CN110655041A - PDS method sulfur high-efficiency refining production process - Google Patents
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- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
- C01B17/027—Recovery of sulfur from material containing elemental sulfur, e.g. luxmasses or sulfur containing ores; Purification of the recovered sulfur
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Abstract
The invention discloses a PDS method sulfur high-efficiency refining production process, which comprises four steps of dissolving and filtering, extraction and separation, solvent regeneration and purification and the like. The invention effectively solves the problem of the purity of the sulfur generated by PDS desulfurization, also solves the problems of catalyst separation and more sewage, further solves the problem of solvent regeneration, and also solves the problem of continuous production of the sulfur. Meanwhile, the problems of metal ions such as Na +, K +, Fe3+ and the like in the sulfur are solved. Also solves the problem of sulfur content in the filter residue after filtration.
Description
Technical Field
The invention relates to a PDS method sulfur high-efficiency refining production process, belonging to the technical field of sulfuration industry.
Background
Coke is widely used as an important energy material in the aspects of metal smelting, casting, gasification and the like. In the coke manufacturing process, certain raw gas can be generated, and the raw gas is widely used as a new resource. The treatment of hydrogen sulfide in raw gas in China can be roughly divided into the following two types; one is dry desulfurization using high-valence iron as a catalyst, and the other is wet oxidation desulfurization using Na2CO3 as an absorbent. Compared with the dry desulphurization of high-valence iron, the wet oxidation desulphurization has the advantages of high desulphurization efficiency, wider coal gas application range, simple operation and the like, and is widely applied to the field of raw coke oven gas purification. Because the raw gas components are very complex, sulfur produced by wet desulphurization contains inorganic salt, tar, ash, a desulphurization catalyst and other substances, the purity is relatively low, the color is mostly black and yellow, the purity is about 70-95%, the price is greatly influenced, the utilization rate of the sulfur is low, even some crude sulfur or sulfur paste of manufacturers is treated by hazardous waste, and the production cost is greatly increased.
The prior art has the following disadvantages: 1. inorganic salt removal has been reported but only in relation to liquid sulfur filtration;
2. the prior art has no report on the treatment of sulfur in the sulfur slag;
3. in the prior report, the process is discontinuous and discontinuous by distillation and reduced pressure distillation without continuity
4. In the prior report, the solvent is rarely regenerated during extraction
5. In the prior report, the generated waste heat is not subjected to recovery research
6. In the existing reports, the continuous output of the sulfur slag is reported less, or the sulfur slag has the sealing property of reporting and answering and the overhaul has no report
Aiming at the problem, a brand-new PDS method sulfur high-efficiency refining production process is urgently needed to be developed so as to meet the requirement of actual use.
Disclosure of Invention
The invention aims to overcome the defects and provide a PDS method sulfur high-efficiency refining production process.
In order to realize the purpose, the invention is realized by the following technical scheme:
a PDS method sulfur high-efficiency refining production process comprises the following steps:
s1, dissolving and filtering, namely adding the sulfur-containing residues generated by PDS desulfurization into a carbon disulfide solvent for mixing to obtain a solid-liquid mixture, pressurizing the solid-liquid mixture through a sulfur foam pump, conveying the solid-liquid mixture to a filtering device for solid-liquid separation, and collecting the separated liquid materials for later use;
s2, performing extraction separation, namely pressurizing the liquid material obtained in the step S1 for the second time, conveying the liquid material into an extraction device, spirally injecting the liquid material into the extraction device along a guide groove in the extraction device, standing, dividing the liquid material flow in the extraction device into a light oil layer, an inorganic salt-containing aqueous solution layer and a sulfur-containing carbon disulfide solution layer from top to bottom along the extraction device, pressurizing the sulfur-containing carbon disulfide solution layer to 0.5MPa by a booster pump, mixing the sulfur-containing carbon disulfide solution layer with 110 ℃ desalted water, and then feeding the mixture into a solvent regeneration system; conveying the light oil and the aqueous solution layer containing inorganic salt to a sewage tank through overflow for collection;
s3, regenerating a solvent, stabilizing the pressure in a regeneration system at 0.2-0.25MPa, conveying the mixture at 110 ℃ in the S2 step to the regeneration system at constant temperature, separating carbon disulfide hydrate from water through the boiling point difference of the carbon disulfide and the water in the high-pressure environment of 0.2-0.25MPa, returning the separated carbon disulfide to the regeneration system, conveying the residual mixture of the sulfur and the water after separation to a flash evaporation system for flash evaporation operation, exchanging heat and condensing desalted water of tail gas containing the carbon disulfide generated in the flash evaporation operation to 25-45 ℃, returning to the S1 step, mixing the tail gas containing the carbon disulfide with the carbon disulfide solvent in the S1 step for use, and collecting the mixture of the sulfur and the water after flash evaporation for later use;
s4, purifying, namely pressurizing the mixture of the sulfur and the water obtained in the step S3 to 0.7MPa, conveying the mixture to a sulfur melting kettle, carrying out sulfur melting operation at the temperature of 140-160 ℃ and under the pressure of 0.5-0.6MPa, feeding liquid sulfur and water generated in the sulfur melting operation into a filtering, liquid separating and desalting system, feeding separated filter residues into a dissolving and filtering system again for sulfur extraction, heating the desalted liquid sulfur to 480 ℃ through heating equipment, purifying the sulfur through a micro reduced pressure distillation device, cooling purified sulfur steam to normal temperature, conveying the cooled sulfur steam to a liquid sulfur tank, collecting and storing the sulfur steam to obtain the finished product of purified sulfur.
