CN117000298A - Catalytic cracking catalyst regeneration system and regeneration method - Google Patents
Catalytic cracking catalyst regeneration system and regeneration method Download PDFInfo
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Abstract
The application relates to a catalytic cracking catalyst regeneration system and a regeneration method, wherein the catalytic cracking catalyst regeneration system comprises a biomass processing unit and a regeneration unit. The regeneration system adopts biomass oil to supply energy to the catalytic cracking device, reasonably applies biomass energy to the catalytic cracking regeneration system, radically changes the energy source of the device, can greatly reduce the carbon emission of the catalytic cracking unit, and can also provide energy for other process units; the concentration of carbon dioxide in the flue gas is higher, which is beneficial to separation and trapping.
Description
Technical Field
The application relates to a regeneration method of a carbon-containing catalyst in a hydrocarbon processing process. More particularly, the application relates to a catalyst regeneration method for realizing carbon dioxide emission reduction and strengthening energy supply of a regeneration device in a catalytic cracking process.
Background
Today, the development of the global oil refining industry faces many challenges such as new energy substitution, energy conservation and emission reduction requirements and the like. Flexible adjustment of cracking production schemes, reduction of carbon dioxide emissions, and reduction of climate change have become necessary routes for the refinery industry to change economic growth and maintain sustainable development. Therefore, the effective reduction of carbon emission in petroleum refining and chemical production processes is particularly important, and the research on low-carbonization catalytic cracking schemes for reducing and increasing oil is an important task in the future of refineries. The carbon emission in the heavy oil processing process is mainly the flue gas emission of equipment such as catalytic cracking and burning, hydrogen production process, boilers and the like and the energy consumption in the technical process. The catalytic cracking device is core equipment in a refinery, carbon emission caused by burning of a catalytic cracking regenerator accounts for 24-55% of carbon emission of the whole plant, the total carbon dioxide emission accounts for nearly 1% of the total national carbon dioxide emission, and the catalytic cracking device is a key point of carbon emission reduction in petrochemical industry.
US5565089 discloses a catalytic cracking catalyst regeneration process, which comprises the steps of firstly burning with air, then recovering carbon dioxide in flue gas, recycling and gradually incorporating the carbon dioxide into an oxygen-containing gas stream until the temperature in a regenerator is normal, and finally injecting only oxygen and carbon dioxide for catalyst regeneration. The process focuses on the regeneration process air intake system and flue gas treatment, but the carbon dioxide produced by the energy supply is still all derived from fossil energy sources.
CN1600431a discloses an incomplete regeneration flue gas combustion technology, which adopts a method of supplementing air in the incomplete regeneration flue gas to enable CO in the non-regenerated flue gas to continue to burn, raise the temperature of the flue gas, improve the recovery efficiency of the flue gas machine, and furthest recover the pressure energy of the flue gas, thereby reducing the energy consumption of the device. The method can improve the energy utilization efficiency, but can not effectively reduce the carbon dioxide emission.
The reaction-regeneration system of the catalytic cracking device is a periodical heat taking-heat releasing heat balance process, and heat generated by burning the regeneration system is used for supplying the reaction system. The production mode of oil reduction and increase is beneficial to promote sustainable development of the oil refining industry, but more reaction heat is also needed. When the scorching amount is insufficient to meet the energy consumption of the device, fossil fuel is usually added for heat compensation, so that the emission amount of carbon dioxide is increased, the resource waste is also caused, and the conflict exists between the development trend and the environmental protection requirement. The carbon dioxide emission can be reduced to a certain extent by optimizing the regeneration process or recycling the discharged carbon dioxide. However, the above-described technical route mainly focuses on reducing carbon dioxide emissions to the atmosphere generated during the regeneration process, and does not reduce carbon dioxide generation.
Therefore, there is a need to develop a catalyst regeneration method that fundamentally reduces carbon dioxide emissions from fossil energy sources, reduces carbon dioxide emissions on the basis of satisfying the energy supply required for the apparatus, and achieves low carbonization development.
Disclosure of Invention
The application aims to provide a catalyst regeneration method for fundamentally reducing carbon dioxide emission from fossil energy based on the prior art.
