CN112938905B - Method for preparing high-purity sulfur by utilizing tail gas containing hydrogen sulfide - Google Patents
Method for preparing high-purity sulfur by utilizing tail gas containing hydrogen sulfide Download PDFInfo
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- CN112938905B CN112938905B CN202110442461.4A CN202110442461A CN112938905B CN 112938905 B CN112938905 B CN 112938905B CN 202110442461 A CN202110442461 A CN 202110442461A CN 112938905 B CN112938905 B CN 112938905B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
- C01B17/04—Preparation of sulfur; Purification from gaseous sulfur compounds including gaseous sulfides
- C01B17/05—Preparation of sulfur; Purification from gaseous sulfur compounds including gaseous sulfides by wet processes
Abstract
The invention relates to a method for preparing high-purity sulfur by utilizing tail gas containing hydrogen sulfide, which comprises the following steps: the tail gas containing hydrogen sulfide is contacted with sulfuric acid through a contact device to react, so that sulfur with purity more than or equal to 99.95% is obtained; the molar ratio of the sulfuric acid to the hydrogen sulfide is (0.1-1): 1; the concentration of sulfuric acid is more than or equal to 75%; and the high-purity ultrafine sulfur is obtained by controlling the relevant parameters of the gas-liquid two phases in the reaction process. The method has the advantages of high absorption reaction efficiency, mild reaction process, no secondary pollution and strong applicability. The purity of the sulfur product is more than or equal to 99.5%, the granularity range is 10-30 mu m, and the sulfur product can be directly applied to the industries of medicine, agriculture, chemical industry and the like; the absorption liquid after treatment can be directly sold or used as a byproduct.
Description
Technical Field
The invention relates to a technology for recycling high-purity ultrafine sulfur from hydrogen sulfide-containing tail gas, in particular to a method for preparing high-purity sulfur from hydrogen sulfide-containing tail gas.
Background
The generation of hydrogen sulfide waste gas comes from a plurality of industries, mainly including purification of natural gas, petroleum refining, gas factories, sewage treatment plants, paper mills and the like, and particularly in some areas where industries are concentrated, a large amount of hydrogen sulfide waste gas with higher concentration can be generated, and therefore, scientific and efficient treatment of the hydrogen sulfide waste gas is required to avoid the harm to human safety and ecological environment.
Currently, the purification methods of hydrogen sulfide exhaust gas mainly include an absorption method, an adsorption method, and an oxidation method. Wherein, the absorption method and the adsorption method adopt a physical or chemical method to fix the hydrogen sulfide waste gas, and do not carry out product conversion on the hydrogen sulfide. The oxidation process oxidizes hydrogen sulfide to elemental sulfur, and is commonly used in the industry as the claus process. The Claus method belongs to dry oxidation, and has the advantages of flexible and convenient operation, high sulfur recovery rate, strong device applicability, and low investment and operation cost. As CN102512937a discloses a method for recycling hydrogen sulfide waste gas, the main steps are as follows: A. waste alkali liquor generated after the alkali fiber is subjected to a squeezing process is filtered by a membrane to obtain secondary waste alkali liquor; B. the secondary alkali liquid is used as alkali absorption liquid and is produced in the production process of viscose fiberDelivering the hydrogen sulfide waste gas to an alkali spray tower together; C. the discharged alkali spray absorption liquid is used as cooking liquid for pulping by a sulfate method, and Na obtained by the reaction is used as a catalyst 2 S and other NaOH solutions are conveyed to the pulp making process, and the method has the advantages of high efficiency of absorbing the hydrogen sulfide waste gas, large treatment capacity in unit time, solving the problems of environmental pollution and production safety hidden trouble caused by the emission of the hydrogen sulfide waste gas, and realizing the purposes of waste preparation by waste and waste recycling by utilizing waste alkali liquor generated by alkali fiber squeezing.
