CN114349091A - Pyrolysis treatment process for desulfurization waste liquid - Google Patents
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Abstract
The invention discloses a desulfurization waste liquid pyrolysis treatment process, which is characterized in that desulfurization waste liquid is concentrated firstly, then high-temperature superheated steam is used as a heat source to carry out pyrolysis conversion on the desulfurization waste liquid, converted tail gas is washed by condensate obtained by evaporation of desulfurization liquid or ammonia water obtained by ammonia distillation and then is merged into a VOC (volatile organic compound) collection system, and liquid generated in the washing process enters a foam tank or a regeneration tower to be used as desulfurization liquid of coal gas after sulfur is recovered. The process is simple, flexible in operation and free of secondary pollution, has outstanding advantages in investment, operation cost, generation and treatment of secondary pollution and treatment effect compared with the prior art, and has important significance in effective treatment of the desulfurization waste liquid.
Description
Technical Field
The invention relates to a pyrolysis treatment process of desulfurization waste liquid, in particular to wet oxidation and H removal by an ammonia method for coal gas2And (3) a treatment process of the desulfurization waste liquid generated in the S process.
Background
The desulfurization waste liquid is a pollutant with great harm generated in the coal gas wet desulfurization process, contains a mixture of various toxic substances, and is listed in national hazardous waste records. Is the key point of environmental protection supervision, so how to effectively treat the desulfurization waste liquid is a difficult problem to be solved urgently by all enterprises adopting a wet oxidation desulfurization process.
At present, the treatment process of the desulfurization waste liquid is mainly divided into three processes, namely a salt extraction process represented by salt extraction, a conversion process represented by acid preparation, and a pyrolysis process represented by coal blending and coking.
The salt extraction method mainly adopts a certain technical means to effectively extract ammonium thiosulfate and ammonium thiocyanate from the desulfurization waste liquid, thereby achieving the dual purposes of saving resources and protecting the environment. At present, two methods are widely adopted in enterprises, namely an evaporative crystallization method and a fractional crystallization method. The evaporative crystallization method is to extract mixed ammonium salt from the desulfurization waste liquid by an evaporative crystallization method, and then return condensate obtained by evaporation to a desulfurization system to achieve the purpose of treating the desulfurization waste liquid. Due to the fact that the mixed ammonium salt is high in toxicity and the market capacity of ammonium thiocyanate, ammonium thiosulfate and the like is limited, the mixed salt does not have a market, and disposal and utilization of the mixed salt are a new problem to be solved. The fractional crystallization method is to recover ammonium thiocyanate and ammonium thiosulfate from the desulfurization waste liquid by using a fractional crystallization method by using a ternary phase diagram theory. In some processes, an acidification and oxidation step is added before decolorization, ammonium thiosulfate in the desulfurization waste liquid is decomposed and oxidized, the desulfurization waste liquid is changed into a two-component solution only containing ammonium thiocyanate and ammonium sulfate from the original three components, and then the ammonium thiocyanate and the ammonium sulfate are extracted from the desulfurization waste liquid through fractional crystallization. The optimization of the process realizes the purpose of extracting high-purity ammonium thiocyanate and ammonium sulfate from the desulfurization waste liquid. However, ammonium thiocyanate obtained from the desulfurization waste liquid cannot be sold due to the problem of the market capacity of the ammonium thiocyanate. Meanwhile, the process also has the problems of large investment, high operating cost, secondary pollution and the like.
The first process in the conversion process is the acid making process. Because coking sulfur also has the problem of difficult sale, enterprises adopt the process of preparing acid from the desulfurization waste liquid to treat the desulfurization waste liquid and the sulfur, the process is to concentrate (or dry) the desulfurization waste liquid containing the sulfur, ammonium thiocyanate and ammonium thiosulfate and then burn and decompose the desulfurization waste liquid and combustion-supporting gas in a combustion furnace, and SO in the waste gas is decomposed by burning2By oxidation to SO3Then absorbing SO with 95% sulfuric acid3And generating 98% concentrated sulfuric acid, and sending the concentrated sulfuric acid to an ammonium sulfate workshop section to be used as a raw material for producing ammonium sulfate.
