专利摘要:
1356289 Desulphurizing Claus off-gases SHELL INTERNATIONALE RESEARCH MAATSCHAPPIJ NV 15 July 1971 [17 July 1970] 33217/71 Heading C1A Off-gases containing sulphur dioxide from a Claus kiln are passed at a temperature above 175‹ C. together with a gas containing free hydrogen and/or free carbon monoxide over a sulphided Group VI and/or Group VIII metal catalyst supported on an inorganic oxide carrier, the reduced gases being then passed through a liquid and regeneratable absorbent for hydrogen sulphide and the unabsorbed portion, optionally after incineration, is discharged to the atmosphere, the hydrogen sulphide enriched absorbent being regenerated for re-use and the hydrogen sulphide rich gas mixture liberated being passed to a Claus process. Group VI metals specified are molybdenum, tungsten and chromium; Group VIII metals specified are iron, cobalt and nickel. The inorganic oxide carrier may be alumina, silica, magnesia, boron oxide, thoria, zirconia or a mixture of these compounds. The sulphiding may be carried out by use of the Claus off-gases themselves, the preferred temperature being between 300 and 400‹ C. The reducing gas preferably contains at least 20% by volume of free hydrogen or an equivalent amount of hydrogen/carbon monoxide mixture. Should any carbonyl sulphide be formed when carbon monoxide is used as the reducing gas it may be decomposed in known manner by passage over a heated bed of alumina. Amines and substituted amines in aqueous solution are the preferred absorbents, in particular alkali metal salts of dialkyl substituted amino acids (e.g. potassium dimethylamino-acetate) and polyalkanolamines such as di- or tri-ethanolamine and diisopropanolamine. After absorption, the H 2 S enriched absorbent is regenerated by heating and/or stripping, the H 2 S enriched gas mixture being recycled to the Claus plant and the regenerated absorbent re-used. Using high gas velocities at temperatures lower than 40‹ C. the selectivity of the H 2 S/CO 2 ratio is enhanced, CO 2 being usually present in the off-gases when the Claus process is operated using air. Other gases present which may be reduced to hydrogen sulphide by the present process include carbonyl sulphide and carbon disulphide.
公开号:SU751318A3
申请号:SU711683575
申请日:1971-07-15
公开日:1980-07-23
发明作者:Кор Пиет Арие;Оиверкерк Корнелиус
申请人:Шелл Интернэшнл Рисерч Маатсхаппий Н.В. (Фирма);
IPC主号:
专利说明:

sa klaus. In principle, you can extract 98% of sulfur, if you use three layers of catalyst Ij
Due to the ever-increasing demands for air pollution prevention, the described waste treatment of the Claus process cannot be considered completely satisfactory. However, it should be taken into account that during such treatment it is not possible to extract all sulfur from the exhaust gases.
The proposed method allows us to significantly reduce the total sulfur content in the exhaust gases by the Claus process or, more generally, in the exhaust gases by processes similar to the Claus process, as a result of which the yield of extracted sulfur is significantly increased. In particular, this Claus process waste gas treatment method is suitable for the case when, along with hydrogen sulfide, these gases contain a relatively large amount of carbon dioxide.
In accordance with the proposed method, the total sulfur content in the waste of the ESCH Claus process gases is reduced due to the fact that these gasses are passed at a temperature higher together with a gas containing hydrogen or carbon monoxide, or both of these gases over the sulphidized cataphizate. -: metal metals of vi .. and uiii groups, periodic table, or a mixture of sulfided metals of both of these groups, moreover, the substrate is an inorganic oxide carrier as the substrate for this catalyst, and after this treatment the waste ase passed through the liquid and capable of regenerating the hydrogen sulfide absorber, whereas the unabsorbed portion of these exhaust gases discharged (preferably after combustion) to the atmosphere. As for the absorber loaded with hydrogen sulfide, it is regenerated and then used again to absorb hydrogen sulphide, while hydrogen sulphide released during regeneration is again subjected to a Claus process.
The term “Claus process off-gas” is understood to be understood to be gases that have not been absorbed by the last layer of catalyst of a Claus unit. Usually in the implementation of the Claus process, two layers of catalyst are used, although the third layer of the catalyst is used quite often.