CN106672918A discloses an energy-saving and environment-friendly design method for an acid making device by a hydrogen sulfide dry method, which comprises the following steps: the first step: the waste gas containing hydrogen sulfide is used as a raw material, and the burnt furnace gas is used for producing steam by recovering waste heat through a fire tube type waste heat boiler and a superheater; and a second step of: the furnace gas temperature is reduced to 320 ℃ and then enters a dynamic wave scrubber of a purification section, and the dynamic wave scrubber is sprayed by dilute acid with the concentration of about 14.4 percent to carry out adiabatic evaporative cooling; and a third step of: cooling the furnace gas to 64.7 ℃ and then entering a cooling tower; fourth step: cooling furnace gas to 38.5 ℃ and sequentially entering a first-stage electric demister and a second-stage electric demister to remove acid mist; fifth step: the content of acid mist in the outlet gas is less than or equal to 0.005g/Nm 3 Feeding into a dry suction section. The energy-saving and environment-friendly design method of the device for preparing the acid by the hydrogen sulfide dry method adopts the Claus method to treat the acid gas containing the hydrogen sulfide to produce sulfur, and takes the acid gas containing the hydrogen sulfide as a raw material to prepare sulfuric acid.
However, the claus process is mainly applied to treatment technology with high concentration of hydrogen sulfide, and strict control of H in process gas is required 2 S and SO 2 The hydrogen sulfide gas is treated, so that the whole process is difficult to control, a certain amount of organic sulfur compounds are generated in the reaction process, the purity of sulfur is low, and the application range is narrow.
Disclosure of Invention
In view of the problems existing in the prior art, one of the purposes of the invention is to provide a method for preparing high-purity sulfur by utilizing hydrogen sulfide-containing tail gas, which adopts sulfuric acid as an absorption liquid to perform contact absorption oxidation on the hydrogen sulfide-containing tail gas to prepare high-purity superfine elemental sulfur and by-produce dilute sulfuric acid. The process has the advantages of simple production equipment, high product purity and good benefit, and has better industrial application prospect.
To achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for preparing high-purity sulfur by utilizing tail gas containing hydrogen sulfide, which comprises the following steps: the tail gas containing hydrogen sulfide is contacted with sulfuric acid through a contact device to react, so that sulfur with purity more than or equal to 99.95% is obtained;
the molar ratio of the sulfuric acid to the hydrogen sulfide is (0.1-1): 1;
the concentration of sulfuric acid is more than or equal to 75%;
an air inlet of the contact device is provided with an aeration structure.
In the invention, the purity of the high purity is more than or equal to 99.95 percent.
In the present invention, the molar ratio of sulfuric acid to hydrogen sulfide is (0.1-1): 1, and may be, for example, 0.1:1, 0.2:1, 0.3:1, 0.4:1, 0.5:1, 0.6:1, 0.7:1, 0.8:1, 0.9:1, or 1:1, etc., but not limited to the recited values, and other non-recited values within this range are equally applicable.
In the present invention, the concentration of sulfuric acid is not less than 75%, for example, 75%, 76%, 77%, 78%, 79%, 80%, 81%, 82%, 83%, 84%, 85%, 86%, 87%, 88%, 89%, 90%, 91%, 92%, 93%, 94%, 95%, 96%, 97% or 98%, etc., but not limited to the above-mentioned values, and other values not mentioned in the above range are equally applicable.
According to the scheme provided by the invention, the comprehensive control of time, temperature and acid concentration in the contact reaction is controlled through the design of the reaction process, and the interaction effect among the four is utilized, so that the preparation of superfine sulfur, the effective separation of hydrogen sulfide in tail gas and the high-value resource development and utilization of the hydrogen sulfide are realized, and the conversion efficiency of the hydrogen sulfide can reach more than 90%.
In the invention, the air inlet of the contact device is the inlet of the hydrogen sulfide tail gas. According to the invention, the aeration plate is arranged at the air inlet of the contact device, so that the size of bubbles is effectively reduced, the mass transfer process is accelerated, and the dispersion degree of gas in liquid is increased.
As a preferable embodiment of the present invention, the molar ratio of sulfuric acid to hydrogen sulfide is (0.1-0.4): 1.
