CN114804033A - Coke oven gas wet desulphurization resource recycling method - Google Patents
Coke oven gas wet desulphurization resource recycling method Download PDFInfo
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- CN114804033A CN114804033A CN202210255786.6A CN202210255786A CN114804033A CN 114804033 A CN114804033 A CN 114804033A CN 202210255786 A CN202210255786 A CN 202210255786A CN 114804033 A CN114804033 A CN 114804033A
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- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000000571 coke Substances 0.000 title claims abstract description 9
- 238000004064 recycling Methods 0.000 title claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 91
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 85
- 239000011593 sulfur Substances 0.000 claims abstract description 84
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 84
- 238000004821 distillation Methods 0.000 claims abstract description 55
- 239000007788 liquid Substances 0.000 claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 claims abstract description 18
- 238000011084 recovery Methods 0.000 claims abstract description 14
- 239000002912 waste gas Substances 0.000 claims abstract description 14
- 239000007789 gas Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 238000004806 packaging method and process Methods 0.000 claims abstract description 6
- 239000002699 waste material Substances 0.000 claims abstract description 5
- 238000002844 melting Methods 0.000 claims abstract description 4
- 230000008018 melting Effects 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims description 18
- 239000002893 slag Substances 0.000 claims description 13
- 238000003860 storage Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000006477 desulfuration reaction Methods 0.000 claims description 6
- 230000023556 desulfurization Effects 0.000 claims description 6
- 238000000746 purification Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- 238000002309 gasification Methods 0.000 claims description 3
- 238000010924 continuous production Methods 0.000 abstract description 4
- 238000000926 separation method Methods 0.000 abstract description 4
- 239000011280 coal tar Substances 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 8
- 239000006227 byproduct Substances 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 239000003921 oil Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000003245 coal Substances 0.000 description 4
- 238000001914 filtration Methods 0.000 description 3
- 239000003345 natural gas Substances 0.000 description 3
- 238000004939 coking Methods 0.000 description 2
- 239000010779 crude oil Substances 0.000 description 2
- 238000010908 decantation Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005188 flotation Methods 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 239000002956 ash Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000010883 coal ash Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000012946 outsourcing Methods 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
- C01B17/0216—Solidification or cooling of liquid sulfur
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0078—Condensation of vapours; Recovering volatile solvents by condensation characterised by auxiliary systems or arrangements
- B01D5/009—Collecting, removing and/or treatment of the condensate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/004—Multifunctional apparatus for automatic manufacturing of various chemical products
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
- C01B17/0221—Melting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00002—Chemical plants
- B01J2219/00027—Process aspects
- B01J2219/00033—Continuous processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00139—Controlling the temperature using electromagnetic heating
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a method for recycling coke oven gas wet desulphurization resources, which comprises the steps of primary low-temperature sulfur melting of crude sulfur, secondary heating, tertiary heating, distillation, a sulfur condenser, a sulfur receiving tank, a closed slicer, a sulfur packaging machine, warehousing, waste gas separation and recovery, and waste residue separation and recovery. Therefore, high-grade sulfur can be continuously produced, and the quality consistency of products is improved. The method can obtain over 99.95% of industrial superior sulfur; the coal tar is recycled, and secondary environmental pollution is avoided. After being recycled, the sulfur resource can be saved, and the foreign exchange expenditure can be saved. In addition, due to the adoption of an electromagnetic heating mode, the electric energy utilization rate is high, the energy is saved, the environment is protected, and each distillation tank is in a normal pressure state in the whole production process, so that the safety and the reliability are realized. Meanwhile, after each tank reaches a set temperature value, the liquid level is controlled by each tank liquid level meter, so that the output of finished products and the input of raw materials reach a balance value, and continuous production in a strict sense is realized.
Description
Technical Field
The invention relates to a method for recycling coke oven gas wet desulphurization resources.