Further, in the step S1, the sulfur-containing residue produced by PDS desulfurization is any one of sulfur paste and crude sulfur.
Furthermore, in the step S1, the mixing ratio of the sulfur-containing substances produced by PDS desulfurization and the carbon disulfide solvent is 1: 1.5-5.
Further, in the step S4, when the liquid sulfur and the water are introduced into the filtration system together, the desalted water at 160 ℃ is not as much as the total amount of the mixture of the liquid sulfur and the water is 0.5 to 3 times as much as the total amount of the mixture of the liquid sulfur and the water.
Further, in the step S4, when the liquid sulfur is heated to 480 ℃, the heating ambient pressure of the liquid sulfur is 0.3 to 0.35 MPa.
Further, in the step S4, the operating pressure of the micro-reduced pressure distillation device is 70-80 KPa.
The invention effectively solves the problem of the purity of the sulfur generated by PDS desulfurization, also solves the problems of catalyst separation and more sewage, further solves the problem of solvent regeneration, and also solves the problem of continuous production of the sulfur. Meanwhile, the problems of metal ions such as Na +, K +, Fe3+ and the like in the sulfur are solved. Also solves the problem of sulfur content in the filter residue after filtration.
Drawings
FIG. 1 is a flow chart of the production process of the present invention.
Detailed Description
The invention will be better understood from the following examples. However, those skilled in the art will readily appreciate that the description of the embodiments is only for illustrating the present invention and should not be taken as limiting the invention as detailed in the claims.
Example 1
As shown in figure 1, the PDS method sulfur high-efficiency refining production process comprises the following steps:
s1, dissolving and filtering, namely adding sulfur paste produced by PDS desulfurization into a carbon disulfide solvent for mixing to obtain a solid-liquid mixture, pressurizing the solid-liquid mixture through a sulfur foam pump, conveying the solid-liquid mixture to a filtering device for solid-liquid separation, and collecting the separated liquid material for later use;
s2, performing extraction separation, namely pressurizing the liquid material obtained in the step S1 for the second time, conveying the liquid material into an extraction device, spirally injecting the liquid material into the extraction device along a guide groove in the extraction device, standing, dividing the liquid material flow in the extraction device into a light oil layer, an inorganic salt-containing aqueous solution layer and a sulfur-containing carbon disulfide solution layer from top to bottom along the extraction device, pressurizing the sulfur-containing carbon disulfide solution layer to 0.5MPa by a booster pump, mixing the sulfur-containing carbon disulfide solution layer with 110 ℃ desalted water, and then feeding the mixture into a solvent regeneration system; conveying the light oil and the aqueous solution layer containing inorganic salt to a sewage tank through overflow for collection;
s3, regenerating a solvent, stabilizing the pressure in a regeneration system at 0.2MPa, conveying the mixture at 110 ℃ in the step S2 to the regeneration system at constant temperature, separating the carbon disulfide hydrate from the mixture through the boiling point difference between the carbon disulfide and water under the high-pressure environment of 0.2MPa, returning the separated carbon disulfide to the regeneration system, conveying the mixture of the separated residual sulfur and water to a flash evaporation system for flash evaporation operation, exchanging heat of desalted water of carbon disulfide-containing tail gas generated in the flash evaporation operation, condensing the desalted water to 25 ℃, returning to the step S1, mixing the desalted water with the carbon disulfide solvent in the step S1, and collecting the mixture of the flash evaporated sulfur and water for later use;
s4, purifying, namely pressurizing the mixture of the sulfur and the water obtained in the step S3 to 0.7MPa, conveying the mixture to a sulfur melting kettle, carrying out sulfur melting operation at the temperature of 140-160 ℃ and under the pressure of 0.5-0.6MPa, feeding liquid sulfur and water generated in the sulfur melting operation into a filtering, liquid separating and desalting system, feeding separated filter residues into a dissolving and filtering system again for sulfur extraction, heating the desalted liquid sulfur to 480 ℃ through heating equipment, purifying the sulfur through a micro reduced pressure distillation device, cooling purified sulfur steam to normal temperature, conveying the cooled sulfur steam to a liquid sulfur tank, collecting and storing the sulfur steam to obtain the finished product of purified sulfur.
