CN109772134B - Circulation desorption H2S and SO2And process for recovering sulfur - Google Patents
Circulation desorption H2S and SO2And process for recovering sulfur Download PDFInfo
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- CN109772134B CN109772134B CN201910021462.4A CN201910021462A CN109772134B CN 109772134 B CN109772134 B CN 109772134B CN 201910021462 A CN201910021462 A CN 201910021462A CN 109772134 B CN109772134 B CN 109772134B
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Abstract
The invention discloses a method for circularly removing H2S and SO2And a method for recovering sulfur, belonging to the field of energy conservation, emission reduction and gas purification. The method of the invention is to mix H2S or SO2With absorption of SO in the column2Or H2The organic base-solvent reaction of S can be simultaneously absorbed by regenerated organic base and organic base not used in the process, and the regenerated organic base and the organic base not used absorb H2S or SO2Then the solid-liquid separation in the separation tower can be directly carried out to the next reaction absorption tower for utilization. The invention realizes the traditional high-temperature gas-phase Claus process under the mild condition of liquid phase, and breaks through the thermal balance limitation of high temperature to Claus reaction so as to improve the conversion rate; and simultaneously solves the problem of removing H by using organic amine in industry2S and SO2The existing desorption energy consumption is high, and the loss of the absorbent is serious; secondly, the method carries out absorption and reaction in a single device, and is more consistent with the concept of green chemistry.
Description
Technical Field
The invention relates to a method for circularly removing H2S and SO2And a method for recovering sulfur, belonging to the field of energy conservation, emission reduction and gas purification.
Background
H2S is a toxic, harmful, strongly irritating, odorous acid gas, which is present in large amounts in oil and gas refinery desulfurization processes, while SO2Is also an acid gas with pungent smell and corrosiveness, and is abundantly present in coal-fired enterprises. H2S and SO2And the coal bed gas exists in the coal bed gas, and the coal bed gas can cause serious pollution to the atmospheric environment, so the coal bed gas must be collected and purified to reach the national emission standard for emission. At present H2S and SO2Mainly through the concentration and the trapping of an organic amine absorbent, and then through medium temperature desorption, the organic amine absorbent is sent to the next process for carrying out the processThe application is as follows. The process has the problem of serious volatilization loss of the absorbent and high energy consumption, and the process is suitable for H2S is utilized to be converted into elemental sulfur by a Claus reaction, and a part of concentrated and trapped H is required to be firstly concentrated in the traditional gas-phase Claus reaction2High temperature oxidation of S to SO2Then the reaction is carried out under the conditions of catalyst and high heat, the high heat condition not only can bring the problem of overhigh energy consumption, but also can inhibit the heat release reaction in the Claus process, thereby causing low conversion rate, finally the tail gas also needs a fine desulfurization process, and the whole process is complex and tedious and has longer flow.
Disclosure of Invention
The invention aims to provide a method for circularly removing H2S and SO2And a process for recovering sulfur which is effective in improving existing H2S and SO2The method has the advantages that the method has the defects of a removal technology and a gas-phase Claus sulfur recovery technology, simultaneously, waste gas resources are comprehensively configured and reasonably utilized to the greatest extent, and the method specifically comprises the following steps:
(1) containing H2Industrial waste gas of S from H2The bottom of the S absorption reaction tower is filled with organic alkali-solvent and SO absorbed from the subsequent process circulation2From H with an organic base-solvent2S flows into the top of the absorption reaction tower and absorbs SO2And H2S is subjected to liquid-phase Claus reaction to generate sulfur simple substance and regenerate organic alkali absorbent, and the unused organic alkali-solvent and the organic alkali regenerated by the liquid-phase Claus reaction can also absorb the introduced H2S, discharging the treated waste gas from the top of the tower and discharging the treated waste gas from H2Introducing the reaction liquid discharged from the bottom of the S absorption reaction tower into a separation tank, extracting elemental sulfur from the bottom of the separation tank, and absorbing H from the top of the separation tank2Organic base-solvent of S is passed through SO2An absorption reaction tower;
(2) containing SO2Industrial waste gas is introduced into SO from the bottom2Absorption in a reaction column at SO2Absorbing H in the absorption reaction tower2Organic base-solvent of S with SO introduced2The liquid-phase Claus reaction is carried out to generate sulfur simple substance and regenerate organic base, and the regenerated organic base and the organic base which is not utilized in the original system can also absorb SO2The treated waste gas is discharged from the top of the tower, and SO is absorbed2And the organic alkali-solvent liquid phase system containing sulfur simple substance is separated from SO2Introducing the bottom of the absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and finally absorbing SO2Is pumped from the top of the separation tank into H2S absorption reaction tower to realize circulation reaction absorption process; the circulating reaction absorption time in the steps (1) and (2) is any time.
Preferably, H in step (1) of the present invention2The S partial pressure is 0.1-10% atm.
Preferably, the organic base in the organic base-solvent of the present invention is: tetramethyl guanidine, 3-pyridine methanol, cyclohexylamine, N-methyl cyclohexylamine, N-dimethyl aniline, 1, 8-diazabicycloundecen-7-ene (DBU), dimethyl ethanolamine and diisopropanolamine, and the solvent is one of sulfolane, diethylene glycol monomethyl ether, ethanol, water and N-methyl pyrrolidone.
Preferably, the organic base in the organic base-solvent of the present invention is 30 to 75 mol%.
Preferably, step (2) SO of the present invention2The partial pressure is 1 to 15 percent atm.