As a preferred embodiment of the present invention, the contacting means comprises 1 or a combination of at least 2 of a gas-liquid spray column, a bubble column, a stirred bubble column or a loop reactor.
As a preferred embodiment of the present invention, the contacting device is a bubble column.
In a preferred embodiment of the present invention, the aeration structure is an aeration plate having pores with a diameter of 15 to 20 μm, and may be, for example, 15 μm, 16 μm, 17 μm, 18 μm, 19 μm or 20 μm, etc., but the aeration structure is not limited to the values recited, and other values not recited in the range are equally applicable. The generation of crystal nucleus in the reaction crystallization process is controlled by controlling the pore diameter of the aeration plate, so that the growth of crystals is controlled, and the generation of superfine sulfur is facilitated.
In a preferred embodiment of the present invention, the contact reaction time is 10-60min, for example, 10min, 12min, 14min, 16min, 18min, 20min, 22min, 24min, 26min, 28min, 30min, 32min, 34min, 36min, 38min, 40min, 42min, 44min, 46min, 48min, 50min, 52min, 54min, 56min, 58min or 60min, etc., but not limited to the recited values, and other non-recited values in the range are equally applicable.
In a preferred technical scheme of the invention, the mode of contacting the tail gas containing hydrogen sulfide with sulfuric acid in the contacting device is countercurrent contact.
As a preferable technical scheme of the invention, the number of the contact reaction stages is 2-5, and the end point of each stage of the contact reaction is that the concentration of sulfuric acid after absorption is 50-52%. In the present invention, the number of the contact reaction stages is 2 to 5, and may be, for example, 2, 3, 4 or 5 stages, etc., but not limited to the recited values, and other non-recited values within this range are equally applicable.
The end point of each stage of the contact reaction is the concentration of sulfuric acid after absorption of 50 to 52%, for example, 50%, 50.1%, 50.2%, 50.3%, 50.4%, 50.5%, 50.6%, 50.7%, 50.8%, 50.9%, 51%, 51.1%, 51.2%, 51.3%, 51.4%, 51.5%, 51.6%, 51.7%, 51.8%, 51.9% or 52%, etc., but not limited to the recited values, and other non-recited values within this range are equally applicable.
The invention adopts countercurrent contact of gas and liquid phases, increases discrete degree and turbulence, accelerates absorption of hydrogen sulfide, accelerates reaction, and is favorable for generation of fine sulfur.
As a preferred technical solution of the present invention, the method includes: carrying out countercurrent contact reaction on the tail gas containing hydrogen sulfide and sulfuric acid through a contact device to obtain sulfur with purity more than or equal to 99.95%;
the molar ratio of the sulfuric acid to the hydrogen sulfide is (0.1-1): 1; the concentration of sulfuric acid is more than or equal to 75%;
the number of the contact reaction stages is 2-5, and the end point of each stage of the contact reaction is that the concentration of sulfuric acid after absorption is 50-52%;
the contacting device comprises 1 or a combination of at least 2 of a gas-liquid spray column, a bubble column, a stirred bubble column, or a loop reactor; the air inlet of the contact device is provided with an aeration plate with air holes with the diameter of 15-20 mu m;
the contact reaction time is 10-60min;
the temperature of the contact reaction is 25-80 ℃.
In the method provided by the invention, the reaction time, the reaction temperature and the reaction end point are greatly influenced by the reaction stage number, and the crystal grain size distribution of the crystal product is increased, the rate of crystal nucleation and secondary nucleation is increased, the rate of crystal growth is reduced and the preparation of superfine sulfur is realized by controlling the reaction parameters in a combined manner.
The method provided by the invention can effectively shorten the growth time of crystals by controlling the reaction time to be 10-60min, reduce the grain size, and simultaneously can control the size of a contact device by the shorter reaction time, thereby being easy for industrial amplification. The reaction temperature is controlled to be 25-80 ℃, so that the gas dissolution speed can be increased, the pressure (gas volume expansion) is increased, the reaction rate is accelerated, and the nucleation reaction of crystals is accelerated.
