CN110876878A - SO2Absorbent and absorption of SO2Method (2) - Google Patents

SO2Absorbent and absorption of SO2Method (2) Download PDF

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Publication number
CN110876878A
CN110876878A CN201811039435.1A CN201811039435A CN110876878A CN 110876878 A CN110876878 A CN 110876878A CN 201811039435 A CN201811039435 A CN 201811039435A CN 110876878 A CN110876878 A CN 110876878A
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China
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absorption
gas
absorbent
diisopropanolamine
temperature
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CN201811039435.1A
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Inventor
刘增让
刘爱华
徐翠翠
刘剑利
陶卫东
常文之
张艳松
吕才山
郝国杨
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China Petroleum and Chemical Corp
Qilu Petrochemical Co of Sinopec
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China Petroleum and Chemical Corp
Qilu Petrochemical Co of Sinopec
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Priority to CN201811039435.1A priority Critical patent/CN110876878A/en
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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
    • B01D53/14—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 absorption
    • B01D53/1456—Removing acid components
    • B01D53/1481—Removing sulfur dioxide or sulfur trioxide
    • 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
    • B01D53/14—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 absorption
    • B01D53/1418—Recovery of products
    • 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
    • B01D53/14—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 absorption
    • B01D53/1425—Regeneration of liquid absorbents
    • 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
    • B01D53/14—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 absorption
    • B01D53/18—Absorbing units; Liquid distributors therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
    • B01D2252/50—Combinations of absorbents
    • B01D2252/504—Mixtures of two or more absorbents

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Treating Waste Gases (AREA)

Abstract

The invention relates to a SO2Absorbent and absorption of SO2Belonging to the technical field of gas purification. SO according to the invention2The absorbent comprises the following raw materials in percentage by weight: 10-30% of diisopropanolamine, 10-25% of compound component and the balance of water; the complex component is one or more of 2-amino-2-methyl-1-propanol, diethylethanolamine or methylethanolamine. SO according to the invention2Absorbent, low cost, SO2High absorption rate and SO in tail gas after absorption2At 30mg/m3Hereinafter, the atmosphere may be directly discharged; the invention also provides the SO absorption method which has the advantages of simple process, low energy consumption, economy, environmental protection and no secondary pollution2The method of (1).

