CN101898143B - Inferior heavy oil cracking and gasifying catalyst - Google Patents
Inferior heavy oil cracking and gasifying catalyst Download PDFInfo
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- CN101898143B CN101898143B CN200910143623A CN200910143623A CN101898143B CN 101898143 B CN101898143 B CN 101898143B CN 200910143623 A CN200910143623 A CN 200910143623A CN 200910143623 A CN200910143623 A CN 200910143623A CN 101898143 B CN101898143 B CN 101898143B
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Abstract
The invention discloses an inferior heavy oil cracking and gasifying catalyst, comprising carrier, binder, gasification active components and cracking active components, wherein the gasification active components are alkali metals and alkaline-earth metals, by taking the catalyst total content as a reference, the oxide content is 2-30%, the atom ratio of the alkali metals to the alkaline-earth metals is (0.05-1.1):1, and the cracking active components are shape selective zeolite with the silica alumina ratio within 20-200. The catalyst aims to the inferior heavy oil processing procedure, considers heavy oil cracking and coke high temperature gasification and improves light oil yield and coke gasification reaction rate obviously.
Description
Technical field
The present invention relates to inferior heavy oil coking and the employed catalyst of coke gasification hydrogen production process.
Background technology
Crude oil heaviness, the development trend of poor qualityization and the increasingly stringent of relevant environmental regulation in the world wide, hydrogenation becomes one of counter-measure.But present hydrogen production process, production cost is higher, and output also is difficult to satisfy the needs of hydrogenation.It is extremely important to develop cheap hydrogen production process.
At present, heavy, inferior feedstock oil have proposed challenge to catalytic cracking process itself and catalyst.The processing of inferior heavy oil on-catalytic comprises delayed coking, fluid coking, flexicoking, solvent deasphalting etc., comes into one's own day by day.But coking process exists liquid to receive the problem that not high and low quality coke is difficult to utilize.What solvent deasphalting also was faced with a large amount of de-oiled asphalts rationally utilizes problem.The liquid of fluid coking, flexicoking is received suitable with delayed coking, but reaction bed is fluid bed or ebullated bed, is convenient to continuous operation.The burning of part coke provides system capacity, and rest parts adopts air or O
2, C0
2, gasification such as water vapour produces the combustible gas with certain calorific value.Ubiquitous problem is: coking predecessor concentration increases in the coking reactor, covers the fluidizing agent surface, mutual viscous between the particle, and the size distribution of particle broadens in the system, the fluid effect variation.The calorific value of combustion gas that gasification furnace produces depends on the gasifying agent that gasification is used, adopts different gasifying agents all to have some shortcomings.In addition, in gasifier, the temperature that gasification reaction needs is higher, and is high to the requirement of equipment material generally at 800～1200 ℃, and in addition, the slag that vanadium, nickel produce causes problems such as the gasifying agent air inlet is not smooth, some component corrosion is serious.
Catalytic cracking, particularly residual oil or RFCC adopt molecular sieve catalyst.Generally about 700 ℃, if regeneration temperature is higher than 750 ℃, then the catalyst hydrothermal stability will receive serious challenge to regeneration temperature.
General molecular sieve catalyst is that acidic site plays main catalytic activity effect in the characteristics of catalytic cracking or the application of other field.CN1216941A utilizes alkali-earth metal modified nonzeolite small pore molecular sieve (SAPO) to make it can be used in the oxygenatedchemicals catalytic conversion process; CN1255474A adopts the metal-modified zeolite that comprises alkaline earth, is used for producing the light olefin technical process by low-carbon alkanes; CN1310222A then is compound in molecular sieve with alkaline-earth metal, improves catalyst selectivity, improves diesel oil and high-knock rating gasoline yield; CN1894037A has also used alkaline-earth metal when preparation alkali magnesium zeolite.