The process technology can effectively treat the desulfurization waste liquid and obtain the product sulfuric acid at the same time, can be used as raw material supply of an ammonium sulfate working section, and has the greatest advantage of simultaneously treating two main pollutants of the desulfurization waste liquid and sulfur mud. However, the process flow is complex, so that the problems of large investment, complex operation, high running cost and the like exist. In the case of the current sulfuric acid market depression, the large application of the technology will inevitably aggravate the sulfuric acid market excess. Meanwhile, the dilute sulfuric acid generated by adopting the technology and the tail gas generated in the incineration process are newly increased environmental protection problems.
The second process of the conversion method is to convert the desulfurization waste liquid into ammonium sulfate, and the method oxidizes ammonium salt and sulfur in the desulfurization waste liquid into ammonium sulfate in an oxidation tower under the conditions of temperature of 273-275 ℃ and pressure of 7000-7500 kPa, and then sends the ammonium sulfate into an ammonium sulfate section for producing the ammonium sulfate. The main problems of the method are high requirement on equipment, large investment, high energy consumption for treating waste liquid and the like, so that the use of the method is limited to a certain extent.
Some sub-enterprises adopt a coal blending coking method to treat the desulfurization waste liquid, and the method mixes the waste liquid into coal as a furnace for coking treatmentAmmonium salt in the desulfurization waste liquid is heated and decomposed in a coke oven, and the final product NH3、H2S、CO 2And N2Enters a subsequent coal-based purification system along with the raw gas, wherein only a small amount of H is contained2The S and the coke react chemically, so that the aim of treating the desulfurization waste liquid is fulfilled. The method is widely adopted by coking enterprises once, some enterprises try to optimize and improve the method by means of uniform spraying, mixing by a mixer, spraying into a coal charging tower and the like, but the final treatment method of the method is the same as that of direct pouring in a coal plant, and is basically the same as that of direct pouring in the coal plant. The method has the problems of influencing moisture of coal as fired, influencing coke quality, causing poor working environment of workers and the like. Particularly, with the comprehensive implementation of the existing large coal yard closed engineering, the defect of the method for treating the desulfurization waste liquid is further shown, and enterprises give up the method for treating the desulfurization waste liquid.
As a result, it has been found that (NH) is the main salt in the desulfurization waste liquid generated in the wet oxidation desulfurization by the ammonia process4)2S2O3，NH4SCN and (NH)4)2SO4However, the salt has poor thermal stability, and an economical and effective desulfurization waste liquid treatment method does not exist at present.
Disclosure of Invention
In order to solve the problems, the invention provides a pyrolysis treatment process of desulfurization waste liquid, which can effectively solve the problems of large investment, high operation cost, serious secondary pollution and the like of the conventional treatment process.
The invention aims at the characteristics of poor thermal stability of pollutants in the ammonia desulphurization waste liquid, and the like, the desulphurization waste liquid is firstly concentrated, then high-temperature superheated steam is used as a heat source to carry out pyrolysis conversion on the desulphurization waste liquid, the converted tail gas is subjected to washing treatment by condensate obtained by evaporating desulphurization liquid or ammonia water obtained by evaporating ammonia and then is merged into a VOC (volatile organic compound) collection system, and liquid generated in the washing process enters a foam tank or a regeneration tower to be used as the desulphurization liquid of coal gas after sulfur is recovered. The process is simple, flexible in operation and free of secondary pollution, and has outstanding advantages in investment, operation cost, secondary pollution generation and treatment effect compared with the prior art.
