CN112010269A - Device and method for preparing acid from hydrogen sulfide-containing acid gas - Google Patents
Device and method for preparing acid from hydrogen sulfide-containing acid gas Download PDFInfo
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- CN112010269A CN112010269A CN202010751163.9A CN202010751163A CN112010269A CN 112010269 A CN112010269 A CN 112010269A CN 202010751163 A CN202010751163 A CN 202010751163A CN 112010269 A CN112010269 A CN 112010269A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/74—Preparation
- C01B17/76—Preparation by contact processes
- C01B17/80—Apparatus
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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
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/74—Preparation
- C01B17/76—Preparation by contact processes
- C01B17/765—Multi-stage SO3-conversion
- C01B17/7655—Multi-stage SO3-conversion with intermediate absorption
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/74—Preparation
- C01B17/76—Preparation by contact processes
- C01B17/80—Apparatus
- C01B17/806—Absorbers; Heat exchangers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention belongs to the technical field of sulfuric acid device process system optimization, and particularly relates to a device and a method for preparing acid from hydrogen sulfide acidic gas. The invention provides an air drying unit, a NOx removal unit and a medium-low temperature two-stage drying unit which are introduced into a hydrogen sulfide acid gas treatment process system, and the water balance of the drying and absorption processes is effectively maintained through the introduction of the air drying unit and the medium-low temperature two-stage drying unit, so that a purification process section with complex flow, large floor area and high investment in the traditional dry acid preparation process flow is omitted, the problem of high difficulty in treating the dilute acid generated in the purification process section is solved, the floor area and the investment of a device are also saved, and the quality of the acid generated cannot change along with seasons and regional humidity. And the NOx is prevented from entering an acid making system by introducing the NOx removing unit, so that the quality of the product acid is effectively improved. The tail gas treatment unit adopts a green oxidant hydrogen peroxide, so that the total sulfur utilization rate is improved.
Description
Technical Field
The invention relates to a method for optimizing a sulfuric acid production process, which is suitable for producing sulfuric acid by taking hydrogen sulfide as a raw material, in particular to a device and a method for preparing acid by using acid gas containing hydrogen sulfide, and belongs to the field of environmental protection of petroleum refining technology.
Background
In the industrial production process such as petroleum refining, natural gas purification and the like, a large amount of hydrogen sulfide-containing acid gas is generated. At present, most petrochemical enterprises adopt a Claus method sulfur recovery process for treating hydrogen sulfide. The other idea of treating the hydrogen sulfide acid gas is to directly prepare the hydrogen sulfide acid gas into sulfuric acid, and the hydrogen sulfide acid gas has the following advantages: firstly, the direct acid preparation process of hydrogen sulfide is simpler than the acid preparation process after sulfur is recovered, so that the loss of an intermediate link is reduced, the energy consumption is reduced, and the economic benefit is increased; secondly, the method can more easily meet the environmental protection requirement. The method for preparing sulfuric acid can be divided into 'wet method' and 'dry method' for preparing acid. The investment of the wet acid making is high, and the requirement on the material of the equipment is high. Compared with the wet method, the dry method acid preparation has smaller investment and low requirements on equipment and pipeline materials.
The prior domestic hydrogen sulfide dry-method acid making device has the following problems: the presence of water, which is greater than the water required for the combination of sulfur into acid, generated by the incineration of hydrogen sulfide in acid gas and other hydrogen-containing substances such as hydrocarbons, and the water brought by combustion air, affects the water balance of the subsequent drying and absorption processes. In summer and coastal areas with high air humidity, the problem is more obvious and even influences the quality of acid production. And the water content in the furnace gas needs to reach 0.1g/Nm before the sulfur dioxide is converted into sulfur trioxide3The normal operation of the catalytic conversion can be guaranteed. In order to solve the problem, the prior hydrogen sulfide dry-method acid making device is matched with furnace gas purification and drying processes, but the purification process is complex, the occupied area is large, the investment is high, and 1-2 t of dilute acid with the mass fraction of about 5-10% can be discharged when 1t of sulfuric acid is produced. Secondly, in the purification process, a large amount of moisture in the furnace gas is removed by adiabatic humidification and cooling, and the temperature of the furnace gas is reduced from 300-380 ℃ to about 40 ℃ for drying. A small amount of SO is contained in the furnace gas in the process3And water vapor, as the temperature drops to the dew point, condense to form acid mist that still requires an electric mist eliminator to remove and corrode equipment and piping. In addition, the dried furnace gas still needs a heat exchanger to exchange heat to 400-450 ℃ and enters a catalytic bed layer for catalytic conversion. Although the process of cooling and then heating the furnace gas achieves the effect of water removal, the energy consumption of the device is increased.
The refinery acid gas is usually composed of 5% -99.5% of H2S, 1-5% NH3Hydrocarbons and other gases, wherein NH3The incomplete combustion of (2) necessarily results in the production of NOx. However, most of denitration units of the domestic sulfuric acid device exist for treating NOx in tail gas at present, and the denitration units have the problem that NOx enters the twice acid making and absorbing units along with the furnace gas and is combined with sulfuric acid to influence the quality of product acid.