Improving the anti-metal of catalyst particularly in the research of pollution of vanadium, also there is the people that alkaline-earth metal is introduced catalyst.CN1125249A introduces zeolite catalyst with the titanate form of alkaline-earth metal with alkaline-earth metal; CN1490287A uses the zeolite catalyst that contains different metal in the method for preparing ethene and propylene, catalyst is matrix with the aluminium oxide, does not contain kaolin, and the purpose that adds metal is to improve acidity of catalyst, thereby reduces coking.The alkaline-earth metal of CN1067670A load 0.1～20% on alumina particle is combined into the hydrocarbon cracking catalyzer that can consolidate vanadium with molecular sieve.CN1186105A then adopts 10～95% sour extracting kaolin, 0～30% rare earth oxide and alkaline earth oxide, 0～40% zeolite molecular sieve, 0～50% protokaolin, 0～15% aluminium chloride to process a kind of catalyst, uses with the synthetic or semi-synthetic full Cracking catalyst combination of another kind then.It is 4: 1～1: 40 mixed solution dipping matrix that CN1542089A has adopted vanadium and alkaline-earth metal mol ratio, processes the hydrocarbon cracking catalyzer that can fall sulphur with the molecular sieve compatibility then.CN1676576A is with a kind of as multiple heat-resisting inorganic oxide in its molecular sieve hydrocarbon cracking catalyzer of alkaline-earth metal.CN1854255A then processes the binding agent slurries with alkaline-earth metal with making beating such as aluminium stone, aluminium colloidal sol, rare earths, mixes making beating then with matrix slurries, molecular sieve pulp, sprays and process the Cracking catalyst of anti-metallic pollution.CN101190416A mixes the part that forms catalytic cracking catalyst with metal oxides such as magnesium, vanadium with aluminium oxide and kaolin, and mixed method has dipping, co-precipitation and mixes and pinch, the preferred method of pinching of mixing.
Summary of the invention
The object of the invention is to provide a kind of prior art that is different from, and is specially adapted to inferior heavy oil, possesses the catalyst of cracking of catalysis hydrocarbon ils and catalytic coke gasification simultaneously.
Inferior heavy oil coking gasifying catalyst provided by the invention; It is characterized in that containing carrier, binding agent, cracking activity component and gasification active component, said cracking activity component is that silica alumina ratio is 20～200 shape-selective molecular sieve, and said gasification reactivity component is alkali metal and alkaline-earth metal; The atomic ratio of alkali metal and alkaline-earth metal is (0.05～1.1): 1; Gross weight with catalyst is a benchmark, and the gasification reactivity component counts 2～30% with oxide, and the cracking activity component is 5～30%.
The present invention also provides above-mentioned Preparation of catalysts method:
1, carrier is mixed with the gasification reactivity component, add deionized water, stir, pull an oar; Obtain slurries A, the solid content of slurries A is 20～50%, carrier with in the mass ratio of the gasification reactivity component of oxide in (1～3.5): 1; Slurry temperature is at 20～80 ℃ during stirring, and the pH value is 3～7;
2, binding agent is mixed with deionized water, solid content adds inorganic acid 20～40%, regulates the pH value 1～5, stirs, and processes slurries B;
3, shape-selective molecular sieve is processed slurries C, make slurry solid content 20～40%;
4, with above-mentioned slurries A, B, C mixing and stirring, spray-drying obtains said catalyst.
Catalyst provided by the invention, elder generation is with carrier and the gasification reactivity component makes up or glue joins, thereby active component is strapped on the carrier.The control alkali metal content, the compound proportion of adjusting and alkaline-earth metal is worked in coordination with gasification reaction is carried out catalytic action simultaneously.At utmost brought into play the catalytic gasification function, the alkalescence of the metal that weakened simultaneously is to the influence of acidity of catalyst.Catalyst aims inferior heavy oil processing procedure of the present invention has been taken into account residual oil cracking and coke high-temperature gasification, has improved the yield and the coke gasification speed of light oil significantly.
