Hydrogen sulfide and/or mercaptan decomposition method

FIELD: gas and petroleum processing.

SUBSTANCE: invention relates to methods for decomposing and utilizing hydrogen sulfide and/or mercaptans, which methods can be used for production of hydrogen and sulfur from hydrogen sulfide as well as for purification of gas mixtures polluted by hydrogen sulfide and/or mercaptans. Method comprises passing hydrogen sulfide and/or mercaptan-containing gas at temperature below 200°C through solid catalyst bed placed in liquid capable of dissolving reaction intermediates and/or sulfur arising on catalyst surface to release hydrogen and/or hydrocarbons.

EFFECT: lowered reaction temperature and eliminated need of frequent solid catalyst regeneration.

7 ex

 

The invention relates to the field of gas and oil, and in particular to methods of decomposition and recycling of hydrogen sulfide and mercaptans (thiols), and can be used for the production of hydrogen and sulfur from hydrogen sulfide, as well as for the purification of gas mixtures of hydrogen sulfide and mercaptans.

Hydrogen sulfide is the main byproduct of oil refining, and hydrometallurgy, in large quantities (up to 50%) is contained in the gas-condensate deposits of natural gas is the main product of decomposition of many mineral and organic substances. Simultaneously, the hydrogen sulfide is a strong toxic poison, causing poisoning of living organisms. Therefore, the exhaust gases of industrial plants must be thoroughly cleaned from hydrogen sulfide. At the same time, the hydrogen sulfide can be the feedstock for production of valuable chemical product hydrogen.

Mercaptans are byproducts of the decomposition of mineral and organic substances which are present as impurities in the gaseous oil products in large quantities may be present in gas condensate natural gas fields. Mercaptans are toxic substances with a very unpleasant smell, so exhaust gases of industrial plants must be thoroughly cleaned from mercaptans. At the same time mercaptans are widely used as odorants household gases, where they are used for detection of leakage. The presence of mercaptans in hydrocarbon gases leads to deactivation of the catalysts for the conversion of these gases into valuable products, so these gases should also be thoroughly cleaned from mercaptans.

Direct thermal decomposition of hydrogen sulfide into hydrogen and sulfur by the reaction:

is a highly endothermic process and can be very noticeable speed to occur only at high temperatures. The known method of thermal decomposition of hydrogen sulfide into hydrogen and sulfur, including the transmission of sulfurous gas through the reaction zone at a temperature 850-1600°where the decomposition of H2S to hydrogen and sulfur, and the subsequent cooling of the specified gas to a temperature of 110-150°for condensing the formed sulfur (US 4302434, 01 17/04, 24.11.81).

The disadvantages of this method are: high temperature required to achieve a high degree of decomposition of hydrogen sulfide; high energy consumption on the implementation of the reaction and the possible compensation of heat losses; the possibility of reducing the degree of decomposition of hydrogen sulfide due to the reverse reaction between hydrogen and sulfur cooling gas; the impossibility of application of the method for processing of gases containing hydrocarbons and other impurities that can experience the change pyrolysis at high temperature; the low efficiency of the process by reducing the concentration of hydrogen sulfide in the hydrogen sulfide-containing source gas; the need to use special expensive structural materials with high temperature resistance for the design of high-temperature reaction zone. Besides, the decomposition reaction of hydrogen sulfide at high temperature leads to the formation of gaseous sulfur consisting of saturated molecules S2. The latter circumstance adversely affect thermodynamics of the whole process, because it is known that obtaining less energy efficient products in the condensed (liquid or solid) state conducive to shift the equilibrium of the reaction towards formation of reaction products.

However, the use of catalysts allows you to direct the reaction (1) by a new route, which can substantially lower the temperature of reaction (1).

It is this possibility inherent in the invention (RF 2216506, 01 17/04, 20.11.03), in which the hydrogen sulfide-containing gas is passed through the layer of solid material capable of decomposing hydrogen sulfide by the reaction (1) at temperatures below 200°and regeneration is produced by passing a regenerating gas containing hydrogen sulfide with a temperature no higher than 350°C.

The disadvantage of this method is the necessity to the frequent regeneration of the particulate material, capable of decomposing hydrogen sulfide, as formed according to reaction (1) sulfur accumulates on the surface and blocks the activation centers of hydrogen sulfide.

