The method of direct allocation of elemental sulfur from hydrogen sulfide-containing gas and the catalyst for its implementation

 

(57) Abstract:

The invention is intended for purification of exhaust gases from hydrogen sulfide to produce elementary sulfur. Gas containing 10 vol.% hydrogen sulfide and molecular oxygen is passed through the catalyst bed to oxidize hydrogen sulfide at elevated temperatures and space velocities of 3000-15000 h-1. To use a catalyst containing chromium oxide - Cr2O3the copper oxide is CuO and alumina - Al2O3when the content, wt.%: Cr2O3- 10-66, SIO-5-34, Al2O3-0-85. The invention improves the performance of the process of direct separation of sulphur from gases with a high degree of conversion and selectivity for sulfur. 2 s and 5 C.p. f-crystals, 1 table.

The invention relates to the field of chemical technology and can be used for purification of exhaust gases from hydrogen sulfide to produce elementary sulfur or for the production of elemental sulfur, for example, from natural gas companies gas, refining, chemical and other industries.

The number of known methods of desulfurization of gases containing up to 5-10%. of hydrogen sulfide, based on his direct selective ASS="ptx2">

Thus, the known method of purification of oxygen-containing gases from hydrogen sulfide by passing them through a layer of catalyst is activated carbon. At the same time in the catalyst bed at a temperature of 20-250oC and space velocities not exceeding 2000 h-1flows through the reaction of partial oxidation of hydrogen sulfide on the surface of activated carbon deposits of elemental sulfur. Otlogetswe sulfur is removed from the layer by processing it with an aqueous solution of ammonium sulfide at normal temperatures or flow of inert gas at 350-400oC [Klein J., Henning K. "Catalytic oxination of hydrogen sulphide on activated carbons" - Fuel-1984, V. 63, N 8, p. 1064-1067]. Due to the fact that the method is carried out at relatively low space velocities, it is characterized by low output sulphur. In addition, at temperatures above 200oC sharp decrease of the selectivity of the process.

A known method of purification of hydrogen sulfide-containing gases "Celecox", which allows to process the sulfur gas streams containing hydrogen sulphide from 0.01 to 5.00%. when the conversion of up to 95% and the depth of sulfur up to 80%. The method is carried out, passing hydrogen sulfide gas through a bed of the catalyst at space velocities of 3000-6000 h-1and poddles 1-30 wt.%, preferably 5-15 wt.%, printed on non-alkaline refractory oxide of aluminum, titanium, silicon and other [U.S. Patent N 4279882, C 01 B 17/04, 1981]. At temperatures of 230 to 270oC high activity of the catalyst of the process "Celecox" the Claus reaction prevents the achievement of high selectivity in the formation of elemental sulfur in the oxidation of sulfide by oxygen due to leakage reverse Claus reaction, therefore, the method has limitations as regards the purification of gases, and in the performance of sulfur.

The known method flue gas cleaning installations Claus "Superclaus" which was conducted by passing the gas containing up to 1% vol. of hydrogen sulfide, 5% vol. oxygen and 30% vol. water through a bed of the catalyst at temperatures of 200-300oC and space velocities of up to 2000 h-1. Using catalysts composed of a mixture of oxides of trivalent iron and trivalent chromium in the ratio of 4: 1, applied on-alumina [Terorde R. J., Brink, P. J., Visser L. M., Dillen, A. J. "Selective oxidation of hydrogen sulfide to elemental sulfur using iron catalysts on various supports" - Catalysis today. - 1993, V. 17, p. 217-224]. For the described process is characterized by a sharp increase in the conversion of hydrogen sulfide at elevated temperature (for example, in the range of 200-300oC level e level of selectivity decreases from 95% to 75%), therefore, the process has a very narrow range of optimal temperatures 290-300oC, which provide for the satisfactory cleaning gas, which imposes strict limitations on the temperature range of the process. For this reason, this method is ineffective, inefficient at temperatures below 290oC. At temperatures above 290oC method cannot be applied for processing of natural gas, due to strong ekzotermicheskie oxidation process and the occurrence of overheating in the catalyst layer, leading to a further decrease in the selectivity for sulfur and undesirable oxidation of hydrocarbons (concomitant oxidation of hydrocarbons begins at temperatures of 320oC).