The application provides a catalytic cracking catalyst regeneration system, comprising:
a biomass processing unit comprising:
a biomass pretreatment device for pretreating biomass,
the biomass liquefying device is used for processing the pretreated biomass to obtain a biomass oil crude product,
the dehydration system is used for carrying out dehydration treatment on the biomass oil crude product to obtain biomass oil;
a storage tank for storing the biomass oil;
a regeneration unit, the regeneration unit comprising:
a regenerator, the regenerator comprising:
a scorch section, and
a dense phase regeneration section,
wherein the dense phase regeneration section is positioned above the scorching section, and an outlet of the scorching section is contained inside the dense phase regeneration section, so that the scorching section is in fluid communication with the dense phase regeneration section;
the scorching section is provided with:
a first oxygen inlet arranged at the bottom of the burning section and used for inputting oxygen into the burning section;
the first circulating flue gas inlet is used for circulating a part of flue gas recovered by the dense-phase regeneration section back into the coking section; and
a spent catalyst inlet for conveying spent catalyst of a catalytic cracking reactor to the interior of the burn-in section;
the to-be-generated catalyst inlet is connected with a to-be-generated inclined tube communicated with the catalytic cracking reaction system, and a mixing tank is arranged in the to-be-generated inclined tube;
the storage tank is communicated with the mixing tank, so that biochar particles in the storage tank are conveyed to the mixing tank, mixed with spent catalyst and then conveyed to the burning section;
the dense phase regeneration section is provided with:
the second oxygen inlet is arranged at the bottom of the dense-phase regeneration section and is used for inputting oxygen into the dense-phase regeneration section;
the second circulating flue gas inlet is used for circulating part of flue gas recovered by the dense-phase regeneration section back to the interior of the dense-phase regeneration section; and
a flue gas outlet arranged at the top of the dense phase regeneration section;
the dense-phase regeneration section is also provided with a heat collector for conveying heat to the outside of the regenerator.
The present application also provides a catalytic cracking catalyst regeneration process, which is carried out in the regeneration system of the present application,
the method comprises the following steps:
s1, conveying biomass to a liquefying device for liquefying after pretreatment to obtain a biomass oil crude product;
s2, dehydrating the biomass oil crude product in a dehydration system to obtain biomass oil, and conveying the biomass oil to a storage tank;
s3, conveying the biomass oil to a mixing tank, mixing the biomass oil with a spent catalyst from a catalytic cracking reactor, conveying the mixture to the inside of a burning section, and contacting the mixture with oxygen to partially burn the spent catalyst;
s4, the materials from the scorching section enter a dense phase regeneration section, and oxygen is injected into the dense phase regeneration section through a second oxygen inlet, so that the catalyst is completely regenerated.
In one embodiment, the liquefaction process comprises a hydrothermal liquefaction process, an alcohol thermal liquefaction process, or a pyrolysis process.
In one embodiment, the hydrothermal liquefaction process is at a temperature of no less than 200 ℃ and a pressure of no less than 4.0MPa; the alcohol thermal liquefaction treatment adopts a solvent selected from methanol and glycol; the pyrolysis treatment is fast pyrolysis or flash pyrolysis, the heating rate is not lower than 100 ℃/s, and the residence time is not higher than 10s.
In one embodiment, the weight ratio of spent catalyst to introduced biomass oil is 10-300:1.
In one embodiment, the temperature of the regenerator bed is controlled by the heat extractor to not exceed 750 ℃, preferably not to exceed 720 ℃.
In one embodiment, the operating conditions of the scorch section are: the temperature is 560-730 ℃, the average residence time of the catalyst is 10-120 seconds, and the apparent linear velocity of the gas is 0.8-3.0m/s.
In one embodiment, the operating conditions of the dense phase regeneration zone are: the temperature is 580-750 ℃, the average residence time of the catalyst is 1.0-5.0 minutes, and the apparent linear velocity of gas is 0.3-0.8m/s.
In one embodiment, the biomass is selected from the group consisting of agricultural and forestry biomass, aquatic plants, and energy crops.
In one embodiment, the oxygen concentration in the char section is no more than 28% by volume; in the dense phase regeneration zone, the oxygen concentration does not exceed 28% by volume.
In one embodiment, the char ratio in the char section is 40-50%; the scorching proportion of the dense phase regeneration section is 50-60%.
In one embodiment, the temperature of the dense phase regeneration zone bed is controlled via the heat extractor to not exceed 750 ℃, preferably not to exceed 720 ℃.
Compared with the existing catalytic cracking catalyst regeneration method, the method has the main advantages that:
(1) Biomass is cheap and easy to obtain, and carbon in the biomass is derived from carbon dioxide captured by plants from air; biomass energy is introduced into a catalytic cracking regeneration system in a proper mode to replace the original fossil fuel energy supply, so that the emission of carbon dioxide can be reduced, and the low carbonization development of oil refining is realized.
(2) Biomass oil can be obtained by biomass liquefaction, the preparation process is simple, the combustion heat value of the biomass is obviously improved compared with that of the biomass, the biomass oil is convenient to uniformly mix with spent catalyst, and the occurrence of local overheating in the burning process can be avoided.
(3) The biomass oil obtained by biomass liquefaction can be used as fuel for energy supply without separation and purification, so that the process is simplified, the cost is saved, and the utilization mode and the way of biomass energy are expanded.
(4) The surplus heat generated by the regeneration system can be used for generating high-pressure steam to supply other devices; after the generated flue gas is subjected to energy recovery, carbon dioxide in the flue gas can be separated and trapped, so that carbon dioxide emission is realized.