Disclosure of Invention
The invention aims to provide a method and a device for preparing acid from acidic gas containing hydrogen sulfide, aiming at the defects of the existing technology for preparing acid from acidic gas containing hydrogen sulfide according to the requirements of the national policies related to energy conservation, emission reduction and environmental protection development. By optimizing the process flow, an air drying unit, an NOx removal unit and a medium-low temperature two-stage drying unit are introduced into a process device for producing sulfuric acid from hydrogen sulfide acidic gas. The process device meets the process production requirement, simultaneously omits the purification process in the traditional dry acid making process flow, effectively simplifies the process flow, reduces the occupied area and the investment, recovers heat as much as possible, and has the advantages of simple process flow, energy conservation, environmental protection, low device investment and the like.
The purpose of the invention can be realized by the following technical scheme:
a device for preparing acid from acidic gas containing hydrogen sulfide comprises an air drying unit, a conversion unit and a first absorption tower, wherein an air output pipeline is connected with an incinerator through the air drying unit, a hydrogen sulfide gas output pipeline is also connected with the incinerator, the output end of the incinerator is connected with a gas mixing tower through a waste heat boiler and a superheater, the output end of the bottom of the gas mixing tower is connected with the bottom of a medium-low temperature two-stage drying tower through a NOx remover and a first economizer, the top of the medium-low temperature two-stage drying tower is connected with the lower part of a nicotinic acid tower and/or the lower part of the first absorption tower through the conversion unit and a second economizer, the output end of the top of the second economizer is respectively connected with the lower part of the nicotinic acid tower and/or the lower part of the first absorption tower, and the output end of the top; the output end of the top of the first absorption tower is connected with the lower part of the second absorption tower through a conversion unit, and the output end of the top of the second absorption tower is connected with an electric demister through a tail absorption tower;
the first absorption tower and the second absorption tower are provided with matched absorption tower circulating grooves, the bottom end of the first absorption tower and the bottom end of the second absorption tower are both connected with the absorption tower circulating grooves, one output end of each absorption tower circulating groove is connected with the upper part of the first absorption tower through a cooler, and the other output end of each absorption tower circulating groove is connected with the upper part of the second absorption tower through a cooler; the nicotinic acid tower is provided with a matched nicotinic acid tower circulating groove, the bottom end of the nicotinic acid tower is connected with the nicotinic acid tower circulating groove, one output end of the nicotinic acid tower circulating groove is connected with the upper part of the nicotinic acid tower circulating groove through a cooler, and the other output end of the nicotinic acid tower circulating groove is used as product acid to be output.
The technical scheme of the invention is as follows: the middle-low temperature two-stage drying tower is provided with a matched drying tower circulating groove, the bottom end of the middle-low temperature two-stage drying tower is connected with the drying tower circulating groove, and the output end of the drying tower circulating groove is respectively connected with the upper part and the middle part of the middle-low temperature two-stage drying tower through a cooler.
The technical scheme of the invention is as follows: the absorption tower circulating groove is also provided with an output end connected with the drying tower circulating groove.
The technical scheme of the invention is as follows: the mixed gas of ammonia gas and air is connected with the gas mixing tower through an ammonia and air mixer. A method for preparing acid from acid gas containing hydrogen sulfide by using the device comprises the following steps:
1) the acid gas containing hydrogen sulfide is fully mixed and combusted in the incinerator 4 through the hydrogen sulfide buffer tank and the dry air which is subjected to freezing adsorption and dehumidification by the air drying unit to generate furnace gas;
2) the furnace gas temperature of the hydrogen sulfide combustion furnace reaches 1050-1200 ℃, the furnace gas temperature is reduced to 300-420 ℃ after heat is recovered by a waste heat boiler and a superheater, and the furnace gas is mixed with mixed gas of ammonia gas and air and then enters a NOx removal reactor to remove NOx;
3) furnace gas from a NOx removal reactor is subjected to waste heat recovery by an economizer, the temperature of the furnace gas is about 180-250 ℃, the furnace gas enters a medium-low temperature two-stage drying tower and is fully contacted with concentrated sulfuric acid sprayed at the top and the middle of the tower, the concentrated sulfuric acid absorbing moisture in sulfur dioxide gas is discharged from the bottom of the tower to an acid circulation tank of the drying tower, and then is sent to an acid cooler of the drying tower by a circulation pump, and is sent to the top and the middle of the tower for spraying after being cooled to 45-55 ℃;
4) SO-treated furnace gas subjected to two-stage medium-low temperature drying2The method comprises the steps of pressurizing a blower, then entering a secondary conversion unit, recycling residual heat from a coal economizer to obtain gas after primary conversion, reducing the temperature to 170-180 ℃, entering a nicotinic acid tower and/or a first absorption tower, and obtaining SO in furnace gas in the first absorption tower3Absorbed by acid sprayed on the top of the tower, and the concentrated sulfuric acid with the temperature of 90-100 ℃ after absorbing sulfur trioxide enters an absorption tower from the bottom of the towerIn the circulating tank, the mixture is sent to a first absorption tower acid cooler by a first absorption tower acid circulating pump to be cooled to 70 ℃, then one part of the mixture enters the top of a first absorption tower to be sprayed, and the other part of the mixture enters a 98% acid finished product tank area after being sent to a 98% finished product acid cooler to be cooled;
5) SO in furnace gas in nicotinic acid tower3Absorbing by 104.5% of nicotinic acid sprayed on the tower top, allowing the nicotinic acid which absorbs 104.8-105.5% of sulfur trioxide and has a temperature of 50-60 ℃ to enter a nicotinic acid tower circulation tank from the tower bottom, then conveying to a nicotinic acid tower acid cooler by a nicotinic acid tower circulation pump to be cooled to 50 +/-5 ℃, allowing a part of the nicotinic acid to enter the tower top of the nicotinic acid tower for spraying, and conveying the other part of the nicotinic acid to a nicotinic acid finished product acid cooler for cooling and then entering a nicotinic acid finished product tank area.
