CN112831341B - Application of rare earth carbonate directly as vanadium passivator and vanadium resistant catalytic cracking catalyst - Google Patents
Application of rare earth carbonate directly as vanadium passivator and vanadium resistant catalytic cracking catalyst Download PDFInfo
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- CN112831341B CN112831341B CN202011625857.4A CN202011625857A CN112831341B CN 112831341 B CN112831341 B CN 112831341B CN 202011625857 A CN202011625857 A CN 202011625857A CN 112831341 B CN112831341 B CN 112831341B
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G11/00—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G11/00—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils
- C10G11/02—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils characterised by the catalyst used
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Abstract
The invention discloses application of rare earth carbonate directly as a vanadium passivator and a vanadium-resistant catalytic cracking catalyst, which has excellent vanadium passivation effect by directly adding the rare earth carbonate into a catalytic cracking system, can also improve the activity of the catalyst, improve the conversion rate of the system, reduce the yield of low-added-value products (coke, dry gas and slurry oil) in a cracked product, improve the yield of high-added-value products (gasoline and liquefied gas) in the cracked product, improve the coke selectivity of the catalyst, flexibly change the using amount of the vanadium passivator according to the change of the property of raw oil, do not need to reprocess the rare earth carbonate, directly purchase commercial products, have convenient use and are worthy of popularization.
Description
Technical Field
The invention belongs to the technical field of catalytic cracking, and particularly relates to an application of rare earth carbonate directly as a vanadium passivator and a vanadium-resistant catalytic cracking catalyst.
Background
Petroleum contains many metal elements such as nickel, vanadium, iron, sodium, calcium, copper, arsenic, etc. in addition to 5 main elements of carbon, hydrogen, sulfur, nitrogen, oxygen, etc., and although their contents are not high, they also have adverse effects in the catalytic cracking process of petroleum.
Crude oil mainly processed by domestic refineries is imported crude oil, wherein the vanadium content is high, the crude oil exists in the form of an organic complex, and the crude oil cannot be removed in an electric desalting process (the crude oil enters a pretreatment procedure before distillation). In the catalytic cracking process, the metal complex in the raw material is decomposed, vanadium is deposited on the cracking catalyst, the activity of the catalyst is reduced, even the catalyst is poisoned (the phenomenon that the activity of the catalyst is obviously reduced or lost), the dosage consumption of the catalyst is increased, and the economical efficiency of processing is influenced.
Therefore, the problem of catalyst pollution caused by vanadium has become a great obstacle for blending of catalytic cracking devices of various refineries, and the toxic effect of high-concentration vanadium in crude oil on the FCC catalyst is a problem to be solved urgently.
In order to reduce the toxic effect of vanadium in crude oil on the FCC catalyst, auxiliary agents such as vanadium resistant agents, vanadium traps and the like are generally added in the catalytic cracking process. The vanadium passivators of the catalytic cracking process currently on the market mainly comprise two types, namely MgO series passivators and rare earth oxide passivators.
The MgO series passivator has a certain vanadium resistant effect, the cost is lower than that of a rare earth vanadium resistant agent, but the catalyst activity is reduced due to the strong alkalinity of the MgO series passivator. Rare earth oxide passivator RE of Grace 2 O 3 /Al 2 O 3 As a representative, has a certain anti-vanadium effect; the rare earth oxide passivator (La 2O 3) developed by Mobil company is taken as a representative (US 4913801A), and has a good vanadium passivation effect; the companies such as medium and petrochemical industry also have a certain vanadium passivation effect by adding rare earth elements into the molecular sieve and the matrix of the catalyst, but Si, al and the like in the rare earth oxide can affect the surface alkalinity of the rare earth compound, so that the vanadium passivation effect is poor, and the improvement is needed.
Disclosure of Invention
The invention mainly solves the technical problem of providing the application of the rare earth carbonate directly as the vanadium passivator and the vanadium resistant catalytic cracking catalyst, which has good vanadium resistant effect and convenient use.
