CN111453703B - Method and device for producing high-concentration hydrogen sulfide by purifying low-temperature methanol - Google Patents
Method and device for producing high-concentration hydrogen sulfide by purifying low-temperature methanol Download PDFInfo
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- CN111453703B CN111453703B CN202010246011.3A CN202010246011A CN111453703B CN 111453703 B CN111453703 B CN 111453703B CN 202010246011 A CN202010246011 A CN 202010246011A CN 111453703 B CN111453703 B CN 111453703B
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- 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
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- B01D53/1425—Regeneration of liquid absorbents
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- B01D53/1456—Removing acid components
- B01D53/1462—Removing mixtures of hydrogen sulfide and carbon dioxide
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Abstract
The invention belongs to the technical field of chemical industry, and relates to a method and a device for purifying and producing high-concentration hydrogen sulfide by using low-temperature methanol, which comprises the steps of obtaining alcohol-washed sulfur-rich methanol after alcohol washing, heat exchange and temperature rise of methanol gas, and obtaining CO-rich after regeneration of the alcohol-washed sulfur-rich methanol 2 And release of CO 2 Is rich in sulfur methanol; rich in CO 2 After cooling, the condensed alcohol solution is continuously regenerated and is rich in CO 2 Discharging the gas and sending the gas to alcohol washing; CO release 2 Is divided into two paths, one path is passed through H 2 H released after S regeneration 2 S and concentrating to obtain high-purity H 2 S gas; the other way is regenerated by methanol heat to generate gas phase and water phase, and the gas phase is upwards used for CO 2 H and H 2 S is regenerated, the water phase is downwards subjected to alcohol-water separation to obtain thermal regeneration qualified methanol and waste water, and the thermal regeneration qualified methanol and the methanol gas are subjected to heat exchange and cooling to be used as lean methanol for alcohol washing. The invention realizes H at low temperature 2 The high-purity enrichment of S can obtain pure methanol at the same time, and the process flow is simple, the energy consumption is low, and the equipment is few.
Description
Technical Field
The invention belongs to the technical field of chemical industry, relates to a method and a device for producing high-concentration hydrogen sulfide gas, and in particular relates to a method and a device for producing high-concentration hydrogen sulfide by purifying low-temperature methanol.
Background
At present, cold methanol is used as an absorption solvent for washing, the excellent characteristic of extremely high solubility of methanol to acid gas at low temperature is utilized for removing the acid gas in raw material gas, the flow generally comprises an absorption tower and a plurality of analysis towers, the absorption tower absorbs the acid gas, the analysis towers analyze the acid gas and the lean methanol is returned to the absorption tower, so that the methanol can be recycled. However, the low-temperature methanol purification process is not easy to obtain high-concentration H 2 S gas, mostly rich in hydrogen sulfide (H therein 2 S is about 25-35%, the rest is CO 2 A small amount of N 2 ) Meanwhile, the purity of the methanol is not high.
Disclosure of Invention
In order to solve the problem of H in the prior low-temperature methanol process 2 The invention provides a method and a device for purifying and producing high-concentration hydrogen sulfide by using low-temperature methanol, which solve the problems of low S concentration and low methanol purity, and realize H at low temperature 2 The high-purity enrichment of S can obtain pure methanol at the same time, and the process flow is simple, the energy consumption is low, and the equipment is few.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a method for producing high-concentration hydrogen sulfide by purifying low-temperature methanol, which comprises the following steps:
1) Alcohol washing, heat exchange and temperature rising are carried out on the methanol gas to obtain alcohol washing sulfur-enriched methanol, and the alcohol washing sulfur-enriched methanol is regenerated to obtain CO-enriched methanol 2 And release of CO 2 Is rich in sulfur methanol; rich in CO 2 After cooling, the condensed alcohol solution is continuously regenerated and is rich in CO 2 Discharging the gas and sending the gas to alcohol washing;
2) CO release in step 2) 2 Is divided into two paths, one path is passed through H 2 H released after S regeneration 2 S and concentrating to obtain high-purity H 2 S gas; the other way is regenerated by methanol heat to generate gas phase and water phase, and the gas phase is upwards used for CO 2 H and H 2 S is regenerated, the water phase is downwards subjected to alcohol-water separation to obtain thermal regeneration qualified methanol and waste water, and the thermal regeneration qualified methanol and the methanol gas are subjected to heat exchange and cooling to be used as lean methanol for alcohol washing.