In the step S1, the mixing ratio of the sulfur paste produced by PDS desulfurization and the carbon disulfide solvent is 1: 1.5.
Meanwhile, when the liquid sulfur and the water are introduced into the filtration system in the step S4, the desalted water at 160 ℃ is not as much as the total amount of the mixture of the liquid sulfur and the water is 0.5 times as much as the total amount of the mixture of the liquid sulfur and the water.
In addition, in the step S4, when the liquid sulfur is heated to 480 ℃, the heating ambient pressure of the liquid sulfur is 0.3 MPa; in the step S4, the operating pressure of the micro-reduced pressure distillation device is 70 KPa.
Example 2
As shown in figure 1, the PDS method sulfur high-efficiency refining production process comprises the following steps:
s1, dissolving and filtering, namely adding crude sulfur produced by PDS desulfurization into a carbon disulfide solvent for mixing to obtain a solid-liquid mixture, pressurizing the solid-liquid mixture through a sulfur foam pump, conveying the solid-liquid mixture to a filter device for solid-liquid separation, and collecting the separated liquid material for later use;
s2, performing extraction separation, namely pressurizing the liquid material obtained in the step S1 for the second time, conveying the liquid material into an extraction device, spirally injecting the liquid material into the extraction device along a guide groove in the extraction device, standing, dividing the liquid material flow in the extraction device into a light oil layer, an inorganic salt-containing aqueous solution layer and a sulfur-containing carbon disulfide solution layer from top to bottom along the extraction device, pressurizing the sulfur-containing carbon disulfide solution layer to 0.5MPa by a booster pump, mixing the sulfur-containing carbon disulfide solution layer with 110 ℃ desalted water, and then feeding the mixture into a solvent regeneration system; conveying the light oil and the aqueous solution layer containing inorganic salt to a sewage tank through overflow for collection;
s3, regenerating a solvent, stabilizing the pressure in a regeneration system at 0.25MPa, conveying the mixture at 110 ℃ in the step S2 to the regeneration system at constant temperature, separating the carbon disulfide from the hydrated carbon disulfide in the mixture through the boiling point difference of the carbon disulfide and a water body under the high-pressure environment of 0.25MPa, returning the separated carbon disulfide to the regeneration system, conveying the mixture of the residual sulfur and the water body after separation to a flash evaporation system for flash evaporation operation, exchanging heat of desalted water of tail gas containing the carbon disulfide generated in the flash evaporation operation, condensing the desalted water to 45 ℃, returning to the step S1, mixing the tail gas containing the carbon disulfide with the carbon disulfide solvent in the step S1 for use, and collecting the mixture of the sulfur and the water body after flash evaporation for later use;
s4, purifying, namely pressurizing the mixture of the sulfur and the water obtained in the step S3 to 0.7MPa, conveying the mixture to a sulfur melting kettle, carrying out sulfur melting operation at the temperature of 140-160 ℃ and under the pressure of 0.5-0.6MPa, feeding liquid sulfur and water generated in the sulfur melting operation into a filtering, liquid separating and desalting system, feeding separated filter residues into a dissolving and filtering system again for sulfur extraction, heating the desalted liquid sulfur to 480 ℃ through heating equipment, purifying the sulfur through a micro reduced pressure distillation device, cooling purified sulfur steam to normal temperature, conveying the cooled sulfur steam to a liquid sulfur tank, collecting and storing the sulfur steam to obtain the finished product of purified sulfur.
