CN107934919B - Process and equipment for continuously preparing sulfur dioxide by low-concentration oleum - Google Patents
Process and equipment for continuously preparing sulfur dioxide by low-concentration oleum Download PDFInfo
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- CN107934919B CN107934919B CN201711364124.8A CN201711364124A CN107934919B CN 107934919 B CN107934919 B CN 107934919B CN 201711364124 A CN201711364124 A CN 201711364124A CN 107934919 B CN107934919 B CN 107934919B
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- C01B17/00—Sulfur; Compounds thereof
- C01B17/48—Sulfur dioxide; Sulfurous acid
- C01B17/50—Preparation of sulfur dioxide
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- C01B17/502—Preparation of sulfur dioxide by reduction of sulfur compounds of sulfur trioxide
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Abstract
The invention belongs to the technical field of inorganic chemical industry, and particularly relates to a process and equipment for continuously preparing sulfur dioxide by low-concentration fuming sulfuric acid. The process comprises the following steps: 1) introducing the gas phase of a converter at the 4 and 5 sections of the sulfuric acid preparation process into a secondary absorption tower from a gas phase input pipeline for absorption, introducing the gas phase into an external absorption system for continuous absorption, introducing the liquid phase obtained by absorption into a circulating tank, continuously pumping the liquid phase into a primary reaction tower through a pump A, and introducing liquid sulfur for reaction, thereby always keeping the state of liquid sulfur shortage; 2) continuously pumping reaction liquid generated in the step 1) back to the circulating tank through a pump B; 3) and (2) allowing the mixed gas generated in the step 1) to enter the lower part of the secondary reaction tower, and introducing liquid sulfur to react to obtain sulfur dioxide gas, wherein the excessive liquid sulfur is always kept in the reaction process. The method is simple and easy to implement, saves energy consumption, reduces production cost and improves product quality; the safety performance is good, and the degree of automation is high.
Description
Technical Field
The invention belongs to the technical field of inorganic chemical industry, and particularly relates to a process and equipment for continuously preparing sulfur dioxide by low-concentration fuming sulfuric acid.
Background
At present, the production process of sulfur dioxide is to prepare sulfur trioxide and then react the sulfur trioxide with liquid sulfur to generate sulfur dioxide.
The preparation of sulfur trioxide is that sulfur dioxide is produced by adopting an incineration method in the sulfuric acid industry, then the sulfur dioxide is catalytically converted into sulfur trioxide through 1,2 and 3 sections of converters, the sulfur trioxide is absorbed by concentrated sulfuric acid to become fuming sulfuric acid, and the fuming sulfuric acid is evaporated to prepare liquid sulfur trioxide. In the sulfur trioxide conversion part, most of sulfur dioxide can be converted in the front, but part of sulfur dioxide is not converted, so concentrated sulfuric acid in a first-stage nicotinic acid tower and a second-stage nicotinic acid tower is used for absorbing and converting the sulfur dioxide into high-concentration fuming acid in the front conversion part, a gas phase enters a first-stage absorption tower for absorption, the sulfur dioxide which is not absorbed in the gas phase continues to enter a 4-stage converter, the sulfur dioxide is converted into sulfur trioxide in a 5-stage converter, and then the sulfur trioxide is absorbed into concentrated sulfuric acid in a second-stage absorption tower, the acid converts low-concentration sulfuric acid into 98% acid by adding water at present, and part of the sulfur trioxide is not recovered.
The above process has the following problems: the process route is longer, and the evaporation and storage of the fuming acid not only bring large investment and high energy consumption, but also bring more potential safety hazards.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a process for continuously preparing sulfur dioxide by using low-concentration oleum, which improves the utilization rate of the low-concentration oleum, improves the added value of sulfur in the sulfuric acid industry, and has the advantages of simple process, low energy consumption and high product quality; the invention also provides equipment for continuously preparing sulfur dioxide by using the low-concentration fuming sulfuric acid, which has high safety performance and is easy to realize automatic control.