At present, the existing application of rare earth carbonate as a vanadium-resistant component requires secondary processing of rare earth carbonate, for example, a rare earth carbonate and a main catalyst component are mixed to prepare a main catalyst containing the rare earth carbonate, the catalyst is often limited in vanadium resistance and cannot adapt to flexible and variable feeding and the situation that the content of heavy metals such as vanadium and the like in mixed feeding is greatly changed or is high, or the rare earth carbonate is mixed with aluminum sol, silica sol and the like to prepare a vanadium-resistant agent which can be independently added, but the vanadium-resistant effect is still poor, the conversion rate is reduced or kept at the same level at most, and an improvement space is still left.
Through long-term research and continuous tests, the inventor unexpectedly finds that the rare earth carbonate is directly added into a catalytic cracking system, so that the catalytic cracking system has an excellent vanadium passivation effect, the system conversion rate can be improved, the yield of low-added-value products (coke, dry gas and oil slurry) in a cracked product is reduced, and the yield of high-added-value products (gasoline and liquefied gas) in the cracked product is improved.
The invention provides an application of rare earth carbonate as a vanadium passivator, which is to directly mix the rare earth carbonate with a reaction system.
In the invention, the rare earth carbonate is directly added into the catalytic cracking system, the vanadium passivation effect is far superior to that of similar products, the rare earth carbonate does not need to be reprocessed, and the use is convenient.
The rare earth carbonate is a salt formed by combining rare earth metal cations and carbonate, and the rare earth metal cations comprise: lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), promethium (Pm), samarium (Sm), europium (Eu), gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), lutetium (Lu), yttrium (Y), and scandium (Sc).
In a specific embodiment of the present invention, the rare earth carbonate is selected from one or more of yttrium carbonate, lanthanum carbonate and cerium carbonate.
Further, the rare earth carbonate is yttrium carbonate.
Most rare earth carbonates have poor wear resistance, for example, the wear indexes of lanthanum carbonate and cerium carbonate are both greater than 98wt%/h, which causes that the wear index of lanthanum carbonate, cerium carbonate and other rare earth carbonates is relatively fast in actual production and needs to be continuously added, but the wear index of yttrium carbonate is only 10.3wt%/h or lower and is significantly lower than that of other rare earth carbonates, the wear index is slow in the production process, and the whole usage amount is significantly reduced. Meanwhile, according to the test results of the application, when yttrium carbonate is used as the vanadium inhibitor, the conversion rate is higher, the yield of gasoline and liquefied gas is higher, the yield of coke and oil slurry is lower, and the performance of the catalyst in catalytic cracking is superior to that of other rare earth carbonates.
The invention also provides a method for resisting vanadium in catalytic cracking, which adds rare earth carbonate into a reaction system.
In a specific embodiment of the present invention, the rare earth carbonate is selected from one or more of yttrium carbonate, lanthanum carbonate and cerium carbonate.
Further, the rare earth carbonate is yttrium carbonate.
Further, the addition amount of the rare earth carbonate is such that the ratio of the rare earth carbonate: the mass ratio of the FCC catalyst is 0.2-10: 99.8 to 90, preferably 0.5 to 5:99.5 to 95.
The FCC catalyst refers to a catalyst which can be applied to catalytic cracking in the field, and the specific type and composition are not limited, and the purpose of vanadium resistance can be achieved by directly adding rare earth carbonate into a catalytic system.
Because the rare earth carbonate is used independently as the vanadium-resistant auxiliary agent, the use amount of the rare earth carbonate can be flexibly adjusted according to the change of the vanadium content in the raw oil, and the use is convenient. In the art, the addition amount of the vanadium resistant additive is generally: and (3) vanadium-resistant auxiliary agent: the mass ratio of the FCC catalyst is 0.2-10: 99.8 to 90, preferably 0.5 to 5:99.5 to 95.
In a specific embodiment of the present invention, the rare earth carbonate: the mass ratio of the FCC catalyst is 2.9:97.1.
the invention also provides a vanadium-resistant catalytic cracking catalyst, which comprises an FCC catalyst and rare earth carbonate.