The invention provides a pyrolysis treatment process of desulfurization waste liquid, which comprises the following steps:
(1) the desulfurization waste liquid is firstly evaporated and concentrated in a concentration kettle or an evaporator, 0.2-0.5MPa saturated steam or tail gas waste heat generated by pyrolysis of the desulfurization waste liquid is used as a heat source in the evaporation process, the salt content in the concentrated liquid after concentration is controlled to be 400-doped 600g/L, and condensate generated in the concentration process is supplemented into a washing tower to be used for washing and purifying the tail gas. In order to improve the evaporation efficiency, the concentration process is carried out under the vacuum condition, and the vacuum degree is 0.05-0.09 MPa.
(2) Spraying the concentrated desulfurization waste liquid into a pyrolysis furnace in a form of mist or liquid drops for pyrolysis, wherein the mass ratio of superheated steam to the desulfurization waste liquid is 0.5-1 in the pyrolysis process, the superheated steam with the temperature of 500-; the superheated steam takes 0.2-0.5MPa saturated steam of enterprises as raw materials, the steam superheating pipe preheats the steam to 400 ℃ plus materials, then the steam is introduced into a steam heating furnace, and the steam is superheated to 800 ℃ plus materials by coal gas, electric heating or enterprise waste heat and then introduced into a pyrolysis furnace.
(3) Gas generated after pyrolysis of the desulfurization waste liquid in the pyrolyzing furnace is primarily cooled through the steam superheater, cooled gas is introduced into the evaporator or the concentration kettle in the step (1) to be cooled again, and heat supply in the concentration process of the desulfurization waste liquid is realized. And (2) introducing a water mixture discharged from the evaporator or the concentration kettle into the middle lower part of the washing tower, wherein the washing tower is in the form of an air spray tower or a packed tower, washing liquid used in the washing process is condensate obtained by evaporating and concentrating desulfurization waste liquid, the washing liquid is extracted from the middle lower part of the washing tower by a pump for recycling, part of liquid is periodically extracted from the bottom of the washing tower and is injected into a regeneration tower or a foam tank of a desulfurization working section, and tail gas at the top of the washing tower is introduced into a VOC tail gas purification system of an enterprise desulfurization working section.
The invention has the beneficial effects that:
the invention provides a pyrolysis treatment process of desulfurization waste liquid, which takes superheated steam as a heat source and produces the desulfurization waste liquid after pyrolysisNH of (2)3、H2S、CO 2And N2The tail gas after washing enters a VOC tail gas collecting system for further treatment and then is discharged after reaching standards, and the liquid generated in the washing process enters a foam tank or a regeneration tower for sulfur recovery and then is used as the desulfurization liquid of the coal gas. The process is simple, flexible in operation and free of secondary pollution, has outstanding advantages in investment, operation cost, generation and treatment of secondary pollution and treatment effect compared with the prior art, and has important significance in effective treatment of the desulfurization waste liquid.
Drawings
FIG. 1 is a diagram of a pyrolysis treatment process of a desulfurized waste liquid.
Detailed Description
The present invention is further illustrated by, but is not limited to, the following examples.
With reference to fig. 1, the pyrolysis treatment process of the desulfurization waste liquid provided by the invention comprises the following steps:
(1) the desulfurization waste liquid is firstly evaporated and concentrated in a concentration kettle or an evaporator, 0.2-0.5MPa saturated steam or the waste heat of tail gas generated by pyrolysis of the desulfurization waste liquid is used as a heat source in the evaporation process, the salt content in the concentrated liquid after concentration is controlled to be 400-600g/L, and condensate generated in the concentration process is supplemented into a washing tower for washing and purifying the tail gas. In order to improve the evaporation efficiency, the concentration process is carried out under the vacuum condition, and the vacuum degree is 0.05-0.09 MPa.
