfurization waste liquid (the effect is better when the pH value is about 4); the level change of the material in the apparatus is observed by the liquid level meter 15.
4) After the desulfurization waste liquid reacts in the device for a period of time and the total retention time is maintained at 5-8 hours, opening a desulfurization waste liquid outlet 6 and a sulfur and waste catalyst discharge port 7, and sequentially discharging the desulfurization waste liquid with the catalytic oxidation and decolorization reaching the reaction end point, sulfur particles and waste catalyst solid mixture generated in the catalytic oxidation and decolorization process; meanwhile, the desulfurization waste liquid is continuously sprayed and a catalyst (active carbon) is added, so that the dynamic balance of the inlet and outlet materials is kept, and the continuous production is realized.
It will be understood by those skilled in the art that the foregoing is merely a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included within the scope of the present invention.
Claims (7)
1. The utility model provides a device of synchronous catalytic oxidation of coking desulfurization waste liquid and decoloration, a serial communication port, including the device shell, the upper portion of device shell is the column district, and the lower part is the toper district, the column district is the jacket formula structure, is equipped with the heating spiral pipe in the jacket formula structure column district lower part is equipped with compressed air and sprays the pipeline the upper portion of device shell is equipped with desulfurization waste liquid import, catalyst and throws with throwing mouthful, tail gas outlet be equipped with desulfurization waste liquid outlet on the device shell of heating spiral pipe below the bottom in toper district is equipped with the solid discharge port.
2. The device for synchronously catalytically oxidizing and decoloring a coking desulfurization waste liquid according to claim 1, wherein a heating medium introduced into the heating spiral pipe is steam or hot oil.
3. The device for synchronously catalyzing, oxidizing and decoloring a coking desulfurization waste liquid according to claim 1, wherein a window, a thermometer, a PH meter and a liquid level meter are further arranged at the upper part of the device shell.
4. The device for synchronously catalytically oxidizing and decoloring coking desulfurization waste liquid according to claim 1, wherein the direction of the desulfurization waste liquid inlet comprises a tangential mode or a radial mode, and the desulfurization waste liquid forms rotational flow by utilizing a columnar structure of the device when entering tangentially; the desulfurization waste liquid inlet is provided with a spray head when entering in the radial direction.
5. The device for synchronously catalyzing, oxidizing and decoloring a coking desulfurization waste liquid according to claim 1, wherein the compressed air injection pipeline comprises a compressed air inlet pipe, a compressed air distribution header and a compressed air distribution branch pipe, the compressed air inlet pipe is communicated with the compressed air pipeline outwards and communicated with the compressed air distribution header inwards, the compressed air distribution header is connected with the compressed air distribution branch pipe above, and the compressed air distribution branch pipe is upwards provided with a compressed air injection outlet.
6. A synchronous catalytic oxidation and decoloration method for coking desulfurization waste liquid is characterized in that a synchronous catalytic oxidation and decoloration device for coking desulfurization waste liquid as in any one of claims 1 to 5 is adopted, sulfate and sulfur in the coking desulfurization waste liquid are catalytically oxidized into sulfate and sulfur in an integrated device, colored substances and impurities in the desulfurization waste liquid are removed by adsorption in an oxidation process, and the desulfurization waste liquid is separated from solid by gravity settling, and the specific method comprises the following steps:
1) the catalytic oxidation and decoloration conditions of the coking desulfurization waste liquid are as follows: reacting for 5-8 h at normal pressure and 90-100 ℃ and pH 4-9;
2) the catalyst used for catalytic oxidation is powdered activated carbon loaded with active components of Fe, Mn and Co, and the dosage of the catalyst is 2.5-5 kg of catalyst/m3Desulfurization waste liquid;
3) when the desulfurization waste liquid enters, the desulfurization waste liquid and the added catalyst are stirred and mixed comprehensively through the rotational flow effect or the spraying effect and the turbulent flow effect formed by the compressed air at the lower part.
7. The method for synchronously catalyzing, oxidizing and decoloring coking desulfurization waste liquid according to claim 1, wherein the conversion rate of thiosulfate oxidized into sulfate in the desulfurization waste liquid is 95-98%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112827759A (en) * | 2020-12-30 | 2021-05-25 | 广东新纪源复合材料股份有限公司 | Composite optical pre-coating film and preparation method thereof |
| CN116444022A (en) * | 2023-05-10 | 2023-07-18 | 广东红海湾发电有限公司 | Supercritical water oxidation treatment system for high-salt-content and high-chlorine-content organic wastewater |
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2020
- 2020-08-25 CN CN202010866006.2A patent/CN112028218A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112827759A (en) * | 2020-12-30 | 2021-05-25 | 广东新纪源复合材料股份有限公司 | Composite optical pre-coating film and preparation method thereof |
| CN116444022A (en) * | 2023-05-10 | 2023-07-18 | 广东红海湾发电有限公司 | Supercritical water oxidation treatment system for high-salt-content and high-chlorine-content organic wastewater |
| CN116444022B (en) * | 2023-05-10 | 2023-12-08 | 广东红海湾发电有限公司 | Supercritical water oxidation treatment system for high-salt-content and high-chlorine-content organic wastewater |
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