The principle of the invention is as follows:
first, acid gas H2S or SO2After the liquid phase system containing the organic base is introduced, the organic base can react with the acidic SO2Or H2S undergoes neutralization reaction to absorb SO2Or H2S; absorption principle using N, N-dimethylaniline as an example: n, N-dimethylaniline and SO2Or H2S is subjected to neutralization reaction to form: electron transfer product N, N-dimethylaniline SO2And proton transfer product N, N-dimethylaniline-hydrosulphate, the specific reaction equation is as follows:
n, N-dimethylaniline and SO2Principle of generating electron transfer product by neutralization reaction:
n, N-dimethylaniline and H2The principle of S neutralization reaction to generate proton transfer products:
then, based on SO2And H2The centering reaction of S:
， SO2or H2After S is absorbed by organic alkali to form corresponding products, the absorbed products and the introduced H2S or SO2Gas is subjected to centering reaction to generate elemental sulfur and water and regenerate absorbent organic alkali at the same time; absorption of SO using N, N-dimethylaniline as example2Or H2S with H2S or SO2The equation for the reaction is as follows:
SO absorption by N, N-dimethylaniline2Formed electron transfer product with H introduced2S reaction equation:
absorption of H by N, N-dimethylaniline2Proton transfer product formed by S and SO introduced2The reaction equation is as follows:
according to the invention, SO is absorbed in each absorption reaction tower2Or H2S organic base-solvent system will not only react with the introduction of H2S or SO2React to form elemental sulfur and regenerate the absorbent to continue absorbing H2S and SO2In each absorption reaction tower, the reaction and the absorption processes are simultaneously carried out to cooperatively remove H2S or SO2And the regenerated organic alkali is absorbedH collection2S or SO2The SO is pumped into the separation tower after the solid-liquid separation of the sediment2Or H2S absorption reaction tower utilization, thus achieving the purpose of circularly removing H2S and SO2The purpose of recovering sulfur.
In addition, the organic base-solvent system of the present invention absorbs H2S or SO2The product formed can be regarded as gaseous H after being dissolved by the solvent2S or SO2So that no solid catalyst is required for the reaction and thus no high temperature conditions are required; in addition, the reaction is an exothermic oxidation-reduction reaction with greatly reduced Gibbs free energy, so that the reaction range of the centering reaction is deeper and the conditions are milder compared with those of a gas phase. Thus, the reaction is faster and the conversion rate is higher.
The invention has the beneficial effects that:
(1) h introduced in the invention2S or SO2With absorption of SO in the column2Or H2The organic base-solvent reaction of S can be simultaneously absorbed by regenerated organic base and organic base not used in the process, and the regenerated organic base and the organic base not used absorb H2S or SO2Then the solid-liquid separation of the separation tower can be directly carried out to enter next SO2Or H2S, utilizing a reaction absorption tower; the circulation process avoids the desorption and regeneration process of the organic alkali, and effectively solves the problems of high desorption energy consumption and serious volatilization loss of the absorbent in the traditional amine absorption process.
(2) H introduced into the process of the invention2S or SO2Two processes of reaction and absorption are simultaneously carried out in the tower, so that the introduced H is introduced2S or SO2The utilization mode is more, the utilization efficiency is higher, and therefore the removal rate of the process is higher than that of the traditional amine absorption process.
(3) The invention realizes the traditional gas phase Claus reaction under the condition of mild liquid phase without adding any catalyst, breaks the thermal balance limit of the gas phase Claus reaction, reduces the reaction energy consumption and greatly improves the H2(ii) the conversion rate of S; and due to the addition of organic base to H2S or SO2Activation of (D), plus Delta of the Claus reactionrGm<<0, the reaction degree is larger, so that the liquid phase Claus reaction in the system is quicker and more efficient, and the reaction is carried out when H is used2S or SO2The method has good effect at lower partial pressure, so that a subsequent fine desulfurization process is not needed, and the method is a great improvement on the traditional gas-phase Claus process.
(4) Conventional complete removal of H2The S process comprises an absorption section and a Claus sulfur recovery section, and the method of the invention carries out absorption and reaction in a single device, namely an absorption tower, with high conversion rate, so that the complex traditional H removal is realized2The S process is simpler and more efficient, and better conforms to the concept of green chemistry.
(5) The process of the invention can be carried out not only in H2S removal field application, and when SO exists in a certain region simultaneously2Or H2When two kinds of waste gas are used, such as coal bed gas exploitation process, the process can play a role in greatly removing H simultaneously, efficiently, quickly and circularly2S and SO2The method has the advantages of simultaneously solving the problem of removing two types of waste gases.
(6) In the process of the invention H2S and SO2Respectively analyzing H by a flue gas analyzer under low partial pressure of 0.1-10 percent and low partial pressure of 1-10 percent2S and SO2The removal rates of the catalyst are 97.7-99.8% and 98.4-99.9% respectively; circulating for a period of time, and then obtaining H by recording the flow of the inlet and outlet flue gas and analyzing by a flue gas analyzer2S and SO2The outlet concentration of the sulfur is 5ppm to 20ppm and 300ppm to 950ppm respectively, and the recovery rate of the sulfur simple substance is 96.2 percent to 99.2 percent.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The invention is described in further detail below with reference to specific process embodiments, without limiting the scope of the invention.
Example 1
Energy-saving high-efficiency recyclable H removal by liquid-phase Claus2S and SO2The process method for recovering sulfur comprises the following specific flow:
(1) h containing 1% atm2S waste gas from H2Introducing a liquid phase consisting of organic alkali and solvent into the bottom of the S absorption reaction tower, and absorbing SO circularly from the subsequent process2From the organic base-solvent liquid phase of H2S flows into the top of the absorption reaction tower and circularly absorbs SO2And H2S is subjected to liquid-phase Claus reaction to generate sulfur simple substance and regenerate organic alkali absorbent, and the unused organic alkali-solvent and the organic alkali regenerated by the liquid-phase Claus reaction can also absorb the introduced H2S, discharging the treated waste gas from the top of the tower; then absorb H2S and sulfur-containing organic base-solvent solid-liquid two-phase system from H2Introducing the bottom of the S absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and absorbing H from the top of the separation tank2Organic base-solvent pumping of S into SO2In the absorption reaction tower, the organic base in the organic base-solvent is N, N-dimethylaniline, the solvent is diethylene glycol monomethyl ether, and the mole percentage content of the organic base in the organic base-solvent is 30%.