In addition to hydrogen sulfide and sulfur dioxide in a ratio of approximately 2: 1, the exhaust gases of this type also contain sulfur, oxygen, and nitrogen, small amounts of inert gases, if the Claus process is carried out using air, and
in addition, water in the form of vapor, carbon dioxide and small amounts of carbon monoxide, carbon dioxide and carbon sulphide. The process can also be used with such waste gases as are emitted during the implementation of the Claus process with insufficient amount of oxygen compared to the stoichiometrically necessary.
After passing through the last catalyst bed and the corresponding condenser to trap free sulfur, the Claus process off-gas typically has a temperature of 130-170 ° C. For a reduction operation with a catalyst from metals of the VJ or VI group (or both of these groups), the exhaust gases must have a higher temperature, and therefore the exhaust gases are first heated to a temperature above 175 ° C. Claus process waste gas temperature. preferably increased to ISO-BSO and even more preferably to 200-300 ° C.
Raising the temperature of the exhaust gases to a temperature above 175 ° C is also important for the reason that these gases contain small amounts of free sulfur in a fog-like state. The undesired fog-like state is eliminated as the temperature rises above the sulfur dew point. It has been found that as a result of increasing the temperature to more than 175 ° C, it is preferable but more than the presence of free sulfur in the gaseous gas does not adversely affect the catalytic effect of the used reduction catalyst.
After heating to a temperature above 175 ° C, the Claus process off-gases together with hydrogen or a mixture of gases containing hydrogen are passed over a catalyst composed of sulfidized metals of group VI or VIII or mixture of sulfided metals of these groups to reduce sulfur dioxide to sulfur dioxide. hydrogen. At the same time, free sulfur is converted to hydrogen sulfide. Reduction catalysts can be catalysts that feed molybdenum, tungsten and (or chromium as Group VI metals. It is desirable that these catalysts also include at least one of the metals from the iron group, such as cobalt, nickel, and / or iron, as group VI11 metals. As an inorganic oxide carrier, one of the oxides or a mixture of two or three oxides, selected from the oxides of such elements as aluminum, silicon, magnesium, boron, thorium, zirconium, can be used. catalyst recovered For use in this method is Ni / Mo / AF, O or Co / Mo / AEjOj. The catalyst, which is a metal of group VI and / or VI, is used in sulfidized form. 1Sulfidation can be carried out in advance using the approach Sulfurising agent, such as a mixture of hydrogen and hydrogen sulfide, containing 10–15% by volume can be sulphided on site using the Claus process off-gases themselves. However, the most suitable sulphidation agent is a mixture consisting of 1: 1: 1 hydrogen, hydrogen sulphide and water, and the temperature suitable for sulphidation is 300-400 ° C. The catalyst, subject to sulphidation, may contain metals of the VI and (or) VII} groups, taken as either an oxide or as an element. The treatment of waste gases with a gas containing hydrogen and (or) carbon monoxide is preferably carried out at 180 -, more preferably at 200-ZOO C. Although the process is carried out mainly at atmospheric pressure, if required, several elevated pressures can be applied. . The volume per velocity (flow rate) of the waste gases of the Vslaus process during the reduction is maintained at 500-10000 l (at normal pressure) per liter of catalyst per hour. As a gas containing water and / or carbon monoxide, it can successfully a gas containing both of these substances is used, for example, domestic gas, water gas, synthesis gas, etc. Pure hydrogen or pure carbon oxides can also be used. Suitable gases or gas containing large amounts of hydrogen may be off-gas from cracking plants for naphtha, gas from plants for producing hydrogen, or gas from a plant for treating saturated crude gas. Hydrogen-containing gas must contain at least 20% by volume of hydrogen IL equivalent amount of hydrogen and (or) carbon monoxide. Hydrogen or Hydrogen-containing gas is used in such an amount that the ratio of hydrogen: di-: sulfur oxide is 3: 1 - 15: 1. The most preferable ratio is 3.5: 1-8: The indicated limits of relationship remain the same when reducing gas mixtures containing both hydrogen and carbon monoxide and only carbon monoxide are used, because carbon monoxide is equivalent to hydrogen. If there is free sulfur in the waste gases from the Claus plant, the required amount of hydrogen and (or) carbon monoxide can be calculated, based on the free sulfur content, as the percentage SOg content. When carbon monoxide