The sulfuric acid is used as the absorption liquid, the concentration of the sulfuric acid at the end point of the absorption reaction is controlled to be 50%, the reaction rate can be accelerated by utilizing the strong oxidizing property of the concentration of more than 50%, the burst nucleation rate of crystals can be increased, the reaction time can be shortened, and the growth process of the crystals can be reduced.
The reaction level is related to the content of hydrogen sulfide in the tail gas and the consumption of the absorption liquid, the higher content of hydrogen sulfide and the lower consumption of the absorption liquid can increase the reaction level, and the reaction level is that the tail gas is serially connected with the absorption level.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) The resource utilization of hydrogen sulfide waste gas with different sources and different concentrations is realized, no secondary pollution is generated, and the high-value conversion of hydrogen sulfide is realized.
(2) The utilization rate of the hydrogen sulfide is high, the prepared sulfur product has high purity, the granularity can reach 10-30 mu m, and the application value is high.
(3) The absorption liquid can be used as a byproduct in the fields of acid washing, mineral leaching and the like or sold.
Detailed Description
For a better illustration of the present invention, which is convenient for understanding the technical solution of the present invention, exemplary but non-limiting examples of the present invention are as follows:
example 1
The method adopts sulfuric acid with the mass concentration of 75% as an absorption liquid to absorb tail gas containing hydrogen sulfide, the content of the hydrogen sulfide is 5%, the molar ratio of the sulfuric acid to the hydrogen sulfide is 0.2:1, the sulfuric acid enters a gas-liquid spray tower from the top and is in countercurrent contact with the tail gas from an aeration plate with the surface pore diameter of 15-20 mu m, the reaction time is controlled to be 30min, the reaction temperature is 80 ℃, the tail gas is subjected to series connection 3 absorption reactions, the concentration of the end-point sulfuric acid of each stage operation is 50%, and after the reaction is finished, the liquid-solid separation is carried out to obtain sulfur and dilute sulfuric acid.
The index of the obtained product is shown in Table 1.
Example 2
The method adopts sulfuric acid with the mass concentration of 85% as an absorption liquid to absorb tail gas containing hydrogen sulfide, the content of the hydrogen sulfide is 30%, the molar ratio of the sulfuric acid to the hydrogen sulfide is 0.4:1, the sulfuric acid enters a bubbling tower from the top and is in countercurrent contact with the tail gas from the bottom through an aeration plate with the surface pore diameter of 15-20 mu m, the reaction time is controlled to be 15min, the reaction temperature is 25 ℃, the tail gas is subjected to series absorption reaction for 3 times, the concentration of the end-point sulfuric acid of each stage operation is 50%, and after the reaction is finished, the liquid-solid separation is carried out to obtain sulfur and dilute sulfuric acid.
The index of the obtained product is shown in Table 1.
Example 3
The method adopts sulfuric acid with the mass concentration of 90% as an absorption liquid to absorb tail gas containing hydrogen sulfide, the content of the hydrogen sulfide is 1%, the molar ratio of the sulfuric acid to the hydrogen sulfide is 0.6:1, the sulfuric acid enters a circulation reactor from the top to be in countercurrent contact with the tail gas from the bottom through an aeration plate with the surface pore diameter of 15-20 mu m, the reaction time is controlled to be 60min, the reaction temperature is 30 ℃, the tail gas is subjected to series connection 2 absorption reactions, the concentration of the end-point sulfuric acid of each stage operation is 50%, and after the reaction is finished, the liquid-solid separation is carried out to obtain sulfur and dilute sulfuric acid.
The index of the obtained product is shown in Table 1.
