• 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:
    A method for regenerating a coke-contaminated cracking catalyst with the simultaneous carefully controlled combustion of CO to CO2 within a regeneration zone to produce regenerated catalyst and flue gas. Novel features of the method include adding to the regeneration zone, independently of the cracking catalyst, a liquid comprising a soluble CO oxidation promoter selected from the group consisting of the noble metals and compounds thereof and combusting CO to CO2 in the presence of the promoter and regenerated catalyst. The liquid may be added to the regeneration zone in amounts to control the CO concentration in the flue gas, a regeneration zone temperature, or the residual carbon concentration on regenerated catalyst.
    公开号:SU1003740A3
    申请号:SU772449507
    申请日:1977-02-02
    公开日:1983-03-07
    发明作者:Лерой Хемлер Чарльз；Оливер Стайн Лоренс
    申请人:Юоп Инк (Фирма)；
    IPC主号:
    专利说明:

    0.12-6.0 h, per 1 million by weight of the catalyst based on metal. Example 1. This example describes tests carried out in the regeneration zone of a pilot catalytic cracking unit in a fluidized bed in order to determine the efficiency of introducing a liquid containing certain activators in a low concentration into the regenerative zone of a catalytic cracking unit in a fluidized bed in relation to a decrease in CO concentration. about flue gas. The tests are carried out in a vertical tubular vessel, in the upper end of which a porous stainless steel filter is inserted to hold a sample of the catalyst introduced into this vessel inside the vessel, and in the lower end of which is an inlet device for introducing a fluidizing medium (nitrogen or air) and inlet A device for injecting a fluid containing an activator. This vessel is heated to a constant temperature and a chromatographic installation is provided for sampling and analyzing flue gas from this vessel to determine if
    it is CO, C02, and 0, so that the results of the analysis can instantly determine the decrease in the concentration of CO. Each test was carried out using 500 g of a sample of a zeolite-containing cracking catalyst, containing about 0.9 wt.% Coke. The fresh catalyst, which is fed to the cracking reactor, consists of macro-spherical particles in the form of a calcined hydrogel matrix consisting of alumina and silicon dioxide, in which crystalline hydrogen ion-exchange resin is suspended as a solid material before gelation of the corresponding hydrosol, containing alumina and silica, around resin crystals. The catalyst contains 8 wt. resin in the composition consisting of 68 wt. silicon dioxide and 32 wt. alumina. Coke is deposited on the catalyst by passing gas oil (as a feedstock) over a pure regenerated catalyst in the hydrocarbon conversion zone of a pilot plant, operating under standard conditions with a preliminarily
    2,
    3.09 04 this sequence of process steps. In test 1, a liquid with an activator is not introduced into the reaction vessel during the course of the process, this test is carried out to establish a standard for comparison with the tests using the proposed method, 500 g of the sample of spent catalyst are introduced into this vessel. and fluidize it with nitrogen introduced from the bottom of the vessel while heating the system to. The nitrogen is then replaced by air, thus initiating the oxidation of the coke. The flue gas leaving this reaction vessel has CO concentrations determined by means of a chromatographic unit and various points in time after entering the air are shown in Table. 1. Table 1 Test 1. Absence of an activator of CO oxidation in the regeneration zone of the pilot plant. CO concentration in flue gas. As can be seen, the CO / CO ratio during the test remains within a rather narrow limit of about 2.5 .3.0. Test 2 is carried out in the same way as test 1, with the difference that 15 seconds after the fluidization with nitrogen, oxygen is turned on, when an increase in CO concentration is observed, 30 cm of a dilute solution of chloroplatinic acid are introduced into the reaction vessel. This solution is prepared by diluting chloroplatinic acid, containing about 28.6 wt.% Pi, with distilled water, into a cut; In this case, a diluted chloroplatinic acid containing 0.1 mg of platinum per cm is obtained. The amount of chloroplatinic acid is equivalent to about 6.0% by weight of the catalyst in the form of free platinum. From the chromatogram obtained instantaneously, it is clear that the concentration of CO is reduced. As the test proceeds, the flue gas has the compositions shown in the table. 2
    Table2 Test 2. Use of diluted chloroplatinic acid (0.1 mg Pt / cM in the regeneration zone of the pilot plant. CO concentration in flue gas
    diluted chloroplatinic acid, equivalent to about 0.5 weight.h. per 1 million catalyst in the form of metallic platinum. This solution is prepared by diluting the pacTw suit of the thief used in Test 2, containing 0.1 mg of platinum per cm, with distilled water, resulting in a more dilute solution of chloroplatinic acid, containing 0.01 mg of platinum per cm. Concentrations were obtained CO in the flue gas are presented in table. 3Table 3 Test 3. Use of dilute chloroplatinic acid in the regeneration zone of the pilot plant. CO concentration in flue gas.
