CN113387333B - Post-treatment method of hydrogen sulfide - Google Patents
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- CN113387333B CN113387333B CN202110676940.2A CN202110676940A CN113387333B CN 113387333 B CN113387333 B CN 113387333B CN 202110676940 A CN202110676940 A CN 202110676940A CN 113387333 B CN113387333 B CN 113387333B
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Abstract
The invention provides a post-treatment method of hydrogen sulfide, which comprises chilling of hydrogen sulfide synthesis gas and refluxing of hydrogen sulfide. The chilling tower is selected, so that polysulfide is prevented from being generated, the post-treatment step of polysulfide is simplified, and meanwhile, the liquefaction of sulfur carried in the hydrogen sulfide synthesis gas can be realized in one step, the purity of the prepared pure hydrogen sulfide reaches 99.95%, and the polysulfide is a trace amount. The low-temperature medium is liquid hydrogen sulfide, and other cooling media are not introduced, so that secondary treatment is avoided. In the process of liquefying hydrogen sulfide, the released heat can be recycled, and solid sulfur or heating and heat preservation of a hydrogen sulfide reactor, a reaction pipeline and the like are carried out.
Description
Technical Field
The invention relates to the field of sulfide synthesis, in particular to a method for post-treating hydrogen sulfide.
Background
Hydrogen sulfide is an industrially important intermediate, for example for the synthesis of methyl mercaptan, dimethyl sulfide, dimethyl disulfide, sulfonic acid, dimethyl sulfoxide and for the reaction of many sulfides.
The preparation method commonly used in industry is the reaction of sulphur and hydrogen to obtain hydrogen sulphide, but the conversion of sulphur and hydrogen is slow and requires the use of a catalyst to achieve high conversion, and these methods are described in large amounts in US5173285, US4629617, WO8200632, US4094961, etc. The process usually includes the step of single-stage or multi-stage condensation of the raw hydrogen sulfide gas collected in the reactor during the synthesis of hydrogen sulfide, wherein polysulfide H is usually generated 2 And Sx is generated. Polysulfanes present in the crude gas stream containing hydrogen sulphide will decompose in the system to hydrogen sulphide and sulphur which will deposit in equipment, pipes, valves etc, affecting the life of the equipment and being difficult to clean.
FR2844208 discloses a crude hydrogen sulphide gas preparation process whereby the hydrogen sulphide synthesizer is passed through a filter containing a solid selected from porous particles of activated carbon, alumina and silica. The filter material is consumed after sulfur loading and must be incinerated or the like. The method has the disadvantages of replacement of the activated carbon bed, large consumption of the activated carbon, high treatment cost, and the need of another treatment device when replacing the activated carbon.
US5686056 provides a method and apparatus for the purification of hydrogen sulphide gas having impurities therein, primarily polysulphides. The purification is achieved by passing hydrogen sulfide gas through the filter media, where the contaminants are trapped as the hydrogen sulfide passes through the filter media. The filter media may be molecular sieves, sand traps, alumina, etc., such that no more than 10ppm of contaminant gases remain in the final hydrogen sulfide. Or firstly decomposing polysulfide into hydrogen sulfide and sulfur by a catalyst, and then trapping impurities such as sulfur by a filter medium. Then, the molecular sieve is regenerated by heating hydrogen, and simultaneously, sulfur in the filter medium is blown off and enters the reactor together with the hydrogen as a raw material.
US7887777 provides a method for treating polysulfides by passing a crude stream of hydrogen sulfide and polysulfides present therein through a catalytic reactor, preferably activated carbon and/or molecular sieves and a hydrogenation catalyst, at a temperature of 135 to 160 ℃ to ensure that the decomposed sulfur can flow into a condenser. The method is used for further catalyzing polysulfide, further decomposing polysulfide, and has high cost and risk of entrainment or deposition of sulfur.
CN1292980C discloses a method for removing polysulfanes from crude gas formed in the process of hydrogen sulfide production, wherein the crude gas of hydrogen sulfide is passed through a multi-stage washing device to contact with water and/or methanol, or a system containing alkaline substances, so that 50-99.5% of the polysulfanes can be consumed to obtain pure gas of hydrogen sulfide. The method has the disadvantages that a large amount of water is used, simultaneously, the sprayed alkaline solution spray is very easy to be entrained by hydrogen sulfide gas, enters the subsequent reaction together and needs to be further removed, and the method is feasible for producing the hydrogen sulfide alkaline substances.