The specific embodiment
This catalyst is primarily aimed at inferior heavy oil fluid coking-gasification technical process, has taken into account residual oil cracking, coke high-temperature gasification, can improve the yield and the coke gasification speed of light oil more significantly.The origin of catalytic cracking effect is the acidic site on the catalyst, and like B acid and L acid, and the active sites of catalytic gasification effect is alkali metal or alkaline-earth metal.Obviously, analyze alkalescence from the physico-chemical property aspect and can weaken the other side each other with acid, still, the inventor finds that from the Preparation of Catalyst aspect, holding quantity or ratio is the key point of dealing with problems.It is exactly that two conflicting aspects are in harmonious proportion together that alkali metal and alkaline-earth metal and molecular sieve compatibility are formed bifunctional catalyst.The purpose of utilizing alkali-earth metal modified molecular sieve is the acidity of regulating catalyst, carries out modification through the acidic site to molecular sieve and can make catalyst applications in different reaction purposes.
In the catalyst provided by the invention, said carrier is selected from kaolin or acid treatment kaolin, and binding agent is selected from one or more the mixture in boehmite, aluminium colloidal sol or the Ludox.
Described catalytic cracking active component is selected from silica alumina ratio at 20～200, preferred 30～100 the selecting property molecular sieve or the selecting property molecular sieve of modification, and like ZSM-5, ZRP etc., ZSM-5 and ZRP are zeolite well-known to those skilled in the art.
Described gasification reactivity component is selected from alkali metal and alkaline-earth metal.Alkali metal such as lithium, sodium, potassium, rubidium, alkaline-earth metal such as magnesium, calcium, strontium, barium.Preferred gasification reactivity component is the combination of sodium or potassium and calcium or magnesium, like sodium and magnesium, sodium and calcium, potassium and magnesium, potassium and calcium, the more preferably combination of potassium and calcium.With the catalyst quality is benchmark, and the oxide addition of alkali metal and alkaline-earth metal is 1～30%, preferred 5～20%.The atomic ratio of alkali metal and alkaline-earth metal is in (0.05～1.1): 1, preferred (0.08～0.8): 1.In catalyst provided by the invention, for the combination of potassium and calcium, the two atomic ratio is preferably (0.1～0.2): 1.
In the method provided by the invention, the Preparation of catalysts process can be divided into steps such as three making beating, mixing, spraying.
First making beating is that carrier mixes making beating with the gasification reactivity component.When carrier and the making beating of gasification reactivity component, both all add slurries by the requirement of catalyst total amount.Slurry solid content is 20～50%, preferred 25～40%.Slurry temperature is at 20～80 ℃ during stirring, the pH value 3～7, preferred 3.5～5.5, mixing time is between 10～60 minutes.Said alkaline-earth metal and alkali-metal compound add with compound forms such as oxide, hydroxide, carbonate, chloride, nitrate, preferred carbonate and chloride.
Second making beating is that binding agent is processed slurries, makes slurry solid content 20～40%, adds proper inorganic acid example hydrochloric acid, acetic acid, regulate the pH value 1～, stirred 10～60 minutes, left standstill 20～60 minutes.
The 3rd making beating is molecular sieve to be pulled an oar separately process slurries, and slurry solid content is 20～50%, preferred 30～45%.The molecular sieve addition is between 5～30%, and according to molecular sieve silica alumina ratio adjustable size whole molecule sieve addition, silica alumina ratio is big, suitably increases additional proportion.
Method provided by the invention is that above-mentioned three kinds of slurries are mixed, and stirs 10～60 minutes, is spray dried to the microspherical catalyst of average grain diameter at 65～90 μ m.
Catalyst contacts with inferior heavy oil in cracker, and the heat transferred oil droplet of self, and catalyzed oil drops in its surface generation cracking reaction.The less molecular hydrocarbon that produces gets into gas phase, and macromolecule hydrocarbon forms coke in the catalyst surface polycondensation.In gasification furnace, the gasification reaction of catalyst activation gasifying agent molecule STRENGTH ON COKE this shows that catalyst should possess certain specific area and acidic site quantity, abrasion resistance, catalytic gasification reactive activity component preferably.Because catalyst circulates in the high and low temperature reaction zone, therefore should possess mechanical strength and hydrothermal stability preferably, catalyst provided by the invention, its wear-resistant index is all less than 1.0%h
-1
Through embodiment the present invention is described further below, but does not therefore limit content of the present invention.