The specific process of the step 1) is that the alcohol washing sulfur-enriched methanol is regenerated by a carbon dioxide regeneration section in a baffle tower to obtain the CO-enriched methanol 2 The condensed alcohol liquid is ejected from a carbon dioxide regeneration section tower of the baffle tower (1) and is cooled, and then flows back to a carbon dioxide regeneration section in the baffle tower, and is rich in CO 2 The gas is discharged and sent to alcohol washing.
The specific process of the step 2) is to release CO 2 The sulfur-enriched methanol after the reaction is divided into two paths, and one path is sent to a hydrogen sulfide regeneration section pair H in a baffle tower 2 S, regenerating; after the heat exchange and cooling of the top gas of the hydrogen sulfide regeneration section and the methanol thermal regeneration section, the liquid phase respectively flows back to the bottom of the carbon dioxide regeneration section and the top of the hydrogen sulfide regeneration section, and the gas phase is concentrated to obtain high-purity H 2 S, S; the other path of the dissolved gas is subjected to methanol thermal regeneration through a methanol thermal regeneration section in the baffle tower, and the dissolved gas upwards enters a carbon dioxide regeneration section and a hydrogen sulfide regeneration section respectively; the water phase enters the alcohol-water separation section downwards to separate water, the wastewater is sent out of the boundary region from the bottom of the baffle tower, and the heat regenerated qualified methanol and the methanol gas are subjected to heat exchange and cooling to be used as lean methanol for alcohol washing.
In the methanol gas, H 2 S and CO 2 The molar ratio of (2) is 1:6-2:1.
A device for purifying and producing high-concentration hydrogen sulfide by using low-temperature methanol comprises a baffle tower, a reflux tank and a reboiler;
the upper part in the baffle tower is provided with a baffle, the baffle divides the upper space in the baffle tower into a left area and a right area, and the two areas are respectively a carbon dioxide regeneration section and a hydrogen sulfide regeneration section;
the reboiler is connected with the carbon dioxide regeneration section; the outlet of the carbon dioxide regeneration section is positioned at the top of the baffle tower, and the outlet of the carbon dioxide regeneration section is connected with the inlet of the carbon dioxide regeneration section; the outlet of the hydrogen sulfide regeneration section is positioned at the top of the baffle tower, the outlet of the hydrogen sulfide regeneration section is connected with the inlet of the reflux tank, and the outlet of the reflux tank is respectively connected with the inlets of the carbon dioxide regeneration section and the hydrogen sulfide regeneration section.
The device for purifying and producing high-concentration hydrogen sulfide by using the low-temperature methanol also comprises a tower top condenser; and the top outlet of the carbon dioxide regeneration section is connected with the inlet of the carbon dioxide regeneration section after passing through the top condenser.
The device for purifying and producing high-concentration hydrogen sulfide by using the low-temperature methanol also comprises a heat exchanger;
the methanol thermal regeneration section is arranged below the carbon dioxide regeneration section and the hydrogen sulfide regeneration section; the outlet of the methanol heat regeneration section is connected with a reboiler, and the inlet of the methanol heat regeneration section is connected with a heat exchanger; and the outlet of the hydrogen sulfide regeneration section is connected with the inlet of the reflux groove through a heat exchanger.
The device for purifying and producing high-concentration hydrogen sulfide by using the low-temperature methanol also comprises a tower bottom condenser; an alcohol-water separation section at the inner bottom of the baffle plate tower; the alcohol-water separation section is positioned below the methanol heat generation section; and the outlet at the bottom of the alcohol-water separation section returns to the alcohol-water separation section after passing through a condenser at the bottom of the tower.
The beneficial effects of the invention are as follows:
1. in the invention, alcohol washing sulfur-rich methanol enters a baffle tower CO 2 The middle lower part of the regeneration section firstly aims at CO 2 Regeneration release is carried out, and then H is entered 2 S regeneration section pair H 2 S is regenerated and recovered and is rich in CO 2 The condensed alcohol liquid cooled at the top of the gas outlet tower flows back to the top of the baffle tower and is rich in CO 2 Discharging the gas and sending the gas to alcohol washing; h can be obtained at low temperature 2 The S gas is concentrated to obtain high-purity hydrogen sulfide, and the process flow is simple and the energy consumption is low.
