CN109852415B - Method for strengthening bimolecular cracking in fluidized catalytic cracking reaction - Google Patents
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Abstract
The invention discloses a method for strengthening bimolecular cracking in a fluid catalytic cracking reaction, wherein a multielement catalytic material is added in a conventional fluid catalytic cracking reaction, and the multielement catalytic material is a mixture of an oxygen-containing compound, animal and vegetable fatty acid or processing residue thereof and an oil-soluble metal soap compound. After the multi-element catalytic material is added in the conventional fluid catalytic cracking reaction, the multi-element catalytic material can be preferentially adsorbed on the catalyst and reacts to generate low-carbon olefin which is easy to generate carbon positive ions, so that the cracking reaction of the conventional catalytic cracking alkane is mainly based on a bimolecular cracking reaction mechanism, the cracking reaction of the conventional catalytic cracking alkane is promoted, and the yield of the product gas hydrocarbon is improved.
Description
Technical Field
The invention relates to the technical field of fluidized catalytic cracking reaction, in particular to a method for strengthening bimolecular cracking in the fluidized catalytic cracking reaction.
Background
Fluid catalytic cracking is the reaction of petroleum catalytic cracking, the main body being petroleum. Catalytic cracking is one of petroleum refining processes, and is a process of converting heavy oil into cracked gas, gasoline, diesel oil and the like through a cracking reaction under the action of heat and a catalyst.
In the 80's of the 20 th century, it was recognized that vegetable oils could be readily cracked in conventional fluid catalytic cracking reactors (abbreviated as fluid catalytic cracking U for english) to yield products very similar to those produced from petroleum feedstocks.
In the prior art, there are many patent documents relating to the catalytic cracking reaction of animal and vegetable oils (the main component of which is oleic acid triglyceride) with an oxygen-containing compound alone or together with an oxygen-containing compound and a hydrocarbon feedstock.
The invention patent application CN1916135 discloses a method for producing fuel oil from biological oil, which is to directly carry out catalytic cracking on the biological oil, or a mixture of the biological oil and a catalytic cracking raw material, or a mixture of the biological oil and catalytic gasoline to generate a liquefied gas, gasoline and diesel oil mixture under the catalytic action of a solid acid catalyst, and the liquefied gas, gasoline and diesel oil products are obtained by distilling and separating the mixed product. The method has high yield, the sum of the liquefied gas, the gasoline and the diesel oil can reach 88-92% by weight, the content of propylene in the liquefied gas can reach more than 40% by weight, and the octane number of the gasoline research method is more than 95. Similarly, there is also an invention patent CN101379166B of International Shell research Co.
The invention patent CN101747134B discloses a method for producing low-carbon olefin by biomass catalytic cracking, which comprises the steps of contacting a biomass raw material or a raw material containing biomass and hydrocarbon oil with a cracking catalyst, and has higher low-carbon olefin yield; however, the production of low-carbon olefins is the main purpose of the patent and is not used for producing fuel oil such as gasoline and diesel.
The invention patent CN102206502B discloses a method for co-refining animal and vegetable oil and oxygen-containing compounds to prepare aromatic hydrocarbon and low-carbon olefin, which comprises introducing the raw materials of animal and vegetable oil and oxygen-containing compounds into a catalytic cracking reactor, and contacting with a catalytic cracking catalyst in the reactor to perform catalytic conversion reaction, wherein the operation temperature is 500-670 ℃, the operation pressure is 0.1-5.0MPa, and the weight hourly space velocity is 0.1-l00h-1The catalyst-oil ratio is 1-50, reaction oil gas and a spent catalyst are separated after reaction, the separated spent catalyst is recycled after steam stripping and coke burning regeneration, the reaction oil gas is fractionated to obtain fractions such as liquefied gas, gasoline and the like, wherein the liquefied gas fraction enters a subsequent gas separation system and is separated to obtain low-carbon olefin; the gasoline fraction is further extracted by aromatic hydrocarbon to obtain aromatic hydrocarbon products. The method has the advantages that the co-refining of the vegetable oil and the oxygen-containing compound is beneficial to controlling the reaction temperature, improving the selectivity of the target product gasoline and reducing the energy consumption; but the production of aromatics and light olefins is the main purpose of the patent and is not used for producing fuel oil such as gasoline and diesel.