The invention relates to a process for continuously preparing sulfur dioxide by low-concentration oleum, which comprises the following steps:
1) introducing the gas phase of a converter at the 4 and 5 sections of the sulfuric acid preparation process into a secondary absorption tower from a gas phase input pipeline for absorption, introducing the gas phase into an external absorption system for continuous absorption, introducing the liquid phase obtained by absorption into a circulating tank, continuously pumping the liquid phase into a primary reaction tower through a pump A, and introducing liquid sulfur through a liquid sulfur pipeline A for reaction to always keep the state of liquid sulfur shortage;
2) continuously pumping reaction liquid generated in the step 1) back to the circulating tank through a pump B;
3) and (3) allowing the mixed gas generated in the step 1) to enter the lower part of the secondary reaction tower, and introducing liquid sulfur through a liquid sulfur pipeline B to react to obtain sulfur dioxide gas, wherein the excessive liquid sulfur is always kept in the reaction process.
And (2) introducing the mixed gas generated in the step 1) into the lower part of a secondary reaction tower, introducing liquid sulfur from a liquid sulfur pipeline B at the upper part of the secondary reaction tower for reaction, and ensuring that the liquid sulfur is fully contacted with unreacted sulfur trioxide in the mixed gas in the secondary reaction tower.
The sulfur dioxide produced by the reaction is used or sold in the gas or liquid phase.
Wherein:
the concentration of the oleum in the step 1) is 100.3-102%.
The mass ratio of the introduction amount of the liquid sulfur to the fuming sulfuric acid in the step 1) is 1: 12-1: 50.
The reaction temperature of the first-stage reaction tower in the step 1) is 70-135 ℃.
The reaction pressure of the primary reaction tower in the step 1) is 0-0.1 MPa.
In the reaction solution in the step 2), the concentration of fuming sulfuric acid is 100.1-101.9%.
The liquid level at the bottom of the secondary reaction tower in the step 3) is always controlled to be 30-80%.
The reaction temperature of the secondary reaction tower in the step 3) is 70-140 ℃.
The reaction pressure of the secondary reaction tower in the step 3) is 0-0.1 MPa.
The equipment for continuously preparing the sulfur dioxide by the fuming sulfuric acid comprises a secondary absorption tower, a primary reaction tower and a secondary reaction tower, wherein an inlet of the secondary absorption tower is connected with a gas phase input pipeline; the top air outlet of the secondary absorption tower is connected with an external absorption system; the bottom outlet of the secondary absorption tower is sequentially connected with a circulating tank and a pump A, and an outlet pipeline of the pump A is respectively connected with a circulating liquid inlet at the upper part of the secondary absorption tower and a feed inlet at the lower part of the primary reaction tower;
the upper part of the first-stage reaction tower is connected with a liquid sulfur pipeline A; the bottom outlet of the first-stage reaction tower is connected with a pump B, and an outlet pipeline of the pump B is connected with an inlet at the upper part of the circulating tank; the top gas phase outlet of the first-stage reaction tower is connected with the lower inlet of the second-stage reaction tower, the top of the second-stage reaction tower is connected with a sulfur dioxide output pipeline, and the upper part of the second-stage reaction tower is connected with a liquid sulfur pipeline B.
In conclusion, the beneficial effects of the invention are as follows:
1. compared with the prior art, the method does not need a sulfuric acid sulfur trioxide preparation process, reduces the sulfur trioxide process, has simple process and low production and operation cost, has high safety performance, is easy to realize automatic control, and meets the energy-saving and safety requirements of chemical production.
2. The sulfur dioxide product produced by the method has high quality, the purity is more than 99.9 percent, the water content is less than or equal to 0.003 percent, and the process for continuously preparing the sulfur dioxide is realized.
3. The invention improves the utilization rate of the low-concentration fuming sulfuric acid and the added value of sulfur in the sulfuric acid industry
4. The invention avoids the defects of insufficient contact and incomplete reaction of sulfur trioxide and liquid sulfur in the kettle-type reactor; meanwhile, the kettle type reactor needs to heat the reaction kettle to bring the damage of jacket leakage, and the direct use of liquid sulfur in the tower type reactor not only saves steam but also can avoid the damage brought by leakage; meanwhile, the reaction is a normal pressure or micro-positive pressure reaction which is safer.