Background
Sulfur is an important chemical raw material, and is widely applied to industrial departments of chemical industry, metallurgy, pesticides, rubber, fuel, paper making and the like. China has large demand for sulfur, but sulfur resources are less, and market supply gaps are larger. In addition, with the development of a large amount of sulfur-containing crude oil and natural gas resources in the world, the sulfur recovery device becomes an indispensable matching device for processing coal, sulfur-containing natural gas and sulfur-containing crude oil in large-scale coal chemical plants, natural gas purification plants, oil refineries and petrochemical plants. In China, the coal chemical industry develops rapidly in recent years, and the recovery situation of sulfur in coal is concerned. Therefore, the coke oven gas of the coke-oven plant can obtain the byproduct of crude sulfur after wet desulphurization. However, because the coke oven gas contains a large amount of coal tar, ash and the like, the substances can enter the crude sulfur, so that the obtained crude sulfur has low sulfur content and black color, cannot be directly used for industrial production and has low value. In addition, the recovered crude sulfur cannot directly enter the market, and the treatment cost is high. Further purification is required to meet the requirements of industrial production and use.
At present, the domestic and foreign desulfurization methods mainly comprise a high-pressure decantation method, a flotation method, a heat filtration method, a granulation screening method, a vacuum distillation method, a solvent method and the like. The sulfur obtained by the high-pressure decantation method, the flotation method and the granulation screening method has low quality. The equipment required by the hot filtration method is complex, the residual sulfur in the filter residue is more, and the yield is not high. The methods can not realize continuous production, have low productivity and high operation cost, and are not suitable for popularization and application of production enterprises. Therefore, it is necessary to improve and perfect the desulfurization method described above.
Disclosure of Invention
In view of the current state of the technology, the invention provides a method for recycling coke oven gas wet desulphurization resources, according to the great difference of physicochemical properties of sulfur and other impurities and the change rule of solid/liquid/gas state of sulfur, the purification is carried out by adopting a low-temperature non-pressure condensation method, the production process is safe and reliable, the product purity reaches more than 99.95 percent, and the problem of byproduct treatment in the coking plant enterprise industry is well solved.
The technical solution of the invention is as follows: a coke oven gas wet desulphurization resource recycling method comprises the following steps:
1. firstly, sorting crude sulfur produced by desulfurization, and conveying the crude sulfur into a low-temperature treatment tank for first heating and melting to complete liquefaction of raw materials, wherein the temperature is required to be 150 degrees;
2. conveying the liquefied sulfur mixture melted at low temperature into a first heating tank through a pipeline for secondary heating liquefaction, wherein the temperature is required to be 250 degrees;
3. conveying the liquefied sulfur mixture subjected to secondary heating to a second heating tank through a pipeline for carrying out tertiary heating liquefaction, wherein the temperature is required to be 350 ℃;
4. and conveying the liquefied sulfur mixture which is completely liquefied by heating for three times into a distillation tank through a pipeline for fourth heating, gasification, distillation and purification. The waste gas is collected and treated by a recovery device and discharged after reaching the standard, the waste residue is collected and transferred to enter downstream enterprises for secondary treatment, and the distillation temperature is required to be 450 degrees;
5. conveying the gasified sulfur in the distillation tank to a condensing device through a pipeline, and forming high-purity liquid sulfur after cooling and condensing, wherein the condensing mode is completed by combining natural air cooling with a water circulation cooling method, and the condensing process is closed operation, so that the reuse of condensed water is ensured;
6. conveying the condensed liquid sulfur to a closed slicer through a pipeline, preparing flaky particles with the particle size of less than 3mm by the slicer, and packaging to obtain a finished product.