Since the price of bio-oil is much higher than that of gasoline and diesel oil, low-carbon olefin and aromatic hydrocarbon, the above patent cannot be practically used for economic reasons.
The invention patent application CN101558135 discloses a process for the short contact time of oxygenated hydrocarbon compounds such as glycerol with bio-oil for fluid catalytic cracking, in which process the oxygenated hydrocarbon compounds are contacted with the fluid cracking catalytic feedstock for a period of less than 3 seconds, the contact time of less than 3 seconds requiring the addition of components for precise control.
Disclosure of Invention
In order to solve the problems, the invention provides a method for strengthening bimolecular cracking in a fluid catalytic cracking reaction.
A method for strengthening bimolecular cracking in a fluid catalytic cracking reaction, when injecting the conventional catalytic cracking raw materials into a fluid catalytic cracking reactor, adding multielement catalytic materials (the materials can be premixed in advance and can also be fed at different positions of a catalytic cracking riser respectively), and contacting the conventional catalytic cracking raw materials and the multielement catalytic materials with a catalyst in the fluid catalytic cracking reactor to carry out the catalytic cracking reaction; the multi-element catalytic material contains a mixture of a catalytic material A and a catalytic material B, wherein the catalytic material A is one or more oxygen-containing compounds and/or animal and vegetable fatty acids, and the catalytic material B is a mixture of one or more oil-soluble metal soap compounds.
After the multi-element catalytic material is added in the conventional fluid catalytic cracking reaction, the multi-element catalytic material can be preferentially adsorbed on the catalyst and reacts to generate low-carbon olefin which is easy to generate carbon positive ions, so that the cracking reaction of the conventional catalytic cracking alkane is mainly based on a bimolecular cracking reaction mechanism, the cracking reaction of the conventional catalytic cracking alkane is promoted, and the yield of the product gas hydrocarbon is improved. Typical products of the bimolecular cracking reaction mechanism are propylene and isobutane.
It is to be noted here that the cracking reaction of the conventional catalytically cracked alkanes without the addition of a multi-component catalyst is mainly based on a single molecular cracking reaction mechanism, and typical products are methane, ethylene and ethane.
Meanwhile, due to the autocatalytic property of the multi-component catalytic material, the conversion of the multi-component catalytic material is accelerated by the existence of the conventional catalytic cracking alkane, the secondary reaction of olefin which is an intermediate product of the conversion of the multi-component catalytic material is promoted to generate high-carbon hydrocarbon, the aromatization reaction of the olefin is particularly accelerated, and the thermal cracking of oxygen-containing compounds and animal and vegetable fatty acids is partially inhibited by the existence of the hydrocarbon.
The results can be verified through a pulse catalytic reaction experiment, the multi-component catalytic material can promote the activation process of alkane, especially has obvious activation effect on alkane molecules with strong adsorption capacity, and the promotion effect of the multi-component catalytic material is more obvious in large pore space and molecular sieve with high B acid site density at low reaction temperature, so that the initial activation and chain growth process in the cracking reaction of conventional catalytic cracking alkane are greatly enhanced by adding the multi-component catalytic material.
Research results of FT-IR and IPSR and catalytic experiments prove that the multi-element catalyst can be preferentially adsorbed on an acid site of a molecular sieve catalyst in a coupling reaction and is immediately converted into a surface alkane oxygen group which can be used as an active site to promote the initial activation of alkane in a hydrogen transfer mode; meanwhile, the conventional catalytic cracking alkane accelerates the catalytic conversion or cracking of the multi-component catalytic material in a coupling reaction to form olefin, a large number of olefin molecules can further promote the chain transfer process of the conventional catalytic cracking alkane in a bimolecular hydrogen transfer mode, and the final product distribution is determined.
The cracking of conventional catalytic cracking alkanes is mainly an endothermic reaction, while the catalytic conversion of the multi-component catalyst into an exothermic reaction, the reaction heats of the two processes have complementarity and cause interaction between the two. The reaction heat provided by the catalytic conversion of the multi-element catalyst can promote the cracking of the conventional catalytic cracking alkane, and the reaction heat absorbed by the cracking of the conventional catalytic cracking alkane can reduce the temperature of the secondary reaction of the oxygenated chemicals and the animal and vegetable fatty acid conversion intermediate products, thus being beneficial to the aromatization reaction.
