RU2140318C1 - Method of removing hydrogen sulfide from gas mixtures - Google Patents
Method of removing hydrogen sulfide from gas mixtures Download PDFInfo
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- RU2140318C1 RU2140318C1 RU98113831A RU98113831A RU2140318C1 RU 2140318 C1 RU2140318 C1 RU 2140318C1 RU 98113831 A RU98113831 A RU 98113831A RU 98113831 A RU98113831 A RU 98113831A RU 2140318 C1 RU2140318 C1 RU 2140318C1
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- hydrogen sulfide
- gas
- gas mixtures
- removing hydrogen
- zinc oxide
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- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 title claims description 20
- 239000007789 gas Substances 0.000 title claims description 19
- 229910000037 hydrogen sulfide Inorganic materials 0.000 title claims description 19
- 238000000034 method Methods 0.000 title claims description 18
- 239000000203 mixture Substances 0.000 title claims description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000011787 zinc oxide Substances 0.000 claims abstract description 13
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 6
- 239000000725 suspension Substances 0.000 claims abstract description 4
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 239000006096 absorbing agent Substances 0.000 claims description 5
- 238000000746 purification Methods 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 3
- 239000002250 absorbent Substances 0.000 abstract description 2
- 230000002745 absorbent Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 12
- 239000011701 zinc Substances 0.000 description 9
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 229910052725 zinc Inorganic materials 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 3
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 230000003993 interaction Effects 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000004246 zinc acetate Substances 0.000 description 3
- 239000005083 Zinc sulfide Substances 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000006477 desulfuration reaction Methods 0.000 description 2
- 230000023556 desulfurization Effects 0.000 description 2
- 238000011086 high cleaning Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910052984 zinc sulfide Inorganic materials 0.000 description 2
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 125000000896 monocarboxylic acid group Chemical group 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
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- Gas Separation By Absorption (AREA)
- Treating Waste Gases (AREA)
Abstract
Description
Изобретение относится к области очистки газов от сероводорода, (в частности, к области обессеривания газов путем химического взаимодействия поглотителя с сероводородом). The invention relates to the field of gas purification from hydrogen sulfide, (in particular, to the field of gas desulfurization by chemical interaction of the absorber with hydrogen sulfide).
Известен широкий круг химических соединений, используемых в качестве поглотителя сероводорода. Наиболее часто для этих целей применяют соединения со щелочной функцией: гидроокиси и карбонаты щелочных металлов, аминосоединений /1. Патент США N 4198378. 2. Патент США N 3941875. 3. А.с. СССР N 814414./ Сероводород поступает в обратимые реакции, что не позволяет достичь высокой глубины очистки. A wide range of chemical compounds are known that are used as an absorbent of hydrogen sulfide. Most often, compounds with an alkaline function are used for these purposes: hydroxides and carbonates of alkali metals, amino compounds / 1. US patent N 4198378. 2. US patent N 3941875. 3. A.S. USSR N 814414./ Hydrogen sulfide enters into reversible reactions, which does not allow to achieve a high cleaning depth.
Абсорбция сероводорода ведется в мягких условиях, без энергетических затрат, технически просто. The absorption of hydrogen sulfide is carried out in mild conditions, without energy costs, technically simple.
Однако к недостаткам этих способов удаления сероводорода, кроме невысокой глубины очистки, следует отнести необходимость проведения следующих стадий процесса - регенерации поглотителя и утилизации сероводорода, что значительно усложняет и удорожает процесс газоочистки. However, the disadvantages of these methods of removing hydrogen sulfide, in addition to a low cleaning depth, include the need for the following stages of the process - regeneration of the absorber and disposal of hydrogen sulfide, which greatly complicates and increases the cost of gas cleaning.
Также широко известны твердые поглотители на основе оксидов металлов, таких как железо, цинк, никель, медь и т.п. В этих процессах происходит химическое взаимодействие по схеме:
ЭО + H2S = ЭS + H2O, где Э = Fe, Ni, Cu, Zn...Solid absorbers based on metal oxides such as iron, zinc, nickel, copper and the like are also widely known. In these processes, a chemical interaction occurs according to the scheme:
EO + H 2 S = ES + H 2 O, where E = Fe, Ni, Cu, Zn ...
Сера необратимо связывается при высокой (250 - 450oC) температуре в сульфид металла, благодаря чему степень очистки газа от сероводорода очень высока. Процесс одностадиен, что также является его достоинством.Sulfur irreversibly binds at high (250 - 450 o C) temperature to a metal sulfide, due to which the degree of gas purification from hydrogen sulfide is very high. The process is one-stage, which is also its advantage.
