CN115041020A - Integrated treatment device and method for complex iron desulfurization sulfur slurry - Google Patents

Integrated treatment device and method for complex iron desulfurization sulfur slurry Download PDF

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Publication number
CN115041020A
CN115041020A CN202110248402.3A CN202110248402A CN115041020A CN 115041020 A CN115041020 A CN 115041020A CN 202110248402 A CN202110248402 A CN 202110248402A CN 115041020 A CN115041020 A CN 115041020A
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outlet
desulfurization
liquid
sulfur slurry
concentrator
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李金环
朱红彬
张千昌
张硕琳
王伟健
王辉
李清方
刘海丽
刘花蕾
董金婷
傅莉
张宁宁
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China Petrochemical Corp
Sinopec Oilfield Service Corp
Sinopec Petroleum Engineering Corp
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Sinopec Oilfield Service Corp
Sinopec Petroleum Engineering Corp
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Priority to CN202110248402.3A priority Critical patent/CN115041020A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/96Regeneration, reactivation or recycling of reactants
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D36/00Filter circuits or combinations of filters with other separating devices
    • B01D36/003Filters in combination with devices for the removal of liquids
    • B01D36/008Means to filter or treat the separated liquid
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/46Removing components of defined structure
    • B01D53/48Sulfur compounds
    • B01D53/52Hydrogen sulfide
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/73After-treatment of removed components
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2258/00Sources of waste gases
    • B01D2258/02Other waste gases

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  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
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  • Environmental & Geological Engineering (AREA)
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Abstract

The invention provides a complex iron desulfurization sulfur slurry integrated treatment device and method, and relates to the technical field of resource recycling. The integrated complex iron desulfurization sulfur slurry treatment device provided by the invention comprises a sulfur slurry cleaning and desulfurization system and a desulfurization solution concentration system; the sulfur slurry cleaning and desulfurizing system comprises: the vacuum filter is provided with a sulfur slurry inlet, a desalted water spraying port, a desulfurized liquid outlet and a sulfur paste outlet; the doctor solution concentration system includes: the device comprises a raw material tank, a concentrator, a flash tank, a condensed water tank, a concentrated medicine outlet and a cooling water tank. The integrated treatment device for the complex iron desulfurization sulfur slurry provided by the invention is compact in equipment, small in occupied area and small in required space, and can realize recycling of a desulfurization agent in the complex iron desulfurization sulfur slurry by treating the complex iron desulfurization sulfur slurry, so that the agent supply of a desulfurization system is reduced, the water balance of the desulfurization system is favorably maintained, the full utilization of energy can be realized, and the energy consumption is reduced.

Description

Integrated treatment device and method for complex iron desulfurization sulfur slurry
Technical Field
The invention relates to the technical field of resource recycling, in particular to a device and a method for integrated treatment of complex iron desulfurization sulfur slurry.
Background
As the amount of natural gas increases, the amount of hydrogen sulfide increases, and the hydrogen sulfide can cause equipment corrosion and catalyst poisoning, resulting in increased production costs and reduced product quality, and thus the hydrogen sulfide needs to be removed by desulfurization techniques. The complex iron desulfurization process has the advantages of simple process flow, high absorption speed, high desulfurization efficiency, no toxicity, simple and convenient equipment, economic and reasonable process and the like, and becomes a widely applied desulfurization technology. The prior art is limited by factors such as low sulfur capacity, large circulation capacity and the like in the aspects of equipment miniaturization, treatment cost reduction and the like, so that the problems of large volume, difficult prying, high treatment cost and the like of treatment equipment are caused. The desulfurization capacity can be improved by increasing the concentration of effective substances in a desulfurization agent system, so that the circulating liquid amount is effectively reduced, the energy consumption is greatly reduced, and meanwhile, the equipment investment and the operation cost are reduced.
A large amount of sulfur generated in the complex iron desulfurization process is dispersed in desulfurization liquid to form sulfur slurry, sulfur can be separated from the sulfur slurry system by diluting the sulfur slurry with water, and the separation of the sulfur from the sulfur slurry system can carry out a large amount of desulfurization liquid (the main component of the desulfurization liquid is a desulfurization agent iron complex, and in addition, a certain amount of sulfate and carbonate can be contained), so that the loss of the desulfurization liquid is large, and the amount of sulfur carried liquid accounts for 63% of the loss of the agent according to the analysis of industrial operation data. And because the desulfurization liquid contains a large amount of dilution water, the concentration of the desulfurization agent is low, and the desulfurization agent cannot be recycled, most enterprises directly discard the desulfurization liquid and supply a large amount of desulfurization agent again in the desulfurization process, and the increase of the volume of the desulfurization system agent is unfavorable for maintaining the water balance of the desulfurization system.
Disclosure of Invention
In view of the above, the invention aims to provide an integrated treatment device and method for complex iron desulfurization sulfur slurry. The device provided by the invention can realize the recycling of the desulfurization agent in the complex iron desulfurization sulfur slurry, avoids resource waste and is beneficial to maintaining the water balance of a desulfurization system.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a complex iron desulfurization sulfur slurry integrated treatment device, which comprises a sulfur slurry cleaning and desulfurization system and a desulfurization solution concentration system;
the sulfur slurry cleaning and desulfurizing system comprises:
the device comprises a vacuum filter 1, wherein the vacuum filter 1 is provided with a sulfur slurry inlet 1-1, a desalted water spraying port 1-2, a desulfurized liquid outlet 1-3 and a sulfur paste outlet 1-4;
the doctor solution concentrating system comprises:
a raw material tank 2 with a feeding port communicated with the desulfurization liquid outlet 1-3, wherein a heater 2-1 is arranged in the raw material tank 2;
the concentrator 3 is communicated with the outlet of the raw material tank 2 through a bottom feeding port, and the concentrator 3 is also provided with a heating steam inlet, a steam condensation outlet and a top discharging port; the steam condensation outlet is communicated with the inlet of the condensation water tank 5;
the flash tank 4 is provided with a top gas outlet and a bottom discharge hole, and the feeding hole is communicated with the top discharge hole of the concentrator 3; a bottom discharge hole pipeline of the flash tank 4 is converged with a bottom feeding hole pipeline of the concentrator 3, and the converged pipeline is also provided with a concentrated chemical outlet 4-1;
a cooling water tank 7 with an inlet in communication with the top gas outlet of the flash tank 4.