(2) SO containing 5% atm2Introducing SO into the waste gas from the bottom2Absorption reaction column in which H is also absorbed2Organic base-solvent of S with SO introduced2The liquid-phase Claus reaction is carried out to generate sulfur simple substance and regenerate organic base, and the regenerated organic base and the organic base which is not utilized in the original system can also absorb SO2The treated waste gas is discharged from the top of the tower, and SO is absorbed2And the organic alkali-solvent liquid phase system containing sulfur simple substance is separated from SO2Introducing the bottom of the absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and finally absorbing SO2Is pumped from the top of the separation tank into H2S absorption reaction tower
After 30min circulation, H is analyzed by a flue gas analyzer and a flow meter at the inlet and the outlet and the mole number of the sulfur simple substance is obtained, and after 30min circulation, H is carried out2The removal rate of S is 99.3%, SO2The removal rate of (A) is 99.4%, H2S outlet concentration is 8ppm, SO2The outlet concentration is 200 ppm; circulating for 30min to obtain element SThe recovery rate was 98.2%.
Example 2
Energy-saving high-efficiency recyclable H removal by liquid-phase Claus2S and SO2The process method for recovering sulfur comprises the following specific flow:
(1) h containing 5% atm2S waste gas from H2Introducing a liquid phase consisting of organic alkali and solvent into the bottom of the S absorption reaction tower, and absorbing SO circularly from the subsequent process2From the top of the column, the organic base-solvent liquid phase of (A) is circulated and SO is absorbed2And H2S is subjected to liquid-phase Claus reaction to generate sulfur simple substance and regenerate organic alkali absorbent, and the unused organic alkali-solvent and the organic alkali regenerated by the liquid-phase Claus reaction can also absorb the introduced H2And S, discharging the treated waste gas from the top of the tower. Then absorb H2S and sulfur-containing organic base-solvent solid-liquid two-phase system from H2Introducing the bottom of the S absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and absorbing H from the top of the separation tank2Organic base-solvent pumping of S into SO2In the absorption reaction tower, the organic base in the organic base-solvent is N, N-dimethylaniline, the solvent is diethylene glycol monomethyl ether, and the mole percentage content of the organic base in the organic base-solvent is 30%.
(2) SO containing 5% atm2Introducing SO into the waste gas from the bottom2Absorption reaction column in which H is also absorbed2Organic base-solvent of S with SO introduced2The liquid-phase Claus reaction is carried out to generate sulfur simple substance and regenerate organic base, and the regenerated organic base and the organic base which is not utilized in the original system can also absorb SO2The treated waste gas is discharged from the top of the tower, and SO is absorbed2And the organic alkali-solvent liquid phase system containing sulfur simple substance is separated from SO2Introducing the bottom of the absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and finally absorbing SO2Is pumped from the top of the separation tank into H2And S absorption reaction tower.
After 40min circulation, H is analyzed by a flue gas analyzer and a flow meter at the inlet and the outlet and the mole number of the sulfur simple substance is obtained, and after 40min circulation, H is carried out2The removal rate of S is 98.7%, SO2The removal rate of (A) was 99.2%, H2The outlet concentration of S is 12ppm, SO2The outlet concentration was 313 ppm; the recovery rate of the element S is 97.6 percent within 40min of circulation.
Example 3
Energy-saving high-efficiency recyclable H removal by liquid-phase Claus2S and SO2The process method for recovering sulfur comprises the following specific flow:
(1) h containing 1% atm2S waste gas from H2Introducing a liquid phase consisting of organic alkali and solvent into the bottom of the S absorption reaction tower, and absorbing SO circularly from the subsequent process2From the top of the column, the organic base-solvent liquid phase of (A) is circulated and SO is absorbed2And H2S is subjected to liquid-phase Claus reaction to generate sulfur simple substance and regenerate organic alkali absorbent, and the unused organic alkali-solvent and the organic alkali regenerated by the liquid-phase Claus reaction can also absorb the introduced H2And S, discharging the treated waste gas from the top of the tower. Then absorb H2S and sulfur-containing organic base-solvent solid-liquid two-phase system from H2Introducing the bottom of the S absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and absorbing H from the top of the separation tank2Organic base-solvent pumping of S into SO2In the absorption reaction tower, the organic base in the organic base-solvent is N, N-dimethylaniline, the solvent is sulfolane, and the mole percentage content of the organic base in the organic base-solvent is 60%.
(2) SO containing 15% atm2Introducing SO into the waste gas from the bottom2Absorption reaction column in which H is also absorbed2Organic base-solvent of S with SO introduced2The liquid-phase Claus reaction is carried out to generate sulfur simple substance and regenerate organic base, and the regenerated organic base and the organic base which is not utilized in the original system can also absorb SO2The treated waste gas is discharged from the top of the tower, and SO is absorbed2And the organic alkali-solvent liquid phase system containing sulfur simple substance is separated from SO2Introducing the bottom of the absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and finally absorbing SO2Is pumped from the top of the separation tank into H2And S absorption reaction tower.
After 60min circulation, H is analyzed by a flue gas analyzer and a flow meter at the inlet and the outlet and the mole number of the sulfur simple substance is obtained, and after 60min circulation, H is carried out2The removal rate of S is 98.5%, SO2The removal rate of (A) was 98.7%, H2The outlet concentration of S is 15ppm, SO2The outlet concentration is 360 ppm; the recovery rate of the element S is 97.3 percent within 60min of circulation.