According to the content of the invention, the rare earth carbonate can be used as an anti-vanadium agent to be added in the catalytic cracking process from the aspect of form, and the rare earth carbonate and the FCC catalyst can also be regarded as a whole and directly mixed to obtain a novel anti-vanadium catalytic cracking catalyst; in either case, the invention is intended to be within the scope of the claims.
In a specific embodiment of the present invention, the rare earth carbonate is selected from one or more of yttrium carbonate, lanthanum carbonate and cerium carbonate.
Further, the rare earth carbonate is yttrium carbonate.
Further, the rare earth carbonate: the mass ratio of the FCC catalyst is 0.2-10: 99.8 to 90, preferably 0.5 to 5:99.5 to 95, more preferably 2.9:97.1.
the invention has the beneficial effects that:
(1) The invention has excellent vanadium passivation effect by directly adding the rare earth carbonate into the catalytic cracking system, can also improve the activity of the catalyst, improve the conversion rate of the system, reduce the yield of low added value products (coke, dry gas and oil slurry) in the cracked products, improve the yield of high added value products (gasoline and liquefied gas) in the cracked products and improve the coke selectivity of the catalyst.
(2) The method can flexibly change the dosage of the vanadium passivator according to the change of the property of the raw oil, does not need to reprocess the rare earth carbonate, can directly purchase the commercial products, is convenient to use and is worth popularizing.
Detailed Description
The technical solutions of the present invention are described clearly and completely below, and it is obvious that the described embodiments are some, not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
In the specific embodiment of the invention, the element composition of the sample is measured by an X-ray fluorescence spectrometer, and the wear index of the sample is measured by a wear index analyzer.
The purity of the commercial rare earth carbonate used in the embodiments of the present invention is greater than 99%.
Comparative example 1
Under the condition of stirring, 4.1 kg (dry basis) of kaolin and 1 kg (dry basis) of alumina sol are added into 5 kg of deionized water, stirred at a high speed for 2 hours, after the kaolin is completely dispersed in the slurry, 1.7 kg (dry basis) of pseudo-boehmite is added, and the pH value of the slurry is adjusted to 2.5-3.5 through HCl, so that the pseudo-boehmite is subjected to gelatinization reaction. After stirring for 30 minutes, a solution containing 3.2 kg (dry basis) of USY molecular sieve (produced by Sichuan Runzhu and New materials catalysis Co., ltd., siO) 2 /Al 2 O 3 A 5 mole ratio), lanthanum chloride solution (containing 0.5 kg lanthanum oxide) and 3.5 kg deionized water. Pulping for 30 minutes, homogenizing the pulp, spray-forming, and roasting at 550 ℃ for 2 hours. Then 8 times of deionized water is added, the mixture is stirred evenly and washed for 15 minutes at 80 ℃, and the catalyst FCC-1 is obtained after filtration and drying.
The FCC-1 catalyst was impregnated by an equal volume impregnation method to have a vanadium content of 3200ppm on the catalyst, and after 10 hours of treatment with 100% steam at 810 deg.C, the cracking performance of the catalyst used in the catalytic cracking process is shown in Table 2.
Comparative example 2
Under the condition of stirring, 4.1 kg (dry basis) of kaolin and 1 kg (dry basis) of alumina sol are added into 5 kg of deionized water, stirred at high speed for 2 hours, after the kaolin is completely dispersed in the slurry, 1.7 kg (dry basis) of pseudo-boehmite is added, and the pH value of the slurry is adjusted to 2.5-3.5 by HCl, so that the pseudo-boehmite is subjected to gelling reaction. After stirring for 30 minutes, a solution containing 3.2 kg (dry basis) of USY molecular sieve (produced by Sichuan Runzhu and New materials catalysis Co., ltd., siO) 2 /Al 2 O 3 A 5 molar ratio), lanthanum chloride solution (containing 0.5 kg lanthanum oxide), yttrium chloride solution (containing 2 kg yttrium oxide) and 3.5 kg deionized water. Pulping for 30 minutes, homogenizing the pulp, spray-forming, and roasting at 550 ℃ for 2 hours. Then 8 times of deionized water is added, the mixture is stirred evenly and washed for 15 minutes at 80 ℃, and the catalyst FCC-2 is obtained after filtration and drying.