According to the existing hydrogen sulfide production technology, the following problems are found: polysulfide which is easily formed in the condensation process of hydrogen sulfide synthesis gas is very unfavorable for subsequent treatment, catalysts or filtering devices such as molecular sieves are mostly used for removing in the prior art, sulfur obtained by decomposition in the process is further recovered, and the catalysts are subjected to regeneration treatment.
Disclosure of Invention
In order to solve the problems, the invention provides a post-treatment method of hydrogen sulfide, and particularly relates to a treatment method of hydrogen sulfide synthesis gas, wherein a catalyst or a filtering device is not used, sulfur carried in the hydrogen sulfide synthesis gas is removed, and the obtained hydrogen sulfide gas has high purity and polysulfide trace.
In order to solve the technical problems, the invention adopts the following technical scheme:
a continuous preparation method of hydrogen sulfide comprises the steps of chilling hydrogen sulfide synthesis gas and refluxing hydrogen sulfide.
The following is a further improvement of the above technical scheme:
the chilling of the hydrogen sulfide synthesis gas comprises directly feeding the hydrogen sulfide synthesis gas obtained in the hydrogen sulfide reactor into a hydrogen sulfide chilling tower, and rapidly cooling to 110-170 ℃, preferably 125-155 ℃. And liquefying sulfur carried in the hydrogen sulfide synthesis gas at low temperature, falling to the bottom of a hydrogen sulfide chilling tower, collecting, and then merging into a sulfur feeding pipe and then entering a hydrogen sulfide reactor.
The chilling of the hydrogen sulfide synthetic gas uses a method of contacting the hydrogen sulfide synthetic gas with a low-temperature medium, and the low-temperature medium used in the invention is reflux liquid hydrogen sulfide at the temperature of-20 ℃ to-10 ℃. The liquid hydrogen sulfide is derived from a hydrogen sulfide reflux step.
The low-temperature medium is preferably-20 ℃ to-15 ℃;
the method for contacting the hydrogen sulfide synthesis gas with the low-temperature medium can use a method for spraying the low-temperature medium, and the returned liquid hydrogen sulfide needs to cover the cross section of the chilling tower after being sprayed, so that the hydrogen sulfide synthesis gas is ensured to be fully contacted. The spraying device can adopt a method of one-time or multiple overlapping spraying, and preferably adopts multiple overlapping spraying. The scheme is carried out under the condition of low pressure, and the pressure is 3 bar-7 bar.
The method for contacting the hydrogen sulfide synthesis gas with the low-temperature medium can adopt a method of directly introducing the hydrogen sulfide synthesis gas into low-temperature liquid hydrogen sulfide in a chilling tower, refluxing liquid hydrogen sulfide is sent into the chilling tower to ensure that the liquid hydrogen sulfide has a certain liquid level, and the hydrogen sulfide synthesis gas is directly introduced into the chilling tower below the liquid hydrogen sulfide liquid level through a pipeline. The scheme needs to be carried out under the condition of high pressure, wherein the pressure is 10-20 bar, and preferably 10-12 bar;
after the hydrogen sulfide synthesis gas is rapidly cooled, the sulfur carried in the hydrogen sulfide synthesis gas is liquefied and falls into the bottom of the chilling tower, and under the condition of a spraying mode, the sulfur is in a low-viscosity state due to the fact that the temperature of the chilling tower is below 160 ℃, cannot be adhered to the bottom of the reactor, and can be collected and recycled. Even if the sulfur is adhered, the treatment is easy, and the reaction is not adversely affected.
Under the condition that hydrogen sulfide synthesis gas is directly introduced into liquid hydrogen sulfide, due to the high-pressure condition, the sulfur falling to the bottom of the chilling tower is solid, is led out by using equipment such as a screw rod and the like, is sent into a storage tank, and is sent into a sulfur feeding pipe after being preheated.
The reflux of the hydrogen sulfide comprises the steps of enabling the hydrogen sulfide synthesis gas to pass through a hydrogen sulfide chilling tower to obtain desulfurized hydrogen sulfide, enabling the desulfurized hydrogen sulfide to partially reflux, enabling the desulfurized hydrogen sulfide to pass through a heat exchanger to obtain liquid hydrogen sulfide at the temperature of minus 20 ℃ to minus 10 ℃, sending the liquid hydrogen sulfide into the chilling tower, and cooling the hydrogen sulfide synthesis gas.
