• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    1. METHOD OF CONSIDERATION OF CRACKING-GASOLINE by contacting a mixture of cracking gasoline and hydrogen containing gas with a catalyst containing metals of the V1B and VIII groups of the Periodic Table of the elements, their oxides, sulfides or mixtures of the listed ingredients on an inorganic oxide carrier containing aluminum oxide at 232 , 2-398 ,, pressure 5.25-42 kg / cm, the ratio of hydrogen - raw materials 36-890 nm of hydrogen per 1 m of weight and the weight feed rate of the raw material is 1-15 hours, about the fact that, with povieni selectivity and simplification of the process technology, Calcium catalyst is used, the carrier of which contains 70-90 wt.% of magnesium oxide.
    公开号:SU1151216A3
    申请号:SU772459305
    申请日:1977-03-04
    公开日:1985-04-15
    发明作者:Джеймс Бертоласини Ральф；Арлингтон Сью-Эй-Кван Тревелайан
    申请人:Стандарт Ойл Компани (Фирма)；
    IPC主号:
    专利说明:

    2. A method according to claim 1, wherein the process is carried out in the vapor phase.
    3. The method according to claim 1, about tl and h and i and the fact that use of catalysts containing ingredient VIB. Groups in an amount corresponding to 10-20 wt.% Metal oxide
    in the catalyst and ingredient VIII
    groups in an amount corresponding to 1-10 wt. metal oxide in the catalyst. 4. The method according to PP. 1-3, of tl ich and y. and using a catalyst containing molybdenum and cobalt as ingredients of VIB and VIII groups, respectively.
    The invention relates to the field of oil refining industry and solves the problem of desulfurizing cracked gasolines, which include gasolines of such secondary refining processes as catalytically cracking and coking. One of the basic components used to produce gasoline is cracking gasolines. Cracking benzines contain sulfur and olefins. Sulfur, which may be present in amounts of the order of 0.3 wt.% And higher, is a potential air pollutant, as well as toxic or toxic material for catalysts, which are used in a catalytic silencer in the exhaust system of an automobile motor. Olefins (the content of fe cracked gasoline is 30% by weight and higher) have octane numbers higher than the octane numbers of the corresponding hardened compounds. Sulfur dioxide, which is absorbed during the combustion of high-sulfur fuels, is the main substance polluting the air, therefore the sulfur concentration in the components of gasoline and, therefore, in cracking gasolines should be reduced. Methods are known for desulfurizing olefin-containing gasoline by contacting gasoline and hydrogen with a catalyst containing silicon, aluminum or magnesium oxides, as well as metal VA, VIB and VIII groups of the Periodic System of Elements. The basis of the carrier of this catalyst is silica fij and 2J, However, to implement the known methods, specific conditions are necessary: pressure 1.4-7 kg / cm and temperature-415-470 ° C; if it is necessary to remove thiophenic sulfur, an even higher temperature is required - 470-525 ° С {2. These methods are carried out with a small load on the raw materials. There is also known a method for the desulfurization of cracked gasolines, in accordance with which the cleaning process is carried out under normal hydrotreating conditions; 232.2-398.9 ° С, total pressure 5.2542. kg / cm, the ratio of hydrogen raw materials 36-890 nm of hydrogen / m of raw materials and weight feed rate of raw materials 1-15 weight units. raw materials per hour per weight unit of catalyst. A feature of this process is recycling a portion of the purified product to the reaction zone to maintain a low concentration of olefins in the reaction zone h. The catalyst used may contain metals of the VIB and VIH groups of the Periodic Table of Elements: it may or may not contain various kinds of stabilizers, promoters or carriers, such as oxides of aluminum, magnesium, silicon, zinc, chromium and t, n. The disadvantages of this method are complicated technology. process: it is envisaged to separate the heavy product from the reactant stream and recycle it to the reaction zone, as well as the selectivity of the process is not high enough. The goal is achieved by haem, that according to the method of desulfurization of cracking gasolines by contacting a mixture of cracked gasolines and a three-stage hydrogen-containing gas with a catalyst containing metals of the VIB and VIT.I groups of the Periodic System of Elements, their oxides, sulfides or mixtures of these ingredients on an inorganic oxide carrier, containing alumina, at 232.2-398.9 ° C, pressure of 5.25-42 kg / cm, hydrogen-raw material ratio of 36-890 nm of hydrogen per 1 m of raw material and weight feed rate of the raw material of 1-15 h, use a catalyst whose carrier contains 70-90 wt .