The equipment used in the production method of the invention is as follows: comprises a primary low-temperature treatment tank, a secondary heating tank, a tertiary heating tank and a distillation tank which are arranged in sequence; the primary low-temperature treatment tank, the secondary heating tank, the tertiary heating tank and the distillation tank are connected with one another through a first pipeline, a second pipeline and a third pipeline, a first high-temperature electric butterfly valve, a second high-temperature electric butterfly valve and a third high-temperature electric butterfly valve are correspondingly arranged on the pipelines, and a raw material conveying device is arranged at a feed inlet of the primary low-temperature treatment tank; a fourth pipeline is arranged at the bottom of the distillation tank and connected with the top of the slag discharging tank, a slag discharging port is arranged at the bottom of the slag discharging tank, and a fourth high-temperature electric butterfly valve is arranged on the fourth pipeline; the tops of the primary low-temperature treatment tank, the secondary heating tank, the tertiary heating tank and the distillation tank are respectively connected with a waste gas pipeline through a first branch pipeline to a fourth branch pipeline, and a fifth high-temperature electric butterfly valve is arranged on the waste gas pipeline positioned on one side of the distillation tank; wherein a fifth pipeline is arranged at the top of the distillation tank and connected with the condenser, a sixth high-temperature electric butterfly valve is arranged on the fifth pipeline, and a storage tank is arranged corresponding to the lower part of the condenser; a feed inlet is arranged on one side of the primary low-temperature treatment tank, and a raw material conveying device is arranged at the feed inlet; a fifth branch pipeline connecting pipeline is arranged at the bottom of the primary low-temperature treatment tank, is communicated with a sixth branch pipeline arranged at the bottom of the tertiary heating tank, and is provided with a seventh high-temperature electric butterfly valve and an eighth high-temperature electric butterfly valve which are arranged on the fifth branch pipeline and the sixth branch pipeline; the bottom of the secondary heating tank is provided with a pipeline connected with the slag discharge recovery tank, and the pipeline is provided with a ninth high-temperature electric butterfly valve.
In the invention, electromagnetic heating systems are respectively arranged outside the primary low-temperature treatment tank, the secondary heating tank, the tertiary heating tank and the distillation tank.
In the invention, the first to fourth branch pipelines and the storage box, which are connected with the waste gas pipeline, of the first to fourth pipelines are provided with a heat conduction oil or steam heating system.
In the invention, a stirrer is arranged in the low-temperature treatment tank, and the stirrer is of a vertical shaft type double-layer stirring blade structure.
In the invention, a liquidometer and a metering pump arranged at the bottom of each tank are respectively arranged in the primary low-temperature treatment tank, the secondary heating tank, the tertiary heating tank and the distillation tank.
1) The product quality meets the admission standard
The latest industrial sulfur standard adopts the national quality standard GB/T2449.1-2014 Industrial Sulfur, and the specific standard technical index requirements are shown in tables 5-4.
TABLE 5-4 technical indices of Industrial Sulfur
First-class qualified product with excellent index name
Sulfur (S) is more than or equal to 99.95 percent, 99.50 percent and 99.00 percent
Water content less than or equal to 0.10%, 0.50%, 1.00%
Ash content is less than or equal to 0.03 percent, 0.10 percent and 0.20 percent
Acidity (calculated by H2SO 4) is less than or equal to 0.003 percent, 0.005 percent and 0.02 percent
Organic matter is less than or equal to 0.03 percent, 0.30 percent and 0.80 percent
Arsenic (As) is less than or equal to 0.0001%, 0.01% and 0.05%
Iron (Fe) is less than or equal to 0.003 percent and 0.005 percent
Sieve residue
Pore diameter of 150um is not more than 3.0
The pore diameter is not less than 75um and not more than 0.51.04.0
Note: the screen residue index in the table is for powdered sulphur only.
2) The resource, the energy consumption, the comprehensive utilization of byproducts and the like completely meet the requirements. The method has the advantages of effectively utilizing the smoke desulfurization byproducts of coking enterprises to produce available national standard sulfur products, meeting the requirement of the circular industry, having advanced production technology, no production wastewater discharge, standard discharge of treated smoke, and adoption of electric energy as a main energy source.