There is also known a method of desulfurization of natural gas by direct partial oxidation of hydrogen sulfide in the presence of iron-chromium-zinc oxide catalyst spinel structure containing (in wt.%): 30-60 Cr2O3, 20-40 Fe2O3, 15-30 ZnO. The method is carried out in the temperature range 250-300oC at space velocities of 3000-15000 h-1[Patent Germany, 3390486 B 01 D 53/46, C 01 B 17/04, 1987]. The described method and catalyst for its implementation adopted by the greatest number similar to disposabe direct allocation of sulfur from hydrogen sulfide-containing gases and catalyst for its implementation.

The disadvantages of the prototype are reduced activity and selectivity of the catalyst with increasing temperature. For example, if 250oC the activity of the catalyst is 94% and the selectivity was 91%, at 275oC activity - 93%, a selectivity of 90% and at 300oC activity - 90%, a selectivity of 87%. Therefore, the process is carried out in a narrow temperature range 250-300oC, i.e. under conditions when the probability of a significant temperature rise in the catalyst bed due to the heat of reaction, which leads to lower selectivity for sulfur and undesirable oxidation of hydrocarbons. At lower temperatures for a method of low productivity.

The invention solves the problem of increasing the productivity of the process of direct allocation of sulfur from hydrogen sulfide-containing gases in a wide range of temperatures, namely at 120-300oC, with a consistently high level of hydrogen sulfide conversion and selectivity.

The task is solved in that the separation of elemental sulfur from hydrogen sulfide-containing gas is carried out, passing the treated gas containing not more than 10% about. hydrogen sulfide and molecular oxygen with respect to their bulk concentrations in the range of 0.5-4,utilizator 120-300oC. using the catalyst composition, wt.%:

Cr2O3- 10-66, CuO - 5 - 34, Al2O3- 0 - 85

The method is as follows. Hydrogen sulfide, for example, natural gas is mixed with air or oxygen so that the resulting gas mixture is called here the treated gas contains about 10% about. of hydrogen sulfide. At the same time maintain the ratio of the volume of hydrogen sulfide concentrations to bulk concentrations of oxygen in the range of 0.5 to 4.0. Then the processed gas is sent to the catalytic reactor and at a flow rate of 3000 - 15000 h-1passed through the catalyst bed supporting therein the temperature of 120-300oC. the temperature in the catalyst bed supported by well-known methods. So, with the lack of heat in the treated gas add fuel, or heat, or it, or a layer of catalyst. The excess heat away, for example, by heat exchange with the coolant. It is expedient if the oxygen content in the treated gas with respect to the hydrogen sulfide is greater than 1 (O2/H2S > 1) to maintain the temperature in the catalyst bed 120-200oC. under these conditions provides a high proizvoditelnosti temperature and bulk velocity. Stable activity and selectivity under these conditions has a catalyst containing chromium oxide, copper and aluminum, wt.%: Cr2O3- 10 - 66, CuO - 5 - 34, Al2O3- 0 - 85.

The catalyst not containing aluminum oxide, is prepared as follows: reactive copper bichromate (CuCr2O72H2O) or a mixture of powders of chromium trioxide CrO3and basic salts of carbonate of copper (Cu(OH)2CuCO3) calcined in air flow at a temperature of 600-700oC for 6 hours To give strength to the catalyst in its composition along with the oxides of chromium and copper enter the aluminum oxide to 85 wt.%. In this case, it is prepared as follows.