is used as a reducing gas, some amount of carbon dioxide is formed. If the presence of carbonyl sulphide in the treated gas is undesirable, it can be decomposed hackily, by passing this gas at elevated temperatures with a layer of alumina. As a liquid and capable of K regeneration absorber of hydrogen sulfide is preferably used an aqueous solution of amine or zhmeshchennogo amine. Absorbers of this type are well known in the art, for example, salts formed by dialkylaminic acids with alkali metals, for example, potassium salt of dimethylaminoacetic acid, and alkanolamines. From alkanolamines one should give preference to polyalkanolamine, such as, for example, diethanolamine, triethanolamine or dipropanolol in. Alkanolamines are preferably used in aqueous solutions with a molar concentration of 0.5-5, and more preferably a molar concentration of 1-3. After absorption (absorption), the absorber enriched with hydrogen sulfide is regenerated by heating and / or desorption, resulting in a mixture of gases with a high content of hydrogen sulfide and a regenerated absorber (absorber .nt), which can be reused. However, since regeneration is never complete, and accumulation of carbon dioxide in the absorber can occur during long-term use, especially if the content of carbon dioxide in the Claus process off-gas is high, these gases after treatment with hydrogen and / or oxide-containing gas carbon, as described, is brought into contact with an aqueous alkanolamine solution at low temperature using high linear gas flow rates. This contact is carried out in an absorption column with twenty or, more preferably, less than 20 contact plates. The purpose of this treatment is to increase the selectivity of the hydrogen sulfide scavenger and thereby reduce the rate of circulation of the solvent. It is most preferable to use absorption columns with 4-15 contact plates. The velocity of the gas stream should be at least 1.5 m / s, preferably 2-4 m / s. The velocity of the gas stream is determined relative to the active; those. blown surface of the plate. The low temperature of the absorber increases the selectivity of the process of separation of hydrogen sulfide and carbon dioxide. The temperature of the scavenger should preferably be lower. The best results are achieved at c. The Claus process off-gas is brought into contact with an alkanolamine aqueous solution at atmospheric or atmospheric pressure. The contacting is preferably carried out in countercurrent. In some cases, the circulation rate of the solution can be further significantly reduced by removing most of the hydrogen sulfide in the column with the contact plates, while the rest is taken in Venturi-type scrubbers, using a relatively small amount of solvent, which may have a different temperature. , different composition and character. Very good results are obtained when using diisopropanolamine as an absorbent. After passing the waste gases04 through the absorption column, their unabsorbed part, which now stitches mainly from nitrogen, carbon dioxide, a very small amount of hydrogen and contains traces of hydrogen sulfide, is released into the atmosphere. If required, this unabsorbed part of the gases can be subjected to combustion in the usual-a1m way before being released into the atmosphere. Gaseous hydrogen sulfide released during regeneration of the absorbent and containing carbon dioxide and water is first cooled to remove water from it by condensation. Typically, at least a portion of this water is sent back to the regeneration site to maintain the amount of water in the aqueous absorber solution at the desired level. After cooling, a gas with a high content of hydrogen sulphide is directed to a Klaus plant to extract free sulfur from the gas. Since the proposed method is designed to treat the Claus process off-gas, the hydrogen sulfide produced during regeneration is best sent back to the same Claus plant. In FIG. Figure 1 shows the basic technological scheme for treating the Claus process off-gas, including its recovery and subsequent absorption of hydrogen sulfide, the regeneration section intended for the regeneration of the absorption of bodies being part of the overall scheme; in fig. 2 shows a modified embodiment of the method in which the regeneration section forms part of the absorption and absorption section located in front of the Claus installation itself, and the absorption of hydrogen sulfide after the recovery of the exhaust gases from the Claus installation takes place with the help of a gas stream withdrawn from this section. By pipeline 1 Sem. FIG. 1) serve the waste of the installation of Claus. These gases have a temperature of 150 ° C, but with the help of heat exchanger 2, their temperature is increased and passed