Example 4
Energy-saving high-efficiency recyclable H removal by liquid-phase Claus2S and SO2The process method for recovering sulfur comprises the following specific flow:
(1) h containing 0.1% atm2S waste gas from H2Introducing a liquid phase consisting of organic alkali and solvent into the bottom of the S absorption reaction tower, and absorbing SO circularly from the subsequent process2From the top of the column, the organic base-solvent liquid phase of (A) is circulated and SO is absorbed2And H2S is subjected to liquid-phase Claus reaction to generate sulfur simple substance and regenerate organic alkali absorbent, and the unused organic alkali-solvent and the organic alkali regenerated by the liquid-phase Claus reaction can also absorb the introduced H2And S, discharging the treated waste gas from the top of the tower. Then absorb H2S and sulfur-containing organic base-solvent solid-liquid two-phase system from H2Introducing the bottom of the S absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and absorbing H from the top of the separation tank2Organic base-solvent pumping of S into SO2In the absorption reaction tower, the organic base in the organic base-solvent is tetramethylguanidine, the solvent is diethylene glycol monomethyl ether, and the molar percentage content of the organic base in the organic base-solvent is 30%.
(2) SO containing 1% atm2Introducing SO into the waste gas from the bottom2Absorption reaction column in which H is also absorbed2Organic base-solvent of S with SO introduced2The liquid-phase Claus reaction is carried out to generate sulfur simple substance and regenerate organic base, and the regenerated organic base and the organic base which is not utilized in the original system can also absorb SO2The treated waste gas is discharged from the top of the tower, and SO is absorbed2And the organic alkali-solvent liquid phase system containing sulfur simple substance is separated from SO2The bottom of the absorption tower is introduced into a separation tank from whichThe sulfur elementary substance is extracted from the bottom, and finally SO is absorbed2Is pumped from the top of the separation tank into H2And S absorption reaction tower.
After 3H of circulation, H is analyzed by the obtained mole number of the sulfur simple substance and a flue gas analyzer and a flow meter at the inlet and the outlet after 3H of circulation2The removal rate of S is 97.7%, SO2Has a removal rate of 98.4, H2The outlet concentration of S is 20ppm, SO2Outlet concentration 950 ppm; within 3 hours of circulation, the recovery rate of the element S is 96.2 percent.
Example 5
Energy-saving high-efficiency recyclable H removal by liquid-phase Claus2S and SO2The process method for recovering sulfur comprises the following specific flow:
(1) h containing 1% atm2S waste gas from H2Introducing a liquid phase consisting of organic alkali and solvent into the bottom of the S absorption reaction tower, and absorbing SO circularly from the subsequent process2From the top of the column, the organic base-solvent liquid phase of (A) is circulated and SO is absorbed2And H2S is subjected to liquid-phase Claus reaction to generate sulfur simple substance and regenerate organic alkali absorbent, and the unused organic alkali-solvent and the organic alkali regenerated by the liquid-phase Claus reaction can also absorb the introduced H2And S, discharging the treated waste gas from the top of the tower. Then absorb H2S and sulfur-containing organic base-solvent solid-liquid two-phase system from H2Introducing the bottom of the S absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and absorbing H from the top of the separation tank2Organic base-solvent pumping of S into SO2In the absorption reaction tower, the organic base in the organic base-solvent is N, N-dimethyl cyclohexylamine, the solvent is water, and the mole percentage content of the organic base in the organic base-solvent is 75%.
(2) SO containing 10% atm2Introducing SO into the waste gas from the bottom2Absorption reaction column in which H is also absorbed2Organic base-solvent of S with SO introduced2The liquid-phase Claus reaction is carried out to generate sulfur simple substance and regenerate organic base, and the regenerated organic base and the organic base which is not utilized in the original system can also absorb SO2The treated waste gas is discharged from the top of the towerTo absorb SO2And the organic alkali-solvent liquid phase system containing sulfur simple substance is separated from SO2Introducing the bottom of the absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and finally absorbing SO2Is pumped from the top of the separation tank into H2And S absorption reaction tower.
After 1H of circulation, H is analyzed by a flue gas analyzer and a flow meter at the inlet and the outlet through obtaining the mole number of the sulfur simple substance2The removal rate of S is 98.8%, SO2The removal rate of (A) was 99.0%, H2S outlet concentration is 10ppm, SO2Outlet concentration was 505 ppm; the recovery rate of the element S is 97.9 percent within 1 hour of circulation.
Example 6
Energy-saving high-efficiency recyclable H removal by liquid-phase Claus2S and SO2The process method for recovering sulfur comprises the following specific flow:
(1) h containing 0.1% atm2S waste gas from H2Introducing a liquid phase consisting of organic alkali and solvent into the bottom of the S absorption reaction tower, and absorbing SO circularly from the subsequent process2From the top of the column, the organic base-solvent liquid phase of (A) is circulated and SO is absorbed2And H2S is subjected to liquid-phase Claus reaction to generate sulfur simple substance and regenerate organic alkali absorbent, and the unused organic alkali-solvent and the organic alkali regenerated by the liquid-phase Claus reaction can also absorb the introduced H2And S, discharging the treated waste gas from the top of the tower. Then absorb H2S and sulfur-containing organic base-solvent solid-liquid two-phase system from H2Introducing the bottom of the S absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and absorbing H from the top of the separation tank2Organic base-solvent pumping of S into SO2In the absorption reaction tower, the organic base in the organic base-solvent is N-methylaniline, the solvent is diethylene glycol monomethyl ether, and the molar percentage content of the organic base in the organic base-solvent is 50%.