Preferably, the concentrator 3 is a rising-film tube-in-tube concentrator, a falling-film tube-in-tube concentrator, a horizontal tube-in-tube concentrator or a plate concentrator.
Preferably, a raw material pump P-1 is arranged on an outlet pipeline of the raw material tank 2; a concentration circulating pump P-2 is arranged on a discharge port pipeline at the bottom of the flash tank 4; and a vacuum pump P-3 is arranged on an inlet pipeline of the cooling water tank 7.
Preferably, the bottom outlet line of the flash tank 4 is also connected to the outlet line of the concentration circulation pump P-2 via an additional line L-1.
Preferably, the concentrated medicament outlet 4-1 is communicated with the inlet of the concentrated medicament tank 6;
or the concentrated medicament outlet 4-1 is communicated with an evaporative crystallization system; the evaporative crystallization system comprises: the secondary steam inlet is communicated with the top gas outlet of the flash tank 4; the evaporative crystallizer 8 is also provided with an external steam inlet, a steam condensation outlet, an upper feeding port and a bottom discharging port; a feeding port at the upper part of the evaporative crystallizer 8 is communicated with a concentrated medicament outlet 4-1; a discharge port at the bottom of the evaporative crystallizer 8 is branched into a crystallization liquid outlet and a crystallization liquid circulating outlet, the crystallization liquid circulating outlet is communicated with a feeding port at the upper part of the evaporative crystallizer 8, and the crystallization liquid outlet is connected to a centrifuge 9; and a steam condensation outlet of the evaporation crystallizer 8 is communicated with an inlet of the condensed water tank 5.
Preferably, an agitator is provided inside the evaporative crystallizer 8.
Preferably, a crystallization circulating pump P-4 is arranged on a crystallization liquid circulating outlet pipeline of the evaporative crystallizer 8.
Preferably, the bottom discharge line of the evaporative crystallizer 8 is also connected to the outlet line of the crystallization circulation pump P-4 via an additional line L-2.
The invention provides an integrated treatment method of complex iron desulfurization sulfur slurry, which comprises the following steps:
the complex iron desulfurization sulfur slurry to be treated enters a vacuum filter 1 from a sulfur slurry inlet 1-1, desalted water is sprayed in through a desalted water spraying port 1-2, the complex iron desulfurization sulfur slurry is cleaned in the vacuum filter 1, and simultaneously, under the suction filtration action of the vacuum filter 1, sulfur paste and desulfurization liquid are formed, and the sulfur paste is discharged from a sulfur paste outlet 1-4;
the desulfurization solution enters a raw material tank 2 from a desulfurization solution outlet 1-3, and is preheated to the saturation temperature under the evaporation pressure in the raw material tank 2 by a heater 2-1;
the preheated desulfurization solution enters a concentrator 3, steam is introduced into the concentrator 3 to heat the desulfurization solution entering the concentrator 3, the desulfurization solution is heated to form a gas-liquid mixture, and the steam is condensed into water to enter a condensate water tank 5;
the gas-liquid mixture enters a flash tank 4 for gas-liquid separation to form separated liquid and secondary steam; the separation liquid is discharged from a bottom discharge hole of the flash tank 4 and is converged with the preheated desulfurization liquid to form a mixed liquid, one part of the mixed liquid enters a bottom feed inlet of the concentrator 3 for cyclic concentration, and the other part of the mixed liquid flows out from a concentrated medicament outlet 4-1; the secondary steam is discharged from the top gas outlet of the flash tank 4 and condensed into the cooling water tank 7.
Preferably, the mixed liquid flowing out from the concentrated medicament outlet 4-1 enters a concentrated medicament tank 6 to be used as a concentrated medicament for the complex iron desulfurization process;
or the mixed liquid flowing out of the concentrated chemical outlet 4-1 enters the evaporative crystallizer 8 from a feeding port at the upper part of the evaporative crystallizer 8, and external steam and secondary steam discharged from the flash tank 4 are introduced into the evaporative crystallizer 8 to evaporate and crystallize the mixed liquid to form a crystallization liquid; the external steam and the secondary steam are condensed and enter a condensed water tank 5; and discharging the crystallization liquid from a discharge port at the bottom of the evaporative crystallizer 8, feeding one part of the crystallization liquid from a circulation outlet of the crystallization liquid into the evaporative crystallizer 8 again for circulation evaporative crystallization, feeding the other part of the crystallization liquid from an outlet of the crystallization liquid into a centrifugal machine 9 for solid-liquid separation to form crystallized salt and a concentrated medicament, and recovering the concentrated medicament in a complex iron desulfurization process.