% magnesium oxide. Preferably, the process is carried out in the vapor phase. Preferably, a catalyst is used containing an ingredient of Group VIB in an amount corresponding to 10-20% by weight of metal oxide in the catalyst, and an ingredient of Group VIII in an amount corresponding to 1-10% by weight of metal oxide in the catalyst. Preferred ingredients of the VIB and VIII groups are molybdenum and cobalt, respectively. The solid support for the catalytic composition contains magnesia. Such a carrier may be exclusively magnesium oxide, it may also include a refractory inorganic oxide selected from the group consisting of catalytically active alumina, mixed silica and alumina. The catalytically active alumina oxide can be y-alumina, D-alumina or mixtures thereof. Such alumina oxide usually has an average pore size above 70 A and can reach 200 A or more. In addition, suitable catalytically active alumina have a surface area of at least 150 and this value can reach 800 or more. The mixture of silica and alumina, which may be used as a refractory inorganic oxide, may be a mixture with a low content of alumina (5-15 wt.%) Or with a low content of alumina (15-40 wt.% ). In the case when the carrier includes alumina in addition to magnesium oxide, the catalytic carrier must contain at least 16L 70 weight.7, magnesium oxide based on the weight of the carrier. The catalytic composition used in the implementation of the proposed method can be obtained by impregnating magnesia with compounds that decompose under the action of heat, which was 1bt hydrogenation metal compounds. As a rule, the carrier is impregnated with a solution containing both metals, or with a solution containing one of the metals, and then with a solution containing the other metal. In the case when the carrier is a combination or a mixture of magnesium oxide and a refractory inorganic oxide, it can be obtained using conventional methods for producing supports for catalysts containing one or more components, and then impregnated with the desired solution or solutions. The impregnated carrier is dried in air at 121 ° C for 1-20 hours, the dried material is burned at 371-593 ° C, preferably 426.7537, 8 ° C, for 1.5-10 hours. Air speed during drying and calcining 0.042 m / h (a different rate can be used). A mixture of powdered magnesium oxide, aqueous solutions of hydrogenation metal compounds and colloidal alumina can be obtained by simple mixing. The resulting mixture is dried, crushed, granularit to the appropriate size and calcined. The conditions described above may be used. The calcination can be carried out in the manner described or by calcining the granules for at least 1-2 hours at 232 ° C (450 ° F), gradually increasing the temperature to 537.8-593 ° C (10001100 ° F) and maintaining such a high temperature. during few hours. Preferred process conditions: temperature 232-399C, total pressure 10.5-28 kg / cm, weight feed rate 3-10. To successfully maintain selectivity, the conditions of the process should be adjusted so that the reaction takes place in the vapor phase. In addition, the partial pressure, hydrogen should be at least 4.2 kg / cm, preferably at least 5.6 kg / s. Typical raw materials that can be used in the proposed method include catalytic cracking and coking gasoline. Such feedstock contains not only paraffins, naphthenes, and aromatics, but also non-saturated compounds, such as acyclic and cyclic olefins, diolefins, as well as cyclic hydrocarbons with olefinic side chains. Such a filter usually has a boiling point of 48.9 ° 0-204 ° C and may have a maximum boiling point. Cracked gasolines usually contain 0.3-0.4 wt.% Sulfur and up to 20-80 ppm of nitrogen. Coking gas may contain up to 1 wt.