CN110052111B - Cleaning and purifying method for sulfur-containing tail gas - Google Patents
Cleaning and purifying method for sulfur-containing tail gas Download PDFInfo
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- CN110052111B CN110052111B CN201910385494.2A CN201910385494A CN110052111B CN 110052111 B CN110052111 B CN 110052111B CN 201910385494 A CN201910385494 A CN 201910385494A CN 110052111 B CN110052111 B CN 110052111B
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D47/00—Separating dispersed particles from gases, air or vapours by liquid as separating agent
- B01D47/06—Spray cleaning
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/002—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23J—REMOVAL OR TREATMENT OF COMBUSTION PRODUCTS OR COMBUSTION RESIDUES; FLUES
- F23J15/00—Arrangements of devices for treating smoke or fumes
- F23J15/08—Arrangements of devices for treating smoke or fumes of heaters
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/102—Carbon
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2257/30—Sulfur compounds
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- B01D2257/30—Sulfur compounds
- B01D2257/304—Hydrogen sulfide
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Abstract
The invention belongs to the technical field of waste gas treatment, and discloses a method for cleaning and purifying sulfur-containing tail gas, which comprises the following steps: firstly, carrying out a second-stage Claus reaction on the acid sulfur-containing tail gas, then conveying the reacted Claus tail gas to the bottom of a spray tower, enabling the gas to move upwards, contacting with clear water sprayed downwards by a spray nozzle at the top of the spray tower, then conveying the gas out of the top of the spray tower, introducing the gas into a first-stage adsorption tower filled with a CuO activated carbon adsorbent for adsorption treatment, cooling by a heat exchanger, introducing the gas into a second-stage adsorption tower filled with a boron-nitrogen double-doped iron oxide activated carbon composite adsorbent for adsorption treatment, and discharging the treated gas. The clean purification method of the sulfur-containing tail gas disclosed by the invention not only can efficiently and stably desulfurize, but also has high process operation stability, the treated gas can be directly discharged into the atmosphere, the diffusion speed is high, and the haze can be effectively prevented from forming.
Description
Technical Field
The invention relates to the technical field of waste gas treatment, in particular to a method for cleaning and purifying sulfur-containing tail gas.
Background
In recent years, along with rapid development of economy, the demand for energy is increasing day by day, the petrochemical industry and the coal chemical industry are rapidly developing and growing, and most petrochemical and coal chemical enterprises can form sulfur-containing process tail gas in production, and the tail gas contains a large amount of H2S and SO2And if toxic and harmful gases are directly discharged, a large amount of sulfur resources are wasted, the ecological environment is polluted and damaged, and the sustainable development of the industry is severely restricted. With the increasing awareness of people on natural environment protection, China pays attention to controlling petrochemical and coal sulfur-containing tail gas pollution and improving environmental air quality, and related emission standards are more and more strict. Therefore, the development of cost-effective exhaust gas purification technology has become a research direction of great interest.
The Claus method is a mature method for treating sulfur-containing tail gas, and is widely applied to the field of processing and treating coal, petroleum and natural gas. However, the sulfur recovery of the conventional Claus process can only reach 90-95%, the sulfur recovery of the improved Claus process can only reach 95-99%, and low-concentration H still exists in the treated tail gas2S and SO2Only, isThe sulfur-containing tail gas is purified by a single Claus process, and the requirements of national environmental protection emission standards cannot be met. In order to meet the national environmental requirements, the low-concentration sulfur-containing tail gas treated by the Claus method needs to be further purified, so that the purified tail gas can be directly discharged into the atmosphere.
At present, a common Claus tail gas purification treatment method is an alkali absorption method, but the method generates a large amount of low-value and secondary-pollution products such as calcium sulfate, sodium sulfate and the like, and the subsequent treatment is difficult. The activated carbon has a developed pore structure, a large amount of sulfur elements can be stored on the surface and inside of the activated carbon, the problem of secondary pollution is solved by adopting the activated carbon for desulfurization, and the activated carbon is favorable for recycling sulfur, so that the activated carbon becomes an alternative scheme for treating the Claus tail gas. However, the desulfurization efficiency of the activated carbon is low, and the activated carbon is easily influenced by the previous treatment process, the activity of micropores is influenced by the blockage of impurities in the tail gas, and the process operation is unstable; in addition, the temperature of the tail gas after the desulfurization of the activated carbon is usually low, which is not beneficial to the rapid diffusion of the tail gas and easily forms haze.