(2) SO containing 10% atm2Introducing SO into the waste gas from the bottom2Absorption reaction column in which H is also absorbed2Organic base-solvent of S with SO introduced2Liquid phase Claus reaction to produce sulfur monoThe regenerated organic alkali can absorb SO and the organic alkali not utilized by the original system2The treated waste gas is discharged from the top of the tower, and SO is absorbed2And the organic alkali-solvent liquid phase system containing sulfur simple substance is separated from SO2Introducing the bottom of the absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and finally absorbing SO2Is pumped from the top of the separation tank into H2And S absorption reaction tower.
After 50min circulation, H is analyzed by a flue gas analyzer and a flow meter at the inlet and the outlet and the mole number of the sulfur simple substance is obtained, and after 50min circulation, H is carried out2The removal rate of S is 99.4%, SO2The removal rate of (A) is 99.6%, H2S outlet concentration of 7ppm, SO2The outlet concentration is 400 ppm; the recovery rate of the element S is 98.9 percent within 50min of circulation.
Example 7
Energy-saving high-efficiency recyclable H removal by liquid-phase Claus2S and SO2The process method for recovering sulfur comprises the following specific flow:
(1) h containing 1% atm2S waste gas from H2Introducing a liquid phase consisting of organic alkali and solvent into the bottom of the S absorption reaction tower, and absorbing SO circularly from the subsequent process2From the top of the column, the organic base-solvent liquid phase of (A) is circulated and SO is absorbed2And H2S is subjected to liquid-phase Claus reaction to generate sulfur simple substance and regenerate organic alkali absorbent, and the unused organic alkali-solvent and the organic alkali regenerated by the liquid-phase Claus reaction can also absorb the introduced H2And S, discharging the treated waste gas from the top of the tower. Then absorb H2S and sulfur-containing organic base-solvent solid-liquid two-phase system from H2Introducing the bottom of the S absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and absorbing H from the top of the separation tank2Organic base-solvent pumping of S into SO2In the absorption reaction tower, the organic base in the organic base-solvent is 3-pyridine methanol, the solvent is ethanol, and the mole percentage content of the organic base in the organic base-solvent is 75%.
(2) SO containing 10% atm2Introducing SO into the waste gas from the bottom2Absorption reaction column in which H is also absorbed2Organic base-solvent of S with SO introduced2The liquid-phase Claus reaction is carried out to generate sulfur simple substance and regenerate organic base, and the regenerated organic base and the organic base which is not utilized in the original system can also absorb SO2The treated waste gas is discharged from the top of the tower, and SO is absorbed2And the organic alkali-solvent liquid phase system containing sulfur simple substance is separated from SO2Introducing the bottom of the absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and finally absorbing SO2Is pumped from the top of the separation tank into H2And S absorption reaction tower.
After 1H of circulation, H is analyzed by a flue gas analyzer and a flow meter at the inlet and the outlet through obtaining the mole number of the sulfur simple substance2The removal rate of S is 99.6%, SO2The removal rate of (A) was 99.3%, H2S outlet concentration 6ppm, SO2Outlet concentration was 425 ppm; within 1h of circulation, the recovery rate of the element S is 99.0 percent.
Example 8
Energy-saving high-efficiency recyclable H removal by liquid-phase Claus2S and SO2The process method for recovering sulfur comprises the following specific flow:
(1) h containing 10% atm2S waste gas from H2Introducing a liquid phase consisting of organic alkali and solvent into the bottom of the S absorption reaction tower, and absorbing SO circularly from the subsequent process2From the top of the column, the organic base-solvent liquid phase of (A) is circulated and SO is absorbed2And H2S is subjected to liquid-phase Claus reaction to generate sulfur simple substance and regenerate organic alkali absorbent, and the unused organic alkali-solvent and the organic alkali regenerated by the liquid-phase Claus reaction can also absorb the introduced H2And S, discharging the treated waste gas from the top of the tower. Then absorb H2S and sulfur-containing organic base-solvent solid-liquid two-phase system from H2Introducing the bottom of the S absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and absorbing H from the top of the separation tank2Organic base-solvent pumping of S into SO2Absorbing the reaction tower, wherein the organic base in the organic base-solvent is 3-pyridinemethanol, the solvent is ethanol, and the organic base in the organic base-solvent isThe content of (a) is 60% by mole.
(2) SO containing 15% atm2Introducing SO into the waste gas from the bottom2Absorption reaction column in which H is also absorbed2Organic base-solvent of S with SO introduced2The liquid-phase Claus reaction is carried out to generate sulfur simple substance and regenerate organic base, and the regenerated organic base and the organic base which is not utilized in the original system can also absorb SO2The treated waste gas is discharged from the top of the tower, and SO is absorbed2And the organic alkali-solvent liquid phase system containing sulfur simple substance is separated from SO2Introducing the bottom of the absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and finally absorbing SO2Is pumped from the top of the separation tank into H2And S absorption reaction tower.
After 30min circulation, H is analyzed by a flue gas analyzer and a flow meter at the inlet and the outlet and the mole number of the sulfur simple substance is obtained, and after 30min circulation, H is carried out2The removal rate of S is 99.8%, SO2The removal rate of (A) was 99.7%, H2S outlet concentration is 5ppm, SO2The outlet concentration was 345 ppm; the recovery rate of the element S is 99.2 percent within 50min of circulation.
Example 9
Energy-saving high-efficiency recyclable H removal by liquid-phase Claus2S and SO2The process method for recovering sulfur comprises the following specific flow:
(1) h containing 10% atm2S waste gas from H2Introducing a liquid phase consisting of organic alkali and solvent into the bottom of the S absorption reaction tower, and absorbing SO circularly from the subsequent process2From the top of the column, the organic base-solvent liquid phase of (A) is circulated and SO is absorbed2And H2S is subjected to liquid-phase Claus reaction to generate sulfur simple substance and regenerate organic alkali absorbent, and the unused organic alkali-solvent and the organic alkali regenerated by the liquid-phase Claus reaction can also absorb the introduced H2And S, discharging the treated waste gas from the top of the tower. Then absorb H2S and sulfur-containing organic base-solvent solid-liquid two-phase system from H2Introducing the bottom of the S absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and absorbing H from the top of the separation tank2Organic of SAlkali-solvent pumping in SO2In the absorption reaction tower, the organic base in the organic base-solvent is 3-pyridine methanol, the solvent is ethanol, and the mole percentage content of the organic base in the organic base-solvent is 60%.