6) Demisting unabsorbed gas in the first absorption tower by a demister at the top of the tower, returning the unabsorbed gas to the conversion unit for secondary conversion, enabling the converted gas subjected to the secondary conversion to enter a second absorption tower at the temperature of 150-175 ℃, and enabling SO in furnace gas to be in the second absorption tower3The concentrated sulfuric acid which is sprayed from the top of the tower is absorbed by 98 percent of acid, the concentration of the concentrated sulfuric acid which absorbs sulfur trioxide reaches 98-98.2 percent, the temperature reaches 70-75 ℃, the concentrated sulfuric acid enters an absorption circulation tank through the bottom of the tower, the concentrated sulfuric acid is pumped to a secondary absorption tower acid cooler through a secondary absorption tower acid circulation pump to be cooled to 70 ℃, and then the concentrated sulfuric acid enters the top of a second absorption tower to be sprayed; and demisting unabsorbed gas by a demister on the tower top, and then treating the gas by a tail gas treatment unit to reach the standard and discharging the gas.
The method comprises the following steps: the concentration of the circulating acid in the drying tower circulating tank and the concentration of the circulating acid in the nicotinic acid circulating tank are adjusted by 98% sulfuric acid from the absorption circulating tank, and the concentration of the circulating acid in the absorption circulating tank is adjusted by 93-98% sulfuric acid from the drying tower circulating tank.
The method comprises the following steps: the dry air is 3-8g of water/kg of dry gas.
The method comprises the following steps: the mass concentration of concentrated sulfuric acid sprayed at the top and the middle of the low-temperature two-stage drying tower in the step 3) is 93-98%, and the mass concentration of concentrated sulfuric acid absorbing moisture in the sulfur dioxide gas is 92.58-97.68%.
The method comprises the following steps: SO in furnace gas in the first absorption tower in the step 4)3The sulfuric acid with the mass concentration of 98 percent sprayed from the top of the tower is absorbed, and the concentration of the sulfuric acid after absorbing sulfur trioxide reaches 98.5 to 99.0 percent。
The method comprises the following steps: the hydrogen sulfide-containing acid gas contains 5 to 99.5 percent of H2S gas containing 1-5% of NH3And a portion of hydrocarbons.
The method comprises the following steps: the NOx removal efficiency of the NOx removal unit reaches 90-95%, and the problem that the quality of product acid is affected due to the fact that NOx enters the two acid making absorption units to react as follows is avoided.
NO2+NO+2H2SO4→2HNOSO4+H2O
The method comprises the following steps: the medium-low temperature two-stage drying unit uses 93-98% sulfuric acid as a drying agent, the furnace gas is respectively dried in the upper section and the lower section of the dryer, and the moisture content in the dried furnace gas is reduced to 15mg/Nm3The acid mist amount of the furnace gas is obviously reduced.
The invention has the beneficial effects that:
the technology optimizes the production process flow of the hydrogen sulfide acid gas dry-method acid making according to the development of the national environmental protection, energy conservation and emission reduction and the requirements of relevant policies. The invention has the beneficial effects that:
1) the air drying unit is introduced, so that the moisture in the air entering the whole system is reduced from the source, and the subsequent drying and absorption process cannot be influenced without entering a subsequent acid making system.
2) The NOx removal unit is introduced before furnace gas enters the medium-low temperature two-stage drying unit, so that the quality of the product acid is obviously improved, the product acid does not contain impurities, the chromaticity is clear and transparent, and the quality reaches the national GB/T534-2014 high-grade product standard.
3) The medium-low temperature two-stage drying adopts 93-98% concentrated sulfuric acid as a drying agent to perform two-stage drying on the furnace gas after incineration, compared with the traditional one-stage drying technology, the process has the advantages that the moisture content and the acid mist amount in the furnace gas are obviously reduced, dew point corrosion does not exist, corrosion to equipment and pipelines is avoided, and the normal operation time of the device can be effectively prolonged.
4) In addition, the tail gas treatment unit adopts a green oxidant hydrogen peroxide to oxidize sulfur dioxide into sulfuric acid, the sulfuric acid enters an acid making system, and the total sulfur utilization rate reaches 99.98%.