Drawings
FIG. 1 is a schematic diagram of the construction of the apparatus of the present invention;
in the figure: 1. a gas phase input line; 2. a secondary absorption tower; 3. a circulation tank; 4. a pump A; 5. a pump B; 6. a first-stage reaction tower; 7. a secondary reaction tower; 8. a liquid sulfur line A; 9. a liquid sulfur line B; 10. a sulfur dioxide output line.
Detailed Description
The present invention will be further described with reference to the following examples.
Referring to fig. 1, the equipment used in the embodiment comprises a secondary absorption tower 2, a primary reaction tower 6 and a secondary reaction tower 7, wherein the inlet of the secondary absorption tower 2 is connected with a gas phase input pipeline 1; the top air outlet of the secondary absorption tower 2 is connected with an external absorption system; the bottom outlet of the secondary absorption tower 2 is sequentially connected with a circulating tank 3 and a pump A4, and an outlet pipeline of the pump A4 is respectively connected with an upper circulating liquid inlet of the secondary absorption tower 2 and a lower feed inlet of the primary reaction tower 6;
the upper part of the first-stage reaction tower 6 is connected with a liquid sulfur pipeline A8; an outlet at the bottom of the first-stage reaction tower 6 is connected with a pump B5, and an outlet pipeline of the pump B5 is connected with an inlet at the upper part of the circulating tank 3; the gas phase outlet at the top of the first-stage reaction tower 6 is connected with the inlet at the lower part of the second-stage reaction tower 7, the top of the second-stage reaction tower 7 is connected with a sulfur dioxide output pipeline 10, and the upper part of the second-stage reaction tower 7 is connected with a liquid sulfur pipeline B9.
Example 1
1) Introducing the gas phase of a converter at the 4 and 5 sections of the sulfuric acid preparation process into a secondary absorption tower 2 from a gas phase input pipeline 1 for absorption, introducing the gas phase into an external absorption system for continuous absorption, introducing the liquid phase obtained by absorption, namely fuming sulfuric acid (the concentration is 101%), into a circulating tank 3, continuously pumping the fuming sulfuric acid into a primary reaction tower 6 through a pump A4, simultaneously introducing liquid sulfur through a liquid sulfur pipeline A8, reacting at 100 ℃ and 0.05MPa, and always keeping the state of liquid sulfur shortage; wherein the mass ratio of the introduction amount of the liquid sulfur to the fuming sulfuric acid is 1: 30.
2) The reaction liquid generated in the step 1) is continuously pumped back to the circulating tank 3 through a pump B5; the concentration of oleum in the reaction solution is 100.5%.
3) The mixed gas generated in the step 1) enters the lower part of a secondary reaction tower 7, meanwhile, liquid sulfur is introduced through a liquid sulfur pipeline B9 to react at 105 ℃ and 0.05MPa to obtain sulfur dioxide gas, the excessive state of the liquid sulfur is always kept in the reaction process, and the liquid level at the bottom of the tower is controlled at 50%.
The obtained sulfur dioxide gas was detected, sampled and analyzed, and the purity was 99.93%, and the water content was 0.003%.
Example 2
1) Introducing the gas phase of a converter at the 4 and 5 sections of the sulfuric acid preparation process into a secondary absorption tower 2 from a gas phase input pipeline 1 for absorption, introducing the gas phase into an external absorption system for continuous absorption, introducing the liquid phase obtained by absorption, namely fuming sulfuric acid (the concentration is 100.3%), into a circulating tank 3, continuously pumping the fuming sulfuric acid into a primary reaction tower 6 through a pump A4, simultaneously introducing liquid sulfur through a liquid sulfur pipeline A8, reacting at 135 ℃ under normal pressure, and always keeping the state of liquid sulfur shortage; wherein the mass ratio of the introduction amount of the liquid sulfur to the fuming sulfuric acid is 1: 50.