(2) Spraying the concentrated desulfurization waste liquid into a pyrolysis furnace in a form of mist or liquid drops for pyrolysis, wherein the mass ratio of superheated steam to the desulfurization waste liquid in the pyrolysis process is 0.5-1, the superheated steam with the temperature of 500-; the superheated steam takes 0.2-0.5MPa saturated steam of enterprises as raw materials, the steam superheating pipe preheats the steam to 400 ℃ plus materials, then the steam is introduced into a steam heating furnace, and the steam is superheated to 800 ℃ plus materials by coal gas, electric heating or enterprise waste heat and then introduced into a pyrolysis furnace.
(3) The gas of the production of desulfurization waste liquid after the pyrolysis of pyrolysis furnace carries out primary cooling through the steam superheater earlier, and the gas after the cooling lets in the evaporimeter or the concentrated cauldron of step (1) and cools off once more, realizes the heat supply of the concentrated process of desulfurization waste liquid simultaneously. And (2) introducing a water mixture discharged from the evaporator or the concentration kettle into the middle lower part of the washing tower, wherein the washing tower is in the form of an air spray tower or a packed tower, washing liquid used in the washing process is condensate obtained by evaporating and concentrating desulfurization waste liquid, the washing liquid is extracted from the middle lower part of the washing tower by a pump for recycling, part of liquid is periodically extracted from the bottom of the washing tower and is injected into a regeneration tower or a foam tank of a desulfurization working section, and tail gas at the top of the washing tower is introduced into a VOC tail gas purification system of an enterprise desulfurization working section.
The process flow of the invention is illustrated by the following specific examples:
example 1:
the salt content collected from the gas desulfurization section of a certain coking enterprise is 256g/L (NH)4SCN 162g/L，(NH4)2S2O3 74g/L,(NH4)2SO4 20 g/L) of the desulfurization waste liquid, concentrating 100L of the desulfurization waste liquid in an evaporation kettle, generating 56L of condensate liquid in the concentration process, increasing the salt content in the concentrated liquid to 581g/L, spraying the concentrated liquid into a pyrolysis furnace through an ejector within one hour, introducing superheated steam with the temperature of 760 ℃ and the flow of 60Kg/h into the pyrolysis furnace from the bottom, directly exchanging heat between the superheated steam and the sprayed desulfurization waste liquid, discharging a gaseous mixture formed by pyrolysis of the desulfurization waste liquid from the top of the pyrolysis furnace, sequentially passing through a steam preheater, the evaporation kettle and a washing tower in the discharging process, and circularly washing the condensate liquid generated in the evaporation process in the washing tower. 0.2MPa saturated steam is preheated to 350 ℃ through a steam preheater, then enters a steam heating furnace to be heated to 760 ℃ and enters from the bottom of a pyrolysis furnace. Finally, the washing liquid in the washing tower is filtered and analyzed, 7.6kg of elemental sulfur and NH in the liquid are generated in the filtering process4SCN 10.13g/L，(NH4)2S2O3 1.05g/L,(NH4)2SO4 1.88g/L。
Example 2:
collected from gas desulfurization section of certain coking enterpriseThe salt content is 256g/L (NH)4SCN 162g/L，(NH4)2S2O3 74g/L,(NH4)2SO4 20 g/L) of the desulfurization waste liquid, concentrating 100L of the desulfurization waste liquid in an evaporation kettle, generating 42L of condensate liquid in the concentration process, increasing the salt content in the concentrated liquid to 441g/L, spraying the concentrated liquid into a pyrolysis furnace through an injector within one hour, introducing superheated steam with the temperature of 560 ℃ and the flow of 80Kg/h from the bottom of the pyrolysis furnace, directly exchanging heat between the superheated steam and the sprayed desulfurization waste liquid, discharging a gaseous mixture formed by pyrolysis of the desulfurization waste liquid from the top of the pyrolysis furnace, sequentially passing through a steam preheater, the evaporation kettle and a washing tower in the discharging process, and circularly washing the condensate liquid generated in the evaporation process in the washing tower. 0.2MPa saturated steam is preheated to 280 ℃ by a steam preheater, then enters a steam heating furnace to be heated to 660 ℃ and enters from the bottom of a pyrolysis furnace. Finally, the washing liquid in the washing tower is filtered and analyzed, 6.9kg of elemental sulfur and NH in the liquid are generated in the filtering process4SCN 13.50g/L，(NH4)2S2O3 4.18g/L，(NH4)2SO4 2.22g/L。
Claims (6)
1. A pyrolysis treatment process for desulfurization waste liquid is characterized by comprising the following steps: concentrating the desulfurization waste liquid, then carrying out pyrolysis conversion on the desulfurization waste liquid by taking high-temperature superheated steam as a heat source, washing the converted tail gas by condensate obtained by evaporating desulfurization liquid or ammonia water obtained by ammonia evaporation, and then merging the tail gas into a VOC (volatile organic compound) collection system, wherein the liquid generated in the washing process enters a foam tank or a regeneration tower to be used as the desulfurization liquid of coal gas after sulfur recovery.