The invention has the beneficial effects that: the whole production process is highly automated, is free from manual field operation, can continuously produce high-grade sulfur, and improves the consistency of product quality. The method can obtain over 99.95% of industrial superior sulfur; coal tar is recycled, and secondary environmental pollution is avoided; over 1000 million tons of sulfur are imported nationwide every year, and sulfur resources and foreign exchange expenses can be saved after the sulfur is recycled. In addition, due to the adoption of an electromagnetic heating mode, the electric energy utilization rate is high, the energy is saved, the environment is protected, and each tank is in a normal pressure state in the whole production process, so that the safety and the reliability are realized. Meanwhile, after each tank reaches a set temperature value, the liquid level of each tank is controlled by a liquid level meter, so that the output of finished products and the input of raw materials reach a balance value, and continuous production in a strict sense is realized.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a schematic view of a process apparatus.
Detailed Description
The present invention will be further described with reference to the process flow and process equipment.
The process flow diagram is given in figure 1, and comprises the following steps:
the method comprises the following steps of primary low-temperature sulfur melting a of crude sulfur, secondary heating b, tertiary heating c, distillation d, a sulfur condenser e, a sulfur storage tank f, a closed slicing machine g, a sulfur packaging machine h, a storage i, waste gas separation and recovery j and waste residue separation and recovery k.
The process equipment shown in figure 2 comprises a primary low-temperature treatment tank 2, a secondary heating tank 6, a tertiary heating tank 10 and a distillation tank 14 which are sequentially arranged, wherein the tanks of the primary low-temperature treatment tank 2, the secondary heating tank 6, the tertiary heating tank 10 and the distillation tank 14 are connected with one another through a first pipeline 4, a second pipeline 8 and a third pipeline 12, and a first high-temperature electric butterfly valve 5, a second high-temperature electric butterfly valve 9 and a third high-temperature electric butterfly valve 13 are respectively arranged on the first pipeline 4, the second pipeline 8 and the third pipeline 12 correspondingly; a fourth pipeline 16 is arranged at the bottom of the distillation retort 14 and connected with the top of a slag discharge tank 18, a slag discharge port is arranged at the bottom of the slag discharge tank 18, and a fourth high-temperature electric butterfly valve 17 is arranged on the fourth pipeline 16; the top of the primary low-temperature treatment tank 2, the secondary heating tank 6, the tertiary heating tank 10 and the distillation tank 14 are respectively connected with an exhaust gas pipeline 23 through a first branch pipeline 3, a second branch pipeline 7, a third branch pipeline 11 and a fourth branch pipeline 15, the exhaust gas pipeline 23 positioned on one side of the distillation tank 14 is provided with a fifth high-temperature electric butterfly valve 24, the top of the distillation tank 14 is provided with a fifth pipeline 20 connected with a condenser 21, the fifth pipeline 20 is provided with a sixth high-temperature electric butterfly valve 25, and the lower part of the condenser 21 is provided with a storage tank 22; a feed inlet 1 is arranged on one side of the primary low-temperature treatment tank 2, and a raw material conveying device is arranged at the feed inlet; a fifth branch pipeline 19 connecting pipeline 27 which is arranged at the bottom of the primary low-temperature treatment tank 2 is communicated with a sixth branch pipeline 31 which is arranged at the bottom of the tertiary heating tank 10, and a seventh high-temperature electric butterfly valve 26 and an eighth high-temperature electric butterfly valve 32 which are arranged on the fifth branch pipeline 19 and the sixth branch pipeline 31; the bottom of the secondary heating tank 6 is provided with a pipeline 28 connected with a slag discharge recovery tank 30, and the pipeline 28 is provided with a ninth high-temperature electric butterfly valve 29.
In the present invention, the primary low-temperature treatment tank 2, the secondary heating tank 6, the tertiary heating tank 10, and the distillation tank 14 are respectively provided with an electromagnetic heating system (not shown in the figure) at the bottom.
In the invention, the first to fourth pipelines, the first to fourth branch pipelines connected with the waste gas pipeline and the storage tank are provided with a heat conducting oil or steam heating system.
In the present invention, a stirrer 33 is provided in the primary low-temperature treatment tank 2, and the stirrer 33 has a vertical shaft type double-layer stirring blade structure.
In this embodiment, the primary low-temperature treatment tank, the secondary heating tank, the tertiary heating tank and the distillation tank are respectively provided with a level gauge and a metering pump installed on the bottom of each tank.