Description

SO2Absorbent and absorption of SO2Method (2)
Technical Field
The invention relates to a SO2Absorbent and absorption of SO2Belonging to the technical field of gas purification.
Background
SO2Is one of the most important environmental pollutants and is the most important cause of acid rain. SO (SO)2Can destroy the physiological function of plants, slow down the growth of crops and forests, and enable human bodies to inhale SO with higher concentration2Gas, which causes strong stimulation of the respiratory tract, SO2Has received wide attention as a main emission treatment technology of atmospheric pollutants. In recent years, SO2The discharge causes that 40 percent of the territorial area of China is damaged by acid rain, and the annual loss caused by the discharge is as high as 1100 billion yuan. SO emitted by the oil refining industry by 2020 according to the current emission control level2Will reach 126993 t/a. Thus, pollution control and SO reduction2The emission is an important task for sustainable development of the economic society of China.
The sulfur emission requirement of industrially developed countries is very strict, and the regulations of the environmental protection agency of the federal government of the United states stipulate heating furnace flue gas, sulfur tail gas and catalytic cracking regeneration flue gas SO of petroleum refining industry2The emission concentration limit is 50ppm (v) and is about 143mg/m3。
According to the requirements of national emission Standard of pollutants for Petroleum refining industry (GB31570-2015), sulfur dioxide with the limit value of emission concentration of atmospheric pollutants of sulfur devices in China is executed to be less than 400mg/Nm from 7-1.7.20173Especially less than 100mg/Nm3。
With the stricter environmental regulations, the development of a novel process for effectively reducing SO2Emission is the root of the enterprise to live. The worldwide research of the desulfurization technology from the 20 th century and the 50 th century has reached more than 200, and the main method is wet desulfurizationSulfur, semi-dry desulfurization, rotary spray-drying desulfurization, electron beam desulfurization and other desulfurization processes.
In the desulfurization technology applied in industry at present, wet desulfurization is the most common, especially the limestone/gypsum method, although the method has high desulfurization rate and cheap and easily available absorbent, the method has large water consumption, waste water is discharged during operation, the comprehensive utilization of the desulfurization gypsum is difficult in some places, most of desulfurization byproduct gypsum is idle and stacked to form a large amount of solid and liquid wastes, thereby occupying valuable land resources and causing secondary pollution. The solvent reproducible wet desulphurization technology can generate high-concentration SO by the regeneration and recycling of the desulfurizer2Has better environmental and economic benefits, but also has SO2Low absorption efficiency, high energy consumption, high cost, immature process and the like. MDEA as absorbent mainly for absorbing H in gas2S, then the MDEA is resolved and regenerated for recycling, but the MDEA cannot be used for absorbing SO2The main reason is SO2The combination with MDEA is an irreversible reaction, difficult to regenerate, and after absorption, the salt content in the solvent increases, foaming and corrosion phenomena occur.
CN103908872 discloses an absorbent for recovering sulfur dioxide from industrial waste gas and a recovery method, which is characterized in that: mixing piperazine and water, stirring uniformly, and adding ethylene oxide to react under the stirring state; reacting the obtained reaction product with boric acid to obtain organic amine salt; finally, dissolving the organic amine salt in water to prepare an amine salt aqueous solution to obtain the absorbent; the absorption method is that the absorbent is contacted with the gas flow containing sulfur dioxide in a countercurrent way, so that the sulfur dioxide is dissolved in the absorbent to remove the sulfur dioxide, and simultaneously, the absorption liquid absorbing the sulfur dioxide is contacted with steam to be regenerated, thereby being capable of recycling. The desulfurizer prepared by the method is easy to foam, has poor fluctuation resistance and large loss in industrial operation, and cannot meet the existing discharge standard.
CN101721884 discloses a method for using piperazine compound as recyclable sulfur dioxide gas absorbent. CN101537300 discloses a method of using an ionic liquid with a multi-nitrogen straight-chain amine as a recyclable sulfur dioxide gas absorbent. However, all of the above methods have disadvantages such as a small absorption capacity and a high solvent price.
Disclosure of Invention
The invention aims to provide SO2Absorbent, low cost, SO2High absorption rate and SO in tail gas after absorption2At 30mg/m3Hereinafter, the atmosphere may be directly discharged; the invention also provides the SO absorption method which has the advantages of simple process, low energy consumption, economy, environmental protection and no secondary pollution2The method of (1).
SO according to the invention2The absorbent comprises the following raw materials in percentage by weight: 10-30% of diisopropanolamine, 10-25% of compound component and the balance of water;
the complex component is one or more of 2-amino-2-methyl-1-propanol, diethylethanolamine or methylethanolamine.
The main function of the diisopropanolamine in the invention is to absorb SO2The main functions of the compound components are to improve the selectivity of the absorbent and reduce the regeneration energy consumption. The sulfur tail gas not only contains SO2And also contains CO2Gas, diisopropanolamine not only absorbs SO2While also absorbing CO2The steric effect of the compound components is utilized to reduce CO2The co-absorption of the absorbent improves the sulfur capacity of the absorbent and reduces the regeneration energy consumption of the absorbent at the same time.
Preferably, the feed comprises the following raw materials in percentage by weight: 25% of diisopropanolamine, 10% of diethylethanolamine, 5% of methylethanolamine and 60% of water.