As a preferable scheme, the conventional catalytic cracking raw material can be one or more of vacuum gas oil, coking heavy distillate oil, deasphalted oil, hydrogenated tail oil, atmospheric residue and vacuum residue.
As a preferable scheme, the oxygen-containing compound in the catalytic material A can be one or more of methanol, dimethyl ether, formaldehyde, furfural, acetic acid, methylal, methyl acetate, ethyl acetate, glycol, polyethylene glycol and glycerol which are relatively low in price.
Preferably, the animal and vegetable fatty acid in the catalytic material A can be finished animal and vegetable fatty acid, and can also be residual residue processed by using animal and vegetable fatty acid. Animal and vegetable fatty acids and their residual residues, also called acidified oil and its oil residue, are obtained by acidifying the byproduct soapstock produced in oil refinery. The fatty acid is long-chain fatty acid, and the carbon chain length is generally between 12 and 24, wherein the carbon chain with the length of 16 to 18 is mainly used. The main source of oil is the by-product of animal and vegetable oil refining, and fatty acid can be divided into saturated fatty acid and unsaturated fatty acid according to the source of oil. The main industrial use of animal and vegetable fatty acids is the manufacture of fatty acid methyl esters (biodiesel), also used for the production of oleic acid, but at a much lower price than animal and vegetable oils. The existence of the organic fatty acid center has a protection effect on the acid center of the catalyst, and the poisoning effect of basic nitrogen in the raw material on the catalyst is prevented.
As a preferable scheme, the content of the catalytic material B in the multi-element catalytic material is 1-2000ppm, wherein the oil-soluble metal soap compound is prepared by saponification reaction of one or more of magnesium, zirconium, molybdenum, tungsten, manganese, nickel, copper, silver, zinc and rare earth metals with one or more oil-soluble acid substances of oleic acid, isooctanoic acid and naphthenic acid, preferably by saponification reaction of one or more of rare earth metals with one or more oil-soluble acid substances of oleic acid, isooctanoic acid and naphthenic acid, and the rare earth metals are preferably cerium and/or lanthanum. The oil-soluble metal soap compound and the phosphorus element compound contained in the multi-element catalytic material can prevent the aromatic hydrocarbon compound from further polycondensation; and researches show that 1-1000ppm of oil-soluble metal soap compounds, particularly rare earth metal soap compounds can reduce the coking of organic oxygen-containing compounds on the catalyst and improve the coking resistance of the catalyst.
The catalyst used in the invention can adopt any catalyst suitable for the conventional fluid catalytic cracking process, and has no special requirements on the active components of the catalyst, such as various modified Y-type zeolites, ZSM-5 series zeolites and the like; likewise, the catalyst support and the binder are not particularly limited. But as a preferable scheme, the catalyst contains one or more of alkaline earth metal, IVB group metal, VIB group metal, VIIB group metal and VlIIB group metal, and the total content of the metal elements is 1-15 percent by weight calculated by oxides based on the mass of the catalyst; furthermore, the catalyst contains one or more of magnesium, zirconium, molybdenum, tungsten, manganese, nickel, copper, silver, zinc and vanadium, and the total content of the metal elements is 2-12% by weight of oxides based on the mass of the catalyst, wherein the content of nickel is less than 12000ppm and/or the content of vanadium is less than 6500 ppm. The substances containing the above-mentioned metal elements, such as salts or oxides, may be added during the preparation of the catalyst or may be prepared separately, for example in the form of auxiliaries, in the FCC unit.
Preheating the conventional catalytic cracking raw material and the multi-element catalytic material at 65-280 ℃, and then injecting the raw material and the multi-element catalytic material into a fluidized catalytic cracking reactor; the catalytic cracking reaction conditions in the fluidized catalytic cracking reactor are that the reaction temperature is 450--1The reaction pressure is 0.10-1.0 MPa; the reaction temperature is preferably 480 ℃ and 650 ℃, the weight hourly space velocity is preferably 2 to 140h, and the reaction pressure (absolute pressure) is preferably 0.10 to 0.5 MPa.