In conclusion, the combination of the air drying unit and the medium-low temperature two-stage drying unit saves a purification unit with complex flow, large occupied area and high investment in the traditional hydrogen sulfide dry-method acid preparation, solves the problem of high difficulty in processing dilute acid generated in the purification process, greatly reduces the occupied area and investment cost of equipment, and ensures that the quality of acid produced cannot change along with the change of the humidity in regions and seasons. The introduction of the NOx removal unit avoids the NOx from entering the acid making unit, thereby improving the quality of the product acid. The tail gas treatment unit adopts a green oxidant hydrogen peroxide, so that the total sulfur utilization rate is improved, and the emission of sulfur-containing salts is reduced.
Drawings
Fig. 1 is a schematic diagram of an apparatus for producing acid from an acid gas containing hydrogen sulfide according to the present invention.
Wherein: 1-air drying unit, 2-air blower, 3-hydrogen sulfide buffer tank, 4-incinerator, 5-waste heat boiler, 6-superheater, 7-ammonia and air mixer, 8-NOx remover, 9-economizer 1, 10-medium and low temperature two-stage drying tower, 11-drying tower circulation tank, 12-drying tower circulation pump, 13-drying tower acid cooler, 14-sulfur dioxide blower, 15-conversion unit, 16-economizer 2, 17-nicotinic acid tower, 18-nicotinic acid tower circulation tank, 19-nicotinic acid tower circulation pump, 20-nicotinic acid tower acid cooler, 21-first absorption tower, 22-absorption tower circulation tank, 23-absorption tower circulation pump, 24-absorption tower acid cooler, 25-second absorption tower, 26-a secondary absorption tower circulating pump, 27-a secondary absorption tower acid cooler, 28-a tail absorption tower, 29-a mother liquor circulating pump, 30-an electric demister, 31-a desulfurization liquid tank, 32-a desulfurization liquid pump, 33-a nicotinic acid finished product acid cooler, 34-a tail gas chimney and 35-98% of a finished product acid cooler.
Detailed Description
The invention is further illustrated by the following examples, without limiting the scope of the invention:
referring to fig. 1, a device for producing acid from acid gas containing hydrogen sulfide comprises an air drying unit 1, a conversion unit 15 and a first absorption tower 21, wherein an air output pipeline is connected with an incinerator 4 after passing through the air drying unit 1 and an air blower 2, an output pipeline of hydrogen sulfide gas is connected with the incinerator 4 after passing through a hydrogen sulfide buffer tank 3, an output end of the incinerator 4 is connected with a gas mixing tower through a waste heat boiler 5 and a superheater 6, the bottom output end of the gas mixing tower is connected with the bottom of a medium-low temperature two-stage drying tower 10 through a NOx removal device 8 and a first economizer 9, the top of the medium-low temperature two-stage drying tower 10 is connected with a second economizer 16 through a blower 14, a conversion unit 15, the output end of the top of the second economizer 16 is respectively connected with the lower part of a nicotinic acid tower 17 and/or the lower part of a first absorption tower 21, and the output end of the top of the nicotinic acid tower 17 is also connected with the lower part of the first absorption tower 21; the output end of the top of the first absorption tower 21 is connected with the lower part of the second absorption tower 25 after passing through the conversion unit 15, and the output end of the top of the second absorption tower 25 is connected with the electric demister 30 through the tail absorption tower 28;
the first absorption tower 21 and the second absorption tower 25 are provided with matched absorption tower circulating grooves 22, the bottom end of the first absorption tower 21 and the bottom end of the second absorption tower 25 are both connected with the absorption tower circulating grooves 22, one output end of the absorption tower circulating groove 22 is connected with the upper part of the first absorption tower 21 through a cooler, and the other output end of the absorption tower circulating groove 22 is connected with the upper part of the second absorption tower 25 through the cooler; the nicotinic acid tower 17 is provided with a matched nicotinic acid tower circulating groove 18, the bottom end of the nicotinic acid tower 17 is connected with the nicotinic acid tower circulating groove 18, one output end of the nicotinic acid tower circulating groove 18 is connected with the upper part of the nicotinic acid tower circulating groove 18 through a cooler, and the other output end is used as product acid to be output. The middle-low temperature two-stage drying tower 10 is provided with a matched drying tower circulating groove 11, the bottom end of the middle-low temperature two-stage drying tower 10 is connected with the drying tower circulating groove 11, and the output end of the drying tower circulating groove 11 is respectively connected with the upper part and the middle part of the middle-low temperature two-stage drying tower 10 through a cooler. The absorption tower circulation tank 22 also has an output end connected to the drying tower circulation tank 11. The mixed gas of ammonia gas and air is connected to the gas mixing tower through an ammonia and air mixer 7.