Drawings
The accompanying drawings are included to provide a further understanding of the application, and are incorporated in and constitute a part of this specification, illustrate the application and together with the description serve to explain, without limitation, the application.
FIG. 1 is a schematic diagram of one embodiment of a regeneration system of the present application.
Detailed Description
The application is further described in detail below by means of the figures and examples. The features and advantages of the present application will become more apparent from the description.
The word "exemplary" is used herein to mean "serving as an example, embodiment, or illustration. Any embodiment described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments. Although various aspects of the embodiments are illustrated in the accompanying drawings, the drawings are not necessarily drawn to scale unless specifically indicated.
In addition, the technical features described below in the different embodiments of the present application may be combined with each other as long as they do not collide with each other.
The application provides a catalytic cracking catalyst regeneration system and a regeneration method performed in the regeneration system. The regeneration process of the present application is further described below in conjunction with the catalytic cracking catalyst regeneration system of the present application. The same applies to the regeneration system with respect to the embodiments of the regeneration method and vice versa.
As shown in fig. 1, the present application provides a catalytic cracking catalyst regeneration system for reducing carbon dioxide emissions, comprising: a biomass processing unit 300 and a regeneration unit 200.
The present application provides a catalytic cracking catalyst regeneration process, which can be performed in the regeneration system of the present application,
the method comprises the following steps:
s1, conveying biomass to a liquefying device for liquefying after pretreatment to obtain a biomass oil crude product;
s2, dehydrating the biomass oil crude product in a dehydration system to obtain biomass oil, and conveying the biomass oil to a storage tank;
s3, conveying the biomass oil to a mixing tank, mixing the biomass oil with a spent catalyst from a catalytic cracking reactor, conveying the mixture to the inside of a burning section, and contacting the mixture with oxygen to partially burn the spent catalyst;
s4, the materials from the scorching section enter a dense phase regeneration section, and oxygen is injected into the dense phase regeneration section through a second oxygen inlet, so that the catalyst is completely regenerated.
As shown in fig. 1, in the catalytic cracking reaction system 100, a catalytic cracking reactor 110 is used to perform catalytic cracking reaction: the bottom inlet 102 of which is fed with a lifting medium to lift the regenerated catalyst (from the regeneration unit 200) entering the regenerated catalyst inlet 103; the feedstock entering from feedstock inlet 101 contacts the catalyst to perform a catalytic cracking reaction. The reacted oil and gas products are separated by the oil agent separating device 120, and the separated oil and gas products are collected by the gas collection chamber 140 and then are input into the product separating device 150 for separation, thus obtaining various products. The separated spent catalyst is stripped by the stripping section 130 of the settler and then conveyed to the regeneration unit 200 for regeneration through the spent catalyst outlet 131, thereby realizing recycling. The catalytic cracking reactor 110 used in the present application may be various reactors commonly used in the art, such as a riser reactor, a fluidized bed reactor, a reducing reactor, a combination thereof, and the like.
The biomass oil used in the application is obtained by conveying biomass after pretreatment to a liquefying device for liquefying treatment to obtain a biomass oil crude product; and carrying out dehydration treatment on the biomass oil crude product in a dehydration system to obtain biomass oil.
The biomass processing unit 300 includes:
a biomass pretreatment device 310 for pretreating biomass,
a biomass liquefying device 320 for processing the pretreated biomass to obtain a biomass oil crude product,
the dewatering system 330 is configured to dewater the crude biomass oil product to obtain biomass oil;
a storage tank 340 for storing the biomass oil.
According to the present application, biomass includes, but is not limited to, agroforestry biomass, forestry biomass, aquatic plants, energy crops, and the like. For example, agricultural biomass including but not limited to straw, chaff, cotton stalks, and the like, forestry biomass including but not limited to firewood, fast-growing forest, forestry processing residues, and the like, aquatic plants including but not limited to reed, algae, and the like, and energy crops including cassava, canola, and the like.
According to the application, the biomass pretreatment process aims at improving the liquefaction efficiency, and the biomass pretreatment method is one or more selected from crushing, drying, baking, compression molding, acid washing and the like, and can be selected according to the category and property of biomass.
According to the present application, the biomass liquefaction process may be selected from the group consisting of hydrothermal liquefaction, pyrolysis, and the like. According to the application, the temperature and pressure of the biomass hydrothermal liquefaction process are not lower than 200 ℃ and not lower than 4.0 MPa. The solvent used for thermal liquefaction of alcohol is selected from methanol, ethylene glycol, etc. The pyrolysis process is fast pyrolysis or flash pyrolysis, the heating rate is not lower than 100 ℃/s, and the residence time is not higher than 10s.
According to the application, biomass is liquefied to obtain a biomass oil crude product, and the biomass oil is obtained after moisture removal and is directly used as a supplementary fuel, wherein the biomass oil is a mixture and comprises acids, aldehydes, ketones, alcohols, esters, ethers, phenols, saccharides, oligomers and the like.