The invention provides a complex iron desulfurization sulfur slurry integrated treatment device, which comprises a sulfur slurry cleaning and desulfurization system and a desulfurization solution concentration system; the sulfur slurry cleaning and desulfurizing system comprises: the device comprises a vacuum filter 1, wherein the vacuum filter 1 is provided with a sulfur slurry inlet 1-1, a desalted water spraying port 1-2, a desulfurized liquid outlet 1-3 and a sulfur paste outlet 1-4; the doctor solution concentrating system comprises: a raw material tank 2, a concentrator 3, a flash tank 4, a condensed water tank 5, a concentrated medicine outlet 4-1 and a cooling water tank 7. The integrated treatment device for the complex iron desulfurization sulfur slurry provided by the invention has the advantages that the device is compact, the occupied area is small, the required space is small, the device provided by the invention is used for treating the complex iron desulfurization sulfur slurry, the recycling of desulfurization agents in the complex iron desulfurization sulfur slurry can be realized, the agent supply of a desulfurization system is reduced, the water balance of the desulfurization system is favorably maintained, the full utilization of energy sources can be realized, the energy consumption is reduced, and particularly, the separation liquid generated by the flash tank 4 is sent to the concentrator 3 to be used as a heating material, so that the feed liquid in the concentrator is kept in a boiling state, the latent heat is recovered, and the thermal efficiency is improved.
Furthermore, the device provided by the invention is used for treating the complex iron desulfurization sulfur slurry, and can also crystallize and separate potassium sulfate in the sulfur slurry, so that the condition that the desulfurization process is influenced due to the fact that the recycled desulfurization agent contains the salt in the recycling process is avoided; and the secondary steam generated by the flash tank 4 is used as a steam source of crystallization, so that the energy of the system is further fully utilized, the supply of external heat sources is reduced, and the energy consumption is reduced.
Drawings
FIG. 1 is a schematic view of an integrated complex iron desulfurization sulfur slurry treatment device provided by the invention;
in figure 1, 1-vacuum filter, 1-1-sulfur slurry inlet, 1-2-desalted water spray port, 1-3-desulfurized liquid outlet, 1-4-sulfur paste outlet, 2-raw material tank, 2-1-heater, 3-concentrator, 4-flash tank, 4-1-concentrated chemical outlet, 5-condensate tank, 6-concentrated chemical tank, 7-cooling water tank, 8-evaporative crystallizer, 9-centrifuge, P-1-raw material pump, P-2-concentration circulating pump, P-3-vacuum pump, P-4-crystallization circulating pump, L-1-connecting pipeline, L-2-connecting pipeline.
Detailed Description
The invention provides a complex iron desulfurization sulfur slurry integrated treatment device, which comprises a sulfur slurry cleaning and desulfurization system and a desulfurization solution concentration system;
the sulfur slurry cleaning and desulfurizing system comprises:
the device comprises a vacuum filter 1, wherein the vacuum filter 1 is provided with a sulfur slurry inlet 1-1, a desalted water spraying port 1-2, a desulfurized liquid outlet 1-3 and a sulfur paste outlet 1-4;
the doctor solution concentration system includes:
a raw material tank 2 with a feeding port communicated with the desulfurization solution outlet 1-3, wherein a heater 2-1 is arranged in the raw material tank 2;
the concentrator 3 is communicated with the outlet of the raw material tank 2 through a bottom feeding port, and the concentrator 3 is also provided with a heating steam inlet, a steam condensation outlet and a top discharging port; the steam condensation outlet is communicated with the inlet of the condensation water tank 5;
the flash tank 4 is provided with a top gas outlet and a bottom discharge hole, and the feeding hole is communicated with the top discharge hole of the concentrator 3; a bottom discharge hole pipeline of the flash tank 4 is converged with a bottom feeding hole pipeline of the concentrator 3, and the converged pipeline is also provided with a concentrated medicament outlet 4-1;
a cooling water tank 7 with an inlet in communication with the top gas outlet of the flash tank 4.
The integrated complex iron desulfurization sulfur slurry treatment device provided by the invention comprises a sulfur slurry cleaning and desulfurization system. In the invention, the sulfur slurry cleaning and desulfurizing system comprises: the vacuum filter 1 is provided with a sulfur slurry inlet 1-1, a desalted water spray port 1-2, a desulfurized liquid outlet 1-3 and a sulfur paste outlet 1-4. The invention has no special requirement on the vacuum filter 1, and can adopt a vacuum filter known by persons skilled in the art, and the filter cloth is distributed in the vacuum filter 1, so that the solid-liquid separation can be carried out on the cleaned sulfur pulp to form sulfur paste and filtrate, wherein the filtrate is the desulfurization solution. In the invention, the desalted water spray ports 1-2 are preferably arranged above the vacuum filter 1, and the desalted water spray ports 1-2 are used for spraying desalted water into mist, so that the number of the desalted water spray ports is not particularly required, and the sulfur slurry can be fully sprayed; in the invention, the desalted water spray ports 1-2 are preferably connected with a desalted water main pipe, namely a spray system is formed in a manner that the desalted water main pipe is connected with a plurality of branch pipes with desalted water spray ports; the desalted water main pipe is preferably provided with a check valve, and the branch pipe is preferably provided with a flow dividing throttle valve. In the present invention, the doctor outlet 1-3 is preferably located below the vacuum filter 1. In the present invention, the sulfur paste outlets 1-4 are preferably connected to a belt conveyor to realize continuous discharge of the sulfur paste.
The integrated treatment device for the complex iron desulfurization sulfur slurry comprises a desulfurization solution concentration system, wherein the desulfurization solution concentration system comprises a raw material tank 2, a feeding port of which is communicated with a desulfurization solution outlet 1-3, and a heater 2-1 is arranged in the raw material tank 2. The invention has no special requirements on the raw material tank 2 and the heater 2-1, and the raw material tank and the heater which are well known by the technical personnel in the field can be adopted; the heater 2-1 is used for preheating the desulfurization solution in the raw material tank. In the present invention, the outlet line of the raw material tank 2 is preferably provided with a raw material pump P-1, and the present invention does not require the raw material pump P-1, and a corresponding pump well known to those skilled in the art may be used.