(2) SO containing 1% atm2Introducing SO into the waste gas from the bottom2Absorption reaction column in which H is also absorbed2Organic base-solvent of S with SO introduced2The liquid-phase Claus reaction is carried out to generate sulfur simple substance and regenerate organic base, and the regenerated organic base and the organic base which is not utilized in the original system can also absorb SO2The treated waste gas is discharged from the top of the tower, and SO is absorbed2And the organic alkali-solvent liquid phase system containing sulfur simple substance is separated from SO2Introducing the bottom of the absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and finally absorbing SO2Is pumped from the top of the separation tank into H2And S absorption reaction tower.
After 3H of circulation, H is analyzed by the obtained mole number of the sulfur simple substance and a flue gas analyzer and a flow meter at the inlet and the outlet after 3H of circulation2The removal rate of S is 98.7%, SO2The removal rate of (A) is 99.9%, H2S outlet concentration is 19ppm, SO2The outlet concentration is 300 ppm; within 3 hours of circulation, the recovery rate of the element S is 97.4 percent.
Example 10
Energy-saving high-efficiency recyclable H removal by liquid-phase Claus2S and SO2The process method for recovering sulfur comprises the following specific flow:
(1) h containing 0.1% atm2S waste gas from H2Introducing a liquid phase consisting of organic alkali and solvent into the bottom of the S absorption reaction tower, and absorbing SO circularly from the subsequent process2From the top of the column, the organic base-solvent liquid phase of (A) is circulated and SO is absorbed2And H2S is subjected to liquid-phase Claus reaction to generate sulfur simple substance and regenerate organic alkali absorbent, and the unused organic alkali-solvent and the organic alkali regenerated by the liquid-phase Claus reaction can also absorb the introduced H2And S, discharging the treated waste gas from the top of the tower. Then absorb H2S and sulfur-containing organic base-solvent solid-liquid two-phase systemH2Introducing the bottom of the S absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and absorbing H from the top of the separation tank2Organic base-solvent pumping of S into SO2In the absorption reaction tower, the organic alkali in the organic alkali-solvent is tetramethylguanidine, the solvent is N-methyl pyrrolidone, and the mole percentage content of the organic alkali in the organic alkali-solvent is 30 percent.
(2) SO containing 10% atm2Introducing SO into the waste gas from the bottom2Absorption reaction column in which H is also absorbed2Organic base-solvent of S with SO introduced2The liquid-phase Claus reaction is carried out to generate sulfur simple substance and regenerate organic base, and the regenerated organic base and the organic base which is not utilized in the original system can also absorb SO2The treated waste gas is discharged from the top of the tower, and SO is absorbed2And the organic alkali-solvent liquid phase system containing sulfur simple substance is separated from SO2Introducing the bottom of the absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and finally absorbing SO2Is pumped from the top of the separation tank into H2And S absorption reaction tower.
After 1H of circulation, H is analyzed by a flue gas analyzer and a flow meter at the inlet and the outlet through obtaining the mole number of the sulfur simple substance2The removal rate of S is 98.2%, SO2The removal rate of (A) was 98.9%, H2S outlet concentration is 10ppm, SO2The outlet concentration was 370 ppm; the recovery rate of the element S is 97.2 percent within 1 hour of circulation.
Example 11
Energy-saving high-efficiency recyclable H removal by liquid-phase Claus2S and SO2The process method for recovering sulfur comprises the following specific flow:
(1) h containing 0.1% atm2S waste gas from H2Introducing a liquid phase consisting of organic alkali and solvent into the bottom of the S absorption reaction tower, and absorbing SO circularly from the subsequent process2From the top of the column, the organic base-solvent liquid phase of (A) is circulated and SO is absorbed2And H2S is subjected to liquid-phase Claus reaction to generate sulfur simple substance and regenerate the organic base absorbent, and the organic base-solvent which is not utilized and the organic base regenerated by the liquid-phase Claus reaction can also be absorbedH in2And S, discharging the treated waste gas from the top of the tower. Then absorb H2S and sulfur-containing organic base-solvent solid-liquid two-phase system from H2Introducing the bottom of the S absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and absorbing H from the top of the separation tank2Organic base-solvent pumping of S into SO2In the absorption reaction tower, the organic base in the organic base-solvent is cyclohexylamine, the solvent is water, and the mole percentage content of the organic base in the organic base-solvent is 75%.
(2) SO containing 10% atm2Introducing SO into the waste gas from the bottom2Absorption reaction column in which H is also absorbed2Organic base-solvent of S with SO introduced2The liquid-phase Claus reaction is carried out to generate sulfur simple substance and regenerate organic base, and the regenerated organic base and the organic base which is not utilized in the original system can also absorb SO2The treated waste gas is discharged from the top of the tower, and SO is absorbed2And the organic alkali-solvent liquid phase system containing sulfur simple substance is separated from SO2Introducing the bottom of the absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and finally absorbing SO2Is pumped from the top of the separation tank into H2And S absorption reaction tower.
After 30min circulation, H is analyzed by a flue gas analyzer and a flow meter at the inlet and the outlet and the mole number of the sulfur simple substance is obtained, and after 30min circulation, H is carried out2The removal rate of S is 98.6%, SO2The removal rate of (A) was 99.3%, H2The outlet concentration of S is 9ppm, SO2The outlet concentration is 328 ppm; the recovery rate of the element S is 97.4 percent within 30min of circulation.