The mass ratio of the conventional catalytic cracking raw material to the multi-element catalytic material is 1:1-150:1, and the mass ratio of the catalyst to a catalytic cracking mixture composed of the conventional catalytic cracking raw material and the multi-element catalytic material is 1:50, preferably 2: 30.
The invention has the beneficial effects that: under the condition of fluid catalytic cracking reaction, the interaction of the multi-component catalyst and the conventional catalytic cracking alkane promotes the cracking reaction of the conventional catalytic cracking alkane, promotes the conversion of the multi-component catalyst and the secondary reaction, especially the aromatization reaction, of the multi-component catalyst and the intermediate product of the conversion of the conventional catalytic cracking alkane; meanwhile, the oil-soluble metal soap compound and the phosphorus element compound contained in the multi-element catalyst can prevent the aromatic hydrocarbon compound from further polycondensation; in short, the multi-element catalytic material is blended in the fluid catalytic cracking reactor, the catalytic cracking reaction mechanism can be partially changed, the characteristics of a final product are improved, the loss is reduced, the specific expression is that the content of aromatic hydrocarbon in gasoline is improved, the octane number of the gasoline is further improved, the yield of light oil and liquefied gas is improved, the yield of coke is reduced, the sulfur content of gasoline and diesel oil is reduced, and the economic benefit is very obvious.
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Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to specific embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Examples 1 to 2
Examples 3 to 4
Examples 5 to 6
Examples 7 to 8
Wherein, the composition of the raw oil is shown in table 1, the composition of the multi-component catalyst is shown in table 2, the chemical composition of the catalyst and related parameters thereof are shown in table 3, and the comparative example is shown in table 4.
TABLE 1
TABLE 2
| Catalyst and process for preparing same | A | B |
| Chemical composition, W% | ||
| Al2O3 | 47 | 50.1 |
| Na2O | 0.2 | 0.054 |
| Fe2O3 | 0.50 | 0.44 |
| Physical Properties | ||
| Specific surface m2/g | 167 | 204 |
| Pore volume ml/g | 0.37 | 0.28 |
| Bulk density g/cm3 | 0.66 | 0.79 |
| Abrasion index w%/h | 2.9 | 1.4 |
| Sieving | ||
| 0～20μm | 0.5 | 4.6 |
| 0～40μm | 6.4 | 15.8 |
| 0～149μm | 95.0 | 90.5 |
| Average particle diameter, μm | 66 | 76.9 |
| Ageing agent Activity, MA | 68 | 74 |
TABLE 3
TABLE 4
The invention has no special requirement on the preheating process, and can adopt the conventional preheating method in the field, such as heat exchange with other high-temperature media through a heat exchanger and the like.
The invention has no special requirements for the type of the fluidized reactor, and the conventional reactor type in the field is applicable to the invention, for example, any one of riser, fluidized bed, downer, reducing riser, moving bed, conveying line and the like or a composite reactor formed by combining the riser, the fluidized bed, the downer, the reducing riser, the moving bed, the conveying line and the like can be selected; the regenerator can be selected from single-stage regeneration, two-stage regeneration, a coke burning tank and the like. Similarly, the invention has no special requirements on the combination mode of the reactor and the regenerator, and can be parallel, coaxial and the like, and the requirement on the reaction residence time is more than 3 seconds.
The other process steps involved in the invention, such as oil separation, product separation, catalyst stripping, regeneration and the like are the same as those of the conventional fluidized catalytic cracking process.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. A method for strengthening bimolecular cracking in a fluid catalytic cracking reaction is characterized in that when a conventional catalytic cracking raw material is injected into a fluid catalytic cracking reactor, a multi-component catalytic material is added at the same time, and the conventional catalytic cracking raw material and the multi-component catalytic material are contacted with a catalyst in the fluid catalytic cracking reactor to carry out the catalytic cracking reaction;
the conventional catalytic cracking raw material is one or more of vacuum gas oil, coking heavy distillate oil, deasphalted oil, hydrogenated tail oil, atmospheric residue and vacuum residue;
the mass ratio of the conventional catalytic cracking raw material to the multi-element catalytic material is 1:1-150:1, and the mass ratio of the catalyst to a catalytic cracking mixture consisting of the conventional catalytic cracking raw material and the multi-element catalytic material is 1: 50;
the multi-component catalyst contains a mixture of a catalyst A and a catalyst B, wherein the catalyst A is one or more oxygen-containing compounds and/or animal and vegetable fatty acids, the catalyst B is a mixture of one or more oil-soluble metal soap compounds, and the content of the catalyst B in the multi-component catalyst is 1-2000 ppm;
the oxygen-containing compound in the catalyst A is one or more of methanol, dimethyl ether, formaldehyde, furfural, acetic acid, methylal, methyl acetate, ethyl acetate, ethylene glycol, polyethylene glycol and glycerol.