Example 1: application in equipment for preparing acid by hydrogen sulfide dry method (100% sulfuric acid yield is 30 ten thousand tons/year)
10825.24Nm from upstream equipment3Acid gas containing hydrogen sulfide (40 ℃, 0.06 MPa), wherein H2S content 79.18%, CO2Content of 16.88%, H2O content 2.1%, NH3The content is 1.00%, and the hydrocarbon content is 0.84%. Hydrogen sulfide acid gas passing through the hydrogen sulfide buffer tank 3 and dry air (3g/kg dry gas) after being refrigerated, adsorbed and dehumidified by the air drying unit 1 are fully mixed and combusted in the incinerator 4 to generate SO with the concentration of about 7.79 percent2And a small amount of SO3The temperature of the furnace gas discharged from the hydrogen sulfide combustion furnace reaches 1050-1200 ℃, the temperature of the furnace gas is reduced to 320 ℃ after heat is recovered by the waste heat boiler 5 and the superheater heat 6, and the furnace gas enters the NOx removal reactor 8 to react with ammonia and air from the air and ammonia mixer 7 to remove NOx. Furnace gas from a NOx removal reactor 8 is subjected to waste heat recovery through an economizer 9, the temperature of the furnace gas is about 200-250 ℃, the furnace gas enters a medium-low temperature two-stage drying tower 10, the furnace gas is fully contacted with 93-98% concentrated sulfuric acid sprayed at the top of the tower, the concentrated sulfuric acid absorbing about 92.58-97.68% of water in sulfur dioxide gas is discharged into an acid circulation tank 11 of the drying tower from the bottom of the tower, and then the concentrated sulfuric acid is sent into an acid cooler 13 of the drying tower through a circulation pump 12, cooled to 50 +/-5 ℃ and then sent to the top of the tower for spraying; the concentration of the circulating acid in the drying tower circulating tank 11 is adjusted by 98% acid passing from the absorption tower acid circulating tank 22 to the drying tower acid circulating tank 11. SO-treated furnace gas subjected to two-stage medium-low temperature drying2The blower 14 is pressurized and then enters a secondary conversion unit 15, the gas after primary conversion is subjected to residual heat recovery by an economizer 16, the temperature of the gas is reduced to 170-180 ℃, the gas enters a first absorption tower 17 and a nicotinic acid tower 21, and SO in furnace gas in the first absorption tower 173The sulfuric acid is absorbed by 98% acid sprayed on the top of the tower, the concentrated sulfuric acid which absorbs 98.5-99.0% of sulfur trioxide and has the temperature of 90-100 ℃ enters an absorption tower circulating tank 22 through the bottom of the tower, and then is sent to an absorption tower acid cooler 24 by an absorption tower acid circulating pump 23 to be cooled to 70 ℃, and then a part of the sulfuric acid enters a first absorption tower 21 to be sprayed on the top of the tower, and the other part of the sulfuric acid enters a finished product tank area after being sent to a 98% finished product acid cooler 35 to be cooled. SO in furnace gas in nicotinic acid tower 213Absorbed by 104.5 percent of nicotinic acid sprayed on the tower top, the nicotinic acid which absorbs 104.8 to 105.5 percent of sulfur trioxide and has the temperature of 50 to 60 ℃ enters a nicotinic acid tower circulating tank 18 through the tower bottom, and then is sent to a nicotinic acid tower acid cooler 20 by a nicotinic acid tower circulating pump 19 to be cooled to 50 ℃, and then a part of the nicotinic acid tower top is sprayed, and the other part of the nicotinic acid tower top is sent to a nicotinic acid finished product acid cooler 33 to be cooled and then enters a nicotinic acid finished product tank area. Unabsorbed gasThe body is demisted by a demister on the top of the tower and then returned to the conversion unit 15 for secondary conversion. The converted gas after the secondary conversion has a temperature of about 158 ℃, enters a second absorption tower 25, and SO in the furnace gas3Absorbed by 98 percent acid sprayed on the top of the tower, the concentrated sulfuric acid absorbing sulfur trioxide enters an absorption circulating tank 22 from the bottom of the tower, is sent to a secondary absorption tower acid cooler 27 by a secondary absorption tower acid circulating pump 30 to be cooled to 70 ℃, and then enters a second absorption tower 25 to be sprayed on the top of the tower. The acid concentration in the acid circulation tank 22 of the absorption tower is adjusted by 93-98% acid which is communicated with the acid circulation tank 22 of the absorption tower from the acid circulation tank 11 of the drying tower. The concentration of the circulating acid in the nicotinic acid tower circulating tank 18 is adjusted by the 98% acid which is fed from the absorption tower acid circulating tank 22 to the nicotinic acid circulating tank 18. And demisting unabsorbed gas by a demister on the tower top, and then treating the gas by a tail gas treatment unit to reach the standard and discharging the gas. SO in the exhaust gas is discharged after the tail gas desulfurization treatment2≤50mg/Nm3，SO3≤3mg/Nm3。
Materials of main nodes:
incinerator outlet gas (temperature: 1150 ℃, pressure: 1.5kpa (g)):
| kg/h | kmol/h | Nm3/h | mol％ | |
| O2 | 14373.4396 | 449.1700 | 10061.4077 | 9.22 |
| N2 | 1104095.5100 | 3943.1968 | 88327.6100 | 80.91 |
| SO2 | 24301.2860 | 379.7076 | 8308.0021 | 7.79 |