2. In the invention, CO is released 2 The sulfur-rich methanol after the process is subjected to methanol thermal regeneration through a methanol thermal regeneration section, and dissolved gas upwards enters CO 2 Regeneration section and H 2 S regeneration section, water phase enters the alcohol-water separation section downwards to separate water, the heat regenerated qualified methanol and methanol gas can be used as lean methanol to remove alcohol washing after heat exchange, the energy consumption is reduced, and high-concentration H is obtained 2 And S is rich, and the methanol can be regenerated and dehydrated simultaneously to obtain pure methanol.
3. In the invention, a baffle tower is adopted to realize methanol regeneration and dehydration and H 2 The S gas has high purity and is rich, few in equipment and simple in device structure.
Drawings
FIG. 1 is a flow chart of a process for producing high-concentration hydrogen sulfide by purifying low-temperature methanol;
wherein:
1-a baffle tower; 2-an overhead condenser; 3-a bottom condenser; 4-a reflux groove; 5-a heat exchanger; 6-reboiler.
Detailed Description
The invention will now be described in detail with reference to the drawings and examples.
Example 1
Referring to fig. 1, the device for purifying and producing high-concentration hydrogen sulfide by using low-temperature methanol provided by the invention comprises a baffle tower 1, a reflux tank 4 and a reboiler 6.
Referring to fig. 1, in this embodiment, a partition is disposed at the upper portion in a partition tower 1, and the partition separates the upper portion in the partition tower 1 into a carbon dioxide regeneration section and a hydrogen sulfide regeneration section, and a methanol thermal regeneration section is disposed below the carbon dioxide regeneration section and the hydrogen sulfide regeneration section; alcohol-water separation section at the inner bottom of the baffle tower 1.
Specifically, the top end in the baffle tower 1 is provided with a foam removing net; dividing the baffle tower into a left area and a right area through an axial baffle, wherein the left area is a carbon dioxide regeneration section, and the right area is a hydrogen sulfide regeneration section; a methanol thermal regeneration section and an alcohol-water separation section are sequentially arranged below the carbon dioxide regeneration section and the hydrogen sulfide regeneration section in the baffle tower 1.
Further, the device for purifying and producing high-concentration hydrogen sulfide by using low-temperature methanol also comprises a tower top condenser 2, a heat exchanger 5 and a tower bottom condenser 3.
Referring to fig. 1, in this embodiment, reboiler 6 is connected to the carbon dioxide regeneration zone; the outlet of the carbon dioxide regeneration section is positioned at the top of the baffle tower 1, and the outlet of the carbon dioxide regeneration section is connected with the inlet of the carbon dioxide regeneration section; the outlet of the hydrogen sulfide regeneration section is positioned at the top of the baffle tower, the outlet of the hydrogen sulfide regeneration section is connected with the inlet of the reflux tank 4, and the outlet of the reflux tank 4 is respectively connected with the inlets of the carbon dioxide regeneration section and the hydrogen sulfide regeneration section.
Specifically, the reboiler 6 is connected with the carbon dioxide regeneration section; the top outlet of the carbon dioxide regeneration section is connected with the carbon dioxide regeneration section after passing through a top condenser 2; the outlet of the top of the hydrogen sulfide regeneration section sequentially passes through a heat exchanger 5 and a reflux groove 4 and then is divided into two paths, one path is connected with the carbon dioxide regeneration section and the hydrogen sulfide regeneration section in the baffle tower 1, the other path is cooled, and the gas phase is used for recycling high-concentration hydrogen sulfide, and the liquid is connected with the reflux groove 4; the methanol heat regeneration section is respectively connected with a reboiler 6 and a heat exchanger 5, and is connected with an inlet of the methanol heat regeneration section after passing through the heat exchanger 5; the outlet of the hydrogen sulfide regeneration section is connected with the inlet of the reflux groove 4 through a heat exchanger 5. The outlet of the bottom of the alcohol-water separation section is connected with the alcohol-water separation section after passing through a bottom condenser 3.