In the invention, stainless steel container tanks (a low-temperature treatment tank, a first heating tank, a second heating tank, a distillation tank, a slag discharge tank, a storage tank and a condensing device) used in the production equipment belong to a processing part, and other related high-temperature electric butterfly valves, liquid level meters, waste gas recovery devices, slicing machines, raw material conveying devices and automatic packaging machines belong to outsourcing equipment.
The specific production method comprises the following steps:
1. dissolving and filtering, namely conveying the crude sulfur produced by desulfurization into a primary low-temperature treatment tank 2 through a spiral quantitative feeder after sorting, heating for the first time, stirring by a vertical shaft type reaction stirrer system in the primary low-temperature treatment tank 2 to ensure that the stirring strength of the crude sulfur is gradually reduced to meet the optimal uniform heating effect, so that the raw material is liquefied within 1 hour, and the temperature in the primary low-temperature treatment tank 2 is required to be 150 degrees; the capacity of the liquefied sulfur mixture in the primary low-temperature treatment tank 2 is not more than 80% of the total capacity of the tank body, when the liquefied sulfur mixture reaches the maximum capacity, a first high-temperature electric butterfly valve 5 on a first pipeline 4 connected between the low-temperature treatment tank and a secondary heating tank 6 is opened, and the liquid sulfur mixture melted at the primary low temperature is conveyed into the secondary heating tank 6 for secondary heating;
2. the liquefied sulfur mixed material is quantitatively conveyed by an automatic control system of a sulfur metering pump, the conveying amount is equal to the input amount of a screw type quantitative feeder of the primary low-temperature treatment tank 2, the capacity of the liquefied sulfur mixture in the primary low-temperature treatment tank 2 is kept at the highest value, the liquefied sulfur mixture in the secondary heating tank 6 is secondarily heated, the heating time is 1 hour, and the secondary heating temperature is required to be 250 degrees; when the capacity of the liquefied sulfur mixture in the secondary heating tank 6 reaches 80% of the total capacity of the tank body, a second high-temperature electric butterfly valve 9 on a second pipeline 8 connected between the secondary heating tank 6 and the tertiary heating tank 10 is opened, and the liquefied sulfur mixture is conveyed into the tertiary heating tank 10 to be heated for three times;
3. the liquefied sulfur mixed material is quantitatively conveyed into a tertiary heating tank 10 for tertiary heating through an automatic control system of a sulfur metering pump; the conveying capacity is equal to that of the secondary heating tank 6 and the primary low-temperature treatment tank, the third heating time is 1 hour, and the heating temperature in the tertiary heating tank 10 is required to be 350 degrees;
4. when the capacity of the liquefied sulfur mixture in the third heating tank 10 reaches 80% of the total capacity of the tank body, a third high-temperature electric butterfly valve 13 on a third pipeline 12 connected between the third heating tank 10 and the distillation tank 14 is opened, the liquefied sulfur mixture is quantitatively conveyed into the distillation tank 14 through an automatic control system of a sulfur metering pump, the conveying amount is equal to the conveying amount of the third heating tank 10, the liquefied sulfur mixture in the distillation tank 14 is heated for four times, the heating time is 1 hour, and the temperature in the distillation tank 14 is required to be 450 degrees;
5. when the temperature in the distillation retort 14 reaches 450 ℃, carrying out gasification distillation purification on sulfur in the liquefied sulfur mixture, opening a sixth electric butterfly valve 25 on a fifth pipeline 20 connected between the distillation retort 14 and the condenser 21, closing a fifth electric butterfly valve 24 on the distillation retort 14 and the waste gas pipeline 23, and conveying the gasified sulfur in the distillation retort 14 to the condenser 21 through a pipeline;
6. after the gasified sulfur in the distillation retort 14 is conveyed to the condenser 21 through a pipeline, the temperature is reduced and condensed by the condenser 21 to form high-purity liquid sulfur, the condensing mode is completed by combining air natural cooling with a water circulation cooling mode, and the condensing process adopts closed operation to ensure the reuse of condensed water.