% Sulfur and up to 100 ppm of nitrogen. FIG. 1 shows a scheme for carrying out the proposed method in FIG. 2 - the change in L octane number with the change in the percentage of desalting. Heavy stabilized cracked gasoline from source 1 is fed through line 2 to the inlet of pump 3 and further through line 4 to mix with reforming gas that enters via line 5 Hydrogen-hydrogen mixture is fed through heat exchanger 6 through line 7 to reactor 8. Reactor 8 contains one or more layers of catalytic compression. An external heat source is required to start the reaction. Since olefins are hydrogenated to some extent, the temperature in the reactor increases from 24 ° to 37.8 ° C. Such an occurrence requires the presence of special control equipment for rapid cooling with hydrogen in order to avoid uncontrolled temperature. If necessary, a hydrogen cooling agent can be obtained on lines 9 and 10.: Products from reactor 8 are fed through line to heat exchanger 6, then through line 12 to condenser 13 and line 14 to stripper column 15 to remove hydrogen sulfide. Stripping is possible with the help of reformin gas fed through line 16. The liquid product from the oTnapHoit column 15 is withdrawn through line 17, sent to condenser 18 and removed through line 19 from the system. The product withdrawn from the stripping column in line 20 contains 0.2-2 mol% hydrogen sulphide. It is directed to the condenser 21, then via line 22 to the compressor 23 to be recompressed. The recompressed gas is withdrawn via line 24. Example 1. Preparation of catalyst A. 164 g of powdered MgO are impregnated; 150 ml of solution is prepared which is prepared by dissolving 36.3 g of ammonium molybdate in 100 ml of hot (about 71 ° C) distilled water and 23.3 g of cobalt nitrate in 50 ml of distilled water, followed by mixing these solutions. The impregnated material is dried in air at 121 ° C for 3 hours, granulated into granules with a size of 0.32 cm and calcined for 3 hours at 537.8 ° C. During the drying and roasting of this substance the flow rate is 0.042 m / h. This catalyst (A) contains 3.1% by weight of cobalt oxide and 16.1% by weight of 7, molybdenum trioxide based on the weight of the catalytic composition. And pm. M p. 2. Use of catalyst A. Cracked gasoline is used as raw material (raw material No. 1). The test was carried out in a battery test facility containing a reactor with an inner diameter of 1.6 cm. This reactor was immersed in a molten salt. Every day, a sample of the product collected in 2 hours and cool is taken from the condenser and cool and dry with ice-acetone. The product is then washed with a solution of cadmium sulfate to remove hydrogen sulfide, analyzed for sulfur content, and the bromine number is determined (the change in bromine number is used as a measure of the saturation of the olefin). In addition, the octane number of the product is periodically measured. 13.1 g of Catalyst A in the form of particles passing through a 12-mesh sieve, but retained in a 20-mesh sieve, is loaded into the reactor. A sample of the catalyst is pre-sulfided with a mixture of 8% vol. hydrogen sulfide in hydrogen. Such sulphidation is carried out for 1 hour at atmospheric pressure, 29 ° C and a gas flow rate of 0.028. The properties of the raw materials are presented in table. 1i Table 48.6 49 Density, API Sulfur content, 0.27 0, wt.% Bromine number, sg / g 51 74 54 76 Nitrogen, ppm Octane number motor fuel without tetraethylvin77, 6 80 tsa Research without 89.3 93 tetraztils lead
    Table 2 of the 33rd day of testing this ratio is increased from 84 to 103 and maintained at this value, and then reduced to 84 ni / m and maintained until the 41st day of the test. First, the catalyst is deactivated at a hydrogen-feed ratio of 89 nor / m ( this is reflected in the increase in sulfur concentration in the product). On the 27th day of testing, when it is. a ratio of up to 103 nn / m, the concentration of sulfur in the product is balanced. By lowering this ratio to 84, the sulfur concentration in the product increases dramatically. Increasing this ratio to 350 leads to a sharp decrease in the sulfur concentration in the product. As the hydrogen ratio of the feedstock drops to 175, the sulfur concentration in the product slightly increases, but there is no perceptible deactivation of the catalyst from the 59th to the 90th day of testing. The average initial desaturation value obtained in the presence of Alizer A over 8 days of testing is 83.1% weight, whereas media: saturation of olefins - 36.5%. Individual saturation values
    In tab. 3 shows the results obtained in experiment I,
    If the octane number of the product is lower than the octane number of the raw material, then the value of the octane number is preceded by a minus sign; if the octane number is incomplete evaporation. Example 3 A permeated hydrodesulfurization catalyst (HDS-2A) containing about 3 wt.% GoO and 15 wt.% MoOj is used. This catalyst consists of metals supported on a refractory inorganic oxide support of alumina (catalyst B).