Impregnating the method of preparation of catalyst

Prepare a water solution of bichromate of copper (CuCr2O72H2O) or dissolved in water jet bichromate, or by dissolving in water chromic anhydride CrO3and subsequent neutralization of the salt solution of the basic carbonate carbonate copper (Cu(OH)2CuCO3). Media - Al2O3pour a solution of bichromate of copper and incubated at room temperature for 2-5 h, the excess solution is sucked off under vacuum. The sample is dried at room temperature for 12-36 h, PI of bichromate of copper contains per individual anhydrous oxides (wt.%): 5-14 CuO, 10-26 Cr2O3that leads to their content in the finished catalyst in the inventive range.

The preparation of the catalyst by the method of mixing

The alumina powder is mixed with aluminum hydroxide pseudoboehmite patterns humidity 755% within 30-60 minutes, add the powder chromic anhydride and stirred for another 10-30 minutes, add the powder basic salts of carbonate of copper (Cu(OH)2CuCO3) and stirred for 30-60 min, after which the mass is formed into an extrusion method and obtain granules with a diameter of 3-5 mm or rings (outer diameter 8-25 mm, inner diameter 4-18 mm), dried at a temperature of 20-110oC for 4-24 h and calcined at a temperature of 600-700oC for 6 h to obtain the finished catalyst. Weight for molding includes a calculating individual anhydrous oxides, wt.%: 10-14 CuO, 20-26 Cr2O3the rest of the Al2O3that leads to their content in the finished catalyst in the inventive range.

This catalyst is sufficiently stably throughout the specified temperature range, providing high activity and selectivity. Thus a positive contribution to his work makes him spinel structure.

To reduce hydraulic sasiga.

The reaction of sulfur oxidation of hydrogen sulfide with oxygen was carried out in flow-through mode with a fixed bed of catalyst at atmospheric pressure the catalyst fraction 0.4-0.8 mm and 3-5 mm, at temperatures 120-300oC, flow rate 3000-15000 h-1composition of the initial gas mixture (% vol.): 0.5 - 6.0 H2S, 0.5-10.0 O2, 12 C3H8N2to balance the ratios of O2/H2S, 0.5-4.0, varying the composition of the initial gas mixture, bulk velocity and temperature. The composition of the initial and final gas mixture is analyzed chromatographically.

The effectiveness of the present invention estimate the quantities of hydrogen sulfide conversion, selectivity and productivity of sulfur. The productivity value of sulfur, which is an indicator of the effectiveness of the process in terms of condensation of sulfur (at temperatures below 200oC) calculate the amount of sulfur deposited on the catalyst surface before the time of breakthrough, referred to unit mass of catalyst. The breakthrough time is determined at the degree of conversion of hydrogen sulphide into sulphur equal to 90%.

Specific conditions for the solution values of hydrogen sulfide conversion, selectivity and productivity sulphur pre C3H8rest N2heated to 120oC, is passed through the catalyst bed with a bulk velocity of 3000 h-1when the ratio of O2/H2S = 0.5.

The catalyst fraction 0.4-0.8 mm composition (wt.%): 34 CuO + 66 Cr2O3prepared from reactive bichromate of copper by calcination in air flow at 600oC for 6 hours Mechanical crushing strength along - 2.0 MPa.

Indicators of the efficiency of the method:

selectivity for the sulfur - 100%,

the performance of sulfur - 210 g sulfur/kg of catalyst.

Example 2. Characteristics of the method according to example 1.

The catalyst fraction 0.4-0.8 mm composition (wt.%): 5 CuO + 10 Cr2O3+ 85 Al2O3were prepared by impregnation of the carrier - Al2O3in the form of Raschig rings (dimensions, mm: length 14, inner diameter 6, the outer diameter of 14) aqueous solution of bichromate of copper concentration of 40 wt.% for 3 h at room temperature and then suction the excess solution under vacuum, drying in air at room temperature for 24 h, then at 110oC for 8 h and calcination in air flow at 700oC for 6 hours Mechanical crushing strength along - 3.4 MPa.

the e - 240 g of sulphur per kilogram of catalyst.

Example 3. Characteristics of the method according to example 1.