The closest is a method of decomposition of hydrogen sulfide and/or mercaptans by hydrogenation, and then oxidation (US 4399112, B 01 D 53/36, 16.08.83). The disadvantages are the high temperature process, as well as the fact that hydrogen is lost in the form of water in the oxidation

The invention solves the problem of developing a more effective method of decomposition of the hydrogen sulfide and/or mercaptoundecanoic gas to produce hydrogen.

The task is solved in that the sulfide - and/or mercaptoacetate gas is passed at a temperature below 200°through the layer of solid catalyst, is placed in a liquid, capable of dissolving formed on the surface of the catalyst intermediate reaction products and/or sulfur with the release of hydrogen and/or hydrocarbons.

The method is as follows.

The hydrogen sulfide and/or mercaptoacetate gas with an initial temperature below 200°To pass through a layer of solid material (catalyst), with the ability to dissociatively chemosensitivity hydrogen sulfide and/or mercaptan in this temperature region. When this is coupled chemisorption of hydrogen sulfide and/or mercaptan with the formation of gaseous hydrogen and/erisoodustused hydrocarbon and sulfur-containing intermediate products chemisorption on the surface of the solid catalyst. The solid catalyst is placed in a layer of liquid capable of dissolving formed on the surface of the catalyst intermediate products of reaction (1) and/or sulfur. Therefore, surface decomposition of hydrogen sulfide and/or mercaptan into solution with the formation of either dissolved or colloidal or solid elemental sulfur. Leaving a layer of solid catalyst, the hydrogen-containing gas and/or the corresponding hydrocarbon is directed to the selection or use any other method. As the filling of the catalyst surface hammarbyhamnen sulfur to such a level, when it comes to blocking of active sites dissociative chemisorption of hydrogen sulfide and/or mercaptan, the catalyst is heated to the boiling point of water or lower, but sufficient to remove surface compounds of sulfur. If the solubility of the surface sulfur compounds is not sufficient to reactivate the catalyst, the liquid substance is replaced by another solvent, which is a good solvent for the surface of the sulfur compounds and/or elemental sulfur. Then again, the catalyst was immersed in a layer of source liquid substances and again serves the original gas mixture.

As the liquid substance may be used any of the following classes of substances and/or with the combination of two or more liquid substances in any proportion: non-polar, for example, hydrocarbons, CS2and so on; polar, for example, water, organic and inorganic acids, alkali solutions, olefin, diene, acetylene, naphthenic and aromatic hydrocarbons, solutions of salts of organic and inorganic acids, nitrogen-, oxygen-, chalcogen-, halogen-containing compounds and solutions of their salts, etc. and also solutions of surface-active substances.

The main advantage of the proposed method is the possibility of decomposition of hydrogen sulfide and/or mercaptans at a low temperature, e.g. room, while the formed sulfur is not accumulated on the catalyst surface, and enters the liquid volume, where, depending on the nature of the liquid sulfur can exist in the form of solids, colloid or solute. Thus, freed the surface of the catalyst and the regeneration of the active component.

The invention is illustrated by the following examples.

Example 1. Processing is subjected to natural gas containing 3 vol.% of hydrogen sulfide, and nitrogen, carbon dioxide and water vapor. The specified gas is passed at a temperature of 75°through a layer of granular graphite-like carbon material (US 4978649, From 01 To 31/10, 18.12.90), which is placed in the benzene layer. Leaving a layer of the specified material gas contains hydrogen at stake is entrale to 3%, as well as nitrogen, carbon dioxide and water vapor, hydrogen sulfide is absent. Formed on the surface of the catalyst intermediate compounds dissolved in benzene, resulting in the formation of elemental sulfur, S8. Because sulfur is poorly soluble in benzene, it floats on the surface of liquid benzene and may be removed by known methods.

Example 2. Processing is subjected to a gas containing 5 vol.% of hydrogen sulfide, and nitrogen, oxygen and a mixture of light hydrocarbons. The specified gas is passed at a temperature of 150°through the layer of molybdenum disulfide (MoS2, which is placed in the layer of liquid diesel fuel. Leaving a layer of the specified material gas contains hydrogen in an amount of 5 vol.%, as well as nitrogen, oxygen and a mixture of light hydrocarbons, hydrogen sulfide is absent. Intermediate products of reaction (1) are dissolved in diesel fuel is transferred from the surface of the catalyst in the solution to form elemental sulfur, which is poorly soluble in diesel fuel, so sulfur accumulates on the surface of the liquid diesel fuel.