    product is higher than the value of the octane number of raw materials. Then before the value of A octane number is a plus sign. The data of experiment I, presented in table. 3, obtained for the samples, when, apparently, the reagents and products were completely evaporated, I
    Table 3 Catalyst B is tested according to the method described for Catalyst A. As a result, gasolines are obtained that are much more serious than in the presence of Catalyst A, which indicates a worse desulfurization rate. For the first 8 days of testing, the average desulfurization value was 66.2 wt.%, With an olefin saturation equal to 26.5 wt.% (See Table 4). In addition, additional data are presented in Table. 3 (experiment II). Test II 85.2 71.5, Average value Example 4. Another part of the catalyst A is tested in equipment similar to that described in Example 2. Test III was carried out at a pressure of 21 kg / cm 273.9 ° -315.6 ° C, the feed rate of raw materials 3-6 wt.ed. carbohydrate and 1 hour per 1 weight The catalyst is based on a ratio of hydrogen raw materials of 89175 nm / m. For the first 8 days of testing, the temperature was 273.9 ° C, the ratio of hydrogen to raw materials was 89 m / m (first period). From the 9th to the 31st day of treatment, the temperature is 290.6 ° C and the hydrogen feed rate is approximately 89 (second period) From the 31st day of treatment to the 45th day, the hydrogen supply is increased to 175 (third period). From the 45th to the 63rd day of the treatment, the temperature is 315.6 ° C, the weight rate is 6 hours, the hydrogen – SFe 142 ratio (the fourth period). From the data presented in table. 3, it can be seen that during the first period poor desulfurization takes place. The temperature seems to be too low and fluid is present in the system. During the second period, an elevated temperature contributes to greater evaporation, but complete evaporation does not occur. During the third period, a higher hydrogen feed rate is used. Perhaps in this case, complete evaporation occurs. During the fourth period, various combinations of operational parameters are used. The value of the supply of hydrogen is reduced to 142 nm / m with the twisting of the temperature and the supply of raw materials. There is almost complete evaporation. In experiment III (Table 3), the process proceeds satisfactorily at a pressure of 21 kg / cm, and the plant operation improves as a result of more complete evaporation of reagents and products in the reaction zone, and maximum efficiency can be achieved by appropriate selection of process conditions, and the activity of catalysts is maintained. high over an extended period of time. A change in the D octane number with a change in the desulfurization percentage is shown in FIG. 2. These data are derived from data provided. Data in the table. 3, and demonstrate that a decrease in the octane number in the presence of catalyst A, i.e. the catalyst used in the implementation of the proposed method occurs to a lesser extent than in the implementation of the usual process. The abscissa axis (Fig. 2) shows the desulfurization depth (wt.%), The ordinate axis shows the change in the octane number (A), the circles indicate the data obtained when the catalyst A was tested, the triangles the data obtained when the catalyst B was tested. four additional catalysts. Three of them are catalysts of the invention (C, D, E), each of which contains magnesium oxide as a carrier. The fourth catalyst, designated as catalyst F, contains alumina as carrier. To obtain a catalyst, C 162 g of heavy powdered magnesium oxide is impregnated with a solution which is prepared by dissolving 38.0 g of ammonium molybdate in 100 ml of hot (about) distilled water and 23.5 g of cobalt (II) nitrate in 50 ml of distilled water with subsequent mixing of these two solutions. The impregnated material is dried in air for 3 hours, crushed to particles passing through a 25-mesh sieve (US Sieve Series), granulated into t / 8 inch (0.318 cm) granules, calcined in air for 2 hours at 232 ° C and then burned in air for 3 hours at 537.8 ° C. During the drying and calcination, an air supply rate of 0.042 m / h is used. Catalyst C contains 3 wt.% Oxide, cobalt and 15 wt.% Molybdenum trioxide based on the weight of the catalytic composition. The carrier consists of 100% magnesium oxide. To obtain catalyst D, 142 g of heavy powdered magnesium oxide is mixed with an aqueous solution obtained by dissolving 38.8 g of ammonium molybdate and 23.5 g of cobalt (II) nitrate in 150 MP of warm (about 37.8 ° C) distilled water. After thoroughly mixing the mixture, it is further mixed with 224.7 g alum min sol, which contains 9 wt.