    Carbon monoxide concentrations are significantly lower and ratios significantly higher than in Test 1 for the same time intervals. To determine how fast platinum loses effectiveness in reducing CO concentration, the regenerated catalyst test 2 is used for additional process cycles in the hydrocarbon conversion reaction zone of the pilot plant, and then in the regeneration zone without adding an activator. After the first three additional cycles of the process, the formation of CO is almost not observed in the hydrocarbon reaction zone and then in the regeneration zone as coke is burned, but during the fourth cycle a large amount of CO is present in the flue gas, although this amount is much less than in test 1, in which the activator is not used. The same test procedure is then repeated using 500 g of a new test catalyst sample 3 with the exception that a more dilute solution is used and the liquid containing the activator is introduced into the reaction vessel just before the fluidizing nitrogen is switched to the air supply. In this test, 25 cm more is introduced into the vessel. Although the reduced amount of oxidation activator in this test yields results comparable to those obtained using higher concentrations of activator in test 2, the regenerated catalyst shows that a significant degree of activator efficiency is lost very quickly with subsequent cycles, as can be seen from the presence of CO in subsequent regeneration processes. After three cycles using this activator, the catalyst leads to the formation of CO, the amount of which is about 2/3 of the amount that is formed in the absence of the activator in test 1. In test k, 25 cm of chloropalladium solution is introduced into the reaction vessel. acid in water containing 0.1 mg of palladium per cm, which is equivalent to about 5 parts by weight per million catalyst in the form of palladium metal, and this solution is introduced in 1 second after the flow of fluidizing nitrogen has been switched to air supply. initiating incineration. By direct chromatographic examination, it is established that the concentration of CO is reduced. As the experience continues, the flue gas has the composition shown in table. k. Table C Test 2. The recovery zone of the pilot plant using diluted chloropalladic acid (0.1 mg pallad. / S / similar time intervals. In order to quickly evaluate the reduction in the effectiveness of palladium at a decrease in CO concentration, the regenerated catalyst is used for additional cycles in the industrial hydrocarbon reaction zone, and After the first complementary cycle, passage through the hydrocarbon reaction zone and the regeneration zone, essentially the formation of CO during coke combustion is not observed, but starting from the subsequent cycles in the flue gas, small amounts of CO are noted, although CO in the flue gas decreases by about one-tenth as compared to the CO concentration in Test 1, in which the promoter is not used for the same period of time. Example 2. In this example, the procedure is described in detail with flowing in the reduction zone industrial fluid catalytic cracking, shortly after added to any small amounts of liquid. containing the oxidation promoter CO, which is the subject of this invention, without any other process changes. In the installation used in this case, approximately 18.670 barrels / day (2k of a mixture of vacuum gas oil and coking gas oil are obtained, and the amount of catalyst circulating in the system (containing catalyst) is approximately 60 tons kg). The installation is brought to typical operating conditions, without trying to partially or significantly reduce the CO concentration in the flue gas and not using the CO conversion activator in the regeneration zone. Some of these operating conditions of the process before entering the activator into the regeneration zone are presented in Table. 5. Then two liters of an aqueous solution of chloroplatinic acid are squeezed out of the cylinder and injected into the regeneration zone within 2-3 minutes through a tap located in the regeneration zone. A dilute solution of chloroplatinic acid is prepared by diluting 61, g of concentrated chloroplatinic acid (128.637 wt.% P-L) to two-liter volume using distilled water. Passing this amount of solution to the regeneration zone provides an input of an activator in an amount equivalent to about 0.32 parts by weight. per 1 million circulating in the system of the catalyst in the form of elemental platinum. The regeneration zone almost immediately responds to the introduction of this activator; The CO concentration in the flue gas is reduced to half the tog of the amount that is reached before entering the solution, and the temperature of the dense phase of the regeneration zone rises by about a temperature before entering such a solution. No other process changes occur. Indicators of the working conditions of the process after the first input of such a solution are summarized in Table 5. A few hours thereafter, a small amount of the solution containing the activator is introduced into the regeneration zone in an amount equivalent to about 0.13 parts by weight. per million of the catalyst circulating in the system in the form of elemental platinum, and this input occurs in the same way, as well as the first one. Apart from the input of actuator 1003740, no other changes in the workflow are made. The performance indicators of the working conditions shortly after this second entry are also summarized in the table.