2) The reaction liquid generated in the step 1) is continuously pumped back to the circulating tank 3 through a pump B5; the concentration of oleum in the reaction solution is 100.1%.
3) The mixed gas generated in the step 1) enters the lower part of a secondary reaction tower 7, meanwhile, liquid sulfur is introduced through a liquid sulfur pipeline B9 to react at 140 ℃ and normal pressure to obtain sulfur dioxide gas, the excessive state of the liquid sulfur is always kept in the reaction process, and the liquid level at the bottom of the tower is controlled at 80%.
The obtained sulfur dioxide gas was detected, sampled and analyzed, and the purity was 99.95% and the water content was 0.002%.
Example 3
1) Introducing the gas phase of a converter at the 4 and 5 sections of the sulfuric acid preparation process into a secondary absorption tower 2 from a gas phase input pipeline 1 for absorption, introducing the gas phase into an external absorption system for continuous absorption, introducing the liquid phase obtained by absorption, namely fuming sulfuric acid (the concentration is 102%), into a circulating tank 3, continuously pumping the fuming sulfuric acid into a primary reaction tower 6 through a pump A4, simultaneously introducing liquid sulfur through a liquid sulfur pipeline A8, reacting at 70 ℃ and 0.1MPa, and always keeping the state of liquid sulfur shortage; wherein the mass ratio of the introduction amount of the liquid sulfur to the fuming sulfuric acid is 1: 12.
2) The reaction liquid generated in the step 1) is continuously pumped back to the circulating tank 3 through a pump B5; the concentration of oleum in the reaction solution is 101%.
3) The mixed gas generated in the step 1) enters the lower part of a secondary reaction tower 7, and meanwhile, liquid sulfur is introduced through a liquid sulfur pipeline B9 to react at 70 ℃ and 0.1MPa to obtain sulfur dioxide gas, the excessive state of the liquid sulfur is always kept in the reaction process, and the liquid level at the bottom of the tower is controlled at 30%.
The obtained sulfur dioxide gas was detected, sampled and analyzed, and the purity was 99.90% and the water content was 0.002%.
Claims (8)
1. A process for continuously preparing sulfur dioxide by low-concentration oleum is characterized in that: the method comprises the following steps:
1) introducing a gas phase of a converter at the 4 and 5 sections of the sulfuric acid preparation process into a secondary absorption tower (2) from a gas phase input pipeline (1) for absorption, introducing the gas phase into an external absorption system for continuous absorption, introducing a liquid phase obtained by absorption into a circulating tank (3), continuously pumping the liquid phase into a primary reaction tower (6) through a pump A (4), and simultaneously introducing liquid sulfur through a liquid sulfur pipeline A (8) for reaction to always keep the state of liquid sulfur shortage;
2) the reaction liquid generated in the step 1) is continuously pumped back to the circulating tank (3) through a pump B (5);
3) the mixed gas generated in the step 1) enters the lower part of a secondary reaction tower (7), and meanwhile, liquid sulfur is introduced through a liquid sulfur pipeline B (9) for reaction to obtain sulfur dioxide gas, and the excessive state of the liquid sulfur is always kept in the reaction process;
wherein:
the concentration of the oleum in the step 1) is 100.3-102%;
the mass ratio of the introduction amount of the liquid sulfur to the fuming sulfuric acid in the step 1) is 1: 12-1: 50.
2. The process for the continuous production of sulfur dioxide with low-concentration oleum according to claim 1, wherein: the reaction temperature of the first-stage reaction tower (6) in the step 1) is 70-135 ℃.
3. The process for the continuous production of sulfur dioxide with low-concentration oleum according to claim 1, wherein: the reaction pressure of the primary reaction tower (6) in the step 1) is 0-0.1 MPa.
4. The process for the continuous production of sulfur dioxide with low-concentration oleum according to claim 1, wherein: in the reaction solution in the step 2), the concentration of fuming sulfuric acid is 100.1-101.9%.