And the desulfurized hydrogen sulfide partially reflows, can be primarily cooled through a heat exchanger, and then is subjected to secondary heat exchange after heat is recovered to obtain low-temperature liquid hydrogen sulfide.
The hydrogen sulfide synthesis gas is directly discharged through a sulfur and hydrogen reactor, and comprises 89-95% of hydrogen sulfide, 5-10% of sulfur steam and other inert gases. The type of the reactor is not limited, and the hydrogenation catalytic reaction of hydrogen sulfide can be carried out by using a tubular reactor, a U-shaped tubular reactor or a catalyst packed tower. The discharging temperature of the hydrogen sulfide synthesis gas is 350-420 ℃. In order to ensure that the temperature of the low-temperature hydrogen sulfide synthesis gas entering the chilling tower is not lower than 350 ℃, preferably not lower than 360 ℃, a heat preservation device such as electric heat tracing, heat preservation cotton and the like is arranged on the discharging pipeline to control the temperature. Meanwhile, the retention time of the hydrogen sulfide synthesis gas in the hydrogen sulfide chilling tower is limited to 0.1-0.35s, preferably 0.1-0.25 s;
the hydrogen sulfide is refluxed, and the desulfurized hydrogen sulfide gas discharged from the hydrogen sulfide chilling tower is divided into refluxed gaseous hydrogen sulfide and a pure hydrogen sulfide product, wherein the reflux ratio is 0.2-1.0; preferably 0.25 to 0.8; the refluxed gaseous hydrogen sulfide enters a heat exchanger for cooling, and the freezing medium can be chilled water with the temperature of minus 30 ℃ for condensing the refluxed hydrogen sulfide to obtain refluxed liquid hydrogen sulfide which is sent into a chilling tower.
The invention rapidly cools the hydrogen sulfide synthesis gas to below 200 ℃, and reasonably avoids the temperature interval in which polysulfide is easy to generate.
The specific heat capacity of liquid hydrogen sulfide is 69.17 (J/mol.k) at-10 ℃, the specific heat capacity of gaseous hydrogen sulfide is 39.27 (J/mol.k) at 400 ℃, and the high latent heat of vaporization of the liquid hydrogen sulfide provides possibility for the liquid hydrogen sulfide to be used as a low-temperature medium for cooling hydrogen sulfide synthesis gas.
The invention further provides a device for continuously preparing hydrogen sulfide, which comprises a hydrogen sulfide reactor A for reacting sulfur and hydrogen, and a hydrogen sulfide synthetic gas chilling tower F connected with a hydrogen sulfide synthetic gas discharge hole B, wherein the hydrogen sulfide synthetic gas chilling tower F comprises a demister E, a chilling tower discharge hole H and a liquid sulfur discharge hole L. The desulfurized hydrogen sulfide discharge pipeline is provided with a bypass, the bypass is connected with a hydrogen sulfide liquefier G, the liquefier is connected with a hydrogen sulfide synthetic gas chilling tower, and the discharge of the liquefier is directly sent into the hydrogen sulfide synthetic gas chilling tower.
The hydrogen sulfide synthetic gas chilling tower F also can comprise a spraying device D, wherein the spraying device D is at least 1 layer, preferably 4 layers, and is arranged in a staggered mode to ensure that the cross section of the chilling tower is covered, and the discharge of the liquefier is directly connected with the spraying device.
On the basis of the above-mentioned apparatus, the hydrogen sulfide synthesis method is further described.
The hydrogen sulfide reactor A discharges hydrogen sulfide synthesis gas 1, the hydrogen sulfide synthesis gas is sent to the lower half section of a hydrogen sulfide chilling tower F and is contacted with refluxing liquid hydrogen sulfide 5 to obtain hydrogen sulfide gas without sulfur, the hydrogen sulfide gas passes through a foam remover E and a chilling tower discharge hole H and is divided into a pure hydrogen sulfide product 4 and refluxing gaseous hydrogen sulfide 3, the refluxing gaseous hydrogen sulfide 3 passes through a hydrogen sulfide liquefier G to obtain refluxing liquid hydrogen sulfide 5, and the refluxing liquid hydrogen sulfide 5 is sent to a spraying device D. Liquid sulfur 6 obtained from the bottom of the chilling tower is fed into a sulfur feed pipe C of the reactor.