Embodiment 1
Get 6 kilograms of kaolin and place in the container, add 18 kilograms of deionized waters, stir and under 30 ℃ of temperature, mix evenly, add the mixture of 2 kilograms of potassium oxides and calcium oxide while stirring, wherein the atomic ratio of potassium and calcium is 0.2, and it is for use to stir.
Get 1 kilogram of silica alumina ratio and be 20 ZRP molecular sieve, it is evenly for use to add 1.5 kilograms of deionized water and stirring.
Get 0.7 kilogram of boehmite, add 1.2 kilograms of deionized waters, stir, add 0.3 kilogram of aluminium colloidal sol, stirred 10 minutes, add appropriate hydrochloric acid, make slurry pH value between 1.2～3.0, left standstill 30 minutes.
Above-mentioned three kinds of slurries are mixed, stirred 20 minutes, and spray-drying makes the solid particle average grain diameter between 65～90 μ m, and 600 ℃ of roastings obtained catalyst in 60 minutes, were numbered Cat-1.
Embodiment 2～7
According to the preparation method of embodiment 1, adjust each amounts of components, prepare catalyst Cat-2, Cat-3, Cat-4, Cat-5, Cat-6, the Cat-7 of different component content respectively.Its composition is seen table 1.
Comparative Examples 1
This comparative catalyst's composition is with the catalyst of embodiment 7, and difference is to contain potassium and the alkali-free earth metal in the gasification reactivity component, forms and sees table 1.
Comparative Examples 2
This comparative catalyst's composition is with the catalyst of embodiment 7, and difference is calcic in the gasification reactivity component and the alkali-free metal, forms and sees table 1.
Test case
Be to carry out poor oil (character is seen table 2) catalytic cracking experiment on the fixed fluidized bed experimental provision of 300 gram scales at catalyst inventory.500 ℃ of reaction temperatures, weight (hourly) space velocity (WHSV) 5h
-1, oil ratio 7, cracked reaction product distribution experiment result is shown in table 3.
Through surface coverage after the cracking reaction catalyst of coke loaded in fixed fluidized bed gasification reactor, under 860 ℃, carry out gasification reaction, gasifying agent is the mist of steam and oxygen, wherein the oxygen molar content is 20%.Reaction product gas is formed and factor of created gase is seen table 4.
Table 2
| Project | Numerical value |
| Density (20 ℃)/(g/cm 3) | 0.9908 |
| Kinematic viscosity/(mm 2/s) | |
| 120℃ | 98.77 |
| 140℃ | 46.90 |
| Carbon residue/w% | 16.8 |
| Mean molecule quantity/(g/mol) | 548 |
| Four components/w% | |
| Saturated hydrocarbons | 29.0 |
| Aromatic hydrocarbon | 32.5 |
| Colloid | 23.8 |
| Asphalitine | 14.7 |
| Elementary analysis/w% | |
| C | 85.68 |
| H | 10.64 |
| S | 2.5 |
| N | 0.35 |
Claims (10)
1. an inferior heavy oil cracking and gasifying catalyst is characterized in that containing carrier, binding agent, cracking activity component and gasification active component, and said cracking activity component is that silica alumina ratio is 20～200 shape-selective molecular sieve; Said gasification reactivity component is alkali metal and alkaline-earth metal, and the atomic ratio of alkali metal and alkaline-earth metal is (0.05～1.1): 1, and be benchmark with the gross weight of catalyst; The gasification reactivity component counts 2～30% with oxide, and the cracking activity component is 5～30%, and this catalyst prepares through following step: carrier is mixed with the gasification reactivity component; Add deionized water, stir, pull an oar, obtain slurries A; The solid content of slurries A is 20～50%; Carrier with in the gasification reactivity constituent mass ratio of oxide in (1～3.5): 1, slurry temperature is at 20～80 ℃ during stirring, the pH value is 3～7; Binding agent is mixed with deionized water, and solid content adds inorganic acid 20～40%, regulates the pH value 1～5, stirs, and processes slurries B; Shape-selective molecular sieve is processed slurries C, make slurry solid content 20～40%; With above-mentioned slurries A, B, C mixing and stirring, spray-drying obtains catalyst.