Preferably, the feed comprises the following raw materials in percentage by weight: 10% of diisopropanolamine, 10% of 2-amino-2-methyl-1-propanol and 80% of water.
Preferably, the feed comprises the following raw materials in percentage by weight: 30% of diisopropanolamine, 5% of 2-amino-2-methyl-1-propanol, 15% of diethylethanolamine, 5% of methylethanolamine and 45% of water.
Using said SO2Absorption of SO by an absorbent2The method of (1) is to contain SO2Is introduced withThe SO2Absorption tower of absorbent, absorbent and SO-containing liquid2Countercurrent contact of the gas stream, SO2Absorbed by the absorbent; absorption of SO2The purified tail gas is discharged; containing SO2The rich solution enters a regeneration tower for regeneration, and the regenerated high-purity SO2Enters a sulfur recovery device for reutilization to produce high-purity liquid SO2Or used as acid-making raw material.
Will contain SO2Before the gas (A) is introduced into the absorption column, the gas (B) contains SO2The gas temperature of the gas is controlled to be 25-45 ℃; the temperature of the absorption tower is controlled to be 25-45 ℃; the temperature of the regeneration tower is controlled to be 110-125 ℃. Ensure the emission of SO in the atmosphere2The content is less than 30mg/m3。
Before being introduced into the absorption tower, contains SO2Is lower than the temperature of the absorption tower to prevent a large amount of water in the gas from condensing into the absorbent and reduce the absorbent concentration, thereby reducing SO2And (4) absorption effect. Preferably, containing SO2The temperature of the gas is 3-5 ℃ lower than that of the absorption tower.
Absorption of SO2SO in the purified tail gas2The content is less than 30mg/m3。
The regenerated high-purity SO of the invention2The sulfur recovery device is used for processing, which means that any part of the sulfur production furnace entering the sulfur recovery device before the hydrogenation reactor can be an air line and an acid gas line of the sulfur production furnace, and can also be a primary converter, a secondary converter and the like.
The specific process flow is as follows: containing SO2The gas is cooled to 25-45 ℃ by a gas cooler and enters a gas cooler filled with the SO2Absorption tower of absorbent, SO at 25-45 deg.C2Is absorbed by amine liquid to absorb SO2SO in the purified tail gas2The content is less than 30mg/m3The tail gas is emptied after purification; containing SO2The rich solution is pumped into a lean and rich solution heat exchanger by a rich solvent pump for heat exchange, then enters the top of a regeneration tower for regeneration, a reboiler at the bottom of the regeneration tower is controlled to control the regeneration temperature to be 110-125 ℃, the regenerated lean absorption solution enters an absorption tower for continuous absorption of SO after heat exchange by a lean and rich solution heat exchanger2Regenerated high-purity SO2The sulfur enters a sulfur recovery device for treatment to produce high-purity liquid SO2Or used as acid-making raw material. See in particular fig. 1.
The invention has the following beneficial effects:
(1) the invention provides a compound organic amine desulfurizer with low cost and SO2High absorption rate, high sulfur capacity up to 25g/L, and absorbed SO in tail gas2At 30mg/m3Can directly discharge the atmosphere to ensure SO2The emission meets the latest national emission requirements, can be applied to sulfur dioxide waste gas generated by burning low-concentration (0-30 percent by volume) hydrogen sulfide, and can also treat various SO-containing flue gas of sulfur devices, catalytic cracking flue gas and the like2Absorbing gas;
(2) the invention provides a method for absorbing SO2The method can realize the recycling of the absorbent, and the regenerated high-purity SO2Can be introduced into a sulfur recovery device for treatment to produce high-purity liquid SO2Or used as acid-making raw materials, can realize the recycling of sulfur resources, and has the advantages of simple process, low energy consumption, economy, environmental protection and no secondary pollution.
Drawings
FIG. 1 is a diagram of SO absorption according to the present invention2The process flow diagram of (1);
in the figure: 1. containing SO2The gas of (4); 2. a gas cooler; 3. an absorption tower; 4. a rich solvent pump; 5. a lean-rich liquid heat exchanger; 6. barren liquor; 7. a regeneration tower; 8. high purity SO2(ii) a 9. A bottom reboiler.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the practice of the invention.
Example 1
As shown in figure 1, the process of the invention is adopted to treat flue gas of a sulfur plant, wherein SO is contained in the flue gas2The concentration is 10000mg/m3Cooling the flue gas to 40 ℃ by a gas cooler, and then feeding the flue gas into an absorption tower, wherein the absorption liquid used by the absorption tower is a compound solution of diisopropanolamine and 2-amino-2-methyl-1-propanol, wherein the diisopropanolamine accounts for 30% (wt), and the 2-amino-2-15 percent (wt) of methyl-1-propanol, the temperature of the absorption tower is 42 ℃, the absorbed rich solution enters a regeneration tower for regeneration, the regeneration temperature is 120 ℃, and the regenerated SO2And feeding the sulfur into an air line of a sulfur making furnace of a Claus sulfur device. The emission of sulfur dioxide in the absorbed tail gas is 15mg/m3。
Compared with the method of directly discharging through a chimney, the method can reduce the SO of the flue gas of the sulfur device2The discharge concentration is 310mg/m3。
Example 2
As shown in figure 1, the process of the invention is used for treating flue gas containing catalytic cracking gas, wherein SO is contained in the flue gas2The concentration is 25000mg/m3Cooling the flue gas to 33 ℃ by a gas cooler, then feeding the cooled flue gas into an absorption tower, wherein absorption liquid used by the absorption tower is a compound solution of diisopropanolamine and diethylethanolamine, wherein the diisopropanolamine accounts for 25 percent (wt), the diethylethanolamine accounts for 25 percent (wt), the absorption temperature is 35 ℃, absorbing rich liquid enters a regeneration tower for regeneration, the regeneration temperature is 125 ℃, and regenerating SO2For producing high-purity liquid SO2. The emission of sulfur dioxide in the absorbed tail gas is 20mg/m3。