According to the application, the energy consumed by the biomass liquefaction process is at least partly or wholly derived from renewable energy sources such as solar energy, green electricity, nuclear energy and the like.
According to the application, the biomass oil is directly introduced into the mixing tank without separation, is uniformly mixed with the catalyst through the nozzle, and is then conveyed to the regenerator to contact with the catalyst for combustion reaction. In one embodiment, the ratio of spent catalyst to introduced biomass oil is from 10 to 300:1 (by weight).
The regeneration unit 200 of the present application is suitable for the above-described catalytic cracking reaction system 100, for regenerating the spent catalyst passing through the catalytic cracking reaction system, and for transferring the regenerated catalyst back to the catalytic cracking reaction system 100, thereby realizing the recycling of the catalyst.
The regeneration unit 200 includes a regenerator 240, the regenerator 240 including a char section 210, and a dense phase regeneration section 250, the dense phase regeneration section 250 being located above the char section 210, and an outlet of the char section being housed inside the dense phase regeneration section such that the char section is in fluid communication with the dense phase regeneration section. Thus, dense phase regeneration zone 250 is coupled to char zone 210 such that material from char zone 210 may enter dense phase regeneration zone 250 for complete regeneration.
The scorch section 210 is provided with:
a first oxygen inlet 211 provided at the bottom of the char section for inputting oxygen into the char section; and
a spent catalyst inlet 216 for delivering spent catalyst of a catalytic cracking reactor to the interior of the burn-in section;
wherein the spent catalyst inlet 216 is connected with a spent inclined tube communicated with the catalytic cracking reaction system, and a mixing tank 350 is arranged in the spent inclined tube;
the storage tank 340 is in communication with the mixing tank 350 such that the biomass oil in the storage tank is delivered to the mixing tank for mixing with spent catalyst prior to delivery to the regenerator 210.
Optionally, a first circulating flue gas inlet 231 is further arranged at the lower part of the burning section, and the first circulating flue gas inlet 231 is used for circulating part of flue gas recovered by the regeneration section back to the inside of the burning section.
The dense phase regeneration section 250 is provided with:
a second oxygen inlet 253 provided at the bottom of the dense-phase regeneration zone for inputting oxygen to the dense-phase regeneration zone;
a second recycle flue gas inlet 252 for recycling a portion of the flue gas recovered from the dense phase regeneration section back into the dense phase regeneration section; and
a flue gas outlet 232 disposed at the top of the dense phase regeneration section;
wherein the dense phase regeneration zone is further configured with a heat extractor 215 for delivering heat to the exterior of the regenerator.
A portion of the char section 210 is located outside of the dense phase regeneration section 250 and a portion is located inside of the dense phase regeneration section 250. The cross-sectional area of the portion of the char section 210 that is located outside of the dense phase regeneration section 250 may be larger than the portion of the char section 210 that is located inside of the dense phase regeneration section 250. In one embodiment, the portion of the char section 210 that is located outside the dense phase regeneration section 250 communicates with the interior of the dense phase regeneration section 250 through a connection pipe 270, and the outlet end of the connection pipe 270 is located inside the dense phase regeneration section 250.
During the regeneration operation, the biomass oil in the storage tank 340 is sprayed into the mixing tank 350 to be mixed with the spent catalyst, then enters the burning section 210, contacts with the first oxygen entering through the oxygen-containing gas inlet 211, and sends partial burning reaction in the burning section; thereafter, the dense phase regeneration zone 250 is entered for complete regeneration. At this time, pure oxygen is supplied through the oxygen inlet 252 to contact the partially burnt catalyst, thereby further regenerating and burning the catalyst and the incompletely regenerated flue gas. After separation by cyclone 220, the regenerated catalyst falls back to the dense phase regeneration zone and is discharged through catalyst outlet 217 and recycled back to the catalytic cracking reactor. A part of the flue gas discharged through the flue gas outlet 232 is subjected to energy recovery through the flue gas energy recovery system 230 and then separated through the carbon dioxide separation system 260, so that carbon dioxide is trapped; and the other part of the flue gas is recycled to the bottom of the coke generation section and the dense phase regeneration section.
In one embodiment, the gases input via the first oxygen inlet 211 and the second oxygen inlet 252 are both oxygen. However, the oxygen input through the first oxygen inlet 211 is mixed with the recirculated flue gas after entering the char section to form an oxy-carbon dioxide mixture, and the amount of oxygen and/or recirculated flue gas is controlled such that the oxygen concentration in the mixture does not exceed 28% by volume. Similarly, the oxygen input through the second oxygen inlet 253 is mixed with the recycled flue gas and the like after entering the regeneration section to form an oxidation-carbon dioxide mixed gas, and the amount of oxygen and/or recycled flue gas is controlled so that the oxygen concentration in the mixed gas is not higher than 28 vol%. The scorching is carried out in the atmosphere, so that the scorching strength is improved; the air inlet does not contain nitrogen, so that the energy consumed by preheating the air can be reduced; and the carbon dioxide concentration of the flue gas at the outlet of the regenerator is higher, so that the separation and the capture of the carbon dioxide are convenient.