2. according to the catalyst of claim 1, it is characterized in that said carrier is selected from kaolin, binding agent is selected from one or more the mixture in boehmite, aluminium colloidal sol or the Ludox.
3. according to the catalyst of claim 1, said shape-selective molecular sieve is ZSM-5 or ZRP.
4. according to the catalyst of claim 3, wherein the silica alumina ratio of said shape-selective molecular sieve is 30～100.
5. according to the catalyst of claim 1, be benchmark with the gross weight of catalyst, vector contg is 10～70%, binder content is 11～30%.
6. according to the catalyst of claim 1 or 5, be benchmark with the gross weight of catalyst, said binding agent is 10～29% boehmite and 1～10% aluminium colloidal sol or Ludox.
7. according to the catalyst of claim 1, it is characterized in that said alkali metal is sodium or potassium, alkaline-earth metal is calcium or magnesium.
8. according to the catalyst of claim 1, wherein said alkali metal is potassium, and alkaline-earth metal is a calcium, and the atomic ratio of potassium and calcium is (0.1～0.2): 1.
9. claim 1 Preparation of catalysts method is characterized in that this method comprises:
1) carrier is mixed with alkali metal compound and alkaline earth metal compound; Add deionized water, stir, pull an oar, obtain slurries A; The solid content of slurries A is 20～50%; Carrier with in the gross mass ratio of the alkali metal compound of oxide and alkaline earth metal compound in (1～3.5): 1, slurry temperature is at 20～80 ℃ during stirring, the pH value is 3～7;
2) binding agent is mixed with deionized water, solid content adds inorganic acid 20～40%, regulates the pH value 1～5, stirs, and processes slurries B;
3) shape-selective molecular sieve is processed slurries C, make slurry solid content 20～40%;
4) with above-mentioned slurries A, B, C mixing and stirring, spray-drying obtains catalyst.
10. according to the preparation method of claim 9, it is characterized in that said alkali metal compound is selected from alkali-metal oxide, carbonate, chloride or nitrate.
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| KR101874152B1 (en) * | 2011-07-27 | 2018-07-03 | 사우디 아라비안 오일 컴퍼니 | Process for the gasification of heavy residual oil with particulate coke from a delayed coking unit |
| CN103566918B (en) * | 2012-07-26 | 2015-09-23 | 中国石油化工股份有限公司 | A kind of multi-functional catalyst composition |
| CN103566962B (en) * | 2012-07-26 | 2016-05-25 | 中国石油化工股份有限公司 | A kind of multi-functional catalyst composition |
| CN103962175B (en) * | 2013-01-24 | 2016-08-03 | 中国科学院过程工程研究所 | A kind of heavy oil cracking and gasifying bifunctional catalyst and preparation method thereof |
| CN104741138B (en) * | 2013-12-31 | 2017-08-22 | 中国石油化工股份有限公司 | A kind of multi-functional catalyst composition |
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| CN106179478B (en) * | 2015-04-29 | 2019-05-21 | 中国石油化工股份有限公司 | A kind of cracking gasification process of cracking gasification catalyst composition, preparation method and petroleum hydrocarbon |
| CN106179456B (en) * | 2015-04-29 | 2019-08-16 | 中国石油化工股份有限公司 | A kind of cracking gasification process of cracking gasification catalyst composition, preparation method and petroleum hydrocarbon |
| CN111686790A (en) * | 2019-03-12 | 2020-09-22 | 中国石油天然气股份有限公司 | Catalytic cracking gasoline octane number auxiliary agent with low liquefied gas yield and preparation method thereof |
| CN115582141B (en) * | 2021-07-06 | 2023-08-22 | 中国石油天然气股份有限公司 | Catalyst for slurry cracking and coke gasification thereof and preparation method thereof |
| CN113522345B (en) * | 2021-07-22 | 2022-05-13 | 太原理工大学 | Ordered mesoporous Al-SBA-15 supported sulfated zirconia solid acid material and preparation and application thereof |
| CN113769727B (en) * | 2021-09-07 | 2023-12-08 | 中海油天津化工研究设计院有限公司 | High-stability solid base catalyst and preparation method thereof |
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