    Table 5
    The susceptibility of the regeneration zone of the industrial catalytic cracking unit in the fluidized bed to the input of the activator. Selected to the operating conditions of the process.
    665 681
    713
    687
    661
    717
    667 678
    703
    511
    510 511
    329
    one.
    17.1
    0.0
    12.2
    0.06
    10 Continued table. five
    As the data in the table. 5, CO concentration in flue gas decreases from 10.5% by volume (before entering any activator solution) to 5.9% by volume after entering the first Ko tt solution quality (0.32 parts by weight per million Pt) , up to 1, vol. after extracting the second amount of solution (0.13 parts by weight per 1 million Pt). The amount of carbon on the regenerated catalyst decreases from 0.30 to 0.16 wt. after entering the first amount of solution, and then decreasing to 0.06 wt.% after entering the second amount of solution; while the temperature of the dense phase of the regeneration zone increases from 655 to 681 after entering the first quantity and up to the second amount of solution after Evod. Temperatures elsewhere in the regeneration zone also increase, but not to the same extent as in the dense phase region.
    Example 3. This example describes the use of this invention and in the same industrial installation, as in Example 2, and shows the advantages of the proposed cno-i self. Before entering these two quantities of activator solution, which was carried out as in Example 2, a fairly complete test 1 was carried out for comparison with subsequent tests carried out with the introduction of the activator solution into the regeneration zone. The next day after the introduction of the first two quantities of the activator solution, two more activator solutions were introduced: containing activator in an amount equivalent, respectively, to approximately 0.13 and 0.32 parts by weight. per million of the metallic Pt catalyst circulating in the system, and the introduction of these solutions is carried out in the same manner as described in example 2. In this case, however, the velocity of the air introduced into the regeneration zone is increased in order to guarantee sufficient oxygen for the almost complete conversion of CO to CO. During the course of the process at steady state, when CO is almost completely oxidized in the regeneration zone in the presence of a mixture of an oxidation activator CO with a regenerated catalyst, impregnates; test 2 is repaired; during test 2, coke; In the regeneration zone, it is mixed with a CO oxidation activator, which is equivalent to about Dj9 weight parts. per 1 million of the catalyst circulating in the system in the form of free P-t. In test 2, the feed rate of the feedstock, the pressure in the regeneration zone and in the hydrocarbon conversion zone are basically the same as in test 1. Before the start of test 2, no attempt was made to achieve the same degree of conversion that was achieved on test 1, and - also optimize the air flow rate required for practical use. chesky complete conversion of CO. The results of tests 1 and 2 are shown in Table 6.