In the embodiment, the device for purifying and producing high-concentration hydrogen sulfide by using low-temperature methanol has few equipment and simple structure.
By adopting the device provided by the embodiment, the method for purifying and producing high-concentration hydrogen sulfide by using low-temperature methanol comprises the following steps:
1) Alcohol washing, heat exchange and temperature rising are carried out on the methanol gas to obtain alcohol washing sulfur-enriched methanol, and the alcohol washing sulfur-enriched methanol is regenerated to obtain CO-enriched methanol 2 And release of CO 2 Is rich in sulfur methanol; rich in CO 2 After cooling, the condensed alcohol solution is continuously regenerated,rich in CO 2 Discharging the gas and sending the gas to alcohol washing;
2) CO release in step 2) 2 Is divided into two paths, one path is passed through H 2 H released after S regeneration 2 S and concentrating to obtain high-purity H 2 S gas; the other way is regenerated by methanol heat to generate gas phase and water phase, and the gas phase is upwards used for CO 2 H and H 2 S is regenerated, the water phase is downwards subjected to alcohol-water separation to obtain thermal regeneration qualified methanol and waste water, and the thermal regeneration qualified methanol and the methanol gas are subjected to heat exchange and cooling to be used as lean methanol for alcohol washing.
In the embodiment, the specific process of the step 1) is that after the alcohol washing sulfur-rich methanol is regenerated by a carbon dioxide regeneration section in the baffle tower 1, the obtained CO-rich methanol is regenerated 2 CO from the baffle tower 1 2 The alcohol solution condensed after the top of the regeneration section is cooled flows back to the carbon dioxide regeneration section in the baffle tower 1 and is rich in CO 2 The gas is discharged and sent to alcohol washing.
In this embodiment, the specific process of step 2) is to release CO 2 The sulfur-enriched methanol after the reaction is divided into two paths, and one path is sent to a hydrogen sulfide regeneration section pair H in a baffle tower 1 2 S, regenerating; after the heat exchange and cooling of the top gas of the hydrogen sulfide regeneration section and the methanol thermal regeneration section, the liquid phase respectively flows back to the bottom of the carbon dioxide regeneration section and the top of the hydrogen sulfide regeneration section, and the gas phase is concentrated to obtain high-purity H 2 S, S; the other path of the dissolved gas passes through a methanol thermal regeneration section in the baffle tower 1 to carry out methanol thermal regeneration, and the dissolved gas upwards enters a carbon dioxide regeneration section and a hydrogen sulfide regeneration section respectively; the water phase enters the alcohol-water separation section downwards to separate water, the wastewater is sent out of the boundary region from the bottom of the baffle tower 1, and the heat regenerated qualified methanol and the methanol gas are subjected to heat exchange and cooling to be used as lean methanol for alcohol washing.
In this example, H in methanol gas 2 S and CO 2 The molar ratio of (2) is 1:6-2:1.
Example 2
The method for producing high-concentration hydrogen sulfide by purifying low-temperature methanol is described by taking a specific application as an example.
In this example, methanol gas from stripping (mainly containing H 2 S and CO 2 )，H 2 S and CO 2 Molar of (2)The ratio was 1:6.