In one embodiment, the operating conditions of the scorch section are: the temperature is 560-730 ℃, the average residence time of the catalyst is 10-120 seconds, and the apparent linear velocity of the gas is 0.8-3.0m/s.
In one embodiment, the operating conditions of the dense phase regeneration zone are: the temperature is 580-750 ℃, the average residence time of the catalyst is 1.0-5.0 minutes, and the apparent linear velocity of gas is 0.3-0.8m/s.
In one embodiment, the char ratio in the char section is 40-50%; the scorching proportion of the dense phase regeneration section is 50-60%. The application adopts pure oxygen regeneration, and the regenerated flue gas only contains carbon dioxide and oxygen, thereby being convenient for separating and capturing the carbon dioxide for further conversion and utilization and realizing carbon emission.
Due to the injection of the biomass oil, a large amount of heat is generated during the regeneration process. If the temperature in the regenerator is too high, the activity of the catalyst may be adversely affected. Therefore, the regeneration unit 200 is further provided with a heat collector 215 for transporting heat to the outside of the regenerator. The heat extractors may be internal heat extractors (disposed inside the regenerator) or/and external heat extractors (disposed outside the regenerator), one or more of which may use excess energy generated by the regenerator to supply other devices. The heat collector can be used for generating high-pressure steam by using the surplus heat of the regeneration system and outputting the high-pressure steam to other devices for energy supply. In one embodiment, the regenerator bed temperature is controlled to not exceed 750 ℃, such as not exceeding 720 ℃, by providing a heat extractor.
The catalyst which can be used comprises zeolite, inorganic oxide and optional clay, wherein the components respectively account for the total weight of the catalyst: 1 to 50 weight percent of zeolite, 5 to 99 weight percent of inorganic oxide and 0 to 70 weight percent of clay. Wherein the zeolite is an active component and is selected from medium pore zeolite and/or optional large pore zeolite, the medium pore zeolite accounts for 10-100 wt% of the total weight of the zeolite, and the large pore zeolite accounts for 0-90 wt% of the total weight of the zeolite; the medium pore zeolite is selected from one or more of ZSM series zeolite and/or ZRP zeolite, and the zeolite can be modified by nonmetal such as phosphorus and/or transition metal such as iron, cobalt and nickel; the macroporous zeolite is one or more selected from hydrogen Y, rare earth hydrogen Y, ultrastable Y, etc.
The application uses the energy of biomass oil combustion generated by biomass to maintain the operation of a catalytic cracking device, is an indirect solar energy utilization process in nature, and the carbon in the biomass is derived from carbon dioxide captured by plants from the atmosphere instead of fossil energy, and the energy consumed by the whole process is derived from solar energy. Therefore, biomass energy utilization is also recycling of carbon element, and is a neutral emission process of carbon. Compared with biomass, the biomass oil has higher heat value and higher energy density, can be well coupled with a catalytic cracking process, and can be preheated on the one hand and prevented from being excessively high in local concentration on the other hand by spraying the biomass oil on a spent catalyst for premixing. The pure oxygen regeneration process ensures that the regenerated flue gas only contains carbon dioxide and oxygen, thereby reducing the separation and trapping cost and realizing the carbon emission.
The application can also use the energy generated by the regeneration system of the catalytic cracking device to supply other operation units to become a power center of the refinery, thereby fundamentally reducing the carbon emission of the refinery. According to the application, biomass is introduced into the power center of the catalytic cracking device, the biomass energy supply device is operated, and the discharged carbon dioxide is not derived from fossil energy, so that the energy source can be radically changed, and the carbon emission reduction is realized.
The application will be further illustrated by the following examples, but the application is not limited thereby. The properties of the raw oil A used in the examples and comparative examples are shown in Table 1, respectively.
Catalyst a is catalyst TCC and is prepared as follows: pulping 969 g of halloysite (product of China Kaolin Co., ltd., solid content of 73%) with 4300 g of decationizing water, adding 781 g of pseudo-boehmite (product of Shandong Zibo Ala mill, solid content of 64%) and 144 ml of hydrochloric acid (concentration of 30%, specific gravity of 1.56), stirring uniformly, standing at 60deg.C for aging for 1 hr, maintaining pH at 2-4, cooling to room temperature, adding 5000 g of prepared mesoporous shape-selective ZSM-5 zeolite slurry with high silica-alumina ratio containing chemical water, stirring uniformly, spray drying, and washing free Na + Used after aging, the aging process: aging in water vapor at 800 deg.C for 15h,the properties are shown in Table 2.