5. The process for the continuous production of sulfur dioxide with low-concentration oleum according to claim 1, wherein: the liquid level at the bottom of the secondary reaction tower (7) in the step 3) is always controlled to be 30-80%.
6. The process for the continuous production of sulfur dioxide with low-concentration oleum according to claim 1, wherein: the reaction temperature of the secondary reaction tower (7) in the step 3) is 70-140 ℃.
7. The process for the continuous production of sulfur dioxide with low-concentration oleum according to claim 1, wherein: the reaction pressure of the secondary reaction tower (7) in the step 3) is 0-0.1 MPa.
8. An apparatus for carrying out the process for the continuous production of sulfur dioxide with low-concentration oleum according to claim 1, wherein: the device comprises a secondary absorption tower (2), a primary reaction tower (6) and a secondary reaction tower (7), wherein the inlet of the secondary absorption tower (2) is connected with a gas phase input pipeline (1); the top air outlet of the secondary absorption tower (2) is connected with an external absorption system; the bottom outlet of the secondary absorption tower (2) is sequentially connected with a circulating tank (3) and a pump A (4), and an outlet pipeline of the pump A (4) is respectively connected with an upper circulating liquid inlet of the secondary absorption tower (2) and a lower feed inlet of a primary reaction tower (6);
the upper part of the first-stage reaction tower (6) is connected with a liquid sulfur pipeline A (8); an outlet at the bottom of the first-stage reaction tower (6) is connected with a pump B (5), and an outlet pipeline of the pump B (5) is connected with an inlet at the upper part of the circulating tank (3); the device is characterized in that a gas phase outlet at the top of the first-stage reaction tower (6) is connected with an inlet at the lower part of the second-stage reaction tower (7), the top of the second-stage reaction tower (7) is connected with a sulfur dioxide output pipeline (10), and the upper part of the second-stage reaction tower (7) is connected with a liquid sulfur pipeline B (9).
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| GB384449A (en) * | 1931-12-18 | 1932-12-08 | Ig Farbenindustrie Ag | Improvements in the manufacture and production of sulphur dioxide |
| GB1002584A (en) * | 1961-05-15 | 1965-08-25 | Saint Gobain | Improvements in or relating to the manufacture of pure sulphur dioxide |
| US3325248A (en) * | 1961-10-24 | 1967-06-13 | Method of preparing sulfur dioxide | |
| US4175112A (en) * | 1978-07-17 | 1979-11-20 | Stauffer Chemical Company | Process for purification of gases containing elemental sulfur |
| CN101020570A (en) * | 2006-03-22 | 2007-08-22 | 蒋胜 | Production process of eliminating simple substance sulphur from SO2 gas |
| CN103626135A (en) * | 2013-12-04 | 2014-03-12 | 山东凯盛新材料股份有限公司 | Method and equipment for producing liquid sulfur dioxide through sulfur trioxide and sulphur |
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- 2017-12-18 CN CN201711364124.8A patent/CN107934919B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB384449A (en) * | 1931-12-18 | 1932-12-08 | Ig Farbenindustrie Ag | Improvements in the manufacture and production of sulphur dioxide |
| GB1002584A (en) * | 1961-05-15 | 1965-08-25 | Saint Gobain | Improvements in or relating to the manufacture of pure sulphur dioxide |
| US3325248A (en) * | 1961-10-24 | 1967-06-13 | Method of preparing sulfur dioxide | |
| US4175112A (en) * | 1978-07-17 | 1979-11-20 | Stauffer Chemical Company | Process for purification of gases containing elemental sulfur |
| CN101020570A (en) * | 2006-03-22 | 2007-08-22 | 蒋胜 | Production process of eliminating simple substance sulphur from SO2 gas |
| CN103626135A (en) * | 2013-12-04 | 2014-03-12 | 山东凯盛新材料股份有限公司 | Method and equipment for producing liquid sulfur dioxide through sulfur trioxide and sulphur |
Non-Patent Citations (1)
| Title |
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| 100%二氧化硫的生产;Lurgi Chemie等人;《硫磷设计与粉体工程》;20050330;图1 * |
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