Однако использование высоких температур в процессе предъявляет серьезные требования к конструкционным материалам установки, повышает себестоимость очистки газа за счет высокой энергоемкости. However, the use of high temperatures in the process places serious demands on the structural materials of the installation, and increases the cost of gas purification due to its high energy intensity.
Совместить достоинства вышеописанных процессов - высокую глубину очистки, низкую энергоемкость, техническую простоту и одностадийность позволяет процесс очистки газов от сероводорода с использованием суспензии оксида металла в водном растворе его соли, как это сделано в процессе "Chemsweet" /4. Manning W.P. "Chemsweet, a new process for sweetening low-value sour gas", Oil and Gas Journal, v. 77, N 42, 1979/. Combining the advantages of the above processes - high cleaning depth, low energy intensity, technical simplicity and one-stage process allows the process of cleaning gases from hydrogen sulfide using a suspension of metal oxide in an aqueous solution of its salt, as was done in the Chemsweet / 4 process. Manning W.P. "Chemsweet, a new process for sweetening low-value sour gas", Oil and Gas Journal, v. 77, N 42, 1979 /.
В этом случае взаимодействие окиси цинка с сероводородом происходит в суспензии, содержащей раствор ацетата цинка. Взаимодействует с H2S в водном растворе ацетат цинка с образованием сульфида цинка и уксусной кислоты. Высвободившаяся уксусная кислота растворяет твердую суспендированную окись цинка, переводя в ионную солевую форму, способную к реакции с сероводородом в водной фазе:
CH3COOH + ZnO ---> Zn(CH3COO)2 + H2O
Таким образом, достигается мгновенное и полное связывание H2S в малодиссоциированное соединение, что обеспечивает глубокую очистку газа. Аппаратурное оформление процесса простое, условия ведения его - мягкие.In this case, the interaction of zinc oxide with hydrogen sulfide occurs in a suspension containing a solution of zinc acetate. Zinc acetate interacts with H 2 S in an aqueous solution to produce zinc sulfide and acetic acid. The released acetic acid dissolves the solid suspended zinc oxide, converting it into an ionic salt form capable of reacting with hydrogen sulfide in the aqueous phase:
CH 3 COOH + ZnO ---> Zn (CH 3 COO) 2 + H 2 O
Thus, instant and complete binding of H 2 S to a slightly dissociated compound is achieved, which ensures deep gas purification. The hardware design of the process is simple, its operating conditions are soft.
Наиболее существенными недостатками этого метода сероочистки являются:
а) высокое пенообразование, вызванное сочетанием неорганического элемента - металла - с органическим радикалом в ацетате цинка;
б) постепенная утрата растворителя в реакционной смеси вследствие уноса летучей уксусной кислоты потоком газа.The most significant disadvantages of this desulfurization method are:
a) high foaming caused by a combination of an inorganic element - a metal - with an organic radical in zinc acetate;
b) the gradual loss of solvent in the reaction mixture due to the entrainment of volatile acetic acid by a gas stream.
Этих недостатков лишен предлагаемый способ очистки газа от H2S, основанный на той же реакции иона Zn++ с растворенным в воде сероводородом, с той разницей, что в качестве растворителя оксида цинка выступает не уксусная кислота, а водный раствор хлорида аммония.The proposed method for gas purification from H 2 S is deprived of these drawbacks, based on the same reaction of the Zn ++ ion with hydrogen sulfide dissolved in water, with the difference that the solution of zinc oxide is not acetic acid, but an aqueous solution of ammonium chloride.
Схема процесса:
ZnO + NH4Cl ⇄ [Zn(NH3)n]Cl2 + H2O
Окись цинка растворяется в водном хлористом аммонии с образованием комплексного соединения - цинкамминхлорида, [Zn(NH3)n]Cl2, растворимого в воде и содержащего цинк в воде комплексного иона [Zn(NH3)n]+2.Process diagram:
ZnO + NH 4 Cl ⇄ [Zn (NH 3 ) n ] Cl 2 + H 2 O
Zinc oxide dissolves in aqueous ammonium chloride to form a complex compound, zincamminchloride, [Zn (NH 3 ) n ] Cl 2 , which is soluble in water and contains the complex ion [Zn (NH 3 ) n ] +2 in water.