In the invention, the doctor solution concentration system comprises a concentrator 3 with a bottom feeding port communicated with an outlet of the raw material tank 2, and the concentrator 3 is also provided with a heating steam inlet, a steam condensation outlet and a top discharging port. In the present invention, the bottom feed inlet line of the concentrator 3 is also preferably provided with a feed throttle valve and a check valve, which are preferably provided on the outlet line of the raw material pump P-1, the feed throttle valve being mainly used to control the feed of the concentrator to adjust the amount of circulating liquid material of the concentrator. In the invention, the heating steam inlet is preferably arranged at the upper part of the concentrator 3, the heating steam inlet is preferably connected with a steam generator, the steam generator is preferably a roots blower or a centrifugal compressor, wherein the roots blower is selected for small-flow steam, the centrifugal compressor is selected for large-flow steam, and the steam generator provides heat source steam for the system; the heating steam inlet pipeline is preferably provided with a steam ball valve. In the present invention, the steam condensation outlet is preferably provided at the lower portion of the concentrator 3; the steam condensation outlet is communicated with the inlet of the condensed water tank 5; the top discharge line is also preferably provided with a pressure relief valve. In the invention, the concentrator 3 is preferably an ascending membrane type tube array concentrator, a falling membrane type tube array concentrator, a horizontal tube shell concentrator or a plate concentrator, and specifically, steam is introduced into the shell side of the concentrator 3 to be condensed; the liquid is introduced into the tube and evaporated. In the present invention, the concentrator 3 serves to heat and concentrate the desulfurization solution introduced into the concentrator 3.
In the invention, the doctor solution concentration system comprises a flash tank 4 with a feed inlet communicated with a discharge outlet at the top of the concentrator 3; the feeding port of the flash tank 4 is preferably arranged at the lower part of the flash tank 4, and the flash tank 4 is provided with a top gas outlet and a bottom discharge port. The present invention does not require the flash tank 4 to be specifically configured, and flash tanks known to those skilled in the art may be used. In the invention, a bottom discharge hole pipeline of the flash tank 4 is converged with a bottom feeding hole pipeline of the concentrator 3, and the converged pipeline is also provided with a concentrated chemical outlet 4-1. In the invention, a bottom discharge port pipeline of the flash tank 4 is preferably provided with a concentration circulating pump P-2, specifically, an inlet of the concentration circulating pump P-2 is connected with a bottom discharge port of the flash tank 4, and an outlet of the concentration circulating pump P-2 is connected with a bottom feed port of the concentrator 3 and a concentrated medicine outlet 4-1. In the present invention, the bottom discharge line of the flash tank 4 and the outlet line of the concentration circulating pump P-2 are preferably connected through an additional line L-1 for adjusting the circulating amount.
In the present invention, the desulfurization solution concentration system includes a cooling water tank 7 having an inlet in communication with the top gas outlet of the flash tank 4. In the present invention, the inlet line of the cooling water tank 7 is preferably provided with a vacuum pump P-3. The present invention has no special requirements for the cooling water tank 7 and the vacuum pump P-3, and a cooling water tank and a vacuum pump well known to those skilled in the art can be used.
As an embodiment of the present invention, the concentrated agent outlet 4-1 communicates with the inlet of the concentrated agent tank 6. The invention does not require any particular canister 6 and may be implemented using a reservoir known to those skilled in the art.
As another embodiment of the present invention, the concentrated medicament outlet 4-1 is in communication with an evaporative crystallization system; the evaporative crystallization system comprises: an evaporation crystallizer 8 with a secondary steam inlet communicated with the top gas outlet of the flash tank 4; the evaporative crystallizer 8 is also provided with an external steam inlet, a steam condensation outlet, an upper feeding port and a bottom discharging port. In the present invention, the external steam inlet and the secondary steam inlet are preferably respectively disposed at the upper portion of the evaporative crystallizer 8, the external steam inlet and the secondary steam inlet pipeline are also preferably provided with a steam ball valve, and the external steam inlet is preferably connected to the steam generator in the above technical solution, which is not described herein again; the vapor condensation outlet is preferably arranged in the lower part of the evaporative crystallizer 8. In the invention, a feeding throttle valve is preferably arranged on a feeding port pipeline at the upper part of the evaporative crystallizer 8, and the feeding throttle valve is mainly used for controlling feeding of the evaporative crystallizer so as to adjust the circulating liquid amount of the evaporative crystallizer; and a feeding port at the upper part of the evaporative crystallizer 8 is communicated with a concentrated medicament outlet 4-1. In the invention, a discharge port at the bottom of the evaporative crystallizer 8 is branched into a crystallization liquid outlet and a crystallization liquid circulating outlet, the crystallization liquid circulating outlet is communicated with a feeding port at the upper part of the evaporative crystallizer 8, and the crystallization liquid outlet is connected to a centrifuge 9; and a steam condensation outlet of the evaporative crystallizer 8 is communicated with an inlet of the condensed water tank 5. In the present invention, the inside of the evaporative crystallizer 8 is preferably provided with a stirrer to prevent clogging; a crystallization circulating pump P-4 is arranged on a crystallization liquid circulating outlet pipeline of the evaporative crystallizer 8, specifically, an inlet of the crystallization circulating pump P-4 is connected with a crystallization liquid circulating outlet of the evaporative crystallizer 8, and an outlet of the crystallization circulating pump P-4 is connected with an upper feeding port and a concentrated medicine outlet 4-1 of the evaporative crystallizer 8. The invention has no special requirements on the structure of the evaporation crystallizer 8, and can adopt the evaporation crystallizer known to a person skilled in the art, wherein steam is introduced into the shell side of the evaporation crystallizer 8 to generate condensation, and feed liquid is introduced into the tube side of the evaporation crystallizer 8 to generate crystallization. In the present invention, the bottom discharge port line of the evaporative crystallizer 8 and the outlet line of the crystallization circulating pump P-4 are further connected through an additional line L-2 for adjusting the circulating amount.