The catalyst b was prepared as follows:
(1) 20 g NH 4 Cl is dissolved in 1000 g of water, 100g (dry basis) of a crystallization product ZRP-1 molecular sieve (manufactured by Qilu petrochemical company catalyst plant, siO) is added into the solution 2 /Al 2 O 3 =30, rare earth content RE 2 O 3 =2.0 wt%) and after 0.5 hours exchange at 90 ℃, filtering to obtain a filter cake; 4.0 g of H are added 3 PO 4 (concentration 85%) and 4.5 g of Fe (NO) 3 ) 3 Dissolving in 90 g of water, mixing with the filter cake, soaking and drying; and roasting at 550 ℃ for 2 hours to obtain the MFI mesoporous molecular sieve containing phosphorus and iron. The elemental analysis chemistry of the resulting molecular sieve is: 0.1Na 2 O·5.1Al 2 O 3 ·2.4P 2 O 5 ·1.5Fe 2 O 3 ·3.8RE 2 O 3 ·88.1SiO 2 。
(2) Pulping 75.4 kg of multi-water kaolin (industrial product of Suzhou porcelain clay Co., ltd., solid content of 71.6 wt.%) with 250 kg of decationized water, adding 54.8 kg of pseudo-boehmite (industrial product of Dongnial Co., ltd., solid content of 63 wt.%) and adjusting pH to 2-4 with hydrochloric acid, stirring uniformly, standing at 60-70deg.C for aging for 1 hr, maintaining pH to 2-4, cooling to below 60deg.C, adding 41.5 kg of alumina sol (catalyst product of Qilu petrochemical Co., al) 2 O 3 The content was 21.7 wt%) and stirred for 40 minutes to obtain a mixed slurry.
(3) Adding the MFI medium pore molecular sieve (dry basis is 2 kg) containing phosphorus and iron prepared in the step (1) into the mixed slurry obtained in the step (2), stirring uniformly, spray drying to form, washing with monoammonium phosphate solution (phosphorus content is 1 wt%) and washing to remove free Na + And drying to obtain a sample of the catalytic conversion catalyst c. Based on the total weight of the dry basis of the catalyst b, the dry basis composition of the catalyst b comprises: 2 wt% MFI mesoporous molecular sieve containing phosphorus and iron, 36 wt% pseudo-boehmite and 8 wt% alumina sol, the balance being kaolin.
Example 1
Example 1 was performed on the apparatus shown in fig. 1, wherein,
the structure of the catalytic cracking reactor can be seen in the reactor 302 of fig. 4 of CN 111718230A.
The biomass oil production process is as follows:
the processing unit 300 includes: grinding and crushing biomass, performing hydrothermal liquefaction treatment on the pretreated biomass, wherein the temperature of a liquefaction device is 300 ℃, the pressure is 12MPa, the residence time is 10 minutes, and the liquefied product is dehydrated to obtain the bio-oil fuel.
The raw oil A is used as a reaction raw material, the catalytic conversion catalyst a is used as a catalyst, and the method provided by the application is used for regenerating the catalyst to be regenerated: firstly, mixing the spent catalyst with biomass oil in a mixing tank, wherein the weight ratio of the spent catalyst to the introduced biomass oil is 50:1; and then introduced into the regenerator. Pure oxygen gas is respectively introduced into the coking section and the dense-phase regeneration section, the catalyst mixed with the biomass oil is firstly partially regenerated in the coking section and then ascends to the dense-phase regeneration section to complete regeneration, and meanwhile, part of flue gas from the cyclone separation system of the regenerator is returned to the coking section and the dense-phase regeneration section, and the oxygen content in the coking section and the dense-phase regeneration section is controlled to be not more than 28 percent. The surplus energy generated by the regenerator is used for supplying energy to the outside through a heat collector.
The temperature of the scorching section is 645 ℃, the residence time is 75 seconds, the temperature of the dense phase regeneration section is 650 ℃, and the residence time is 2.5 minutes. The regenerated catalyst is circulated back to the reactor and is contacted with raw oil to carry out catalytic cracking reaction. The regeneration conditions, reaction conditions, and carbon dioxide emissions are shown in table 3.
Comparative example 1
Comparative example 1 was carried out on the same apparatus as example 1, except that no biomass treatment unit was included, with fuel oil as a supplemental source of energy, introduced from the char section. The temperature of the scorching section is 645 ℃, the residence time is 75 seconds, the temperature of the dense phase regeneration section is 650 ℃, and the residence time is 2.5 minutes. The regenerated catalyst is circulated back to the reactor and is contacted with raw oil to carry out catalytic cracking reaction. The regeneration conditions, reaction conditions, and carbon dioxide emissions are shown in table 3.
Example 2
Example 2 was carried out on the apparatus shown in fig. 1, wherein,
the structure of the catalytic cracking reactor can be seen in the reactor 302 of fig. 4 of CN 111718230A.