Example 3. Processing is subjected to natural gas, containing 40 vol.% of hydrogen sulfide. The specified gas is passed at a temperature of 40°through the layer hemosorption-catalytic material is a sulfide of cobalt COxSysupported on silica gel. This hemosol the UNT - the catalyst is placed in a layer of a solution containing 10% diethanolamine in water. Exiting sulfide catalyst natural gas contains up to 40% of the hydrogen sulfide is absent. Surface of the intermediate reactions (1) and the formed elemental sulfur is well dissolved in this solution. When saturated solution of sulfur formed elemental sulfur floats on the surface of the solution and may be removed by known methods.

Example 4. Processing is subjected to gas consisting of a mixture of synthesis gas (CO+H2) and 1 vol.% of hydrogen sulfide. The specified gas is passed at room temperature through a layer of sulfide catalyst composition of COxMoySzdeposited on alumina. This catalyst is placed in a layer of a solution containing 5% of monoethanolamine in water. The output from the layer specified recyclable material gas contains CO and hydrogen, hydrogen sulfide is absent. Exiting sulfide catalyst synthesis gas contains CO and hydrogen, hydrogen sulfide is absent. Surface of the intermediate reactions (1) and the formed elemental sulfur is well dissolved in this solution. When saturated solution of sulfur formed elemental sulfur floats on the surface of the solution and may be removed by known methods.

Example 5. Processing powergallery gas, containing methane, 5% vol. hydrogen sulfide and 0.3 vol.% the mercaptan (methanethiol). The specified gas is passed at room temperature through a layer of sulfide catalyst composition of COxMOySzdeposited on a porous carrier is alumina. This catalyst is placed in a layer of concentrated ammonia. The output from the layer specified recyclable material gas contains methane and hydrogen, hydrogen sulfide and methanethiol are missing. Surface of the intermediate reaction (1) are easily dissolved in this solution, but the resulting sulfur is poorly soluble in the liquid, thus forming elemental sulfur floats on the surface of concentrated ammonia and can be removed by known methods.

Example 6. Processing is subjected to water saturated with hydrogen sulfide. A saturated aqueous solution of hydrogen sulfide is passed through a layer of graphite-like carbon material at a temperature of 20°C. At the outlet of the layer of this material, the sulfide is absent, and in the gas phase hydrogen appears. Since the intermediate reaction (1) poorly soluble in water and practically insoluble elemental sulfur, the sulfur accumulates on the surface of the graphite-like carbon material, so after 40 min of accumulated sulfur begins to block the active surface of the carbon is on the material and at the end there is a sulfide. Therefore, the flow saturated with hydrogen sulfide aqueous solution stop and a layer of graphite-like material is placed in the layer of liquid hydrazine hydrate is added at room temperature. Surface of the intermediate reactions (1) and the formed elemental sulfur is well dissolved in the liquid hydrazinehydrate, so after 5 min hydrazinehydrate merge and begin to re-submit a saturated aqueous solution of hydrogen sulfide. After saturation of the surface of graphite-like material grey it again placed in a layer of hydrazine hydrate is added. Such operations combination hemosorption-catalytic stage with stage reactivation of the catalyst is repeated many times without reducing the capacity of the carbon material.

Example 7. Processing is subjected to ethyl alcohol saturated with ethyl mercaptan (echantillon). Specified liquid solution is passed through a layer of sulfide catalyst (Ni,W)/Al2O3at room temperature. At the output layer of this catalyst ethyl mercaptan is absent in the gas phase appears ethane. Since the solubility of the intermediates of the reaction (1) and sulfur in ethanol is limited, then after 2 h after start of the reaction flow saturated solution of ethyl mercaptan in ethanol stopped and the catalyst are placed in a layer of liquid carbon disulfide CS2. Surface of the intermediate soedineniyami (1) and the formed elemental sulfur is well dissolved in liquid carbon disulfide, so they pass into the solution, releasing the activation centers of ethyl mercaptan. After 10 min the disulphide merge and begin to re-submit ethyl alcohol saturated with ethyl mercaptan. Such operations combination hemosorption-catalytic stage with stage reactivation of the catalyst is repeated many times without reducing the capacity of the catalyst.