The complex iron desulfurization sulfur slurry integrated processing device provided by the invention has compact equipment, small occupied area and small required space, can also adopt an industrial personal computer and a PLC to form an MVR series real-time monitoring center, and can acquire state signals of various sensors in real time through software programming, so that the closing and adjustment of a valve and the control and adjustment of the flow speed, the flow rate, the temperature and the pressure of liquid are automatically controlled, the system can work to reach a dynamic balance state, and meanwhile, the device also has various functions of automatically alarming, automatically recording parameters and providing reports.
The invention provides an integrated treatment method of complex iron desulfurization sulfur slurry, which comprises the following steps:
the complex iron desulfurization sulfur slurry to be treated enters a vacuum filter 1 from a sulfur slurry inlet 1-1, desalted water is sprayed in through a desalted water spraying port 1-2, the complex iron desulfurization sulfur slurry is cleaned in the vacuum filter 1, and simultaneously, under the suction filtration effect of the vacuum filter 1, sulfur paste and desulfurization liquid are formed, and the sulfur paste is discharged from a sulfur paste outlet 1-4;
the desulfurization solution enters a raw material tank 2 from a desulfurization solution outlet 1-3, and is preheated to the saturation temperature under the evaporation pressure in the raw material tank 2 by a heater 2-1;
the preheated desulfurization solution enters a concentrator 3, steam is introduced into the concentrator 3 to heat the desulfurization solution entering the concentrator 3, the desulfurization solution is heated to form a gas-liquid mixture, and the steam is condensed into water to enter a condensate water tank 5;
the gas-liquid mixture enters a flash tank 4 for gas-liquid separation to form separated liquid and secondary steam; the separation liquid is discharged from a discharge port at the bottom of the flash tank 4 and is converged with the preheated desulfurization liquid to form a mixed liquid, one part of the mixed liquid enters a feed port at the bottom of the concentrator 3 for cyclic concentration, and the other part of the mixed liquid flows out from a concentrated chemical agent outlet 4-1; the secondary steam is discharged from the top gas outlet of the flash tank 4 and condensed into the cooling water tank 7.
The complex iron desulfurization sulfur slurry to be treated enters a vacuum filter 1 from a sulfur slurry inlet 1-1, desalted water is sprayed in from a desalted water spraying port 1-2, the complex iron desulfurization sulfur slurry is cleaned in the vacuum filter 1, and simultaneously, under the suction filtration action of the vacuum filter 1, sulfur paste (filter cake) and desulfurization liquid (filtrate) are formed, and the sulfur paste is discharged from a sulfur paste outlet 1-4. In the invention, the desalted water is water for removing strong electrolyte or reducing the strong electrolyte to a certain degree, in particular deionized water with the residual salt content of 1 mg/L-5 mg/L; the invention has no special requirement on the flow of the sprayed desalted water, and can fully clean the complex iron desulfurization sulfur slurry to be treated. In the complex iron desulfurization process, a large amount of sulfur is generated and dispersed in a desulfurization solution to form sulfur slurry, and the sulfur slurry is cleaned by desalted water and subjected to solid-liquid separation by a vacuum filter to separate sulfur from the sulfur slurry to form sulfur paste; the main component of the desulfurization solution is a desulfurization agent iron complex, and in addition, a certain amount of sulfate and carbonate can be contained, and potassium sulfate is taken as the main component.
After the doctor solution is obtained, the doctor solution enters the raw material tank 2 from the doctor solution outlet 1-3, and is preheated to the saturation temperature under the evaporation pressure in the raw material tank 2 by the heater 2-1, and the doctor solution is preheated to the temperature, so that the doctor solution can be ensured to have a good evaporation and concentration effect when entering the concentrator 3, and more steam in the concentrator 3 has the effect of stabilizing the temperature.
After the desulfurization solution is preheated, the preheated desulfurization solution preferably enters a concentrator 3 through a raw material pump P-1, steam is introduced into the concentrator 3 to heat the desulfurization solution entering the concentrator 3, the desulfurization solution is heated to form a gas-liquid mixture, and the steam is condensed into water to enter a condensate water tank 5. In the present invention, the process parameters of the concentrator 3 are preferably: tube side design/operating temperature: 80 ℃/60 ℃, tube side pressure/operating pressure: atmospheric pressure/atmospheric pressure, shell pass design/operating temperature: 120 ℃/100 ℃, shell side design/operating pressure: atmospheric/atmospheric. In the invention, the main component of the gas in the gas-liquid mixture is water vapor, and the main component of the liquid is concentrated medicament; further, the gas-liquid mixture is depressurized by a pressure reducing valve arranged on a discharge port pipeline at the top of the concentrator 3 to form a low-pressure two-phase flow, and the low-pressure two-phase flow is discharged from the concentrator 3.