Compared with the conventional limestone/gypsum wet desulphurization process, the SO can be reduced2Discharge 85mg/m3And low value-added products such as desulfurized gypsum and the like are not generated, and secondary pollution is avoided.
Example 3
As shown in figure 1, the process of the invention is adopted to treat flue gas of a sulfur plant, wherein SO is contained in the flue gas2The concentration is 20000mg/m3Cooling the tail gas to 36 ℃ by a gas cooler, then feeding the tail gas into an absorption tower, wherein the absorption liquid used by an absorption unit is a compound solution of diisopropanolamine, diethylethanolamine and methylethanolamine, wherein the diisopropanolamine accounts for 25 percent (wt), the diethylethanolamine accounts for 10 percent (wt), the methylethanolamine accounts for 5 percent (wt), the absorption temperature is 38 ℃, the absorbed rich solution is fed into a regeneration tower for regeneration, the regeneration temperature is 115 ℃, and the regenerated SO is2The re-returning device is used as acid-making raw material. The emission of sulfur dioxide in the tail gas after absorption is 10mg/m3。
Compared with the conventional limestone/gypsum wet desulphurization process, the SO can be reduced2Discharge 78mg/m3And does not generateDesulfurized gypsum and other low value-added products, and no secondary pollution.
Example 4
As shown in figure 1, the process of the invention is used for treating sulfur dioxide gas generated by burning certain low-concentration hydrogen sulfide, wherein SO is2The concentration is 23000mg/m3Cooling the gas to 30 ℃ by a gas cooler, then feeding the gas into an absorption tower, wherein absorption liquid used by the absorption tower is a compound solution of diisopropanolamine and methylethanolamine, wherein the diisopropanolamine accounts for 25 percent (wt), the methylethanolamine accounts for 15 percent (wt), the absorption temperature is 35 ℃, absorbing pregnant solution enters a regeneration tower for regeneration, the regeneration temperature is 110 ℃, and regenerating SO2For producing high-purity liquid SO2. At this time, the sulfur dioxide emission of the device is 15mg/m3。
Compared with the conventional limestone/gypsum wet desulphurization process, the SO can be reduced2Discharge 90mg/m3And low value-added products such as desulfurized gypsum and the like are not generated, and secondary pollution is avoided.
Example 5
As shown in figure 1, the process of the invention is adopted to treat the flue gas of a sulfur device, the flue gas is cooled to 32 ℃ by a gas cooler and then enters an absorption tower, absorption liquid used by the absorption tower is a compound solution of diisopropanolamine and diethylethanolamine, wherein the diisopropanolamine is 18 percent (wt), the diethylethanolamine is 24 percent (wt), the absorption temperature is 33 ℃, the absorbed rich liquid enters a regeneration tower for regeneration at the regeneration temperature of 119 ℃, and the regenerated SO is regenerated2Feeding into the inlet of a first-stage condenser of a Claus sulfur device sulfur production furnace. At this time, the sulfur dioxide emission of the device is 20mg/m3。
Compared with the method of directly discharging through a chimney, the method can reduce the SO of the flue gas of the sulfur device2Emission concentration 180mg/m3。
Example 6
As shown in figure 1, the process of the invention is adopted to treat flue gas containing catalytic cracking, the flue gas is cooled to 25 ℃ by a gas cooler and then enters an absorption tower, absorption liquid used by the absorption tower is a compound solution of diisopropanolamine and 2-amino-2-methyl-1-propanol, wherein the diisopropanolamine accounts for 30 percent (wt), the 2-amino-2-methyl-1-propanol accounts for 10 percent (wt) and the absorption temperature is 28 ℃,the absorbed rich solution enters a regeneration tower for regeneration at the regeneration temperature of 110 ℃, and regenerated SO2Feeding into the inlet of a secondary converter of a Claus sulfur device sulfur production furnace. The emission of sulfur dioxide in the tail gas after absorption is 11mg/m3。
Compared with the conventional limestone/gypsum wet desulphurization process, the SO can be reduced2Discharge 69mg/m3And low value-added products such as desulfurized gypsum and the like are not generated, and secondary pollution is avoided.
Example 7
As shown in figure 1, the catalytic cracking flue gas is treated by the process of the invention, the gas is cooled to 43 ℃ by a gas cooler and then enters an absorption tower, absorption liquid used by the absorption tower is a compound solution of diisopropanolamine, 2-amino-2-methyl-1-propanol and methylethanolamine, wherein the diisopropanolamine accounts for 20% (wt), the 2-amino-2-methyl-1-propanol accounts for 10% (wt), the methylethanolamine accounts for 15% (wt), the absorption temperature is 45 ℃, the absorbed rich solution enters a regeneration tower for regeneration, the regeneration temperature is 118 ℃, and the regenerated SO2The returning device is used as acid-making raw material. The emission of sulfur dioxide in the tail gas after absorption is 23mg/m3。
Compared with the conventional limestone/gypsum wet desulphurization process, the SO can be reduced2Discharge 42mg/m3And low value-added products such as desulfurized gypsum and the like are not generated, and secondary pollution is avoided.
Example 8
As shown in figure 1, the process of the invention is adopted to treat certain gas containing sulfur dioxide, the flue gas is cooled to 32 ℃ by a gas cooler and then enters an absorption tower, absorption liquid used by the absorption tower is a compound solution of diisopropanolamine and 2-amino-2-methyl-1-propanol, wherein the diisopropanolamine accounts for 10 percent (wt), the 2-amino-2-methyl-1-propanol accounts for 15 percent (wt), the absorption temperature is 34 ℃, the absorbed rich solution enters a regeneration tower for regeneration, the regeneration temperature is 115 ℃, and the regenerated SO2Feeding into the inlet of a secondary converter of a Claus sulfur device sulfur production furnace. The emission of sulfur dioxide in the tail gas after absorption is 19mg/m3。
Compared with the conventional limestone/gypsum wet desulphurization process, the SO can be reduced2Discharge 35mg/m3And low additive such as desulfurized gypsum is not generatedNo secondary pollution.