As seen from the above examples, the proposed method allows to decompose the hydrogen sulfide and/or mercaptans at a low temperature, for example, at room, while the formed sulfur is not accumulated on the catalyst surface, and enters the liquid volume, where, depending on the nature of the liquid sulfur can exist in the form of solids, colloid or solute. Thus, freed the surface of the catalyst and the regeneration of the active component, i.e. the proposed method does not require frequent reactivation and regeneration of the used catalyst.

The method of decomposition of hydrogen sulfide and/or mercaptans, characterized in that the hydrogen sulfide and/or mercaptoacetate gas is passed at a temperature below 200°through the layer of solid catalyst, is placed in a liquid, capable of dissolving formed on the surface of the catalyst intermediate reaction products and/or sulfur with hydrogen gas and/or using hydrocarbon is.



 

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The invention relates to a device for producing sulfur from gases containing sulfur dioxide or hydrogen sulfide, and can be used for gas processing nonferrous metallurgy, oil and gas industries, and also in the construction of gas-phase reactors in the chemical industry
The invention relates to the field of gas and oil, and in particular to methods of decomposition and recycling of hydrogen sulfide, and can be used for the production of hydrogen and sulfur from hydrogen sulfide, and also for purification from hydrogen sulfide gas mixtures
The invention relates to the field of gas and oil, and in particular to methods of decomposition and recycling of hydrogen sulfide and/or mercaptans, and can be used for the production of hydrogen and sulfur from hydrogen sulfide, and also for purification from hydrogen sulfide and mercaptans gas mixtures

The invention relates to a method of catalytic reduction of sulfur dioxide from a gas mixture containing at least 10 vol.% water, whereby the gas mixture is passed over the surface resistant to sulfur hydrogenation catalyst in sulfide form with a bulk velocity component at least 2000 h-1in the presence of a reducing component, preferably at least partially consisting of hydrogen, with the molar ratio of the reducing component and sulfur dioxide, comprising more than 10 and up to 100 at a temperature of from 125 to 300With, the gas mixture is passed after the specified recovery through dry oxidizing layer for oxidation of sulfur compounds, more specifically hydrogen sulfide, to produce elementary sulfur

The invention relates to the field of chemical technology and can be used for purification of exhaust gases from sulfur compounds, carbon monoxide and organic compounds in the gas, oil refining, chemical and other industries

The invention relates to a process for recovering sulfur from a gas containing hydrogen sulfide, which includes: i) oxidation of part of the hydrogen sulfide in the gas stream of oxygen or oxygen-containing gas phase oxidation to sulfur dioxide; (ii) the interaction of the gas obtained at the stage of oxidation of at least two catalytic stages, in accordance with the Claus reaction; (iii) catalytic reduction of SO2in Gaza, leaving the latter at least two catalytic stages, and catalytic reduction takes place in the catalyst bed, located after the last catalytic stage of the Claus process

The invention relates to the production of elemental sulfur from gases of non-ferrous metallurgy, containing mainly nitrogen and sulfur dioxide, and can be used at the enterprises of chemical, petrochemical, gas processing and metallurgical industry

The invention relates to the field of chemistry, and in particular to methods of decomposition of hydrogen sulfide, and can be used for the production of hydrogen and sulfur from hydrogen sulfide, and also for purification from hydrogen sulfide industrial gas emissions
The invention relates to chemical technology, in particular the acidic hydrogen sulfide gas coking, and can be used in coke, oil and gas industry, ferrous and nonferrous metallurgy

The invention relates to a device for producing sulfur from gases containing sulfur dioxide or hydrogen sulfide, and can be used for gas processing nonferrous metallurgy, oil and gas industries, and also in the construction of gas-phase reactors in the chemical industry

FIELD: gas and petroleum processing.

SUBSTANCE: invention relates to methods for decomposing and utilizing hydrogen sulfide and/or mercaptans, which methods can be used for production of hydrogen and sulfur from hydrogen sulfide as well as for purification of gas mixtures polluted by hydrogen sulfide and/or mercaptans. Method comprises passing hydrogen sulfide and/or mercaptan-containing gas at temperature below 200°C through solid catalyst bed placed in liquid capable of dissolving reaction intermediates and/or sulfur arising on catalyst surface to release hydrogen and/or hydrocarbons.

EFFECT: lowered reaction temperature and eliminated need of frequent solid catalyst regeneration.

7 ex

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