The catalyst fraction 0.4-0.8 mm composition (wt.%): 14 CuO + 26 Cr2O3+ 60 Al2O3were prepared by mixing 275 g of aluminum hydroxide and 165 g of alumina powder for 30 min, followed by addition of 45 g of chromic anhydride with stirring for 10-15 min and the addition of 60 g of malachite (Cu(OH)2CuCO3) and stirring 45 min, the molded mass by extrusion in the form of Raschig rings and calcination in air flow at 600oC for 6 hours Mechanical crushing strength along - 3.4 MPa.

Indicators of the efficiency of the method:

selectivity for the sulfur - 100%,

the performance of sulfur - 240 g sulfur/kg of catalyst.

Example 4. Gas mixture composition (% vol.): 6 H2S 3 O2, 12 C3H8rest N2heated to 120oC, is passed through the catalyst bed with a bulk velocity of 3000 h-1when the ratio of O2/H2S = 0.5.

The catalyst of example 1 were prepared by calcination in a stream of air at a temperature of 600-700oC for 6 h in a mixture of 41 g of a powder of chromium trioxide (CrO3) and 53 g of powder basic salts of carbonate of copper (Cu(OH)2CuCO3
the performance of sulfur - 215 g sulfur/kg of catalyst.

Example 5. Gas mixture composition (% vol.): 2 H2S, 2 O2, 12 C3H8rest N2heated to 120oC, is passed through the catalyst bed with a bulk velocity of 3000 h-1when the ratio of O2/H2S = 1.0.

The catalyst according to example 4.

Indicators of the efficiency of the method:

selectivity for the sulfur - 100%,

the performance of sulfur - 209 g sulfur/kg of catalyst.

Example 6. Characteristic of the method according to example 4.

The catalyst according to example 3.

Indicators of the efficiency of the method:

selectivity for the sulfur - 100%,

the performance of sulfur - 240 g sulfur/kg of catalyst.

Example 7. Gas mixture composition (% vol.): 6 H2S, 6 O2, 12 C3H8rest N2heated to 120oC, is passed through the catalyst bed with a bulk velocity of 3000 h-1when the ratio of O2/H2S = 1.0.

The catalyst according to example 3.

Indicators of the efficiency of the method:

selectivity for the sulfur - 100%,

the performance of sulfur - 106 g sulfur/kg of catalyst.

Example 8. Gas mixture composition (% vol.): 2 H2S, 8 O2-1when the ratio of O2/H2S = 4.0.

The catalyst according to example 3.

Indicators of the efficiency of the method:

selectivity for the sulfur - 100%,

the performance of sulfur - 543 g sulfur/kg of catalyst.

Example 9. Gas mixture composition (% vol.): 6 H2S, 3.6 O2, 12 C3H8rest N2heated to 300oC, is passed through the catalyst bed with a bulk velocity of 6000 h-1when the ratio of O2/H2S = 0.6.

The catalyst of example 1.

Indicators of the efficiency of the method:

the conversion of hydrogen sulfide - 98.5%,

selectivity for the sulfur - 94.7%.

Example 10. Characteristics of the method according to example 12.

The catalyst according to example 2.

Indicators of the efficiency of the method:

the conversion of hydrogen sulfide to 100%,

selectivity for the sulfur - 93.9 per cent.

Example 11. Gas mixture composition (% vol.): 0.5 H2S, 1 O2, 12 C3H8rest N2heated to 200oC, is passed through the catalyst bed with a bulk velocity of 3000 h-1when the ratio of O2/H2S = 2.0.

The catalyst according to example 3.

Indicators of the efficiency of the method:

the conversion of hydrogen sulfide to 100%

selection the steel N2heated to 200oC, is passed through the catalyst bed with a bulk velocity of 3000 h-1when the ratio of O2/H2S = 0.6.

The catalyst according to example 3.

Indicators of the efficiency of the method:

the conversion of hydrogen sulfide to 100%,

selectivity for the sulfur - 100%.

Example 13. Gas mixture composition (% vol.): 2 H2S, 1.2 O2, 12 C3H8rest N2heated to 300oC, is passed through the catalyst bed with a bulk velocity of 3000 h-1when the ratio of O2/H2S = 0.6.