Example 12
Energy-saving high-efficiency recyclable H removal by liquid-phase Claus2S and SO2The process method for recovering sulfur comprises the following specific flow:
(1) h containing 0.1% atm2S waste gas from H2Introducing a liquid phase consisting of organic alkali and solvent into the bottom of the S absorption reaction tower, and absorbing SO circularly from the subsequent process2From the top of the column, the organic base-solvent liquid phase of (A) is circulated and SO is absorbed2And H2S generation of liquid phase Claus reaction productThe sulfur simple substance is generated and the organic base absorbent is regenerated, and the unused organic base-solvent and the organic base regenerated by the liquid-phase Claus reaction can also absorb the introduced H2And S, discharging the treated waste gas from the top of the tower. Then absorb H2S and sulfur-containing organic base-solvent solid-liquid two-phase system from H2Introducing the bottom of the S absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and absorbing H from the top of the separation tank2Organic base-solvent pumping of S into SO2In the absorption reaction tower, the organic base in the organic base-solvent is 1, 8-diazabicycloundec-7-ene (DBU), the solvent is ethanol, and the mole percentage content of the organic base in the organic base-solvent is 50%.
(2) SO containing 10% atm2Introducing SO into the waste gas from the bottom2Absorption reaction column in which H is also absorbed2Organic base-solvent of S with SO introduced2The liquid-phase Claus reaction is carried out to generate sulfur simple substance and regenerate organic base, and the regenerated organic base and the organic base which is not utilized in the original system can also absorb SO2The treated waste gas is discharged from the top of the tower, and SO is absorbed2And the organic alkali-solvent liquid phase system containing sulfur simple substance is separated from SO2Introducing the bottom of the absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and finally absorbing SO2Is pumped from the top of the separation tank into H2And S absorption reaction tower.
After 30min circulation, H is analyzed by a flue gas analyzer and a flow meter at the inlet and the outlet and the mole number of the sulfur simple substance is obtained, and after 30min circulation, H is carried out2The removal rate of S is 99.5%, SO2The removal rate of (A) was 99.2%, H2S outlet concentration 6ppm, SO2Outlet concentration 381 ppm; the recovery rate of the element S is 98.9 percent within 30min of circulation.
Example 13
Energy-saving high-efficiency recyclable H removal by liquid-phase Claus2S and SO2The process method for recovering sulfur comprises the following specific flow:
(1) h containing 5% atm2S waste gas from H2The liquid phase consisting of organic alkali and solvent is introduced from the bottom of the S absorption reaction tower and circulated from the subsequent processAbsorb SO2From the top of the column, the organic base-solvent liquid phase of (A) is circulated and SO is absorbed2And H2S is subjected to liquid-phase Claus reaction to generate sulfur simple substance and regenerate organic alkali absorbent, and the unused organic alkali-solvent and the organic alkali regenerated by the liquid-phase Claus reaction can also absorb the introduced H2And S, discharging the treated waste gas from the top of the tower. Then absorb H2S and sulfur-containing organic base-solvent solid-liquid two-phase system from H2Introducing the bottom of the S absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and absorbing H from the top of the separation tank2Organic base-solvent pumping of S into SO2In the absorption reaction tower, the organic alkali in the organic alkali-solvent is dimethylethanolamine, the solvent is N-methyl pyrrolidone, and the mole percentage content of the organic alkali in the organic alkali-solvent is 50 percent.
(2) SO containing 10% atm2Introducing SO into the waste gas from the bottom2Absorption reaction column in which H is also absorbed2Organic base-solvent of S with SO introduced2The liquid-phase Claus reaction is carried out to generate sulfur simple substance and regenerate organic base, and the regenerated organic base and the organic base which is not utilized in the original system can also absorb SO2The treated waste gas is discharged from the top of the tower, and SO is absorbed2And the organic alkali-solvent liquid phase system containing sulfur simple substance is separated from SO2Introducing the bottom of the absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and finally absorbing SO2Is pumped from the top of the separation tank into H2And S absorption reaction tower.
After 10min circulation, H is analyzed by a flue gas analyzer and a flow meter at the inlet and the outlet and the mole number of the sulfur simple substance is obtained, and after 10min circulation, H is carried out2The removal rate of S is 99.6%, SO2The removal rate of (A) was 99.1%, H2S outlet concentration is 8ppm, SO2Outlet concentration is 394 ppm; the recovery rate of the element S is 99.0 percent within 10min of circulation.
Example 14
Energy-saving high-efficiency recyclable H removal by liquid-phase Claus2S and SO2The process method for recovering sulfur comprises the following specific flow:
(1) h containing 0.1% atm2S waste gas from H2Introducing a liquid phase consisting of organic alkali and solvent into the bottom of the S absorption reaction tower, and absorbing SO circularly from the subsequent process2From the top of the column, the organic base-solvent liquid phase of (A) is circulated and SO is absorbed2And H2S is subjected to liquid-phase Claus reaction to generate sulfur simple substance and regenerate organic alkali absorbent, and the unused organic alkali-solvent and the organic alkali regenerated by the liquid-phase Claus reaction can also absorb the introduced H2And S, discharging the treated waste gas from the top of the tower. Then absorb H2S and sulfur-containing organic base-solvent solid-liquid two-phase system from H2Introducing the bottom of the S absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and absorbing H from the top of the separation tank2Organic base-solvent pumping of S into SO2In the absorption reaction tower, organic alkali in the organic alkali-solvent is diisopropanolamine, the solvent is diethylene glycol monomethyl ether, and the molar percentage content of the organic alkali in the organic alkali-solvent is 40%.