| SO3 | 244.9726 | 3.0622 | 68.5923 | 0.06 |
| CO2 | 4128.7328 | 93.8348 | 2088.7635 | 1.93 |
| NOx | 198.2100 | 4.8344 | 108.2900 | 0.10 |
| ∑ | 153593.3034 | 4873.8057 | 108962.6636 | 100 |
| H2O | 7929.9042 | 440.5502 | 9868.3253 |
the outlet gas of the NOx removal device (temperature: 380 ℃, pressure: 2.5kPa (G)):
| kg/h | kmol/h | Nm3/h | mol％ | |
| O2 | 14373.4396 | 449.1700 | 10061.4077 | 9.22 |
| N2 | 110544.8724 | 3948.0312 | 88435.8979 | 81.01 |
| SO2 | 24301.2860 | 379.7076 | 8308.0021 | 7.79 |
| SO3 | 244.9726 | 3.0622 | 68.5923 | 0.06 |
| CO2 | 4128.7328 | 93.8348 | 2088.7635 | 1.93 |
| NOx | 12.05 | 0.294 | 6.583 | 0.006 |
| ∑ | 153593.3034 | 4873.8057 | 108969.2466 | 100 |
| H2O | 7929.9042 | 440.5502 | 9868.3253 |
the outlet gas of the medium-low temperature two-stage dryer (temperature: 55 ℃, pressure: 9.0kPa (G)):
| kg/h | kmol/h | Nm3/h | mol％ | |
| O2 | 14373.4396 | 449.1670 | 10061.4100 | 9.22 |
| N2 | 110544.8724 | 3948.0312 | 88435.9000 | 81.06 |
| SO2 | 24301.28597 | 379.7076 | 8308.0020 | 7.77 |
| CO2 | 4128.732819 | 93.8348 | 2088.7630 | 1.93 |
| NOx | 12.05 | 0.294 | 6.583 | 0.006 |
| ∑ | 153348.3308 | 4870.7436 | 108900.6830 | 100 |
| H2O | 1.6334 | 0.0907 | 2.0327 |
the technical and economic indexes of the purification unit in the traditional hydrogen sulfide dry-method acid making process are as follows:
detail investment:
energy consumption:
| name of item | Unit of |
| (I) electricity | kW |
| Circulating pump of humidifier | 110 |
| Circulating pump of cooling tower | 110 |
| Elevated |
15 |
| Degassing tower pump | 11 |
| Liquid discharge tank pump | 7.5 |
| Electric fog washing pump | 45 |
| Sewage pump | 22 |
| First and second stage electric demister | 22×2 |
| First, second stage |
4×7.5 |
| Total of | 394.5 |
| (II) Water | t/h |
| Circulating water | 1480 |
| Production water | 1 |
| (III) draining | |
| 7％H2SO4 |
4 |
The technical and economic indexes of the newly added air drying unit are as follows:
investment: 12465000 yuan, energy consumption:
electricity: 509.4kW × h, circulating water: 5t/h, 0.4MPa steam: 1.84 t/h.
The method can greatly reduce investment, save the land used by the device and does not influence the quality of the acid and the steam of the product. Only the power consumption is about 30 percent higher than that of the traditional method, and the consumption of the circulating water is greatly reduced.
Example 2: application in equipment for preparing acid by hydrogen sulfide dry method (98% sulfuric acid yield is 10 ten thousand tons/year)
In this example, the flow rate was 1200kg/H, H2S：30.35％，CO2：49.64％，N2：19.9％，CH3OH:0.0948% is acid raw material gas data, and supplementary combustion sulfur is 3250 kg/h. Hydrogen sulfide acid gas passing through the hydrogen sulfide buffer tank 3, supplementary liquid sulfur and dry air (3g/kg dry gas) after being refrigerated, adsorbed and dehumidified by the air drying unit 1 are mixed and combusted in the incinerator 4 to generate SO-containing gas2Furnace gas with concentration of about 8.44% and a small amount of SO3And the furnace gas temperature of the hydrogen sulfide combustion furnace reaches 1050-1200 ℃, the furnace gas temperature is reduced to 320 ℃ after heat is recovered by the waste heat boiler 5 and the superheater heat 6, and then the furnace gas enters the NOx removal reactor 8 to react with the ammonia and the air from the air and ammonia mixer 7 to remove NOx. Furnace gas from a NOx removal reactor 8 is subjected to waste heat recovery through an economizer 9, the temperature of the furnace gas is about 200-250 ℃, the furnace gas enters a medium-low temperature two-stage drying tower 10, the furnace gas is fully contacted with 93-98% concentrated sulfuric acid sprayed on the top of the tower, the concentrated sulfuric acid absorbing about 92.58-97.68% of water in sulfur dioxide gas is discharged into an acid circulation tank 11 of the drying tower from the bottom of the tower, and then the concentrated sulfuric acid is sent into an acid cooler 13 through a circulation pump 12, cooled to 50 ℃ and then sent to the top of the tower for spraying; the concentration of the circulating acid in the drying tower circulating tank 11 is adjusted by 98% acid passing from the absorption tower acid circulating tank 22 to the drying tower acid circulating tank 11. SO-treated furnace gas subjected to two-stage medium-low temperature drying2The blower 14 is pressurized and then enters a secondary conversion unit 15, the gas after primary conversion is subjected to residual heat recovery by an economizer 16, the temperature of the gas is reduced to 170-180 ℃, the gas enters a first absorption tower 17 and a nicotinic acid tower 21, and SO in furnace gas in the first absorption tower 173The sulfuric acid is absorbed by 98% acid sprayed on the top of the tower, the concentrated sulfuric acid which absorbs 98.5-99.0% of sulfur trioxide and has the temperature of 90-100 ℃ enters an absorption tower circulating tank 22 through the bottom of the tower, and then is sent to an absorption tower acid cooler 24 by an absorption tower acid circulating pump 23 to be cooled to 70 ℃, and then a part of the sulfuric acid enters a first absorption tower 17 to be sprayed on the top of the tower, and the other part of the sulfuric acid enters a 98% acid finished product tank area after being sent to a 98% finished product acid cooler 35 to be cooled. SO in furnace gas in nicotinic acid tower 