    Table Comparison of catalytic cracking processes in the fluidized bed before and after the introduction of the CO conversion activator,
    Process conditions
    Hydrocarbon reaction zone
    Temperature, C 10
     Comparison of the test data shows that when using this invention, the CO concentration in the flue gas decreases from 10.5% by volume. Continuation of the table.6 Mixed raw product temperature, C 328 313 Regeneration zone Dense phase temperature, ° C Temperature of fluidized ({) element , C Flue gas temperature, C Carbon on regenerated catalyst, wt.% 0.28 0.11 Flue gas analysis, o6,% 131, 1 rd, residual carbon content on regenerated catalyst decreases from 0.28 dp to 0.11 dp (showing the best regeneration recuperators), and an overall increase of the regeneration zone temperature is from about 38 to. Although the temperatures in the Reaction Zone (or conversion) of the hydrocarbon are not exactly the same, utilizing part of the heat of burning CO in the regeneration zone in Test 2 reduces the temperature of the mixed feedstock. Although the conversion rate in test 2 is about 1.7% less than in test 1, a comparison of the yields indicates that in test 2, cracking is more suitable for producing more valuable products than in test 1. The coke yield of test 2 is (", 3% by weight compared to 5, weight in test 1, and even if the conversion rate in test 2 is 1.7% lower than in test 1, the yield of gasoline fractions in test 2 % by volume compared to 57.6% by volume in test 1. Subsequent tests carried out on the same industrial installation show that almost complete conversion of CO can be achieved by passing an average daily volume of the activator solution containing into the regeneration zone an activator in an amount .. equivalent to about 0.12 pbw of 1 million calories catalyst in the system in the form of metal P. An analysis (for platinum content) of catalyst samples from this industrial installation shows that a significant part of the activator remains on the cracking catalyst. So, for example, at the time when this industrial installation is completely injected a solution of chloroplatinic acid containing the total amount of activator, equivalent to 75 grams of P-fe, a sample of the equilibrium catalyst is removed from the installation and analyzed to determine the concentration of Pfc. The platinum concentration measured is 1.0 pbw. per 1 million. If all 75 g of platinum, which was introduced into the installation, were evenly distributed over the entire quantity of 60 tons (t6B kg) of the reversible 3 catalyst system, then a concentration of 1, k weight per 1 million Pf– could be achieved in the equilibrium Catalyst Example. This example illustrates the problem of chemical instability of a solution. In particular, it illustrates the chemical instability of a solution of chloroplatinic acid in a mixture of water and the usual freezing point of a water depressant, ethylene glycol. Chlorplatinic acid, containing 25.6% by weight of P-fc, is dissolved in the mixture (in a 1: 1 weight ratio of technical ethylene glycol with distilled water and tap water, resulting in two solutions, each containing 0, wt.% PLY: Tina. These two solutions are analyzed for solubility characteristics at -29 ° C and for thermal stability at, 3 ° C and 63 ° C. The data presented in Table 7 show that these solutions are liquid at , but they do not; possess the required chemical resistance BONE in 30 days at 63 ° C, black precipitate It is called approximately 11 days later at 22 ° C and only after 0.7 days at 63 ° C. This black precipitate is separated by centrifugation, washed with water and analyzed for Pt content. The content of elemental platinum in this black precipitate is The chemical analysis by electron spectroscopy shows mainly Pt with an example of "Extraction of platinum from the precipitate, glass parts and a clear solution of 100.3% (of the initial platinum used. These data show that the black precipitate is P-t, which indicates the reduction of Pt in chloroplatinic acid, P, and oxidation of ethylene glycol. Ethylene glycol oxidation products have not been identified. Table 7 The persistence of chloroplatinic acid in a mixture of ethylene glycol and water. Example 5. This example illustrates freezing temperatures and chemical resistances at, 27. C, 63 With ten solutions of chloroplatinic acid (CPA7, having concentrations equivalent to O.O. ZchwesD P-b in various chemically pure primary, secondary or tertiary alcohols or their mixtures. The temperature of -3C With is chosen with the aim of artificially reproducing the lowest temperature, which resistance is the chemical resistance of chloroplatinic acid, is best in the case of saturated aliphatic primary alcohols (except methyl alcohol) and significantly weaker in the case of saturated aliphatic secondary and tertiary alcohols. Along with unsuitability due to poor chemical resistance, chloroplatinic acid2-methyl-2-propanol solution is in solid state. In order for chloroplatinic acid 5 in different solvents at different temperatures can take place under practical conditions, a temperature of 22 ° C is chosen to reproduce the average environmental conditions; and a temperature of 63 ° C is selected for artificial reproduction of average storage conditions (indoors and outdoors. For each temperature, the number of days before the appearance of a black precipitate is determined; most likely °. The data obtained are summarized in Table 8. Table. C and reduce their chemical resistance with 2-ethyl-1-hexanol (more than 60 days) 1-propanol (more than 58 days), 1-butanol (50 days); ethanol and 1-hexanol (day); 2-methyl- 2-propanol (13 days); 2-propanol and 2-butanol (1-2 days) and methanol (0.25 days). Example 6. A linear example describes testing in the regenerator zone pilot plant installations, which were performed to determine the effectiveness of pactsopa containing chloroplatinic acid in 1-butanol,