The FCC-2 catalyst was impregnated by an equal volume impregnation method to have a vanadium content of 3200ppm, and after 10 hours of treatment with 100% steam at 810 deg.C, the cracking performance of the catalyst used in the catalytic cracking process is shown in Table 2.
Comparative example 3
Under the stirring condition, 4.1 kg (dry basis) of kaolin and 1 kg (dry basis) of alumina sol are added into 5 kg of deionized water, stirred at high speed for 2 hours, after the kaolin is completely dispersed in the slurry, 1.7 kg (dry basis) of pseudo-boehmite and yttrium carbonate (containing 2 kg of yttrium oxide) are added, and the pH of the slurry is adjusted to 2.5-3.5 by HCl, so that the pseudo-boehmite is subjected to gelling reaction. After stirring for 30 minutes, 3.2 kg (dry basis) of USY molecular sieve (produced by Sichuan Runhe & catalytic New materials Co., ltd., siO) was added 2 /Al 2 O 3 A 5 mole ratio), lanthanum chloride solution (containing 0.5 kg lanthanum oxide) and 3.5 kg deionized water. Pulping for 30 minutes, homogenizing the pulp, spray-forming,then the mixture is baked for 2 hours at 550 ℃. Then adding 8 times of deionized water, stirring uniformly, washing for 15 minutes at 80 ℃, filtering and drying to obtain the catalyst FCC-3.
The FCC-3 catalyst was impregnated by an equal volume impregnation method to have a vanadium content of 3200ppm, and after 10 hours of treatment with 100% steam at 810 deg.C, the cracking performance of the catalyst used in the catalytic cracking process is shown in Table 2.
Comparative example 4
Cracking performance of 100 g of the FCC-1 catalyst of comparative example 1 for catalytic cracking was shown in table 2, after adding 2 g (dry basis) of commercial MgO (VP-1), impregnating the catalyst by an equivalent-volume impregnation method to a vanadium content of 3200ppm, and treating the catalyst with 100% steam at 810 ℃ for 10 hours.
Comparative example 5
Adding 8 kg lanthanum oxide and 2 kg (dry basis) alumina sol into 12 kg deionized water under stirring, stirring at high speed for 2 hours, homogenizing the slurry, spray forming, and calcining at 550 deg.C for 2 hours to obtain 80% La2O3 passivator VP-2. The abrasion index of VP-2 was 6.1wt%/h, and the average particle size was 82.1um.
100 g of the FCC-1 catalyst of comparative example 1 was added with a passivating agent VP-2 (containing 2 g of La) 2 O 3 ) Then, the catalyst was impregnated by an equal volume impregnation method to have a vanadium content of 3200ppm, and after 10 hours of treatment with 100% steam at 810 ℃, the cracking performance of the catalyst in the catalytic cracking process is shown in table 2.
Comparative example 6
Adding 8 kg lanthanum oxide and 2 kg (dry basis) silica sol into 12 kg deionized water under stirring, stirring at high speed for 2 hours, homogenizing the slurry, spray forming, and calcining at 550 deg.C for 2 hours to obtain 80% La2O3 passivator VP-3. The wear index of VP-3 was 10.2wt%/h, and the average particle size was 78.3um.
Comparative example 1 FCC-1 catalyst was supplemented with passivating agent VP-3 (containing 2 g of La) 2 O 3 ) Then impregnating by using an equal-volume impregnation method to ensure that the vanadium content on the catalyst is 3200ppm, and treating for 10 hours by 100 percent steam at 810 ℃, wherein the catalyst is used in the catalytic cracking processThe cracking performance is shown in Table 2.
Comparative example 7
The passivating agent prepared by the method in example 1 of patent CN102228838A is named VP-4.