7. The condensed liquid sulfur is stored in a storage tank 22 at the lower end of a condenser 21, a heat conduction oil or steam heating system is arranged in the storage tank 22, the temperature of the liquid sulfur is controlled to be 130-150 degrees, the liquid sulfur in the storage tank 22 is quantitatively conveyed to a closed slicing machine through an automatic control system of a sulfur metering pump, and is made into flaky particles with the diameter of more than 3 millimeters through the slicing machine, and the flaky particles are packaged and stored in a warehouse through an automatic packaging machine.
In the invention, when the distillation residue in the distillation tank 14 reaches a certain amount and affects normal production, the third high-temperature electric butterfly valve 13 on the third pipeline 12 between the distillation tank 14 and the third heating tank 10 is closed, the fourth high-temperature electric butterfly valve 17 on the fourth pipeline 16 connected between the distillation tank 14 and the residue discharge tank 18 is opened, the distillation residue in the distillation tank 14 is discharged into the residue discharge tank 18, and the distillation residue is discharged from the residue discharge port 19 of the residue discharge tank 18 and collected after being cooled.
According to the invention, the impurities in the liquid sulfur mixture are gradually purified by controlling different temperature points of each tank according to the principle of different boiling points of different substances. And collecting the distillation residue in the distillation tank as a byproduct and selling the byproduct to downstream production enterprises for secondary treatment. And the waste gas is collected by the recovery device and then discharged after reaching the standard.
In the present invention, the exhaust gas from each tank is collected by a recovery device (not shown) and then discharged after reaching standards.
In the invention, the pipelines connected with the tanks and the waste gas pipelines of the tanks are provided with heat conducting oil or steam heating systems to ensure the normal operation of the system.
In the invention, each tank is in a normal pressure state in the whole production process. And after each tank reaches a set temperature value, the liquid level is controlled by a liquid level meter of each tank, so that the output of the finished product and the input of the raw material reach an average value. Thereby realizing the continuous production in strict sense.
Claims (6)
1. A method for recycling coke oven gas wet desulphurization resources comprises the following steps:
1) firstly, sorting crude sulfur produced by desulfurization, and conveying the crude sulfur into a primary low-temperature treatment tank for primary heating and melting to complete liquefaction of raw materials, wherein the temperature is required to be 150 degrees;
2) conveying the liquefied sulfur mixture melted at low temperature into a secondary heating tank through a pipeline for secondary heating liquefaction, wherein the temperature is required to be 250 degrees;
3) conveying the liquefied sulfur mixture subjected to secondary heating to a tertiary heating tank through a pipeline for tertiary heating liquefaction, wherein the temperature is required to be 350 ℃;
4) conveying the liquefied sulfur mixture completely liquefied by three times of heating to a distillation tank through a pipeline for four times of heating, gasification, distillation and purification, collecting and treating waste gas by a recovery device to reach the standard, discharging, collecting and storing waste residues, and allowing the waste residues to enter downstream enterprises for secondary treatment, wherein the distillation temperature is required to be 450 degrees;
5) conveying the gasified sulfur in the distillation tank to a condensing device through a pipeline, and forming high-purity liquid sulfur after cooling and condensing, wherein the condensing mode is completed by combining natural air cooling with a water circulation cooling method, and the condensing process is closed operation, so that the reuse of condensed water is ensured;
6) conveying the condensed liquid sulfur to a closed slicer through a pipeline, preparing the liquid sulfur into flaky particles with the particle size of less than 3mm by the slicer, and packaging the flaky particles into finished products.