% Alumina. The mixture is thoroughly mixed, air dried for 3 hours at, ground to 25 mesh particles (U.S. Sieve Series) passing through CIto with openings of 25 mesh and granulated to 1.8 inches (Oj32 cm) in size. The granules are calcined in air for 2 hours at 232 ° C. the temperature is gradually raised to 537.8 ° C and then burned in air for 3 hours at 537.8 ° C, Catalyst D contains, wt%: cobalt oxide 3, molybdenum trioxide 16, magnesium oxide 70 and alumina 11 per on the weight of the catalyst. For the preparation of catalyst E, 106.5 tons of powdered magnesium oxide are mixed with an aqueous solution obtained by dissolving 38.8 g of ammonium molybdate and 23.5 g of cobalt nitrate (I in 150 ml of warm (about 37.8 ° C) distilled water. After careful mixing the mixture is mixed with 398.8 g of alumina sol containing 9% by weight of alumina. The mixture is thoroughly mixed, dried in air for 3 hours at 121 ° C, crushed to form particles passing through a 25-mesh sieve mesh (US Sieve Series), and granulated into 1/8 inch granules ( 0.32 cm.) The granules are calcined in air for 2 hours at 232 ° C, gradually raising the temperature to 537.8 ° C, and calcined in air for 3 hours at 537.8 ° C. A catalyst E is obtained, containing, by weight. %: cobalt oxide 3, molybdenum trioxide 16, magnesium oxide 58 and alumina 23 are calculated on the weight of the catalyst. To obtain a catalyst F 1820 g of alumina sol containing approximately 8.9% by weight of alumina is mixed with an aqueous solution which is obtained by dissolving 38.6 g of ammonium molybdate and 23.3 g of cobalt (II) nitrate in 500 ml of distilled water. The mass obtained is dried overnight in air at a temperature of about 135 ° C, shifted from 4% Sterotex, dried for 2 h in air at 232 ° C, gradually raising the temperature to 537.8 ° C, and then burned in air at 537 , 8 ° C for 3 hours. A catalyst F is obtained, which contains by weight%: cobalt oxide. 3, molybdenum trioxide 16 and alumina 81, based on the weight of the catalyst. And p im e r 5. Catalysts C, D, E, and F are tested for the ability to desulfurize high-sulfur catalytic cracking gasoline (raw material K 2, whose properties are listed in Table 2). Each of the experiments was carried out on a battery-type installation, as described in Example 2, in a flow-type reactor with one pass of hydrogen. The collected product is cooled with wet ice. 13 g of catalyst in the form of particles that pass through a 12-mesh sieve (U.S. Sieve Series) are loaded into the reactor and are not trapped by a 20-mesh sieve. The catalyst sample is precipitated with a mixture of 8% hydrogen sulfide (8 vol.%) In hydrogen, for 1 h at atmospheric pressure and 296 ° C. The rate of the sulfur gas is maintained at 0.028. Conditions for each experiment: total pressure 10.5 kg / cm, temperature SOZC, hydrogen to raw materials ratio | 75 nm / m,
    weight speed of the raw material drop is 2.53. Each of the samples of the hydrotreated product is then collected for 2 hours and washed with a solution
    the sulfur content and the bromine number are determined.
    The test results are presented in Table. five.
    g
    Table 5 cadmium sulfate for the removal of hydrogen sulfide. Product analyzed
    权利要求:
    Claims (4)
    [1]
    1. METHOD FOR SULFURING CRACKING-GASOLINE by contacting a mixture of cracked gasoline and hydrogen containing gas with a catalyst containing metals of groups VIB and VIII of the Periodic system of elements, their oxides, sulfides, or mixtures of the listed ingredients on an inorganic oxide carrier containing aluminum oxide, 232.2-398.9 ° C, a pressure of 5.25-42 kg / cm 2 , the ratio of hydrogen - raw materials 36-890 nm 3 hydrogen per 1 m 3 of raw materials and a weight feed rate of 1-15 h ', about t l characterized in that, in order to increase the selectivity and simplify the process technology, using the catalyst, the carrier of which contains 70-90 wt.% magnesium oxide.
    [2]
    2. The method according to p. ^ Characterized in that the process is carried out in the vapor phase.
    [3]
    3. The method according to p. ^ Characterized in that they use catalysts containing the ingredient VIB. group in an amount corresponding to 10-20 wt.% metal oxide in the catalyst, and ingredient VIII! group in an amount corresponding to 1 to 10 wt.% metal oxide in the catalyst.
    [4]
    4. The method according to PP. 1-3, on t lich a y u. with the fact that they use a catalyst containing molybdenum and cobalt as groups of ingredients VIB and VIII, respectively.
    类似技术:
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    同族专利:
    公开号 | 公开日
    DE2709098A1|1977-09-08|
    FR2343042A1|1977-09-30|
    NL7701738A|1977-09-06|
    US4140626A|1979-02-20|
    IT1086671B|1985-05-28|
    AU513580B2|1980-12-11|
    FR2343042B1|1982-09-03|
    JPS52107008A|1977-09-08|
    PL113664B1|1980-12-31|
    CA1098472A|1981-03-31|
    GB1577821A|1980-10-29|
    AU2209277A|1978-08-17|
    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
    US66401876A| true| 1976-03-04|1976-03-04|
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