Claims (10)

1. SO (SO)2The absorbent is characterized by comprising the following raw materials in percentage by weight: 10-30% of diisopropanolamine, 10-25% of compound component and the balance of water;
the complex component is one or more of 2-amino-2-methyl-1-propanol, diethylethanolamine or methylethanolamine.
2. SO according to claim 12The absorbent is characterized by comprising the following raw materials in percentage by weight: 25% of diisopropanolamine, 10% of diethylethanolamine, 5% of methylethanolamine and 60% of water.
3. SO according to claim 12The absorbent is characterized by comprising the following raw materials in percentage by weight: 10% of diisopropanolamine, 10% of 2-amino-2-methyl-1-propanol and 80% of water.
4. SO according to claim 12The absorbent is characterized by comprising the following raw materials in percentage by weight: 30% of diisopropanolamine, 5% of 2-amino-2-methyl-1-propanol, 15% of diethylethanolamine, 5% of methylethanolamine and 45% of water.
5. Use of a SO as claimed in any one of claims 1 to 42Absorption of SO by an absorbent2The method of (2), characterized by: will contain SO2Is introduced with the SO2Absorption tower of absorbent, absorbent and SO-containing liquid2Countercurrent contact of the gas stream, SO2Absorbed by the absorbent; absorption of SO2The purified tail gas is discharged; containing SO2The rich solution enters a regeneration tower for regeneration, and the regenerated high-purity SO2And the sulfur enters a sulfur recovery device for reutilization.
6. SO absorption according to claim 52The method of (2), characterized by: will contain SO2Is introduced into the gas channelBefore entering the absorption tower, containing SO2The gas temperature of the gas is controlled to be 25-45 ℃; the temperature of the absorption tower is controlled to be 25-45 ℃.
7. SO absorption according to claim 52The method of (2), characterized by: the temperature of the regeneration tower is controlled to be 110-125 ℃.
8. SO absorption according to claim 52The method of (2), characterized by: before being introduced into the absorption tower, contains SO2The temperature of the gas of (a) is lower than the temperature of the absorption column.
9. SO absorbed according to claim 82The method of (2), characterized by: containing SO2The temperature of the gas is 3-5 ℃ lower than that of the absorption tower.
10. SO absorption according to claim 52The method of (2), characterized by: absorption of SO2SO in the purified tail gas2The content is less than 30mg/m3。
CN201811039435.1A 2018-09-06 2018-09-06 SO2Absorbent and absorption of SO2Method (2) Pending CN110876878A (en)

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刘克友等: "MDEA法炼厂气脱硫", 《炼油设计》 *

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Application publication date: 20200313