After a gas-liquid mixture is obtained, the gas-liquid mixture enters a flash tank 4 for gas-liquid separation to form separated liquid and secondary steam. In the present invention, the process parameters of the flash tank 4 are preferably: design/operating temperature: 80 ℃/60 ℃, design/operating pressure: -100/-80 kPa. In the present invention, the secondary steam is discharged from the top gas outlet of the flash tank 4, preferably condensed into the cooling water tank 7 after exchanging heat with the tap water introduced into the vacuum pump P-3. In the invention, the separation liquid is discharged from a bottom discharge hole of a flash tank 4, preferably joins with the preheated desulfurization liquid through a concentration circulating pump P-2 to form a mixed liquid, a part of the mixed liquid enters a bottom feed inlet of a concentrator 3 for circulating concentration, and in the process, the separation liquid formed by the flash tank 4 is used as a heating material of the concentrator 3 to maintain the feed liquid in the concentrator 3 in a boiling state, so that the potential energy of the heat of the system is recycled, and the supply of external steam is reduced; the other part of the mixed solution flows out from a concentrated medicament outlet 4-1.
As an embodiment of the invention, the mixed liquid flowing out from the concentrated chemical outlet 4-1 enters the concentrated chemical tank 6 to be used as a concentrated chemical for the complex iron desulphurization process, so that the concentration of the circulating liquid is kept stable and the requirement of the complex iron desulphurization process on the concentration of the concentrated chemical is met.
As another embodiment of the present invention, when the desulfurization solution further contains a certain amount of sulfate and carbonate, which are usually mainly potassium sulfate in actual conditions, the present invention preferably introduces the mixed solution flowing out from the concentrated chemical agent outlet 4-1 into the evaporative crystallizer 8 from the upper feeding port of the evaporative crystallizer 8. In the invention, the mixed solution is evaporated and crystallized by introducing external steam into the evaporation crystallizer 8 and secondary steam discharged from the flash tank 4 to form a crystallization solution; the external steam and the secondary steam are condensed and enter a condensed water tank 5; and discharging the crystallization liquid from a discharge port at the bottom of the evaporative crystallizer 8, discharging one part of the crystallization liquid from a circulation outlet of the crystallization liquid, preferably, feeding the crystallization liquid into the evaporative crystallizer 8 again through a crystallization circulating pump P-4 for circulation evaporative crystallization, and feeding the other part of the crystallization liquid from an outlet of the crystallization liquid into a centrifugal machine 9 for solid-liquid separation to form crystallized salt and a concentrated medicament, wherein the concentrated medicament is recovered in a complex iron desulfurization process. In the present invention, the process parameters of the evaporative crystallizer are preferably: vessel design/operating temperature: 80 ℃/60 ℃, vessel design/operating pressure: atmospheric pressure/atmospheric pressure, jacket design/operating temperature: 120 ℃/100 ℃, jacket design/operating pressure: atmospheric pressure/atmospheric pressure. In the crystallization and evaporation process, the secondary steam generated by the flash tank 4 is used as a steam source of crystallization, so that the energy of the system is fully utilized, the latent heat is recovered, and the heat efficiency is improved.
The device provided by the invention is used for treating the complex iron desulfurization sulfur slurry, and the recycling of the desulfurization agent in the complex iron desulfurization sulfur slurry can be realized, so that the agent supply of a desulfurization system is reduced, the maintenance of the water balance of the desulfurization system is facilitated, the full utilization of energy can be realized, and the energy consumption is reduced. In addition, the potassium sulfate in the sulfur slurry can be crystallized and separated, and the condition that the recycled desulfurization agent contains the salt to cause system blockage in the recycling process and influence the desulfurization process is avoided.
The integrated complex iron desulfurized slurry treatment apparatus and method of the present invention will be described in detail with reference to the following examples, which should not be construed as limiting the scope of the present invention.
Example 1
The integrated complex iron desulfurization sulfur slurry treatment device has a structure as shown in figure 1: in figure 1, 1-vacuum filter, 1-1-sulfur slurry inlet, 1-2-desalted water spray port, 1-3-desulfurized liquid outlet, 1-4-sulfur paste outlet, 2-raw material tank, 2-1-heater, 3-concentrator, 4-flash tank, 4-1-concentrated agent outlet, 5-condensed water tank, 6-concentrated agent tank, 7-cooling water tank, P-1-raw material pump, P-2-concentration circulating pump, P-3-vacuum pump.
The device shown in figure 1 is adopted to carry out integrated treatment on the complex iron desulfurization sulfur slurry, and the complex iron desulfurization sulfur slurry comprises the following main components: iron complex and potassium sulfate, and the treatment method comprises the following steps:
feeding the complex iron desulfurization sulfur slurry into a vacuum filter 1 from a sulfur slurry inlet 1-1, spraying desalted water into the vacuum filter 1 through a desalted water spraying port 1-2, cleaning the complex iron desulfurization sulfur slurry in the vacuum filter 1, forming sulfur paste and desulfurization liquid under the suction filtration action of the vacuum filter 1, and discharging the sulfur paste from a sulfur paste outlet 1-4;
the desulfurization solution enters a raw material tank 2 from a desulfurization solution outlet 1-3, and is preheated to the saturation temperature (80 ℃) under the evaporation pressure in the raw material tank 2 by a heater 2-1;
the preheated desulfurization solution enters a concentrator 3 through a raw material pump P-1, steam is introduced into the concentrator 3 to heat the desulfurization solution entering the concentrator 3 (the temperature is 80 ℃), the desulfurization solution is heated to form a gas-liquid mixture, and the steam is condensed into water to enter a condensate water tank 5;
the gas-liquid mixture enters a flash tank 4 (the temperature is 80 ℃, and the pressure is 80kPa) for gas-liquid separation to form separated liquid and secondary steam; the separation liquid is discharged from a bottom discharge hole of a flash tank 4, and is converged with the preheated desulfurization liquid by a concentration circulating pump P-2 to form a mixed liquid, one part of the mixed liquid enters a bottom feed inlet of a concentrator 3 for circulating concentration, and the other part of the mixed liquid enters a concentrated medicament tank 6 from a concentrated medicament outlet 4-1 to be used as a concentrated medicament (the medicament concentration is the same as the original desulfurization medicament concentration used by the complex iron desulfurization system) for the complex iron desulfurization process; the secondary steam is discharged from a gas outlet at the top of the flash tank 4, exchanges heat with tap water introduced into the vacuum pump P-3, and is condensed into the cooling water tank 7.