The biomass oil production process is as follows:
the processing unit 300 includes: grinding and crushing biomass, performing hydrothermal liquefaction treatment on the pretreated biomass, wherein the temperature of a liquefaction device is 300 ℃, the pressure is 12MPa, the residence time is 10 minutes, and the liquefied product is dehydrated to obtain the bio-oil fuel.
The C5-C8 mixed olefin is taken as a reaction raw material (the mol ratio of C5 to C6 to C7 to C8 is 1:1:1), and the catalytic conversion catalyst b is taken as a catalyst. The method provided by the application is used for regenerating the catalyst to be regenerated: spraying biomass oil onto the catalyst in a mixing tank on a spent circuit, and uniformly mixing, wherein the weight ratio of the spent catalyst to the introduced biomass oil is 135:1; the spent catalyst mixed with biomass oil is introduced into a regenerator to be contacted with pure oxygen diluted by circulating flue gas, and a combustion reaction occurs. Partial regeneration is carried out in the coke burning section, then the partial regeneration is carried out in the dense phase regeneration section, the partial regeneration is finished, and meanwhile, the flue gas from the cyclone separation system of the regenerator is partially returned to the coke burning section and the dense phase regeneration section, and the oxygen content in the coke burning section and the dense phase regeneration section is controlled to be not more than 28%. The surplus energy generated by the regenerator is used for supplying energy to the outside through a heat collector.
The temperature of the scorching section is 640 ℃, the residence time is 90 seconds, the temperature of the dense phase regeneration section is 655 ℃, and the residence time is 1.5 minutes. The regenerated catalyst is circulated back to the reactor and is contacted with raw oil to carry out catalytic cracking reaction. The regeneration conditions, reaction conditions, and carbon dioxide emissions are shown in table 4.
Comparative example 2
Comparative example 2 was carried out on the same apparatus as example 2, except that no biomass treatment unit was included, with fuel oil as a supplemental source of energy, introduced from the char section. The temperature of the scorching section is 640 ℃, the residence time is 90 seconds, the temperature of the dense phase regeneration section is 655 ℃, and the residence time is 1.5 minutes. The regenerated catalyst is circulated back to the reactor and is contacted with raw oil to carry out catalytic cracking reaction. The regeneration conditions, reaction conditions, and carbon dioxide emissions are shown in table 4.
From the data in tables 3 and 4, it can be seen that the example uses biomass oil as the source of supplemental energy, and the amount of carbon dioxide emitted is significantly reduced when the regeneration system generates the same amount of energy as compared to the comparative example, which is advantageous for substantially reducing the amount of carbon dioxide emitted.
In the description of the present application, it should be noted that the directions or positional relationships indicated by the terms "upper", "lower", "inner", "outer", "front", "rear", "left", "right", etc. are directions or positional relationships based on the operation state of the present application are merely for convenience of describing the present application and simplifying the description, and do not indicate or imply that the devices or elements to be referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present application.
In the description of the present application, it should be noted that the terms "mounted," "connected," and "connected" are to be construed broadly, unless otherwise specifically defined and limited. The specific meaning of the above terms in the present application will be understood in specific cases by those of ordinary skill in the art.
The application has been described above in connection with preferred embodiments, which are, however, exemplary only and for illustrative purposes. On this basis, the application can be subjected to various substitutions and improvements, and all fall within the protection scope of the application.
TABLE 1
| Feed Properties | Raw oil A |
| Density, kg/cubic meter (20 ℃ C.) | 843.7 |
| C, wt% | 86.59 |
| H, wt% | 13.41 |
| S，μg/g | 5800 |
| N，μg/g | 62 |
| Initial point of distillation, DEG C | 226 |
| 50% distillation temperature, DEG C | 287 |
| Paraffin, weight percent | 40.5 |
| Naphthene, weight percent | 33.3 |
| Aromatic hydrocarbon, weight percent | 26.2 |
TABLE 2
TABLE 3 Table 3
The calculation was performed based on 100g of the raw material processed.
The carbon dioxide emission index refers to the amount of carbon dioxide from fossil energy emitted per 1MJ energy produced by the coke burning of the regeneration system; the carbon dioxide produced by biomass oil is derived from carbon dioxide present in the atmosphere and is a neutral carbon emission process.
TABLE 4 Table 4
The calculation was performed based on 100g of the raw material processed.