В ионном виде цинк мгновенно связывает сероводород в сульфид цинка, обеспечивая высокую глубину очистки. Высвободившийся при этой реакции NH4Cl вновь растворяет суспендированную окись цинка, переводя цинк в ионную форму.In its ionic form, zinc instantly binds hydrogen sulfide to zinc sulfide, providing a high degree of purification. The NH 4 Cl released during this reaction re-dissolves the suspended zinc oxide, converting the zinc to its ionic form.
Процесс продолжается до полного срабатывания оксида цинка. Конверсия ZnO практически 100%. The process continues until zinc oxide is fully activated. The conversion of ZnO is almost 100%.
Глубина очистки газа от H2S - 5 - 7 ppm.Depth of gas purification from H 2 S - 5 - 7 ppm.
Технически процесс крайне прост, условия проведения его - мягкие, т.к. обусловлены температурным интервалом существования водных растворов. Technically, the process is extremely simple, its conditions are soft, because due to the temperature range of the existence of aqueous solutions.
Сказанное иллюстрируется примерами:
Пример 1. В цилиндрический реактор, снабженный трубками для подачи и вывода газа, загружали 8,1 г (0,1 моля) оксида цинка и 160 г 20%-го водного раствора хлорида аммония. Через смесь барботировали при комнатной температуре газ состава: CH4 95 об.%, H2S 5 об.%, с объемной скоростью 4,5 л/час (30 час-1).The foregoing is illustrated by examples:
Example 1. In a cylindrical reactor equipped with tubes for supplying and removing gas, was loaded 8.1 g (0.1 mol) of zinc oxide and 160 g of a 20% aqueous solution of ammonium chloride. A gas of the following composition was bubbled through the mixture at room temperature: CH 4 95 vol.%, H 2 S 5 vol.%, With a space velocity of 4.5 l / h (30 h -1 ).
На выходе определяли содержание H2S в мг/м3 прибором - анализатором сероводорода "Рикэн Кэйки".The output was determined by the content of H 2 S in mg / m 3 instrument - analyzer of hydrogen sulfide "Ricken Keyki".
Сероводород в потоке газа после очистки отсутствовал. Hydrogen sulfide in the gas stream after purification was absent.
Пример 2 - 11. В цилиндрический реактор, снабженный трубками для подачи и вывода газа, загружали определенную навеску оксида цинка и определенное количество раствора хлорида аммония указанных ниже концентраций. Example 2 - 11. In a cylindrical reactor equipped with tubes for supplying and removing gas, a certain weighed portion of zinc oxide and a certain amount of a solution of ammonium chloride of the concentrations indicated below were loaded.
Через смесь барботировали газ, содержащий метан, диоксид углерода, сероводород в указанных ниже количествах с заданной скоростью, при заданной температуре. A gas containing methane, carbon dioxide, hydrogen sulfide in the amounts indicated below was bubbled through the mixture at a given speed at a given temperature.
На выходе определяли состав газа. Содержание метана, диоксида углерода определяли хроматографически; содержание сероводорода определяли прибором "Рикэн Кэйки". The gas composition was determined at the outlet. The content of methane, carbon dioxide was determined chromatographically; the hydrogen sulfide content was determined with a Ricken Keykey instrument.