2. The apparatus for the production method according to claim 1, which comprises a primary low-temperature treatment tank, a secondary heating tank, a tertiary heating tank and a distillation tank arranged in sequence; the primary low-temperature treatment tank, the secondary heating tank, the tertiary heating tank and the distillation tank are connected with one another through a first pipeline, a second pipeline and a third pipeline, and a first high-temperature electric butterfly valve, a second high-temperature electric butterfly valve and a third high-temperature electric butterfly valve are correspondingly arranged on the pipelines; a fourth pipeline is arranged at the bottom of the distillation tank and connected with the top of the slag discharging tank, a slag discharging port is arranged at the bottom of the slag discharging tank, and a fourth high-temperature electric butterfly valve is arranged on the fourth pipeline; the tops of the primary low-temperature treatment tank, the secondary heating tank, the tertiary heating tank and the distillation tank are respectively connected with a waste gas pipeline through a first branch pipeline to a fourth branch pipeline, and a fifth high-temperature electric butterfly valve is arranged on the waste gas pipeline positioned on one side of the distillation tank; wherein a fifth pipeline is arranged at the top of the distillation tank and connected with the condenser, a sixth high-temperature electric butterfly valve is arranged on the fifth pipeline, and a storage tank is arranged corresponding to the lower part of the condenser; a feed inlet is arranged on one side of the primary low-temperature treatment tank, and a raw material conveying device is arranged at the feed inlet; a fifth branch pipeline connecting pipeline is arranged at the bottom of the primary low-temperature treatment tank, is communicated with a sixth branch pipeline arranged at the bottom of the tertiary heating tank, and is provided with a seventh high-temperature electric butterfly valve and an eighth high-temperature electric butterfly valve which are arranged on the fifth branch pipeline and the sixth branch pipeline; the bottom of the secondary heating tank is provided with a pipeline connected with the slag discharge recovery tank, and the pipeline is provided with a ninth high-temperature electric butterfly valve.
3. The production equipment according to claim 2, wherein the primary low-temperature treatment tank, the secondary heating tank, the tertiary heating tank and the distillation tank are externally provided with electromagnetic heating systems respectively.
4. The production equipment as claimed in claim 2, wherein the first to fourth branch pipes and the storage tank connected with the first to fourth pipes and the exhaust gas pipe are provided with a heat conducting oil or steam heating system.
5. The production facility as claimed in claim 2, wherein a stirrer of a vertical shaft type double-layer stirring blade structure is provided in the low-temperature treatment tank.
6. The production apparatus as claimed in claim 2, wherein the liquid level meter and the metering pump are provided in the primary low-temperature treatment tank, the secondary heating tank, the tertiary heating tank and the distillation tank, respectively.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115180596A (en) * | 2022-08-02 | 2022-10-14 | 张桂芬 | Method and equipment for continuously refining and purifying sulfur from crude sulfur |
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| US2961301A (en) * | 1958-02-18 | 1960-11-22 | Blaw Knox Co | Method and apparatus for processing sulfur |
| CN107673313A (en) * | 2017-09-30 | 2018-02-09 | 杨波 | The processing recovery process of sulfur waste sulphur in a kind of chloride |
| CN110304609A (en) * | 2018-03-27 | 2019-10-08 | 中国科学院过程工程研究所 | A kind of sulphur purification schemes suitable for coal gas direct-reduction metallurgical gas production |
| CN212855681U (en) * | 2020-05-27 | 2021-04-02 | 湖北鄂中生态工程股份有限公司 | Multi-stage heating sulfur melting device |
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2022
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2961301A (en) * | 1958-02-18 | 1960-11-22 | Blaw Knox Co | Method and apparatus for processing sulfur |
| CN107673313A (en) * | 2017-09-30 | 2018-02-09 | 杨波 | The processing recovery process of sulfur waste sulphur in a kind of chloride |
| CN110304609A (en) * | 2018-03-27 | 2019-10-08 | 中国科学院过程工程研究所 | A kind of sulphur purification schemes suitable for coal gas direct-reduction metallurgical gas production |
| CN212855681U (en) * | 2020-05-27 | 2021-04-02 | 湖北鄂中生态工程股份有限公司 | Multi-stage heating sulfur melting device |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115180596A (en) * | 2022-08-02 | 2022-10-14 | 张桂芬 | Method and equipment for continuously refining and purifying sulfur from crude sulfur |
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