In comparative example 1, after adding a passivating agent VP-4 (containing 2.9 g of lanthanum carbonate) to the FCC-1 catalyst, the catalyst was impregnated by an equivalent volume impregnation method to have a vanadium content of 3200ppm, and then treated with 100% steam at 810 ℃ for 10 hours, the cracking performance of the catalyst in the catalytic cracking process is shown in Table 2.
Example 1
Yttrium carbonate YC-VP-2 was purchased commercially with an abrasion index of 10.3wt%/h and an average particle size of 45.6um.
In comparative example 1, 2.9% of passivating agent YC-VP-2 was added to the FCC-1 catalyst, and then the catalyst was impregnated by an equivalent volume impregnation method to have a vanadium content of 3200ppm, and then treated with 100% steam at 810 ℃ for 10 hours, and the cracking performance of the catalyst in the catalytic cracking process was as shown in Table 2.
Example 2
Commercially available lanthanum carbonate LaC-VP-3 with an attrition index >98wt%/h and an average particle size of 23.6um.
In comparative example 1, 2.9% of a passivating agent LaC-VP-3 was added to the FCC-1 catalyst, and then the catalyst was impregnated by an equivalent volume impregnation method to have a vanadium content of 3200ppm, and then treated with 100% steam at 810 c for 10 hours, and the cracking performance of the catalyst in a catalytic cracking process was shown in table 2.
Example 3
Commercially available cerium carbonate CeC-VP-4 with an attrition index >99wt%/h and an average particle size of 22.9um.
In comparative example 1, 2.9% of a passivating agent LaC-VP-4 was added to the FCC-1 catalyst, and then the catalyst was impregnated by an equivalent volume impregnation method to have a vanadium content of 3200ppm, and then treated with 100% steam at 810 ℃ for 10 hours, and the cracking performance of the catalyst in a catalytic cracking process was as shown in table 2.
Test example 1
The FCC catalysts impregnated with vanadium solution of comparative examples 1 to 7, the FCC catalysts impregnated with vanadium solution of examples 1 to 3 and the auxiliary agents were used for catalytic cracking, and evaluated on a micro fluidized bed reactor (ACE) and a supporting gas chromatograph, and the properties of the feedstock oil were measured as in table 1, and the catalytic cracking performance of the samples of examples and comparative examples was measured as in table 2.
TABLE 1 Properties of the stock oils
TABLE 2 catalytic cracking performance of different catalysts
Coke index = coke yield/conversion (100% -conversion)
Comparative example 1 does not add any vanadium-resistant component or vanadium-resistant auxiliary, comparative example 2 adds rare earth oxide component to the main catalyst, comparative example 3 adds rare earth carbonate component to the main catalyst, comparative examples 2 to 6 are vanadium-resistant auxiliary prepared by additionally adding rare earth oxide, and comparative example 7 is vanadium-resistant auxiliary prepared by adding rare earth carbonate and silica sol. As can be seen from the data in Table 2, the catalytic cracking performance of examples 1 to 3 is significantly better than that of comparative examples 1 to 7, and compared with other vanadium-resistant methods, the method of the present invention of directly adding rare earth carbonate to a catalytic cracking system can improve the conversion rate of the system, improve the yield of gasoline and liquefied gas, reduce the yield of coke, dry gas and slurry oil, have more excellent coke selectivity, and generally improve the utilization rate of raw oil and the device benefit.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. The application of the rare earth carbonate as the vanadium passivator is characterized in that the rare earth carbonate is directly mixed with a catalytic cracking reaction system, and the rare earth carbonate is yttrium carbonate.
2. A method for resisting vanadium in catalytic cracking is characterized in that rare earth carbonate is added into a reaction system, and the rare earth carbonate is yttrium carbonate.
3. The method according to claim 2, wherein the ratio of rare earth carbonate: the mass ratio of the FCC catalyst is 0.2-10: 99.8 to 90.
4. The process according to claim 3, wherein the ratio of rare earth carbonate: the mass ratio of the FCC catalyst is 0.5-5: 99.5 to 95.
5. The process according to claim 4, characterized in that the rare earth carbonate: the mass ratio of the FCC catalyst is 2.9:97.1.
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