The carbon dioxide emission index refers to the amount of carbon dioxide from fossil energy emitted per 1MJ energy produced by the coke burning of the regeneration system; the carbon dioxide produced by biomass oil is derived from carbon dioxide present in the atmosphere and is a neutral carbon emission process. />
Claims (12)
1. A catalytic cracking catalyst regeneration system comprising:
a biomass processing unit comprising:
a biomass pretreatment device for pretreating biomass,
the biomass liquefying device is used for processing the pretreated biomass to obtain a biomass oil crude product,
the dehydration system is used for carrying out dehydration treatment on the biomass oil crude product to obtain biomass oil;
a storage tank for storing the biomass oil;
a regeneration unit, the regeneration unit comprising:
a regenerator, the regenerator comprising:
a scorch section, and
a dense phase regeneration section,
wherein the dense phase regeneration section is positioned above the scorching section, and an outlet of the scorching section is contained inside the dense phase regeneration section, so that the scorching section is in fluid communication with the dense phase regeneration section;
the scorching section is provided with:
a first oxygen inlet arranged at the bottom of the burning section and used for inputting oxygen into the burning section;
the first circulating flue gas inlet is used for circulating a part of flue gas recovered by the dense-phase regeneration section back into the coking section; and
a spent catalyst inlet for conveying spent catalyst of a catalytic cracking reactor to the interior of the burn-in section;
the to-be-generated catalyst inlet is connected with a to-be-generated inclined tube communicated with the catalytic cracking reaction system, and a mixing tank is arranged in the to-be-generated inclined tube;
the storage tank is communicated with the mixing tank, so that biochar particles in the storage tank are conveyed to the mixing tank, mixed with spent catalyst and then conveyed to the burning section;
the dense phase regeneration section is provided with:
the second oxygen inlet is arranged at the bottom of the dense-phase regeneration section and is used for inputting oxygen into the dense-phase regeneration section;
the second circulating flue gas inlet is used for circulating part of flue gas recovered by the dense-phase regeneration section back to the interior of the dense-phase regeneration section; and
a flue gas outlet arranged at the top of the dense phase regeneration section;
the dense-phase regeneration section is also provided with a heat collector for conveying heat to the outside of the regenerator.
2. A catalytic cracking catalyst regeneration process, said process being carried out in a regeneration system according to claim 1,
the method comprises the following steps:
s1, conveying biomass to a liquefying device for liquefying after pretreatment to obtain a biomass oil crude product;
s2, dehydrating the biomass oil crude product in a dehydration system to obtain biomass oil, and conveying the biomass oil to a storage tank;
s3, conveying the biomass oil to a mixing tank, mixing the biomass oil with a spent catalyst from a catalytic cracking reactor, conveying the mixture to the inside of a burning section, and contacting the mixture with oxygen to partially burn the spent catalyst;
s4, the materials from the scorching section enter a dense phase regeneration section, and oxygen is injected into the dense phase regeneration section through a second oxygen inlet, so that the catalyst is completely regenerated.
3. The method of claim 2, wherein the liquefaction process comprises a hydrothermal liquefaction process, an alcohol thermal liquefaction process, or a pyrolysis process.
4. A method according to claim 3, wherein the hydrothermal liquefaction process is at a temperature of not less than 200 ℃ and a pressure of not less than 4.0MPa; the alcohol thermal liquefaction treatment adopts a solvent selected from methanol and glycol; the pyrolysis treatment is fast pyrolysis or flash pyrolysis, the heating rate is not lower than 100 ℃/s, and the residence time is not higher than 10s.
5. The method of claim 2, wherein the weight ratio of spent catalyst to introduced biomass oil is 10-300:1.
6. A method according to claim 2, wherein the temperature of the regenerator bed is controlled by the heat extractor to not exceed 750 ℃, preferably not to exceed 720 ℃.
7. The method of claim 2, wherein the operating conditions of the scorch section are: the temperature is 560-730 ℃, the average residence time of the catalyst is 10-120 seconds, and the apparent linear velocity of the gas is 0.8-3.0m/s.
8. The process of claim 2, wherein the operating conditions of the dense phase regeneration zone are: the temperature is 580-750 ℃, the average residence time of the catalyst is 1.0-5.0 minutes, and the apparent linear velocity of gas is 0.3-0.8m/s.
9. The method of claim 2, wherein the biomass is selected from the group consisting of agroforestry biomass, forestry biomass, aquatic plants, energy crops.
10. The method of claim 2, wherein in the char section, the oxygen concentration does not exceed 28% by volume; in the dense phase regeneration zone, the oxygen concentration does not exceed 28% by volume.
11. The method of claim 2, wherein the char fraction in the char section is 40-50%; the scorching proportion of the dense phase regeneration section is 50-60%.
12. A process according to claim 2, wherein the temperature of the dense phase regeneration zone bed is controlled via the heat extractor to not exceed 750 ℃, preferably not to exceed 720 ℃.
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| CN202210476000.3A CN117000298A (en) | 2022-04-29 | 2022-04-29 | Catalytic cracking catalyst regeneration system and regeneration method |
| PCT/CN2023/091038 WO2023208085A1 (en) | 2022-04-29 | 2023-04-27 | Catalytic cracking catalyst regeneration method and system using bio-based liquid-phase fuel |
| TW112115713A TW202342173A (en) | 2022-04-29 | 2023-04-27 | Catalytic cracking catalyst regeneration method and system using bio-based liquid-phase fuel |
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