Disclosure of Invention
The invention aims to make up for the defects of the prior art and provides a clean purification method for sulfur-containing tail gas, which not only can efficiently and stably desulfurize, but also has high process operation stability, and the treated gas can be directly discharged into the atmosphere, has high diffusion speed and can effectively prevent haze.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for cleaning and purifying sulfur-containing tail gas comprises the following steps:
(1) introducing the acid sulfur-containing tail gas into a combustion furnace for treatment at the temperature of 1100-1300 ℃, introducing the treated gas into a waste heat boiler for waste heat recovery, then sequentially introducing the gas into a primary Claus reactor, a primary condenser, a secondary Claus reactor and a secondary condenser, collecting liquid sulfur obtained by condensation and separation through a liquid sulfur trap, and introducing the Claus tail gas after liquid sulfur separation into the next treatment process;
(2) sending the Claus tail gas to the bottom of a spray tower, enabling the gas to move upwards, contacting with clear water sprayed downwards by a spray nozzle at the top of the spray tower, discharging the gas from the top of the spray tower, heating to 230-;
(3) introducing the heated gas into a primary adsorption tower loaded with a CuO activated carbon adsorbent for adsorption treatment, and then cooling to 120-160 ℃ through a heat exchanger;
(4) and introducing the gas subjected to temperature reduction treatment into a secondary adsorption tower filled with a boron-nitrogen double-doped iron oxide activated carbon composite adsorbent for adsorption treatment, and discharging the treated gas.
Preferably, the temperature of the gas at the inlet of the primary Claus reactor is 235-245 ℃, the gas is cooled to 150-160 ℃ through a primary condenser after the reaction in the primary Claus reactor, the gas is heated to 225-235 ℃ through a heat exchanger, the gas is introduced into a secondary Claus reactor for reaction, the gas is cooled to 150-160 ℃ through a secondary condenser after the reaction, and the discharged Claus tail gas is introduced into the next treatment process.
Preferably, the average pore diameter of the CuO-loaded activated carbon adsorbent is 10-30 nm.
Preferably, the preparation method of the CuO-loaded activated carbon adsorbent is as follows: adding 1-2kg of activated carbon in 50-100L of Cu (NO) with concentration of 5-10%3)2·3H2Dipping in O solution for 12-24h, filtering, roasting at 400 ℃ for 2-4h under the protection of inert gas, and cooling to obtain the CuO-loaded activated carbon adsorbent.
Preferably, the average pore diameter of the boron-nitrogen double-doped iron oxide activated carbon composite adsorbent is 2-5 nm.
Preferably, the preparation method of the boron-nitrogen double-doped iron oxide activated carbon composite adsorbent comprises the following steps: firstly, metal iron is taken as a target material, and high-purity N is obtained2And Ar is working gas, the surface of the activated carbon is subjected to magnetron sputtering, then the activated carbon is soaked in 0.5-1% borax solution for 0.5-1h, the solution is taken out and washed, dried, then treated at 400-600 ℃ for 2-4h, and cooled to obtain the boron-nitrogen double-doped iron oxide activated carbon composite adsorbent.
Preferably, said N is2And Ar in a flow ratio of (2-4): 1.
preferably, the specific conditions of the magnetron sputtering are as follows: the vacuum degree is 2-2.5 multiplied by 10-4Pa, the sputtering pressure is 0.5-1Pa, the sputtering power is 50-100W, and the sputtering time is 30-60 s.