The catalyst according to example 3.

Indicators of the efficiency of the method:

the conversion of hydrogen sulfide to 100%,

selectivity for the sulfur - 82.0%.

Example 14. Gas mixture composition (% vol.): 2 H2S, 1.4 O2, 12 C3H8rest N2heated to 200oC, is passed through the catalyst bed with a bulk velocity of 6000 h-1when the ratio of O2/H2S = 0.7.

The catalyst according to example 3.

Indicators of the efficiency of the method:

the conversion of hydrogen sulfide to 100%,

selectivity for the sulfur - 100%.

Example 15. Gas mixture composition (% vol.): 2 H2S, 1.4 O2, 12 C3H8rest N2heated to 300 = 0.7.

The catalyst according to example 3.

Indicators of the efficiency of the method:

the conversion of hydrogen sulfide to 100%,

selectivity for the sulfur - 78.3%.

Example 16. Characteristics of the method according to example 19.

The catalyst fractions 3-5 m in example 3.

Indicators of the efficiency of the method:

the conversion of hydrogen sulfide to 100%,

selectivity for the sulfur - 100%

Example 17. Characteristics of the method according to example 20.

The catalyst fractions 3-5 mm in example 3.

Indicators of the efficiency of the method:

the conversion of hydrogen sulfide to 100%,

selectivity for the sulfur - 85.1%.

Example 18. Gas mixture composition (% vol.): 2 H2S, 1.4 O2, 12 C3H8rest N2heated to 200oC, is passed through the catalyst bed with a bulk velocity of 10,000 h-1when the ratio of O2/H2S = 0.7

The catalyst according to example 3.

Indicators of the efficiency of the method:

the conversion of hydrogen sulfide to 100%,

selectivity for the sulfur - 99.1%.

Example 19. Gas mixture composition (% vol.): 2 H2S, 1.4 O2, 12 C3H8rest N2heated to 300oC, is passed through the catalyst bed with a bulk velocity of 10,000 h-1when sootnosheniya hydrogen sulphide 100%,

selectivity for the sulfur - 84,0%.

Example 20. Gas mixture composition (% vol.): 2 H2S, 12 O2, 12 C3H8rest N2heated to 300oC, is passed through the catalyst bed with a bulk velocity of 10,000 h-1when the ratio of O2/H2S = 1.0.

The catalyst according to example 3.

Indicators of the efficiency of the method:

the conversion of hydrogen sulfide to 100%,

selectivity for the sulfur - 81.8%.

Example 21. Gas mixture composition (% vol.): 6 H2S, 4 O2, 12 C3H8rest N2heated to 200oC, is passed through the catalyst bed with a bulk velocity of 3000 h-1when the ratio of O2/H2S = 0.7

The catalyst according to example 3.

Indicators of the efficiency of the method:

the conversion of hydrogen sulfide to 100%,

selectivity for the sulfur - 95.9%.

Example 22. Gas mixture composition (% vol.): 6 H2S, 4 O2, 12 C3H8rest N2heated to 300oC, is passed through the catalyst bed with a bulk velocity of 3000 h-1when the ratio of O2/H2S = 0.7

The catalyst according to example 3.

Indicators of the efficiency of the method:

the conversion of hydrogen sulfide to 100%,

selectivity for the sulfur - 72.8% of the thuja 300oC, is passed through the catalyst bed with a bulk velocity of 6000 h-1when the ratio of O2/H2S = 0.7

The catalyst according to example 3.

Indicators of the efficiency of the method:

the conversion of hydrogen sulfide to 100%,

selectivity for the sulfur - 87.0%.

Example 24. Gas mixture composition (% vol.): 6 H2S 3 O2, 12 C3H8rest N2heated to 200oC, is passed through the catalyst bed with a bulk velocity of 10,000 h-1when the ratio of O2/H2S = 0.5

The catalyst according to example 3.

Indicators of the efficiency of the method:

the conversion of hydrogen sulfide to 74.5%,

selectivity for the sulfur - 100%.