Meanwhile, in the step S1, the mixing ratio of the crude sulfur produced by PDS desulfurization and the carbon disulfide solvent is 1: 5.
It should be noted that, when the liquid sulfur and the water are introduced into the filtration system in the step S4, the total amount of the desalted water at 160 ℃ in the mixture of the liquid sulfur and the water is not 3 times of the total amount of the mixture of the liquid sulfur and the water.
Further preferably, in the step S4, when the liquid sulfur is heated to 480 ℃, the heating ambient pressure of the liquid sulfur is 0.35 MP; in the step S4, the operating pressure of the micro-reduced pressure distillation device is 80 KPa.
Example 3
As shown in figure 1, the PDS method sulfur high-efficiency refining production process comprises the following steps:
s1, dissolving and filtering, namely adding a sulfur paste produced by PDS desulfurization and a crude sulfur mixture into a carbon disulfide solvent for mixing to obtain a solid-liquid mixture, pressurizing the solid-liquid mixture through a sulfur foam pump, conveying the solid-liquid mixture to a filter device for solid-liquid separation, and collecting the separated liquid material for later use;
s2, performing extraction separation, namely pressurizing the liquid material obtained in the step S1 for the second time, conveying the liquid material into an extraction device, spirally injecting the liquid material into the extraction device along a guide groove in the extraction device, standing, dividing the liquid material flow in the extraction device into a light oil layer, an inorganic salt-containing aqueous solution layer and a sulfur-containing carbon disulfide solution layer from top to bottom along the extraction device, pressurizing the sulfur-containing carbon disulfide solution layer to 0.5MPa by a booster pump, mixing the sulfur-containing carbon disulfide solution layer with 110 ℃ desalted water, and then feeding the mixture into a solvent regeneration system; conveying the light oil and the aqueous solution layer containing inorganic salt to a sewage tank through overflow for collection;
s3, regenerating a solvent, stabilizing the pressure in a regeneration system at 0.23MPa, conveying the mixture at 110 ℃ in the step S2 to the regeneration system at constant temperature, separating the carbon disulfide hydrate from the carbon disulfide through the boiling point difference between the carbon disulfide and water in the high-pressure environment of 0.24MPa, returning the separated carbon disulfide to the regeneration system, conveying the mixture of the separated residual sulfur and water to a flash evaporation system for flash evaporation operation, exchanging heat of desalted water of carbon disulfide-containing tail gas generated in the flash evaporation operation, condensing the desalted water to 30 ℃, returning to the step S1, mixing the desalted water with the carbon disulfide solvent in the step S1, and collecting the mixture of the flash evaporated sulfur and water for later use;
s4, purifying, namely pressurizing the mixture of the sulfur and the water obtained in the step S3 to 0.7MPa, conveying the mixture to a sulfur melting kettle, carrying out sulfur melting operation at the temperature of 140-160 ℃ and under the pressure of 0.5-0.6MPa, feeding liquid sulfur and water generated in the sulfur melting operation into a filtering, liquid separating and desalting system, feeding separated filter residues into a dissolving and filtering system again for sulfur extraction, heating the desalted liquid sulfur to 480 ℃ through heating equipment, purifying the sulfur through a micro reduced pressure distillation device, cooling purified sulfur steam to normal temperature, conveying the cooled sulfur steam to a liquid sulfur tank, collecting and storing the sulfur steam to obtain the finished product of purified sulfur.
In the step S1, the mixing ratio of the sulfur paste and the crude sulfur produced by PDS desulfurization to the carbon disulfide solvent is 1: 3.
In addition, when the liquid sulfur and the water are introduced into the filtration system in the step S4, the desalted water at 160 ℃ is not as much as the total amount of the mixture of the liquid sulfur and the water is 2.5 times as much as the total amount of the mixture of the liquid sulfur and the water.
Preferably, in the step S4, when the liquid sulfur is heated to 480 ℃, the heating ambient pressure of the liquid sulfur is 0.32 MPa.
In this embodiment, in the step S4, the operating pressure of the micro reduced pressure distillation apparatus is 75 KPa.