Example 2
The integrated complex iron desulfurization sulfur slurry treatment device has a structure as shown in figure 1: in figure 1, 1-vacuum filter, 1-1-sulfur slurry inlet, 1-2-desalted water spray port, 1-3-desulfurized liquid outlet, 1-4-sulfur paste outlet, 2-raw material tank, 2-1-heater, 3-concentrator, 4-flash tank, 4-1-concentrated chemical outlet, 5-condensate water tank, 7-cooling water tank, 8-evaporative crystallizer, 9-centrifuge, P-1-raw material pump, P-2-concentration circulating pump, P-3-vacuum pump, P-4-crystallization circulating pump.
The device shown in figure 1 is adopted to carry out integrated treatment on the complex iron desulfurization sulfur slurry, and the complex iron desulfurization sulfur slurry comprises the following main components: iron complex and potassium sulfate, and the treatment method comprises the following steps:
feeding the complex iron desulfurization sulfur slurry into a vacuum filter 1 from a sulfur slurry inlet 1-1, spraying desalted water into the vacuum filter 1 through a desalted water spraying port 1-2, cleaning the complex iron desulfurization sulfur slurry in the vacuum filter 1, forming sulfur paste and desulfurization liquid under the suction filtration action of the vacuum filter 1, and discharging the sulfur paste from a sulfur paste outlet 1-4;
the desulfurization solution enters a raw material tank 2 from a desulfurization solution outlet 1-3, and is preheated to the saturation temperature (80 ℃) under the evaporation pressure in the raw material tank 2 by a heater 2-1;
the preheated desulfurization solution enters a concentrator 3 through a raw material pump P-1, steam is introduced into the concentrator 3 to heat the desulfurization solution entering the concentrator 3 (at the temperature of 80 ℃), the desulfurization solution is heated to form a gas-liquid mixture, and the steam is condensed into water to enter a condensate water tank 5;
the gas-liquid mixture enters a flash tank 4 (the temperature is 80 ℃, and the pressure is 80kPa) for gas-liquid separation to form separated liquid and secondary steam; wherein, the secondary steam is discharged from a top gas outlet of the flash tank 4, exchanges heat with tap water introduced into the vacuum pump P-3 and then enters the cooling water tank 7; the separated liquid is discharged from a discharge port at the bottom of the flash tank 4, and is converged with the preheated desulfurization liquid by a concentration circulating pump P-2 to form a mixed liquid, one part of the mixed liquid enters a feed port at the bottom of the concentrator 3 for cyclic concentration, the other part of the mixed liquid flows out from a concentrated chemical agent outlet 4-1 and enters an evaporative crystallizer 8 from a feed port at the upper part of the evaporative crystallizer 8, external steam is introduced into the evaporative crystallizer 8, and secondary steam discharged from the flash tank 4 is used for evaporative crystallization (at the temperature of 80 ℃) of the mixed liquid to form a crystallization liquid; condensing the external steam and the secondary steam into a condensed water tank 5; the crystal liquid is discharged from a discharge port at the bottom of the evaporative crystallizer 8, one part of the crystal liquid enters the evaporative crystallizer 8 again through a crystal liquid circulating outlet via a crystal circulating pump P-4 for circulating evaporative crystallization, the other part of the crystal liquid enters a centrifuge 9 from a crystal liquid outlet for solid-liquid separation to form crystal salt and a concentrated medicament, wherein the concentrated medicament (the concentration of which reaches 1.4 times of the original medicament) is recovered in a complex iron desulfurization process (the concentrated medicament can be diluted by adding water and pumped back to a complex iron desulfurization system).
The embodiment shows that the device provided by the invention is used for carrying out integrated treatment on the complex iron desulfurization sulfur slurry, and can realize recycling of the desulfurization agent in the complex iron desulfurization sulfur slurry, so that agent supply of a desulfurization system is reduced, maintenance of water balance of the desulfurization system is facilitated, full utilization of energy can be realized, and energy consumption is reduced; the potassium sulfate in the sulfur slurry can be crystallized and separated, and the condition that the desulfurization agent obtained by recovery contains the salt, so that the system is blocked in the recycling process and the desulfurization process is influenced is avoided.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (10)

1. The integrated complex iron desulfurization sulfur slurry treatment device is characterized by comprising a sulfur slurry cleaning desulfurization system and a desulfurization solution concentration system;
the sulfur slurry cleaning and desulfurizing system comprises:
the device comprises a vacuum filter (1), wherein the vacuum filter (1) is provided with a sulfur slurry inlet (1-1), a desalted water spraying port (1-2), a desulfurized liquid outlet (1-3) and a sulfur paste outlet (1-4);
the doctor solution concentration system includes:
a raw material tank (2) with a feeding port communicated with the doctor solution outlet (1-3), wherein a heater (2-1) is arranged in the raw material tank (2);
the concentrator (3) is communicated with the outlet of the raw material tank (2) through a bottom feeding port, and the concentrator (3) is also provided with a heating steam inlet, a steam condensation outlet and a top discharge port; the steam condensation outlet is communicated with the inlet of the condensation water tank (5);
the flash tank (4) is communicated with the feed inlet and the top discharge port of the concentrator (3), and the flash tank (4) is provided with a top gas outlet and a bottom discharge port; a bottom discharge port pipeline of the flash tank (4) is converged with a bottom feed port pipeline of the concentrator (3), and the converged pipeline is also provided with a concentrated chemical outlet (4-1);
and the inlet of the cooling water tank (7) is communicated with the top gas outlet of the flash tank (4).