Условия и результаты эксперимента приведены в таблице. The conditions and results of the experiment are shown in the table.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| RU98113831A RU2140318C1 (en) | 1998-07-14 | 1998-07-14 | Method of removing hydrogen sulfide from gas mixtures |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| RU98113831A RU2140318C1 (en) | 1998-07-14 | 1998-07-14 | Method of removing hydrogen sulfide from gas mixtures |
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| RU2140318C1 true RU2140318C1 (en) | 1999-10-27 |
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| RU98113831A RU2140318C1 (en) | 1998-07-14 | 1998-07-14 | Method of removing hydrogen sulfide from gas mixtures |
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Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1904428A1 (en) * | 1969-01-30 | 1970-08-13 | Basf Ag | Aqueous methyldiethanolamine |
| US3941875A (en) * | 1972-04-26 | 1976-03-02 | Nittetu Chemical Engineering Ltd. | Process for treating gas containing hydrogen sulfide |
| US4147212A (en) * | 1978-03-27 | 1979-04-03 | The Sherwin-Williams Co. | Control of hydrogen sulfide gas to reduce toxicity and corrosion due to exposures thereto |
| US4198378A (en) * | 1976-11-12 | 1980-04-15 | Giuseppe Giammarco | Process for removing CO2, H2 S and other gaseous impurities from gaseous mixtures |
| SU814414A1 (en) * | 1979-01-03 | 1981-03-23 | Северо-Кавказский Научно-Исследова-Тельский Институт Природных Газов | Method of cleaning gas from hydrogen sulphide and carbon dioxide |
| US4259301A (en) * | 1979-07-30 | 1981-03-31 | Exxon Research And Engineering Co. | Removal of acidic compounds from gaseous mixtures |
| EP0088485A1 (en) * | 1982-01-18 | 1983-09-14 | Exxon Research And Engineering Company | A process for the removal of hydrogen sulfide from gaseous mixtures with strongly basic tertiary amino compounds |
| US4435371A (en) * | 1982-02-26 | 1984-03-06 | The Goodyear Tire & Rubber Company | Sulfur removal from a gas stream |
| EP0214814A2 (en) * | 1985-08-30 | 1987-03-18 | Exxon Research And Engineering Company | Absorbent composition containing a severely hindered amino compound and an amine salt and process for the absorption of H2S using the same |
| EP0568003A3 (en) * | 1992-04-28 | 1993-12-29 | Phillips Petroleum Co | Absorption of hydrogen sulfide and absorbent composition therefor |
| RU2042402C1 (en) * | 1990-07-02 | 1995-08-27 | Производственный кооператив "Экологически обоснованная химическая технология" | Coke-oven gas processing method |
| GB2287714A (en) * | 1994-03-23 | 1995-09-27 | Us Energy | Removing H2S from a gas stream |
| US5538703A (en) * | 1993-10-29 | 1996-07-23 | Massachusetts Institute Of Technology | Hot gas desulfurization by injection of regenerable sorbents in gasifier-exit ducts |
-
1998
- 1998-07-14 RU RU98113831A patent/RU2140318C1/en active
Patent Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1904428A1 (en) * | 1969-01-30 | 1970-08-13 | Basf Ag | Aqueous methyldiethanolamine |
| US3941875A (en) * | 1972-04-26 | 1976-03-02 | Nittetu Chemical Engineering Ltd. | Process for treating gas containing hydrogen sulfide |
| US4198378A (en) * | 1976-11-12 | 1980-04-15 | Giuseppe Giammarco | Process for removing CO2, H2 S and other gaseous impurities from gaseous mixtures |
| US4147212A (en) * | 1978-03-27 | 1979-04-03 | The Sherwin-Williams Co. | Control of hydrogen sulfide gas to reduce toxicity and corrosion due to exposures thereto |
| SU814414A1 (en) * | 1979-01-03 | 1981-03-23 | Северо-Кавказский Научно-Исследова-Тельский Институт Природных Газов | Method of cleaning gas from hydrogen sulphide and carbon dioxide |
| US4259301A (en) * | 1979-07-30 | 1981-03-31 | Exxon Research And Engineering Co. | Removal of acidic compounds from gaseous mixtures |
| EP0088485A1 (en) * | 1982-01-18 | 1983-09-14 | Exxon Research And Engineering Company | A process for the removal of hydrogen sulfide from gaseous mixtures with strongly basic tertiary amino compounds |
| US4435371A (en) * | 1982-02-26 | 1984-03-06 | The Goodyear Tire & Rubber Company | Sulfur removal from a gas stream |
| EP0214814A2 (en) * | 1985-08-30 | 1987-03-18 | Exxon Research And Engineering Company | Absorbent composition containing a severely hindered amino compound and an amine salt and process for the absorption of H2S using the same |
| RU2042402C1 (en) * | 1990-07-02 | 1995-08-27 | Производственный кооператив "Экологически обоснованная химическая технология" | Coke-oven gas processing method |
| EP0568003A3 (en) * | 1992-04-28 | 1993-12-29 | Phillips Petroleum Co | Absorption of hydrogen sulfide and absorbent composition therefor |
| US5538703A (en) * | 1993-10-29 | 1996-07-23 | Massachusetts Institute Of Technology | Hot gas desulfurization by injection of regenerable sorbents in gasifier-exit ducts |
| GB2287714A (en) * | 1994-03-23 | 1995-09-27 | Us Energy | Removing H2S from a gas stream |
Non-Patent Citations (1)
| Title |
|---|
| W.P. Manning "Chemsweet, a new process for sweetening low-value sour gas", oil and gas Journal, 1979, v.77, N 42, p.122-124. * |
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