(2) SO containing 10% atm2Introducing SO into the waste gas from the bottom2Absorption reaction column in which H is also absorbed2Organic base-solvent of S with SO introduced2The liquid-phase Claus reaction is carried out to generate sulfur simple substance and regenerate organic base, and the regenerated organic base and the organic base which is not utilized in the original system can also absorb SO2The treated waste gas is discharged from the top of the tower, and SO is absorbed2And the organic alkali-solvent liquid phase system containing sulfur simple substance is separated from SO2Introducing the bottom of the absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and finally absorbing SO2Is pumped from the top of the separation tank into H2And S absorption reaction tower.
After 2H of circulation, H is analyzed by the obtained mole number of the sulfur simple substance and a flue gas analyzer and a flow meter at the inlet and the outlet after 2H of circulation2The removal rate of S is 97.9%, SO2The removal rate of (A) was 98.7%, H2S outlet concentration is 19ppm, SO2Outlet concentration is 880 ppm; within 2h of circulation, the recovery rate of the element S is 96.5 percent.
Example 15
Energy-saving high-efficiency recyclable H removal by liquid-phase Claus2S and SO2The process method for recovering sulfur comprises the following specific flow:
(1) h containing 1% atm2S waste gas from H2Introducing a liquid phase consisting of organic alkali and solvent into the bottom of the S absorption reaction tower, and absorbing SO circularly from the subsequent process2From the top of the column, the organic base-solvent liquid phase of (A) is circulated and SO is absorbed2And H2S is subjected to liquid-phase Claus reaction to generate sulfur simple substance and regenerate organic alkali absorbent, and the unused organic alkali-solvent and the organic alkali regenerated by the liquid-phase Claus reaction can also absorb the introduced H2And S, discharging the treated waste gas from the top of the tower. Then absorb H2S and sulfur-containing organic base-solvent solid-liquid two-phase system from H2Introducing the bottom of the S absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and absorbing H from the top of the separation tank2Organic base-solvent pumping of S into SO2In the absorption reaction tower, the organic base in the organic base-solvent is N, N-dimethylaniline, the solvent is water, and the mole percentage content of the organic base in the organic base-solvent is 45%.
(2) SO containing 15% atm2Introducing SO into the waste gas from the bottom2Absorption reaction column in which H is also absorbed2Organic base-solvent of S with SO introduced2The liquid-phase Claus reaction is carried out to generate sulfur simple substance and regenerate organic base, and the regenerated organic base and the organic base which is not utilized in the original system can also absorb SO2The treated waste gas is discharged from the top of the tower, and SO is absorbed2And the organic alkali-solvent liquid phase system containing sulfur simple substance is separated from SO2Introducing the bottom of the absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and finally absorbing SO2Is pumped from the top of the separation tank into H2And S absorption reaction tower.
After 40min circulation, H is analyzed by a flue gas analyzer and a flow meter at the inlet and the outlet and the mole number of the sulfur simple substance is obtained, and after 40min circulation, H is carried out2The removal rate of S is 99.6%, SO2The removal rate of (A) was 98.9%, H2S outlet concentration of 7ppm, SO2The outlet concentration is 688 ppm; the recovery rate of the element S is 98.6 percent within 40min of circulation.
Claims (4)
1. Circulation desorption H2S and SO2The method for recovering sulfur is characterized by comprising the following steps:
(1) containing H2Industrial waste gas of S from H2The bottom of the S absorption reaction tower is filled with organic alkali-solvent and SO absorbed from the subsequent process circulation2From H with an organic base-solvent2S flows into the top of the absorption reaction tower and absorbs SO2And H2S is subjected to liquid-phase Claus reaction to generate sulfur simple substance and regenerate organic alkali absorbent, and the unused organic alkali-solvent and the organic alkali regenerated by the liquid-phase Claus reaction can also absorb the introduced H2S, discharging the treated waste gas from the top of the tower and discharging the treated waste gas from H2Introducing the reaction liquid discharged from the bottom of the S absorption reaction tower into a separation tank, extracting elemental sulfur from the bottom of the separation tank, and absorbing H from the top of the separation tank2Organic base-solvent of S is passed through SO2An absorption reaction tower;
(2) containing SO2Industrial waste gas is introduced into SO from the bottom2Absorption in a reaction column at SO2Absorbing H in the absorption reaction tower2Organic base-solvent of S with SO introduced2Liquid-phase Claus reaction is carried out to generate sulfur simple substance and regenerate organic base, and the regenerated organic base and the organic base which is not utilized in the original system are used for absorbing SO2From SO, treated exhaust gases2The absorption reaction tower is discharged from the top of the tower, and SO is absorbed2And the organic alkali-solvent liquid phase system containing sulfur simple substance is separated from SO2Introducing the bottom of the absorption tower into a separation tank, extracting sulfur elementary substance from the bottom of the separation tank, and finally absorbing SO2Is pumped from the top of the separation tank into H2S absorption reaction tower to realize circulation reaction absorption process;
organic bases in the organic base-solvent are: tetramethyl guanidine, 3-pyridine methanol, cyclohexylamine, N-methyl cyclohexylamine, N-dimethyl aniline, 1, 8-diazabicycloundecen-7-ene, dimethyl ethanolamine and diisopropanolamine, and the solvent is one of sulfolane, diethylene glycol monomethyl ether, ethanol, water and N-methyl pyrrolidone.
2. The cyclic removal of H according to claim 12S and SO2And a process for recovering sulfur, characterized by: step (1) H2The S partial pressure is 0.1-10% atm.
3. The cyclic removal of H according to claim 12S and SO2And a process for recovering sulfur, characterized by: the mol percentage content of the organic base in the organic base-solvent is 30-75%.
4. The cyclic removal of H according to claim 12S and SO2And a process for recovering sulfur, characterized by: step (2) SO2The partial pressure is 1 to 15 percent atm.
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