2. The method for enhancing bimolecular cracking in fluid catalytic cracking according to claim 1, wherein the oil-soluble metal soap compound in the catalyst material B is obtained by saponification of one or more of magnesium, zirconium, molybdenum, tungsten, manganese, nickel, copper, silver, zinc and rare earth metals with one or more oil-soluble acid substances such as oleic acid, isooctanoic acid and naphthenic acid.
3. The method for enhancing bimolecular cracking in fluid catalytic cracking according to claim 2, wherein the oil-soluble metal soap compound in the catalytic material B is obtained by saponification of one or more rare earth metals with one or more oil-soluble acid substances selected from oleic acid, isooctanoic acid and naphthenic acid.
4. The method for enhancing bimolecular cracking in a fluidized catalytic cracking reaction according to claim 2 or 3, wherein cerium and/or lanthanum is used as the rare earth metal.
5. The method for enhancing bimolecular cracking in a fluidized catalytic cracking reaction according to claim 1, wherein the catalyst contains one or more of alkaline earth metals, group IVB metals, group VIB metals, group VIIB metals, group VlIIB metals, and the total content of the above metal elements is 1-15% by mass of the catalyst in terms of oxides.
6. The method for enhancing bimolecular cracking in a fluidized catalytic cracking reaction according to claim 5, wherein the catalyst contains one or more of magnesium, zirconium, molybdenum, tungsten, manganese, nickel, copper, silver, zinc and vanadium, and the total content of the above metal elements is 2-12% by mass of the catalyst in terms of oxides.
7. The method of enhancing bimolecular cracking in a fluidized catalytic cracking reaction according to claim 6, wherein the catalyst has a nickel content of less than 12000ppm and/or a vanadium content of less than 6500 ppm.
8. The method for enhancing bimolecular cracking in a fluidized catalytic cracking reaction according to claim 1, wherein the conventional catalytic cracking feedstock and the multi-component catalytic feedstock are preheated at 65-280 ℃ and then injected into the fluidized catalytic cracking reactor; the catalytic cracking reaction conditions in the fluidized catalytic cracking reactor are that the reaction temperature is 450--1And the reaction pressure is 0.10-1.0 MPa.
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| CN102206503A (en) * | 2010-03-31 | 2011-10-05 | 中国石油化工股份有限公司 | Gasoline preparing method by refining plant oil and oxygenated chemicals together |
| CN104557377A (en) * | 2013-10-28 | 2015-04-29 | 中国石油化工股份有限公司 | Method for producing ethylene and propylene from oxygen-containing compound and naphtha by coupled reaction |
| CN109423322A (en) * | 2017-08-24 | 2019-03-05 | 中国石油化工股份有限公司 | A kind of method of coal derivative catalytic pyrolysis |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101239866A (en) * | 2007-02-07 | 2008-08-13 | 中国石油化工股份有限公司 | Method for producing ethylene and propylene from oxygen-containing compounds |
| CN101314724A (en) * | 2007-05-31 | 2008-12-03 | 中国石油化工股份有限公司 | Combined catalytic conversion method for biological oil and fat and mineral oil |
| CN102206503A (en) * | 2010-03-31 | 2011-10-05 | 中国石油化工股份有限公司 | Gasoline preparing method by refining plant oil and oxygenated chemicals together |
| CN104557377A (en) * | 2013-10-28 | 2015-04-29 | 中国石油化工股份有限公司 | Method for producing ethylene and propylene from oxygen-containing compound and naphtha by coupled reaction |
| CN109423322A (en) * | 2017-08-24 | 2019-03-05 | 中国石油化工股份有限公司 | A kind of method of coal derivative catalytic pyrolysis |
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