The refluxed liquid hydrogen sulfide 5 can also be directly introduced into the lower end of the chilling tower and fall to the bottom of the chilling tower, and the liquid level is ensured to be higher than the inlet of the hydrogen sulfide synthesis gas 1.
Compared with the prior art, the invention has the beneficial effects that:
1) The chilling tower is selected, so that the generation of polysulfide is avoided, the post-treatment step of the polysulfide is simplified, meanwhile, the liquefaction of sulfur carried in the hydrogen sulfide synthesis gas can be realized in one step, the purity of the prepared pure hydrogen sulfide product reaches over 99.95 percent, and the polysulfide is trace.
2) The low-temperature medium is liquid hydrogen sulfide, and other cooling media are not introduced, so that secondary treatment is avoided.
3) In the process of liquefying the hydrogen sulfide, the released heat can be recycled, and solid sulfur or heating and heat preservation of a hydrogen sulfide reactor, a reaction pipeline and the like are carried out.
Description of the drawings:
FIG. 1 is a flow diagram of the purification of hydrogen sulfide corresponding to examples 1-4;
FIG. 2 is a flow chart of the purification of hydrogen sulfide corresponding to example 3.
In the figure:
a to L are reaction equipment:
a is hydrogen sulfide reactor; b-hydrogen sulfide synthetic gas discharge port; c-sulfur feed pipe; d, a spraying device; e-demister; h-a discharge hole of the chilling tower; g-hydrogen sulfide liquefier; l is a liquid sulfur discharge port; f-a chilling tower;
1-6 are reactant streams:
1-hydrogen sulfide synthesis gas; 2-desulfurization of hydrogen sulfide gas; 3-refluxing gaseous hydrogen sulfide; 4-pure hydrogen sulfide; 5-liquid hydrogen sulfide under reflux; 6-sulphur.
Detailed Description
The preferred embodiments of the present invention are described below, and it should be understood that the preferred embodiments described herein are only for illustrating and explaining the present invention and are not to be construed as limiting the present invention.
Example 1A method for the aftertreatment of Hydrogen sulfide
Discharging sulfur obtained from a chilling tower from a liquid sulfur discharge port L, preheating the discharged sulfur 6 to 100 ℃, enabling the sulfur to enter a hydrogen sulfide reactor A from a sulfur feed pipe C, mixing the sulfur with hydrogen, and then passing through a catalytic tube to obtain hydrogen sulfide synthetic gas 1, wherein the hydrogen sulfide synthetic gas 1 is discharged from a hydrogen sulfide synthetic gas discharge port B at 678.35kg/h (the hydrogen sulfide synthetic gas 1 comprises 92.44% of hydrogen sulfide, 7.48% of sulfur and 0.08% of impurities), the discharging temperature is 379 ℃, and the temperature of 7bar entering a hydrogen sulfide chilling tower F is 375 ℃ under the condition of pipeline heat preservation;
the refluxed gaseous hydrogen sulfide 3 passes through a hydrogen sulfide liquefier G to obtain refluxed liquid hydrogen sulfide 5, the temperature of the refluxed liquid hydrogen sulfide 5 is-16 ℃, the refluxed liquid hydrogen sulfide 5 enters a spraying device D inside a hydrogen sulfide chilling tower F and contacts with the high-temperature hydrogen sulfide synthetic gas 1 to obtain desulfurized hydrogen sulfide gas 2, and the high-temperature hydrogen sulfide synthetic gas 1 stays in the chilling tower F for 0.20s;
the temperature of the chilling tower F is 154.65 ℃, and the reaction pressure is 6.5bar;
the desulfurized hydrogen sulfide gas 2 is discharged from a chilling tower discharge hole H at the speed of 967.82kg/H, and the reflux ratio is 0.54.
The purity of the pure hydrogen sulfide product 4 is 99.99%, and the polysulfide is trace.