over the reduction catalyst in reactor 3, now they have a temperature of 225 ° C. The hydrogen required for reduction can be supplied to the catalyst bed separately or added directly to the Claus off-gas in the pipeline 1. The exhaust gases leave reactor 3 via line 4 and are cooled in Heat Exchanger 5. The exhaust gases enter the absorption column B at a temperature . This column contains a liquid absorber of hydrogen sulfide, capable of regeneration. If required, a condenser can be installed to remove water that may be in the exhaust gases. The installation site of the condenser is between the heat exchanger 5 and the absorption column 6. The unabsorbed components of the exhaust gases, consisting mainly of carbon dioxide and nitrogen, are discharged through line 7. In order to avoid traces of hydrocarbons and hydrogen sulphide in the gases emitted into the atmosphere, the gas mixture left unabsorbed is heated in a heat exchanger 8 and its combustible components are burned at a temperature of 400 ° C in a furnace 9 for burning before being discharged to the exhaust pipe through a pipeline 10. absorber enriched hydrogen sulfide m, are sent for regeneration via conduit 11 to desorption column 12 equipped with a preheater 13. The regenerated absorber (absorbent) is returned to absorption tower 6 via conduit 14 equipped with a condenser 15, and the released hydrogen sulfide containing relatively small amount of carbon dioxide is fed to the unit Claus through line 16. In desorption column 12, the absorbent is regenerated at elevated temperature by heating with steam supplied to the preheater 13. Since it is regenerated the first absorbent is used at a low temperature. between this absorbent and the absorbent to be regenerated, heat is exchanged in the heat exchanger 17, after which the regenerated absorbent is further cooled in the refrigerator 15 Hydrogen-containing gas entering through the pipeline 16 is cooled in the refrigerator 18 in order to condense all the water vapor entrained in the gas stream and the condensate is returned to the desorption column via line 19. In the combined scheme, a gas stream with a high content of hydrogen sulfide is supplied to the absorption column 20 with an absorbent hydrogen sulphide capable of regeneration via pipeline 21. A gas stream with a low content of hydrogen sulphide is discharged through conduit 22, while absorbent saturated with hydrogen sulphide is supplied via conduit 23 to desorption column 12 for regeneration. Pipelines 23 and 11 (from the absorption column b) are connected at point A and at this point the common pipeline, also designated as 11, leads to columns 12. The regenerated absorbent is discharged through pipeline 14, heat is transferred to exchanger 17 in heat exchanger which should be subjected to regeneration. At point B in the direction opposite to the flow from cooler 15, pipe 14 is split in two, and along the branch part of the regenerated absorbent is withdrawn into the absorption tower where it comes into contact with the recovered Claus off-gases. The main stream is sent back to the absorption column 20 through line 24. Hydrogen sulfide released from the sorbent during regeneration cools down in refrigerator 18 to remove water and is directed to Claus unit 25. The waste gases in this installation are discharged through conduit 1 and then processed as described. The proposed method is especially suitable for the treatment of Claus off-gas, if these gases, in addition to hydrogen sulfide, contain relatively large amounts of carbon dioxide; Containing 1 carbon dioxide in these gases may be higher than 5 vol.%, For example, it may be 8-15 vol.% Without causing any technical difficulties in applying this method, and from an economic point of view the method will remain acceptable. Example. A synthetic gae of the Claus type waste gas type is reduced over a sulfided catalyst consisting of Co / Mo / A 20z (3.2 parts by weight of Co, 13.4 parts by weight of Mo, and 100 parts by weight of AfjOa) a mixture of hydrogen and carbon monoxide is used for reduction. Synthetic flue gas containing sulfur dioxide in different quantities is passed through with a reducing gas with a bulk velocity of 1700 liters (at normal pressure) per hour per liter of catalyst. The whole gas mixture has the following composition, vol.