The invention has the advantages that:
(1) the optimum desulfurization temperature of the industrial boiler flue gas is 120-250 ℃, and the desulfurization efficiency is higher at the temperature, and the flue gas is favorable for the rapid diffusion of the stack exhaust. The method firstly introduces 230-250 ℃ gas into the CuO-loaded activated carbon adsorbent, and efficiently removes H in the gas by utilizing the characteristic of higher removal efficiency of CuO at higher temperature2S, and preliminary removal of SO2Then, the gas is cooled to 120-150 ℃, and the boron-nitrogen double-doped iron oxide activated carbon composite adsorbent is used for desulfurization with high desulfurization activity, multiple active sites and uniform distribution to SO2Good removing effect, and deep removal of residual SO in gas2And H2And S. Through the combination of the processes, the desulfurization efficiency can be improved, the aim of efficient desulfurization is fulfilled, the desulfurization and purification effects of waste gas are good, the discharge temperature of the purified gas can be ensured to be higher, the exhaust gas of a chimney can be rapidly diffused, and the haze can be prevented from being formed;
(2) the invention firstly sprays the Claus tail gas through a spray tower to remove most of dust, oil mist and other particle impurities in the tail gas and reduce the adverse effect of impurities on the subsequent adsorption tower process, then orderly combines the adsorption towers with active carbon adsorbents with different pore diameters in series, so that the gas firstly passes through a first-stage adsorption tower with a CuO-loaded active carbon adsorbent with larger pore diameter. Through the gradient dust removal and desulfurization treatment of the process, the interference of particle impurities on the desulfurization process is effectively reduced, the stability of the process operation is improved, the desulfurization efficiency is greatly improved, and the desulfurization effect is improved.
In conclusion, the method for cleaning and purifying the sulfur-containing tail gas overcomes the defects that the conventional activated carbon tail gas desulfurization method is low in efficiency, unstable in desulfurization effect, poor in process operation stability, low in chimney exhaust temperature and easy to form haze, can be used for efficiently and stably desulfurizing, is high in process operation stability, can directly discharge treated gas into the atmosphere, is high in diffusion speed, and can effectively prevent the haze from forming.
Detailed Description
The technical solution of the present invention is further described with reference to the following specific examples.
Example 1
A method for cleaning and purifying sulfur-containing tail gas comprises the following steps:
(1) introducing the acid sulfur-containing tail gas into a combustion furnace for treatment at 1100 ℃, introducing the treated gas into a waste heat boiler for waste heat recovery, introducing the gas into a primary Claus reactor, wherein the inlet temperature of the primary Claus reactor is 235 ℃, performing reaction in the primary Claus reactor, cooling the gas to 150 ℃ through a primary condenser, heating the gas to 225 ℃ through a heat exchanger, introducing the gas into a secondary Claus reactor for reaction, cooling the gas to 150 ℃ through a secondary condenser after the reaction, performing condensation separation to obtain liquid sulfur, collecting the liquid sulfur through a liquid sulfur trap, and introducing the Claus tail gas after the liquid sulfur separation into the next treatment process;
(2) sending the Claus tail gas to the bottom of a spray tower, enabling the gas to move upwards, contacting with clear water sprayed downwards by a spray nozzle at the top of the spray tower, discharging the gas from the top of the spray tower, heating to 230-;
(3) introducing the heated gas into a first-stage adsorption tower filled with a CuO-loaded activated carbon adsorbent with the average pore diameter of 10nm for adsorption treatment, and then cooling to 120 ℃ through a heat exchanger, wherein the preparation method of the CuO-loaded activated carbon adsorbent comprises the following steps: 1kg of activated carbon was treated with 50L of 5% Cu (NO)3)2·3H2Dipping in O solutionTreating for 12h, filtering, roasting for 2h at 300 ℃ under the protection of inert gas, and cooling to obtain a CuO-loaded activated carbon adsorbent;
(4) introducing the gas subjected to temperature reduction treatment into a secondary adsorption tower filled with a boron-nitrogen double-doped iron oxide activated carbon composite adsorbent with the average pore diameter of 2nm for adsorption treatment, and discharging the treated gas, wherein the preparation method of the boron-nitrogen double-doped iron oxide activated carbon composite adsorbent comprises the following steps: firstly, metal iron is taken as a target material, and high-purity N is obtained2And Ar is a working gas, in N2And Ar in a flow ratio of 2: 1, soaking the surface of the activated carbon in a 0.5% borax solution for 0.5h, taking out, washing, drying, treating at 400 ℃ for 2h, and cooling to obtain the boron-nitrogen double-doped iron oxide activated carbon composite adsorbent.