    in relation to reducing the CO concentration in the flue gas. The tests are carried out using the apparatus described in Example 1. As in Example 1, the apparatus is heated to a constant temperature and a chromatographic apparatus for continuous sampling and analysis of flue gas from the vessel for CO, C02 and 02 contents. Instantly using them to determine the chromatogram of CO, CO and 02: allows to characterize the degree of combustion CO during this test. From the chromatograms for each test, a characteristic ratio is considered that is considered the minimum ratio by first determining the maximum CO concentration for a particular test (which is usually carried out within 2/3 min after initiating the combustion), determining the C0 concentration; 2 at the time of the maximum CO concentration, and the subsequent calculation of the CO. / CO ratio for the concentrations found in this way is considered as the minimum CO / CO ratio, since from the results of many such tests it was found but, that if one builds a relationship dependence curve (at each moment of time) against time for each test, then this curve passes through the minimum value of the ratio, having a value calculated as indicated above. This minimal CO2UO ratio best describes the ability of any solution containing a CO oxidation activator to catalyze the burning of CO. The tests were carried out using 500 g samples of an equilibrium zeolite-containing fluid cracking catalyst, which was first worked by passing the initial gas oil feed over a sample of an equilibrium catalyst in the hydrocarbon reaction zone of the pilot plant, in which standard conditions were created and in which the process steps predetermined sequence. A sample of each spent catalyst contains about 0.9 wt.% Coke.
    In Test 1, no solution containing an activator was used; the test is carried out in order to establish a standard for comparing the
    a subsequent test in which a solution containing an activator was used. 500 g of spent catalyst are introduced into the reaction vessel, and fluidization is created by nitrogen, which is introduced from the bottom of the vessel while heating the system to. Then the nitrogen supply is switched to the air supply, thus initiating the oxidation of coke in this way. The flue gas leading out of this reaction vessel is analyzed for CO-2, CO and 0 using a chromatographic system, and from CO amounts. and CO calculate the minimum ratio. To establish the reproducibility of the results obtained by this test method, this test is repeated.
    with individual samples of spent catalyst four times. The minimum values of the C0 "/ C0 ratios in the range from 2.5 to 3.3 are shown in Table. 9.
    Test 2 was carried out in the same way as test 1, with the difference that just before the flow of fluidized nitrogen was switched to oxygen, 25 g of a sample of chloroplatinic acid solution in 1-butanol was introduced into the regeneration zone. The concentration of chloroplatinic acid in this sample is equivalent to O, 008 Bec.Ht, and the amount
    platinum in the sample is 2 mg or weight.h. on 1 million (in a sample of the catalyst of 500 g). A minimum ratio of 52.1 is obtained and then to determine the speed, with
    which a mixture of particles of activator and particles of the generated catalyst
    loses effectiveness in relationships
    reducing the CO concentration in the flue gas, this mixture is passed through a greater number of cycles. In particular, to complete the next cycle, the mixture is tested in the reaction zone of the hydrocarbons of the pilot plant, as described above, and the test in the regeneration zone is repeated without adding additional quantities of activator solution. At the end of the seventh cycle, the minimum ratio of CO2 / CO mixture is 45.1, thus showing that it maximally retains its activity as a catalyst for burning CO. The results of tests 2 and 1 are summarized on the table. 9.
    t9 Table 9
    Cycle
    Minimum COj / CO ratios
    .LTflillinLlL
    Test 1 without using an activator solution
    Test 2 (25 g of chloroplatinic Chislota-β-butanol solution, 0.008 wtD)
    pt);
    10037 0
    20
    Solutions of chloroplatinic acid. In other suitable solvents, they behave in the same manner as the solutions of chloroplatinic acid 5 in 1-butanol used in this example.
    权利要求:
    Claims (2)
    [1]
    1.Patent of France tf 2186293 cl. In 01 J P / O, published. 197.
    [2]
    2.US Patent fZZPPZb,
    ,five
    , cl. 208-120, publ. 1968 (prototype).
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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
    US65426076A| true| 1976-02-02|1976-02-02|
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