1) Methanol gas enters a carbon dioxide regeneration section from the middle part of the carbon dioxide regeneration section on a baffle tower after being subjected to alcohol washing, the pressure of the baffle tower is about 0.05MPa, and CO in the methanol gas is released 2 Gas, released CO 2 Condensing the gas phase of the carbon dioxide regeneration section from the top outlet of the carbon dioxide regeneration section through a top condenser to obtain a gas phase rich in CO 2 The gas can be collected and utilized, the temperature is 22 ℃, the carbon dioxide in the gas phase is 91%, and the hydrogen sulfide is 5%; the liquid phase is alcohol liquid from baffle tower CO 2 The upper part of the regeneration section returns into the baffle tower;
2) CO release 2 Is divided into two paths:
one path enters a hydrogen sulfide regeneration section on the right side of the top of the baffle tower to carry out H 2 S regeneration, released H 2 The outlet of the tower top of the S hydrogen sulfide regeneration section exchanges heat with the methanol thermal regeneration section through a heat exchanger 5, then enters a reflux tank 4, liquid phase respectively returns to the top of the hydrogen sulfide regeneration section in the baffle tower and the bottom of the carbon dioxide regeneration section in the baffle tower through reflux, and a small part of liquid phase carried by the condensed gas phase is sent to the reflux tank 4, H 2 S gas is collected, the temperature of the gas phase is minus 10 ℃, the hydrogen sulfide is 93%, and the carbon dioxide is 2%; and concentrating to obtain high-concentration H 2 S gas;
the other path of the methanol is fed into a methanol thermal regeneration section for methanol thermal regeneration, dissolved gas upwards enters a carbon dioxide regeneration section and a hydrogen sulfide regeneration section, after a liquid phase comes out of the methanol thermal regeneration section, part of qualified methanol is subjected to reboiler 6 and then is used as lean methanol for alcohol washing; the water phase enters an alcohol-water separation section downwards to separate water to obtain pure methanol, and the separated wastewater is separated from the bottom of the baffle tower through a tower bottom condenser and is sent out of the boundary region.
Example 3
In this example, methanol gas from stripping (mainly containing H 2 S and CO 2 )，H 2 S and CO 2 The molar ratio of (2) is 1:2, the pressure of the baffle tower is about 0.15MPa, and the gas phase is rich in CO 2 The gas can be collected (cooled) for use, the temperature is 30 ℃, the carbon dioxide in the gas phase is 92%, and the hydrogen sulfide is 3%; h 2 The S gas (after cooling) is collected,and the temperature of the gas phase is 2 ℃, the hydrogen sulfide is 94%, the carbon dioxide is 2%, and H 2 S gas can be further concentrated to obtain high-concentration H 2 S gas is recycled.
Example 4
In this example, methanol gas from stripping (mainly containing H 2 S and CO 2 )，H 2 S and CO 2 The molar ratio of (2) to (1), the pressure of the baffle tower is about 0.25MPa, and the gas phase is rich in CO 2 The gas (after cooling) can be collected and utilized, the temperature is 15 ℃, the carbon dioxide in the gas phase is 90%, and the hydrogen sulfide is 3.5%; h 2 S gas (after cooling) is collected, the temperature of the gas phase is 15 ℃, hydrogen sulfide is 95%, carbon dioxide is 2.5%, H 2 S gas can be further concentrated to obtain high-concentration H 2 S gas is recycled.
The method for purifying and producing high-concentration hydrogen sulfide by using low-temperature methanol is simple in process flow and lowest in energy consumption, and the methanol can be regenerated and dehydrated while the hydrogen sulfide gas is enriched in high concentration, so that pure methanol is obtained, and the whole device has few equipment.
Claims (7)
1. A method for producing high-concentration hydrogen sulfide by purifying low-temperature methanol is characterized by comprising the following steps: the method comprises the following steps:
1) Alcohol washing, heat exchange and temperature rising are carried out on the methanol gas to obtain alcohol washing sulfur-enriched methanol, and the alcohol washing sulfur-enriched methanol is regenerated to obtain CO-enriched methanol 2 And release of CO 2 Is rich in sulfur methanol; rich in CO 2 After cooling, the condensed alcohol solution is continuously regenerated and is rich in CO 2 Discharging the gas and sending the gas to alcohol washing;
2) CO release 2 Is divided into two paths, one path is passed through H 2 S releases H after regeneration 2 S and concentrating to obtain high-purity H 2 S gas; the other way is regenerated by methanol heat to generate gas phase and water phase, and the gas phase is upwards used for CO 2 H and H 2 S, regenerating, namely separating alcohol from water downwards from the water phase to obtain hot qualified methanol and waste water, and performing heat exchange and cooling on the hot qualified methanol and the methanol gas to obtain lean methanol for alcohol washing;
the specific process of the step 2) is to release CO 2 The sulfur-enriched methanol after the reaction is divided into two paths, and one path is sent to a hydrogen sulfide regeneration section pair H in a baffle tower (1) 2 S, regenerating; after the heat exchange and cooling of the top gas of the hydrogen sulfide regeneration section and the methanol thermal regeneration section, the liquid phase respectively flows back to the bottom of the carbon dioxide regeneration section and the top of the hydrogen sulfide regeneration section, and the gas phase is concentrated to obtain high-purity H 2 S, S; the other path of the dissolved gas passes through a methanol thermal regeneration section in a baffle tower (1) to carry out methanol thermal regeneration, and the dissolved gas upwards enters a carbon dioxide regeneration section and a hydrogen sulfide regeneration section respectively; the water phase enters the alcohol-water separation section downwards to separate water, the wastewater is sent out of the boundary region from the bottom of the baffle tower (1), and the heat regenerated qualified methanol and the methanol gas are subjected to heat exchange and cooling to be used as lean methanol for alcohol washing.