Wherein, the specific conditions of magnetron sputtering are as follows: vacuum degree of 2X 10-4Pa, sputtering pressure of 0.5Pa, sputtering power of 50W, and sputtering time of 30 s.
Example 2
A method for cleaning and purifying sulfur-containing tail gas comprises the following steps:
(1) introducing the acid sulfur-containing tail gas into a combustion furnace for treatment at 1300 ℃, introducing the treated gas into a waste heat boiler for waste heat recovery, then introducing the gas into a primary Claus reactor, wherein the inlet temperature of the primary Claus reactor is 245 ℃, cooling the gas to 160 ℃ through a primary condenser after the reaction in the primary Claus reactor, heating the gas to 235 ℃ through a heat exchanger, introducing the gas into a secondary Claus reactor for reaction, cooling the gas to 160 ℃ through a secondary condenser after the reaction, performing condensation separation to obtain liquid sulfur, collecting the liquid sulfur through a liquid sulfur trap, and introducing the Claus tail gas after the liquid sulfur separation into the next treatment process;
(2) sending the Claus tail gas to the bottom of a spray tower, enabling the gas to move upwards, contacting with clear water sprayed downwards by a spray nozzle at the top of the spray tower, discharging the gas from the top of the spray tower, heating to 250 ℃ through a heat exchanger, enabling spray water to flow into an acid outlet tank, and concentrating and collecting through a concentration system;
(3) introducing the heated gas into a container with the average pore diameter ofAdsorbing in a first-stage adsorption tower of 30nm CuO-loaded activated carbon adsorbent, and then cooling to 1160 ℃ through a heat exchanger, wherein the preparation method of the CuO-loaded activated carbon adsorbent comprises the following steps: 2kg of activated carbon was added to 100L of 10% Cu (NO)3)2·3H2Soaking in O solution for 24h, filtering, roasting at 400 ℃ for 4h under the protection of inert gas, and cooling to obtain a CuO-loaded activated carbon adsorbent;
(4) introducing the gas subjected to temperature reduction treatment into a secondary adsorption tower filled with a boron-nitrogen double-doped iron oxide activated carbon composite adsorbent with the average pore diameter of 5nm for adsorption treatment, and discharging the treated gas, wherein the preparation method of the boron-nitrogen double-doped iron oxide activated carbon composite adsorbent comprises the following steps: firstly, metal iron is taken as a target material, and high-purity N is obtained2And Ar is a working gas, in N2And Ar at a flow ratio of 5: 1, soaking the surface of the activated carbon in a borax solution with the concentration of 1% for 1h, taking out, washing, drying, treating at 600 ℃ for 4h, and cooling to obtain the boron-nitrogen double-doped iron oxide activated carbon composite adsorbent.
Wherein, the specific conditions of magnetron sputtering are as follows: the degree of vacuum was 2.5X 10-4Pa, sputtering pressure of 1Pa, sputtering power of 100W, and sputtering time of 60 s.
Comparative example 1
The comparative example only differs from example 1 in that the average pore diameter of the boron-nitrogen double-doped iron oxide activated carbon composite adsorbent is 10 nm.
Comparative example 2
The comparative example only differs from example 1 in that the average pore size of the CuO activated carbon adsorbent is 2 nm.
Comparative example 3
The difference between the comparative example and the example 1 is only that the CuO active carbon adsorbent with the average pore diameter of 2nm replaces the boron-nitrogen double-doped iron oxide active carbon composite adsorbent with the average pore diameter of 2 nm.