Example 4
The method adopts sulfuric acid with the mass concentration of 98% as an absorption liquid to absorb tail gas containing hydrogen sulfide, the content of the hydrogen sulfide is 15%, the molar ratio of the sulfuric acid to the hydrogen sulfide is 0.1:1, the sulfuric acid enters a stirring bubbling tower from the top and is in countercurrent contact with the tail gas from the bottom through an aeration plate with the surface pore diameter of 15-20 mu m, the reaction time is controlled to be 10min, the reaction temperature is 60 ℃, the tail gas is subjected to series connection 5 absorption reactions, the concentration of the end-point sulfuric acid of each stage operation is 50%, and after the reaction is finished, the liquid-solid separation is carried out to obtain sulfur and dilute sulfuric acid.
The index of the obtained product is shown in Table 1.
Example 5
The method comprises the steps of absorbing tail gas containing hydrogen sulfide by using sulfuric acid with the mass concentration of 95% as an absorption liquid, wherein the content of the hydrogen sulfide is 50%, the molar ratio of the sulfuric acid to the hydrogen sulfide is 1:1, the sulfuric acid enters a bubbling tower from the top to be in countercurrent contact with the tail gas from the bottom through an aeration plate with the surface pore diameter of 15-20 mu m, the reaction time is controlled to be 20min, the reaction temperature is 25 ℃, the tail gas is subjected to series connection for 5 absorption reactions, the concentration of the end-point sulfuric acid of each operation is 50%, and after the reaction is finished, the liquid-solid separation is carried out to obtain sulfur and dilute sulfuric acid.
The index of the obtained product is shown in Table 1.
Comparative example 1
The sulfuric acid concentration in example 4 was changed to 30% and the other conditions were the same. The index of the obtained product is shown in Table 1.
Comparative example 2
The reaction time was changed to 120min in example 2, and the other conditions were the same. The index of the obtained product is shown in Table 1.
Comparative example 3
The reaction temperature in comparative example 2 was changed to 100℃and the other conditions were the same as in comparative example 3. The index of the obtained product is shown in Table 1.
Comparative example 4
The molar ratio of sulfuric acid to hydrogen sulfide in example 4 was varied to be 5:1, with the remaining conditions being the same. The index of the obtained product is shown in Table 1.
Comparative example 5
The reaction temperature in example 4 was changed to 100℃and the other conditions were the same. The index of the obtained product is shown in Table 1.
Comparative example 6
The reaction temperature in comparative example 4 was changed to 100℃and the other conditions were the same. The index of the obtained product is shown in Table 1.
Comparative example 7
The aeration panel in example 4 was changed to be disposed at the inlet of sulfuric acid, and the other conditions were the same. The index of the obtained product is shown in Table 1.
Comparative example 8
The aeration panel in modified example 4 was disposed in the middle of the contact device, and the other conditions were the same. The index of the obtained product is shown in Table 1.
Comparative example 9
The aeration plate pores in example 4 were changed to have a diameter of 30. Mu.m, and the other conditions were the same. The index of the obtained product is shown in Table 1.
TABLE 1
As is apparent from the results of the above examples and comparative examples, the solution provided by the present invention greatly affects the crystal size distribution of the crystalline product by the reaction time, reaction temperature, reaction end point and reaction progression, and realizes the preparation of fine sulfur particles by controlling the nucleation of crystals, the rate of secondary nucleation and the reduction of the growth rate of crystals by adding an aeration plate to the contact device and controlling the diameter of the air holes.
The applicant states that the detailed structural features of the present invention are described by the above embodiments, but the present invention is not limited to the above detailed structural features, i.e. it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be apparent to those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope of the present invention and the scope of the disclosure.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.
In addition, the specific features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described further.
Moreover, any combination of the various embodiments of the invention can be made without departing from the spirit of the invention, which should also be considered as disclosed herein.
Claims (5)
1. A method for preparing high-purity sulfur by utilizing tail gas containing hydrogen sulfide, which is characterized by comprising the following steps: the tail gas containing hydrogen sulfide is contacted with sulfuric acid through a contact device to obtain sulfur with the purity of more than or equal to 99.95 percent and the granularity of 10-30 mu m;
the molar ratio of the sulfuric acid to the hydrogen sulfide is (0.1-0.3): 1;
the concentration of sulfuric acid is more than or equal to 75%;
the contact reaction time is 10-60min; the temperature of the contact reaction is 25-80 ℃; the number of the contact reaction stages is 2-5, and the end point of each stage of the contact reaction is that the concentration of sulfuric acid after absorption is 50-52%;
the air inlet of the contact device is provided with an aeration structure, and the aeration structure is an aeration plate with air holes with the diameter of 15-20 mu m on the surface.