%: Variable amounts 0.5-0.6 0.3-0.4 Else The catalyst is used in the form of particles 0.3-0.6 mm in size (30-50 mesh). The sulphidation of the catalyst is carried out at a maximum temperature and pressure of 10 kg / cm using a mixture of gases consisting of hydrogen and hydrogen sulfide, in which the hydrogen sulfide content is 12.5% by volume. At the same time, the catalyst is heated to the specified temperature in 4 hours, starting from room temperature (in the first hour from 20 to 100 ° C, in the second and third hours from 100 to 250 ° C and in the fourth hour from 250 to 375 ° WITH). After sulphidation, the catalyst is cooled to 100 ° C, and the supply of sulfur-containing, gas-containing mixture of gases is continuous. continue, then only hydrogen is passed through, and finally, gases such as the Claus off-gas are reduced. The experiment was carried out at different temperatures of recovery. The results are shown in table 1. Ta b- persons 1 P and Measures 2. A Claus process flue gas, containing, in addition to sulfur dioxide and hydrogen sulfide, also a small amount of gaseous free sulfur, is reduced by hydrogen using the same sulfided catalyst, namely Co / Mo. / AfgOg, which was used in the experiments described in the example. Gas such as the Claus process off-gas is passed over a specified catalyst / and the volume transmission rate of 1400 liters (at normal pressure) of gas per hour per 1 liter of catalyst. The composition of the gas mixture before and after the reduction is given in Table. 2. The Total Conversion table calculated on the basis of consumed hydrogen. equal to 45%. Froze The Claus process flue gas is reduced using oxide and carbon over the same sulfidir catalysts and mash, namely Co / Mo / APjO, which was used in the two previous examples. The reduction is carried out at a temperature of 230 ° C, and the volumetric flow rate of gases such as the Claus process off-gas, together with carbon monoxide, is maintained at 1700 (at normal pressure) per hour for 1 liter of catalyst. The total gas mixture before the restoration has a composition of ed., About. %: The rest of the conversion, calculated on the basis of consumed carbon monoxide, was 35%. When repeating the same experiment with a volumetric gas transmission rate equal to 900 liters (at normal pressure) of gas per 1 hour per 1 liter of catalyst at the same temperature as in the previous experiment, the conversion was 9-0%. EXAMPLE 4 Claus process off-gas containing a large amount of carbon dioxide is reduced (hydrogen is poured by passing over a sulfided catalyst, which is Co / Mo / AtgO at 220 ° C. The gas mixture obtained after reduction has the following , composition, vol.%: HjS2.5 Gas of this composition is passed at a speed of 2.0 m / s through a column containing 11–12 plates, and a 27% (by weight) aqueous solution of diisopropanolamine circulates in this column. dialkanolamine before it was brought into contact The composition of the treated gas, i.e. the gas after it passed through a solution of diisopropanolamine, and the composition of the gas with a high content of hydrogen sulfide, after this gas was obtained after regeneration of the indicated amine solution is given in Table 3. The treated gas is removed to the incineration furnace, and the gas with a high content of hydrogen sulfide is sent back to the Claus plant, from which the waste gases come. Table 3 As can be seen from the results of the experiment, under the conditions of the proposed method, hydrogen sulfide is absorbed with a high degree of selectivity and in the presence of a large amount of carbon dioxide. Example 5. A mixture of gases containing 2.37% by volume of hydrogen sulphide and 10.38% by volume of carbon dioxide is brought into contact with a two molar aqueous solution of diisopropanolamine in a column with contact plates under different conditions. Conditions, such as temperature, the gas flow rate, the number of plates in the column, and the height of the spray solution on these plates, are changed so as to maintain the hydrogen sulfide concentration in. processed gas is about 0.05% by volume. The results are shown in Table. four. . T a b l and c a 4
Based on the data in this table, it can be concluded that at low temperatures it is advisable to carry out the process at relatively high gas flow rates and apply a relatively large spray height of the solution relative to the columns of the column. This ensures optimal selectivity in the absorption of hydrogen sulfide using relatively small amounts of solution.
权利要求:
Claims (1)
[1]
1. Patent of Great Britain 1138437, C 1 A, published. 1969.
60
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同族专利:
公开号 | 公开日
IE35451L|1972-01-17|
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AU459768B2|1975-04-10|
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CH580982A5|1976-10-29|
IT941574B|1973-03-10|
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引用文献:
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法律状态:
优先权:
申请号 | 申请日 | 专利标题
NLAANVRAGE7010604,A|NL171144B|1970-07-17|1970-07-17|PROCESS FOR REDUCING THE TOTAL SULFUR CONTENT OF CLAUSE GASES.|
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