The sulfur-containing tail gas purification methods of the above examples 1 to 2 and comparative examples 1 to 3 are adopted to purify acidic sulfur-containing tail gas, and the purified tail gas is sampled, detected and evaluated after the system runs for 0d and 60d respectively. The acid sulfur-containing tail gas comprises the following components:
H2S 29％，SO21.7％，COS 1.4％，CO219.3％，N213.4％，H2O 35.2％。
after treatment, the detection results of the tail gas are as follows:
comparing the example 1 with the comparative example 1, it is shown that in the secondary adsorption tower fine desulfurization process, the active carbon adsorption material with small pore diameter is needed to achieve the effect of fine desulfurization of tail gas with low sulfur concentration, so that the tail gas can reach the standard and be discharged; comparing the example 1 with the comparative example 2, the results show that the stable operation time of the system can be prolonged and the desulfurization efficiency can be kept stable for a long time by orderly and serially combining the adsorption towers of the activated carbon adsorbents with different pore diameters; comparing example 1 with example 3, it is demonstrated that the boron-nitrogen double-doped iron oxide activated carbon composite adsorbent used in the invention has high desulfurization efficiency, especially for SO2The removal effect is good, thereby achieving the purpose of high-efficiency desulfurization.
Claims (6)
1. The method for cleaning and purifying the sulfur-containing tail gas is characterized by comprising the following steps of:
(1) introducing the acid sulfur-containing tail gas into a combustion furnace for treatment at the temperature of 1100-1300 ℃, introducing the treated gas into a waste heat boiler for waste heat recovery, then sequentially introducing the gas into a primary Claus reactor, a primary condenser, a secondary Claus reactor and a secondary condenser, collecting liquid sulfur obtained by condensation and separation through a liquid sulfur trap, and introducing the Claus tail gas after liquid sulfur separation into the next treatment process;
(2) sending the Claus tail gas to the bottom of a spray tower, enabling the gas to move upwards, contacting with clear water sprayed downwards by a spray nozzle at the top of the spray tower, discharging the gas from the top of the spray tower, heating to 230-;
(3) introducing the heated gas into a primary adsorption tower loaded with a CuO activated carbon adsorbent for adsorption treatment, and then cooling to 120-160 ℃ through a heat exchanger;
(4) introducing the gas subjected to temperature reduction treatment into a secondary adsorption tower filled with a boron-nitrogen double-doped iron oxide activated carbon composite adsorbent for adsorption treatment, and discharging the treated gas;
the average pore diameter of the CuO-loaded activated carbon adsorbent is 10-30 nm;
the average pore diameter of the boron-nitrogen double-doped iron oxide activated carbon composite adsorbent is 2-5 nm.
2. The method as claimed in claim 1, wherein the temperature of the gas at the inlet of the primary Claus reactor is 235-245 ℃, the gas is cooled to 150-160 ℃ through the primary condenser after the reaction in the primary Claus reactor, the gas is heated to 225-235 ℃ through the heat exchanger, the gas is introduced into the secondary Claus reactor for the reaction, the gas is cooled to 150-160 ℃ through the secondary condenser after the reaction, and the discharged Claus tail gas is introduced into the next treatment process.
3. The method for cleaning and purifying sulfur-containing tail gas according to claim 1, wherein the preparation method of the CuO-loaded activated carbon adsorbent comprises the following steps: adding 1-2kg of activated carbon in 50-100L of Cu (NO) with concentration of 5-10%3)2·3H2Dipping in O solution for 12-24h, filtering, roasting at 400 ℃ for 2-4h under the protection of inert gas, and cooling to obtain the CuO-loaded activated carbon adsorbent.
4. The method for cleaning and purifying the sulfur-containing tail gas according to claim 1, wherein the preparation method of the boron-nitrogen double-doped iron oxide activated carbon composite adsorbent comprises the following steps: firstly, taking metallic iron as a target material, taking high-purity N2 and Ar as working gases, carrying out magnetron sputtering on the surface of activated carbon, then soaking in a borax solution with the concentration of 0.5-1% for 0.5-1h, taking out, washing, drying, then treating at 400-ion 600 ℃ for 2-4h, and cooling to obtain the boron-nitrogen double-doped iron oxide activated carbon composite adsorbent.
5. The method for cleaning and purifying the sulfur-containing tail gas according to claim 4, wherein the flow ratio of N2 to Ar is (2-4): 1.
6. the method for cleaning and purifying sulfur-containing tail gas according to claim 4, wherein the specific conditions of the magnetron sputtering are as follows: the vacuum degree is 2-2.5 multiplied by 10-4Pa, sputtering pressure 0.5-1Pa, sputtering power of 50-100W and sputtering time of 30-60 s.
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