2. The pyrolysis treatment process of desulfurization waste liquid according to claim 1, characterized by comprising the steps of:
(1) the desulfurization waste liquid is firstly evaporated and concentrated in a concentration kettle or an evaporator, 0.2-0.5MPa saturated steam or the waste heat of tail gas generated by pyrolysis of the desulfurization waste liquid is used as a heat source in the evaporation process, the salt content in the concentrated liquid after concentration is controlled at 400-600g/L, and condensate generated in the concentration process is supplemented into a washing tower for washing and purifying the tail gas;
(2) spraying the concentrated desulfurization waste liquid into a pyrolysis furnace in a form of mist or liquid drops for pyrolysis, wherein superheated steam is used as a heat source in the pyrolysis process, the mass ratio of the superheated steam to the desulfurization waste liquid is 0.5-1, and the temperature is 500-;
(3) gas generated after pyrolysis of the desulfurization waste liquid in the pyrolysis furnace is primarily cooled through a steam superheater, the cooled gas is introduced into an evaporator or a concentration kettle to be cooled again, and heat supply in the concentration process of the desulfurization waste liquid is realized; the gas-water mixture discharged from the evaporator or the concentration kettle is introduced into the middle lower part of the washing tower, the washing liquid used in the washing process is condensate obtained by the desulfurization waste liquid through the evaporation concentration process, the washing liquid is extracted from the middle lower part of the washing tower by a pump for recycling, part of liquid is extracted from the bottom of the washing tower periodically and is injected into a regeneration tower or a foam tank of a desulfurization working section, and the tail gas at the top of the washing tower is introduced into a VOC tail gas purification system of the enterprise desulfurization working section.
3. The desulfurization waste liquid pyrolysis treatment process according to claim 2, characterized in that: in the step (1), the concentration process is carried out under vacuum condition, and the vacuum degree is 0.05-0.09 MPa.
4. The desulfurization waste liquid pyrolysis treatment process according to claim 2, characterized in that: in the step (2), a steam superheater tube is arranged at the upper part of the pyrolysis furnace, a nozzle for desulfurization waste liquid is arranged at the middle part of the pyrolysis furnace, and a high-temperature-resistant packing layer and a superheated steam distributor are arranged at the bottom of the pyrolysis furnace.
5. The desulfurization waste liquid pyrolysis treatment process according to claim 2, characterized in that: in the step (2), the superheated steam takes saturated steam with 0.2-0.5MPa in an enterprise as a raw material, the steam temperature is preheated to 400 ℃ by a steam superheating pipe, then the steam is introduced into a steam heating furnace, and the steam is superheated to 800 ℃ by coal gas, electric heating or enterprise waste heat and then introduced into a pyrolysis furnace.
6. The desulfurization waste liquid pyrolysis treatment process according to claim 2, characterized in that: in the step (3), the washing tower is an air-jet tower or a packed tower.
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