2. The integrated complex iron desulfurization sulfur slurry treatment device according to claim 1, wherein the concentrator (3) is a rising-film tube array concentrator, a falling-film tube array concentrator, a horizontal shell-and-tube concentrator or a plate concentrator.
3. The integrated complex iron desulfurization sulfur slurry treatment device according to claim 1, characterized in that a raw material pump (P-1) is arranged on the outlet pipeline of the raw material tank (2); a concentration circulating pump (P-2) is arranged on a bottom discharge port pipeline of the flash tank (4); and a vacuum pump (P-3) is arranged on an inlet pipeline of the cooling water tank (7).
4. The integrated complex iron desulfurization sulfur slurry treatment device according to claim 3, wherein the bottom discharge line of the flash tank (4) is further connected with the outlet line of the concentration circulating pump (P-2) through an additional line (L-1).
5. The integrated complex iron desulfurization sulfur slurry treatment device according to claim 1, wherein the concentrated agent outlet (4-1) is communicated with an inlet of a concentrated agent tank (6);
or the concentrated medicine outlet (4-1) is communicated with an evaporative crystallization system; the evaporative crystallization system comprises: the secondary steam inlet is communicated with the top gas outlet of the flash tank (4) to form an evaporation crystallizer (8); the evaporation crystallizer (8) is also provided with an external steam inlet, a steam condensation outlet, an upper feeding port and a bottom discharging port; a feeding port at the upper part of the evaporation crystallizer (8) is communicated with a concentrated medicament outlet (4-1); a discharge port at the bottom of the evaporative crystallizer (8) is branched into a crystallization liquid outlet and a crystallization liquid circulating outlet, the crystallization liquid circulating outlet is communicated with a feeding port at the upper part of the evaporative crystallizer (8), and the crystallization liquid outlet is connected to a centrifuge (9); and a steam condensation outlet of the evaporation crystallizer (8) is communicated with an inlet of the condensed water tank (5).
6. The integrated complex iron desulfurization sulfur slurry treatment device according to claim 5, characterized in that a stirrer is arranged inside the evaporative crystallizer (8).
7. The integrated complex iron desulfurization sulfur slurry treatment device according to claim 5 or 6, characterized in that a crystallization circulating pump (P-4) is arranged on a crystallization liquid circulating outlet pipeline of the evaporative crystallizer (8).
8. The integrated complex iron desulfurization sulfur slurry treatment device according to claim 7, wherein the bottom discharge line of the evaporative crystallizer (8) is further connected with the outlet line of the crystallization circulation pump (P-4) through an additional line (L-2).
9. The integrated treatment method of the complex iron desulfurization sulfur slurry is characterized by comprising the following steps of:
the complex iron desulfurization sulfur slurry to be treated enters a vacuum filter (1) from a sulfur slurry inlet (1-1), desalted water is sprayed in through a desalted water spraying port (1-2), the complex iron desulfurization sulfur slurry is cleaned in the vacuum filter (1), and simultaneously, under the suction filtration action of the vacuum filter (1), sulfur paste and desulfurization liquid are formed, and the sulfur paste is discharged from a sulfur paste outlet (1-4);
the desulfurization solution enters the raw material tank (2) from a desulfurization solution outlet (1-3), and is preheated to the saturation temperature under the evaporation pressure in the raw material tank (2) by the heater (2-1);
the preheated desulfurization solution enters a concentrator (3), steam is introduced into the concentrator (3) to heat the desulfurization solution entering the concentrator (3), the desulfurization solution is heated to form a gas-liquid mixture, and the steam is condensed into water to enter a condensate water tank (5);
the gas-liquid mixture enters a flash tank (4) for gas-liquid separation to form separated liquid and secondary steam; the separation liquid is discharged from a discharge port at the bottom of the flash tank (4) and is converged with the preheated desulfurization liquid to form a mixed liquid, one part of the mixed liquid enters a feed port at the bottom of the concentrator (3) for cyclic concentration, and the other part of the mixed liquid flows out from a concentrated chemical outlet (4-1); and the secondary steam is discharged from a top gas outlet of the flash tank (4) and condensed into a cooling water tank (7).
10. The integrated treatment method according to claim 9, wherein the mixed liquid flowing out from the concentrated medicament outlet (4-1) enters a concentrated medicament tank (6) to be used as a concentrated medicament for the complex iron desulfurization process;
or the mixed solution flowing out of the concentrated chemical outlet (4-1) enters the evaporation crystallizer (8) from a feeding port at the upper part of the evaporation crystallizer (8), and external steam and secondary steam discharged from the flash tank (4) are introduced into the evaporation crystallizer (8) to evaporate and crystallize the mixed solution to form a crystallization liquid; the external steam and the secondary steam are condensed and enter a condensed water tank (5); and the crystallized liquid is discharged from a discharge hole at the bottom of the evaporation crystallizer (8), one part of the crystallized liquid enters the evaporation crystallizer (8) again from a crystallized liquid circulating outlet for circulating evaporation crystallization, the other part of the crystallized liquid enters a centrifugal machine (9) from a crystallized liquid outlet for solid-liquid separation to form crystallized salt and a concentrated medicament, and the concentrated medicament is recovered in a complex iron desulfurization process.
CN202110248402.3A 2021-03-08 2021-03-08 Integrated treatment device and method for complex iron desulfurization sulfur slurry Pending CN115041020A (en)

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CN202110248402.3A CN115041020A (en) 2021-03-08 2021-03-08 Integrated treatment device and method for complex iron desulfurization sulfur slurry

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