213Absorbed by 104.5 percent of nicotinic acid sprayed on the tower top, the nicotinic acid which absorbs 104.8 to 105.5 percent of sulfur trioxide and has the temperature of 50 to 60 ℃ enters a nicotinic acid tower circulating tank 18 from the tower bottom, then is sent to a nicotinic acid tower acid cooler 20 by a nicotinic acid tower circulating pump 19 to be cooled to 50 ℃, then a part of the nicotinic acid tower top is sprayed, and the other part of the nicotinic acid tower top is sent to a nicotinic acid finished product acid cooler 33 to be cooled and then enters a nicotinic acid finished product tankAnd (4) a zone. The gas that is not absorbed is demisted by a demister at the top of the tower and then returned to the conversion unit 15 for secondary conversion. The converted gas after the secondary conversion has a temperature of about 158 ℃, enters a second absorption tower 25, and SO in the furnace gas3Absorbed by 98 percent acid sprayed on the top of the tower, the concentrated sulfuric acid absorbing sulfur trioxide enters an absorption circulating tank 22 from the bottom of the tower, is sent to a secondary absorption tower acid cooler 27 by a secondary absorption tower acid circulating pump 26 to be cooled to 70 ℃, and then enters a second absorption tower 25 to be sprayed on the top of the tower. The acid concentration in the acid circulation tank 22 of the absorption tower is adjusted by 93-98% of acid flowing from the acid circulation tank 11 of the drying tower to the acid circulation tank 22 of the absorption tower, and the acid concentration in the acid circulation tank 18 of the nicotinic acid tower is adjusted by 98% of acid flowing from the acid circulation tank 22 of the absorption tower to the acid circulation tank 18 of the nicotinic acid tower. And demisting unabsorbed gas by a demister on the tower top, and then treating the gas by a tail gas treatment unit to reach the standard and discharging the gas. SO in the exhaust gas is discharged after the tail gas desulfurization treatment2≤50mg/Nm3，SO3≤3mg/Nm3。
Claims (9)
1. The utility model provides a device of sour is made to sour containing hydrogen sulfide sour gas which characterized in that: the device comprises an air drying unit (1), a conversion unit (15) and a first absorption tower (21), an air output pipeline is connected with an incinerator (4) through the air drying unit (1), a hydrogen sulfide gas output pipeline is also connected with the incinerator (4), the output end of the incinerator (4) is connected with a gas mixing tower through a waste heat boiler (5) and a superheater (6), the bottom output end of the gas mixing tower is connected with the bottom of a medium-low temperature two-stage drying tower (10) through a NOx remover (8) and a first economizer (9), the top of the medium-low temperature two-stage drying tower (10) is connected with a second economizer (16) through a conversion unit (15), the output end of the top of the second economizer (16) is respectively connected with the lower part of the nicotinic acid tower (17) and/or the lower part of the first absorption tower (21), and the output end of the top of the nicotinic acid tower (17) is also connected with the lower part of the first absorption tower (21); the output end of the top of the first absorption tower (21) is connected with the lower part of the second absorption tower (25) after passing through the conversion unit (15), and the output end of the top of the second absorption tower (25) is connected with the electric demister (30) through the tail absorption tower (28);
the first absorption tower (21) and the second absorption tower (25) are provided with matched absorption tower circulating grooves (22), the bottom end of the first absorption tower (21) and the bottom end of the second absorption tower (25) are both connected with the absorption tower circulating grooves (22), one output end of each absorption tower circulating groove (22) is connected with the upper part of the first absorption tower (21) through a cooler, and the other output end of each absorption tower circulating groove is connected with the upper part of the second absorption tower (25) through a cooler; the nicotinic acid tower (17) is provided with a matched nicotinic acid tower circulating groove (18), the bottom end of the nicotinic acid tower (17) is connected with the nicotinic acid tower circulating groove (18), one output end of the nicotinic acid tower circulating groove (18) is connected with the upper part of the nicotinic acid tower circulating groove (18) through a cooler, and the other output end is used as product acid to be output.
2. The apparatus for producing acid from a hydrogen sulfide-containing acid gas of claim 1, wherein: the middle-low temperature two-stage drying tower (10) is provided with a matched drying tower circulating groove (11), the bottom end of the middle-low temperature two-stage drying tower (10) is connected with the drying tower circulating groove (11), and the output end of the drying tower circulating groove (11) is respectively connected with the upper part and the middle part of the middle-low temperature two-stage drying tower (10) through a cooler.
3. The apparatus for producing acid from a hydrogen sulfide-containing acid gas of claim 2, wherein: the absorption tower circulating groove (22) is also provided with an output end connected with the drying tower circulating groove (11).