The spraying device D is provided with 4 layers of spraying pipes, and sprayed liquid drops cover the whole cross section of the chilling tower F
Example 2A method for the aftertreatment of Hydrogen sulfide
Discharging sulfur obtained by a chilling tower from a liquid sulfur discharge port L, preheating the discharged sulfur 6 to 100 ℃, feeding the sulfur into a hydrogen sulfide reactor A from a sulfur feeding pipe C, mixing the sulfur with hydrogen, passing through a catalytic pipe to obtain hydrogen sulfide synthetic gas 1, discharging the hydrogen sulfide synthetic gas 1 from a hydrogen sulfide synthetic gas discharge port B at 678.35kg/h (the hydrogen sulfide synthetic gas 1 comprises 92.24% of hydrogen sulfide, 7.41% of sulfur and 0.35% of impurities), wherein the discharging temperature is 378 ℃ and 7bar, and the temperature is 375 ℃ when the sulfur enters a hydrogen sulfide chilling tower F under the condition of pipeline heat preservation and pressure preservation;
and the refluxed gaseous hydrogen sulfide 3 passes through a hydrogen sulfide liquefier G to obtain refluxed liquid hydrogen sulfide 5, the temperature of the refluxed liquid hydrogen sulfide 5 is-15 ℃, the refluxed liquid hydrogen sulfide enters a spraying device D in a hydrogen sulfide chilling tower F and contacts with the high-temperature hydrogen sulfide synthetic gas 1 to obtain desulfurized hydrogen sulfide gas 2, and the retention time of the hydrogen sulfide synthetic gas 1 in the chilling tower F is 0.15s.
The temperature of the chilling tower F is 125.83 ℃, and the reaction pressure is 6.5bar;
desulfurized hydrogen sulfide gas 2 was withdrawn from quench tower outlet H at a rate of 1018.92kg/H with a reflux ratio of 0.625.
627.03kg/h of pure hydrogen sulfide 4 with a purity of 99.95% and a trace amount of polysulfide is obtained.
The spraying device D is provided with 4 layers of spraying pipes, and sprayed liquid drops cover the whole cross section of the chilling tower F.
Example 3A method for the aftertreatment of Hydrogen sulfide
Discharging sulfur obtained by a chilling tower from a liquid sulfur discharge port L, preheating discharged sulfur 6 to 100 ℃, feeding the sulfur into a hydrogen sulfide reactor A from a sulfur feeding pipe C, mixing the sulfur with hydrogen, passing through a catalytic tube to obtain hydrogen sulfide synthesis gas 1, discharging the hydrogen sulfide synthesis gas 1 from a hydrogen sulfide synthesis gas discharge port B at 678.35kg/h (the hydrogen sulfide synthesis gas 1 comprises 92.24% of hydrogen sulfide, 7.41% of sulfur and 0.35% of impurities), wherein the discharging temperature is 375 ℃,4bar, and the temperature when the sulfur enters a hydrogen sulfide chilling tower F is 365 ℃ under the condition of pipeline heat preservation;
and the refluxed gaseous hydrogen sulfide 3 passes through a hydrogen sulfide liquefier G to obtain refluxed liquid hydrogen sulfide 5, the temperature of the refluxed liquid hydrogen sulfide 5 is-10 ℃, the refluxed liquid hydrogen sulfide enters a spraying device D in a hydrogen sulfide chilling tower F and contacts with the high-temperature hydrogen sulfide synthetic gas 1 to obtain desulfurized hydrogen sulfide gas 2, and the retention time of the hydrogen sulfide synthetic gas 1 in the chilling tower F is 0.25s.
The temperature of the chilling tower F is 155.2 ℃, and the reaction pressure is 4bar;
the desulfurized hydrogen sulfide gas 2 is discharged from a discharge hole H of the chilling tower at the speed of 1168.39kg/H, and the reflux ratio is 0.8
626.12kg/h of pure hydrogen sulfide 4 with a purity of 99.92% and traces of polysulfide are obtained.
The spraying device D is provided with 4 layers of spraying pipes, and sprayed liquid drops cover the whole cross section of the chilling tower F.