2. The process of claim 1, wherein the contacting means comprises 1 or a combination of at least 2 of a gas-liquid spray column, a bubble column, a stirred bubble column, or a loop reactor.
3. The method of claim 2, wherein the contacting device is a bubble column.
4. The method of claim 1, wherein the hydrogen sulfide containing tail gas is contacted with sulfuric acid in a countercurrent contact in the contacting device.
5. The method of claim 1, wherein the method comprises: carrying out countercurrent contact reaction on the tail gas containing hydrogen sulfide and sulfuric acid through a contact device to obtain sulfur with purity more than or equal to 99.95%;
the molar ratio of the sulfuric acid to the hydrogen sulfide is (0.1-0.3): 1; the concentration of sulfuric acid is more than or equal to 75%;
the number of the contact reaction stages is 2-5, and the end point of each stage of the contact reaction is that the concentration of sulfuric acid after absorption is 50-52%;
the contacting device comprises 1 or a combination of at least 2 of a gas-liquid spray column, a bubble column, a stirred bubble column, or a loop reactor; the air inlet of the contact device is provided with an aeration structure, and the aeration structure is an aeration plate with air holes with the diameter of 15-20 mu m on the surface;
the contact reaction time is 10-60min;
the temperature of the contact reaction is 25-80 ℃.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04362008A (en) * | 1991-06-07 | 1992-12-15 | Idemitsu Kosan Co Ltd | Treatment of hydrogen sulfide containing gas |
| EP0612556A1 (en) * | 1993-02-25 | 1994-08-31 | Idemitsu Kosan Company Limited | Process for removal of hydrogen sulfide |
| WO1995021790A1 (en) * | 1994-02-14 | 1995-08-17 | Exxon Research And Engineering Company | Method and apparatus for recovering elemental sulfur from flue gas |
| WO1995022394A1 (en) * | 1994-02-18 | 1995-08-24 | Ivo Giovanni Dalla Lana | A method for removing hydrogen sulfide from gas streams |
| CN102198365A (en) * | 2011-05-11 | 2011-09-28 | 北京丰汉工程咨询有限公司 | Processing method of acid gas |
| CN106145058A (en) * | 2015-03-24 | 2016-11-23 | 上海宝钢化工有限公司 | Saturated hydrog en sulphide solution safely prepare apparatus and method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ITMI20022705A1 (en) * | 2002-12-20 | 2004-06-21 | Enitecnologie Spa | ORGANIC CHEMICAL PROCESS FOR THE DESULFURATION OF H2S CONTAINING GASEOUS CURRENTS. |
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2021
- 2021-04-23 CN CN202110442461.4A patent/CN112938905B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04362008A (en) * | 1991-06-07 | 1992-12-15 | Idemitsu Kosan Co Ltd | Treatment of hydrogen sulfide containing gas |
| EP0612556A1 (en) * | 1993-02-25 | 1994-08-31 | Idemitsu Kosan Company Limited | Process for removal of hydrogen sulfide |
| WO1995021790A1 (en) * | 1994-02-14 | 1995-08-17 | Exxon Research And Engineering Company | Method and apparatus for recovering elemental sulfur from flue gas |
| WO1995022394A1 (en) * | 1994-02-18 | 1995-08-24 | Ivo Giovanni Dalla Lana | A method for removing hydrogen sulfide from gas streams |
| CN102198365A (en) * | 2011-05-11 | 2011-09-28 | 北京丰汉工程咨询有限公司 | Processing method of acid gas |
| CN106145058A (en) * | 2015-03-24 | 2016-11-23 | 上海宝钢化工有限公司 | Saturated hydrog en sulphide solution safely prepare apparatus and method |
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