4. The apparatus for producing acid from a hydrogen sulfide-containing acid gas of claim 1, wherein: the mixed gas of ammonia gas and air is connected with a gas mixing tower through an ammonia and air mixer (7).
5. A method for preparing acid from acid gas containing hydrogen sulfide by using the device of claim 1, which is characterized by comprising the following steps: the method comprises the following steps:
1) the acid gas containing hydrogen sulfide is fully mixed and combusted in the incinerator 4 through the hydrogen sulfide buffer tank and the dry air which is subjected to freezing adsorption and dehumidification by the air drying unit to generate furnace gas;
2) the furnace gas temperature of the hydrogen sulfide combustion furnace reaches 1050-1200 ℃, the furnace gas temperature is reduced to 300-420 ℃ after heat is recovered by a waste heat boiler and a superheater, and the furnace gas is mixed with mixed gas of ammonia gas and air and then enters a NOx removal reactor to remove NOx;
3) recovering waste heat of furnace gas from a NOx removal reactor through an economizer, reducing the temperature of the furnace gas to about 180-250 ℃, enabling the furnace gas to enter a medium-low temperature two-stage drying tower, fully contacting with concentrated sulfuric acid sprayed at the top and the middle of the tower, discharging the concentrated sulfuric acid absorbing moisture in sulfur dioxide gas from the bottom of the tower to an acid circulation tank of the drying tower, sending the concentrated sulfuric acid into an acid cooler of the drying tower through a circulation pump, cooling to 45-55 ℃, and sending the concentrated sulfuric acid to the top and the middle of the tower for spraying;
4) SO-treated furnace gas subjected to two-stage medium-low temperature drying2The method comprises the steps of pressurizing a blower, then entering a secondary conversion unit, recycling residual heat from a coal economizer to obtain gas after primary conversion, reducing the temperature to 170-180 ℃, entering a nicotinic acid tower and/or a first absorption tower, and obtaining SO in furnace gas in the first absorption tower3Absorbing by acid sprayed on the top of the tower, enabling concentrated sulfuric acid with the temperature of 90-100 ℃ after absorbing sulfur trioxide to enter an absorption tower circulation tank through the bottom of the tower, then sending the concentrated sulfuric acid to an absorption tower acid cooler through an absorption tower acid circulation pump to be cooled to 70 ℃, enabling one part of the concentrated sulfuric acid to enter the top of a first absorption tower for spraying, and sending the other part of the concentrated sulfuric acid to a 98% finished product acid cooler for cooling and then entering a 98% acid finished product tank area;
5) SO in furnace gas in nicotinic acid tower3Absorbing by 104.5% of nicotinic acid sprayed on the tower top, allowing the nicotinic acid which absorbs 104.8-105.5% of sulfur trioxide and has a temperature of 50-60 ℃ to enter a nicotinic acid tower circulation tank from the tower bottom, then conveying to a nicotinic acid tower acid cooler by a nicotinic acid tower circulation pump to be cooled to 50 +/-5 ℃, allowing a part of the nicotinic acid to enter the tower top of the nicotinic acid tower for spraying, and conveying the other part of the nicotinic acid to a nicotinic acid finished product acid cooler for cooling and then entering a nicotinic acid finished product tank area.
6) Demisting unabsorbed gas in the first absorption tower by a demister at the top of the tower, returning the unabsorbed gas to the conversion unit for secondary conversion, enabling the converted gas subjected to the secondary conversion to enter a second absorption tower at the temperature of 150-175 ℃, and enabling SO in furnace gas to be in the second absorption tower3Absorbed by 98 percent acid sprayed on the tower top, the concentrated sulfuric acid absorbing sulfur trioxide with the concentration of 98-98.2 percent and the temperature of 70-75 ℃ enters an absorption circulation tank through the tower bottom, is pumped to a secondary absorption tower acid cooler by a secondary absorption tower acid circulation pump to be cooled to 70 ℃, and then enters the tower top of a second absorption towerSpraying; and demisting unabsorbed gas by a demister on the tower top, and then treating the gas by a tail gas treatment unit to reach the standard and discharging the gas.
6. The method of claim 5, wherein: the concentration of the circulating acid in the drying tower circulating tank and the concentration of the circulating acid in the nicotinic acid circulating tank are adjusted by 98% sulfuric acid from the absorption circulating tank, and the concentration of the circulating acid in the absorption circulating tank is adjusted by 93-98% sulfuric acid from the drying tower circulating tank.
7. The method of claim 5, wherein: the dry air is 3-8g of water/kg of dry gas.
8. The method of claim 5, wherein: the mass concentration of concentrated sulfuric acid sprayed at the top and the middle of the low-temperature two-stage drying tower in the step 3) is 93-98%, and the mass concentration of concentrated sulfuric acid absorbing moisture in the sulfur dioxide gas is 92.58-97.68%.
9. The method of claim 5, wherein: SO in furnace gas in the first absorption tower in the step 4)3The mass concentration of the sulfuric acid sprayed by the tower top is 98 percent, and the concentration of the sulfuric acid after absorbing sulfur trioxide reaches 98.5 to 99.0 percent.
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