Example 4A method for the aftertreatment of Hydrogen sulfide
Discharging sulfur obtained from a chilling tower from a liquid sulfur discharge port L, preheating discharged sulfur 6 to 100 ℃, enabling the sulfur to enter a hydrogen sulfide reactor A from a sulfur feed pipe C, mixing the sulfur with hydrogen, and then passing through a catalytic tube to obtain hydrogen sulfide synthetic gas 1, wherein the hydrogen sulfide synthetic gas 1 is discharged from a hydrogen sulfide synthetic gas discharge port B at 678.35kg/h (the hydrogen sulfide synthetic gas 1 comprises 92.24% of hydrogen sulfide, 7.41% of sulfur and 0.35% of impurities), the discharging temperature is 375 ℃,4bar, and the temperature is 360 ℃ when the sulfur enters a hydrogen sulfide chilling tower F under the condition of pipeline heat preservation;
and the refluxed gaseous hydrogen sulfide 3 passes through a hydrogen sulfide liquefier G to obtain refluxed liquid hydrogen sulfide 5, the temperature of the refluxed liquid hydrogen sulfide 5 is-20 ℃, the refluxed liquid hydrogen sulfide enters a spraying device D in a hydrogen sulfide chilling tower F and contacts with the high-temperature hydrogen sulfide synthetic gas 1 to obtain desulfurized hydrogen sulfide gas 2, and the retention time of the hydrogen sulfide synthetic gas 1 in the chilling tower F is 0.10s.
The temperature of the chilling tower F is 150.5 ℃, and the reaction pressure is 4bar;
the desulfurized hydrogen sulfide gas 2 is discharged from a discharge hole H of the chilling tower at the speed of 795.29kg/H, and the reflux ratio is 0.25
626.2kg/h of pure hydrogen sulfide 4 with a purity of 99.95% and traces of polysulfide are obtained.
The spraying device D is provided with 4 layers of spraying pipes, and sprayed liquid drops cover the whole cross section of the chilling tower F.
Example 5A method for the working-up of Hydrogen sulfide
Discharging sulfur obtained by a chilling tower from a liquid sulfur discharge port L, preheating discharged sulfur 6 to 100 ℃, feeding the sulfur into a hydrogen sulfide reactor A from a sulfur feeding pipe C, mixing the sulfur with hydrogen, passing through a catalytic pipe to obtain hydrogen sulfide synthetic gas 1, discharging the hydrogen sulfide synthetic gas 1 from a hydrogen sulfide synthetic gas discharge port B at 678.35kg/h (the hydrogen sulfide synthetic gas 1 comprises 92.24% of hydrogen sulfide, 7.41% of sulfur and 0.35% of impurities), wherein the discharging temperature is 380 ℃ and 7bar, and the temperature when the sulfur enters a hydrogen sulfide chilling tower F is 375 ℃ under the condition of pipeline heat preservation; and (2) the desulfurized hydrogen sulfide gas 2 is formed in the liquid hydrogen sulfide at the bottom of the chilling tower F of the hydrogen sulfide, the retention time of the hydrogen sulfide synthesis gas 1 in the chilling tower F is 0.15s, and the desulfurized hydrogen sulfide gas 2 is discharged from a discharge hole H of the chilling tower at the speed of 1018.92 kg/H. And the reflux ratio of the heat exchanger is 0.625, the refluxed gaseous hydrogen sulfide 3 passes through a hydrogen sulfide liquefier G to obtain refluxed liquid hydrogen sulfide 5, the refluxed liquid hydrogen sulfide 5 enters a chilling tower F at the temperature of-15 ℃, the pressure in the tower is 10bar, and the temperature is 125.83 ℃. The purity of the obtained pure hydrogen sulfide product 4 was 99.95%.
It is necessary to ensure that the hydrogen sulfide synthesis gas 1 inlet is submerged below the liquid hydrogen sulfide. The specific operation is as follows: firstly, ensuring that a certain liquid level exists in a chilling tower F and ensuring that a hydrogen sulfide inlet is immersed; then the liquid hydrogen sulfide 5 which flows back is changed into gas after contacting with the hydrogen sulfide synthesis gas 1, and the liquid level is kept by adjusting the reflux ratio.
EXAMPLE 6 aftertreatment device for Hydrogen sulfide
The invention further provides a post-treatment device of hydrogen sulfide, which comprises a hydrogen sulfide reactor A for reacting sulfur and hydrogen, and a hydrogen sulfide synthetic gas chilling tower F connected with a hydrogen sulfide synthetic gas discharge hole B, wherein the hydrogen sulfide synthetic gas chilling tower F comprises a demister E, a chilling tower discharge hole H and a liquid sulfur discharge hole L. The desulfurized hydrogen sulfide discharge pipeline is provided with a bypass, the bypass is connected with a hydrogen sulfide liquefier, the liquefier is connected with a hydrogen sulfide synthetic gas chilling tower F, and the discharge of the liquefier is directly sent to the hydrogen sulfide synthetic gas chilling tower F.