Example 25. Gas mixture composition (% vol.): 6 H2S 3 O2, 6.0 C2H6, 6.0 C3H8rest N2heated to 300oC, is passed through the catalyst bed with a bulk velocity of 10,000 h-1when the ratio of O2/H2S = 0.5

The catalyst according to example 3.

Indicators of the efficiency of the method:

the conversion of hydrogen sulfide - 98.2%,

selectivity for the sulfur - 99.0%

For comparison with the invention of the prototype examples 26-32

Example 26. Characteristics of the method according to example 5.

The catalyst from the simple efficiency of the method:

selectivity for the sulfur - 100%,

the performance of sulfur - 105 g sulfur/kg of catalyst.

Example 27. Characteristics of the method according to example 6.

The catalyst according to example 26.

Indicators of the efficiency of the method:

selectivity for the sulfur - 100%,

the performance of sulfur - 112 g sulfur/kg of catalyst

Example 28. Characteristics of the method according to example 8.

The catalyst according to example 26.

Indicators of the efficiency of the method:

selectivity for the sulfur - 100%,

the conversion of hydrogen sulphide does not exceed 71%.

Example 29. Characteristics of the method according to example 15.

The catalyst according to example 26.

Indicators of the efficiency of the method:

the conversion of hydrogen sulfide - 68.0%,

selectivity for the sulfur - 93.1%.

Example 30. Characteristics of the method according to example 16.

The catalyst according to example 26.

Indicators of the efficiency of the method:

the conversion of hydrogen sulfide - 90.0%,

selectivity for the sulfur - 86.9%.

Example 31. Gas mixture composition (% vol.): 6 H2S, 4 O2, 12 C3H8rest N2heated to 200oC, is passed through the catalyst bed with a bulk velocity of 3000 h-1when the ratio of O2/H2S hydrogen - 13%,

selectivity for the sulfur - 100%.

Example 32. Gas mixture composition (% vol.): 6 H2S, 4 O2, 12 C3H8rest N2heated to 300oC, is passed through the catalyst bed with a bulk velocity of 3000 h-1 with a ratio of O2/H2S = 0.7

The catalyst according to example 26.

Indicators of the efficiency of the method:

the conversion of hydrogen sulfide - 84.6%,

selectivity for the sulfur - 80.0%.

Initial conditions and results of experiments are summarized in table.

Thus, as can be seen from the examples, the proposed method and the catalyst in order to improve productivity of the process of direct allocation of sulfur from hydrogen sulfide-containing gases in a wide range of temperatures with a consistently high degree of conversion and selectivity and can be widely used in gas, oil refining, chemical industries.

1. The method of direct separation of sulphur from gases containing up to 10% vol. of hydrogen sulfide, comprising passing the treated gas containing hydrogen and molecular oxygen through a bed of catalyst for the oxidation of hydrogen sulfide containing chromium oxide, at elevated temperatures and volumetric skorov> - 10 - 66, CuO - 5 - 34, Al2O3- 0 - 85.

2. The method according to p. 1, characterized in that the ratio of the volume concentrations of molecular oxygen volumetric concentration of hydrogen sulfide is 0.5 to 4.0.

3. The method according to PP.1 and 2, characterized in that the process is carried out at 120 - 300oC.

4. The method according to PP.1 to 3, characterized in that when the oxygen content in the treated gas with respect to the hydrogen sulfide content of more than 1 (O2/H2S > 1) the process is carried out at 120 - 200oC.

5. The catalyst for implementing the method of direct separation of sulphur from gases containing up to 10% vol. of hydrogen sulfide, comprising chromium oxide, characterized in that it additionally contains copper oxide CuO and aluminum oxide Al2O3when the content, wt. %: Cr2O3- 10 - 66, CuO - 5 - 34, Al2O3- 0 - 85.

6. The catalyst p. 5, characterized in that it has a spinel structure.

7. The catalyst PP.5 and 6, characterized in that it is made in the form of Raschig rings.

 

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