2. The method for producing high-concentration hydrogen sulfide by purifying low-temperature methanol according to claim 1, wherein: the specific process of the step 1) is that alcohol washing sulfur-rich methanol is regenerated by a carbon dioxide regeneration section in a baffle tower (1) to obtain CO-rich methanol 2 The condensed alcohol liquid is ejected from a carbon dioxide regeneration section tower in the baffle tower (1) and is returned to a carbon dioxide regeneration section in the baffle tower (1) after being cooled, and is rich in CO 2 The gas is discharged and sent to alcohol washing.
3. The method for producing high-concentration hydrogen sulfide by purifying low-temperature methanol according to claim 1 or 2, characterized in that: in the methanol gas, H 2 S and CO 2 The molar ratio of (2) is 1:6-2:1.
4. An apparatus for carrying out the method for producing high concentration hydrogen sulfide by purifying low temperature methanol according to claim 1, characterized in that: the device for purifying and producing high-concentration hydrogen sulfide by using low-temperature methanol comprises a baffle tower (1), a reflux tank (4) and a reboiler (6);
the upper part in the baffle tower (1) is provided with a baffle, the baffle divides the upper space in the baffle tower (1) into a left area and a right area, and the two areas are respectively a carbon dioxide regeneration section and a hydrogen sulfide regeneration section;
the reboiler (6) is connected with the carbon dioxide regeneration section; the outlet of the carbon dioxide regeneration section is positioned at the top of the baffle tower (1), and the outlet of the carbon dioxide regeneration section is connected with the inlet of the carbon dioxide regeneration section; the outlet of the hydrogen sulfide regeneration section is positioned at the top of the baffle tower, the outlet of the hydrogen sulfide regeneration section is connected with the inlet of the reflux tank (4), and the outlet of the reflux tank (4) is respectively connected with the inlets of the carbon dioxide regeneration section and the hydrogen sulfide regeneration section.
5. The apparatus for purifying low-temperature methanol to produce high-concentration hydrogen sulfide according to claim 4, wherein: the device for purifying and producing high-concentration hydrogen sulfide by using low-temperature methanol also comprises a tower top condenser (2); and the top outlet of the carbon dioxide regeneration section is connected with the inlet of the carbon dioxide regeneration section after passing through the top condenser.
6. The apparatus for purifying low-temperature methanol to produce high-concentration hydrogen sulfide according to claim 4, wherein: the device for purifying and producing high-concentration hydrogen sulfide by using low-temperature methanol also comprises a heat exchanger (5);
the methanol thermal regeneration section is arranged below the carbon dioxide regeneration section and the hydrogen sulfide regeneration section; the outlet of the methanol heat regeneration section is connected with a reboiler (6), and the inlet of the methanol heat regeneration section is connected with a heat exchanger (5); the outlet of the hydrogen sulfide regeneration section is connected with the inlet of the reflux groove (4) through a heat exchanger (5).
7. The apparatus for purifying low-temperature methanol to produce high-concentration hydrogen sulfide according to claim 4, wherein: the device for purifying and producing high-concentration hydrogen sulfide by using low-temperature methanol also comprises a tower bottom condenser (3); by a means of
The inner bottom of the baffle tower (1) is provided with an alcohol-water separation section; the alcohol-water separation section is positioned below the methanol thermal regeneration section;
and the outlet at the bottom of the alcohol-water separation section returns to the alcohol-water separation section after passing through a bottom condenser (3).
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| CN111453703A (en) | 2020-07-28 |
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