The hydrogen sulfide synthetic gas chilling tower F also can comprise a spraying device D, wherein the spraying devices are at least 1 layer, preferably 4 layers, and are arranged in a staggered mode to ensure that the cross section of the chilling tower F is covered, and the discharge of the liquefier is directly connected with the spraying device D.
Claims (6)
1. A method for post-treating hydrogen sulfide, characterized in that: the method comprises chilling of hydrogen sulfide synthesis gas and refluxing of hydrogen sulfide;
chilling the hydrogen sulfide synthesis gas, and rapidly cooling the hydrogen sulfide synthesis gas to 110-170 ℃;
the hydrogen sulfide synthesis gas is chilled, and the hydrogen sulfide synthesis gas is contacted with a low-temperature medium in a chilling tower to form a desulfurization hydrogen sulfide gas; the low-temperature medium is reflux liquid hydrogen sulfide at the temperature of-20 ℃ to-10 ℃;
the temperature of the hydrogen sulfide synthesis gas entering the chilling tower is not lower than 350 ℃, and the retention time of the hydrogen sulfide synthesis gas in the chilling tower is 0.1-0.35s;
the hydrogen sulfide synthesis gas comprises 89-95% of hydrogen sulfide and 5-10% of sulfur steam by mass percentage.
2. A method for the post-treatment of hydrogen sulphide according to claim 1, characterized in that: and refluxing the hydrogen sulfide, namely refluxing the desulfurized hydrogen sulfide gas at a reflux ratio of 0.2-1, condensing the refluxed hydrogen sulfide to be used as a low-temperature medium, and sending the low-temperature medium to a chilling tower.
3. A method for the post-treatment of hydrogen sulphide according to claim 1, characterized in that: the contact mode is that the spraying low-temperature medium is in reverse contact with the hydrogen sulfide synthetic gas, and the pressure in the chilling tower is 3 bar-7 bar.
4. A method for the post-treatment of hydrogen sulphide according to claim 3, characterized in that: and the sprayed low-temperature medium needs to cover the cross section of the chilling tower.
5. A method for the post-treatment of hydrogen sulphide according to claim 1, characterized in that: the contact mode is that the hydrogen sulfide synthesis gas is directly introduced below the low-temperature medium liquid level in the chilling tower, and the pressure in the chilling tower is 10 bar-20 bar.
6. A method for the post-treatment of hydrogen sulphide according to claim 1, characterized in that: chilling the hydrogen sulfide synthesis gas, separating sulfur from the hydrogen sulfide synthesis gas by liquefying or solidifying the sulfur, and discharging the sulfur for synthesizing the hydrogen sulfide synthesis gas.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0339818A1 (en) * | 1988-04-07 | 1989-11-02 | JGC Corporation | Process for the manufacture of hydrogen sulfide |
| CN102502523A (en) * | 2011-11-03 | 2012-06-20 | 烟台大学 | Method for preparing hydrogen sulfide |
| CN102500285A (en) * | 2011-11-03 | 2012-06-20 | 烟台大学 | Hydrogen sulfide synthesis device |
| CN112408336A (en) * | 2020-11-25 | 2021-02-26 | 泰安科赛尔化学科技有限公司 | Method and equipment for purifying hydrogen sulfide |
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| JPH04208386A (en) * | 1990-11-30 | 1992-07-30 | Kyocera Corp | Gas purifying method |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0339818A1 (en) * | 1988-04-07 | 1989-11-02 | JGC Corporation | Process for the manufacture of hydrogen sulfide |
| CN102502523A (en) * | 2011-11-03 | 2012-06-20 | 烟台大学 | Method for preparing hydrogen sulfide |
| CN102500285A (en) * | 2011-11-03 | 2012-06-20 | 烟台大学 | Hydrogen sulfide synthesis device |
| CN112408336A (en) * | 2020-11-25 | 2021-02-26 | 泰安科赛尔化学科技有限公司 | Method and equipment for purifying hydrogen sulfide |
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