The invention effectively solves the problem of the purity of the sulfur generated by PDS desulfurization, also solves the problems of catalyst separation and more sewage, further solves the problem of solvent regeneration, and also solves the problem of continuous production of the sulfur. Meanwhile, the problems of metal ions such as Na +, K +, Fe3+ and the like in the sulfur are solved. The problem of sulfur content in filter residue after filtration is also solved, the purity of the produced sulfur reaches 99.98 percent, and Na +, K + and Fe3+ in the sulfur are respectively 19.21ppm, 1.38ppm and 4.68 ppm.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. A PDS method sulfur high-efficiency refining production process is characterized in that: the PDS method sulfur efficient refining production process comprises the following steps:
s1, dissolving and filtering, namely adding the sulfur-containing residues generated by PDS desulfurization into a carbon disulfide solvent for mixing to obtain a solid-liquid mixture, pressurizing the solid-liquid mixture through a sulfur foam pump, conveying the solid-liquid mixture to a filtering device for solid-liquid separation, and collecting the separated liquid materials for later use;
s2, performing extraction separation, namely pressurizing the liquid material obtained in the step S1 for the second time, conveying the liquid material into an extraction device, spirally injecting the liquid material into the extraction device along a guide groove in the extraction device, standing, dividing the liquid material flow in the extraction device into a light oil layer, an inorganic salt-containing aqueous solution layer and a sulfur-containing carbon disulfide solution layer from top to bottom along the extraction device, pressurizing the sulfur-containing carbon disulfide solution layer to 0.5MPa by a booster pump, mixing the sulfur-containing carbon disulfide solution layer with 110 ℃ desalted water, and then feeding the mixture into a solvent regeneration system; conveying the light oil and the aqueous solution layer containing inorganic salt to a sewage tank through overflow for collection;
s3, regenerating a solvent, stabilizing the pressure in a regeneration system at 0.2-0.25MPa, conveying the mixture at 110 ℃ in the S2 step to the regeneration system at constant temperature, separating carbon disulfide hydrate from water through the boiling point difference of the carbon disulfide and the water in the high-pressure environment of 0.2-0.25MPa, returning the separated carbon disulfide to the regeneration system, conveying the residual mixture of the sulfur and the water after separation to a flash evaporation system for flash evaporation operation, exchanging heat and condensing desalted water of tail gas containing the carbon disulfide generated in the flash evaporation operation to 25-45 ℃, returning to the S1 step, mixing the tail gas containing the carbon disulfide with the carbon disulfide solvent in the S1 step for use, and collecting the mixture of the sulfur and the water after flash evaporation for later use;
and S4, purifying, namely pressurizing the mixture of the sulfur and the water obtained in the step S3 to 0.7MPa, conveying the mixture to a sulfur melting kettle, performing sulfur melting operation at the temperature of 140-160 ℃ and under the pressure of 0.5-0.6MPa, sequentially feeding liquid sulfur and water generated in the sulfur melting operation into a filtering, liquid separating and desalting system, feeding separated filter residues into a dissolving and filtering system again for sulfur extraction, heating the desalted liquid sulfur to 480 ℃ through heating equipment, purifying the sulfur through a micro reduced pressure distillation device, cooling purified sulfur steam to normal temperature, conveying the cooled sulfur steam to a liquid sulfur tank, collecting and storing the sulfur steam, and obtaining the finished product of purified sulfur.
2. The PDS process for efficient refining production of sulfur according to claim 1, wherein: in the step S1, the sulfur-containing residue produced by PDS desulfurization is any one of sulfur paste and crude sulfur.
3. The PDS process for efficient refining production of sulfur according to claim 1, wherein: in the step S1, the mixing ratio of the sulfur-containing substances produced by PDS desulfurization and the carbon disulfide solvent is 1: 1.5-5.
4. The PDS process for efficient refining production of sulfur according to claim 1, wherein: in the step S4, when the liquid sulfur and the water enter the filtering system together, the total amount of the desalted water at 160 ℃ in the mixture of the liquid sulfur and the water is not 0.5 to 3 times of the total amount of the mixture of the liquid sulfur and the water.
5. The PDS process for efficient refining production of sulfur according to claim 1, wherein: in the step S4, when the liquid sulfur is heated to 480 ℃, the heating ambient pressure of the liquid sulfur is 0.3-0.35 MPa.
6. The PDS process for efficient refining production of sulfur according to claim 1, wherein: in the step S4, the operating pressure of the micro-reduced pressure distillation device is 70-80 KPa.
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