Method and system for conducting carbon black through LCO

By cutting catalytic cracked diesel into different components and performing a cracking reaction in a high-temperature cracking reactor, combined with electromagnetic induction heating and cooling and cooling technology, the problem of insufficient productivity and quality of conductive carbon black in the prior art is solved, and efficient and simple preparation of conductive carbon black is achieved.

CN119899544AActive Publication Date: 2025-04-29CHINA PETROLEUM & CHEMICAL CORP +1
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Patent Information

Application Number
CN202311402844.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2023-10-26
Publication Date
2025-04-29
Estimated Expiration
2043-10-26

AI Technical Summary

Technical Problem

In the prior art, when producing conductive carbon black, it is difficult to effectively improve the yield and quality of carbon black, and there is a lack of effective recycling methods.

Method used

Conductive carbon black is prepared by cutting catalytic cracked diesel (LCO) into aromatic hydrocarbon components and non-aromatic components, and performing cracking reactions in a high-temperature cracking reactor, combining electromagnetic induction heating and cooling and cooling technology.

Benefits of technology

The yield of carbon black and the effective utilization rate of catalytic cracked diesel are improved, and conductive carbon black is prepared easily and efficiently, and high yield carbon black production is achieved.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to a method and a system for conducting carbon black by utilizing LCO, components in the LCO are reasonably utilized, and the LCO is subjected to high-temperature cracking in different reaction zones according to the property composition of fractions, so that the yield of the carbon black is improved, and the effective utilization rate of the LCO is also improved. According to the method for producing the carbon black, the conductive carbon black can be simply, conveniently and efficiently prepared, and the yield of the carbon black is high.
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Description

Technical Field

[0001] The invention relates to the field of petrochemical industry, and in particular to a method and system for preparing conductive carbon black from LCO. Background Art

[0002] In my country, due to the reduction of crude oil reserves and the gradual strengthening of environmental awareness, the availability of inferior oil and the increase in processing profits have reduced the market share of low-quality gasoline and diesel. At the same time, the demand for high-quality gasoline has gradually increased. The slowdown in economic growth has led to a structural surplus of diesel, and the market share of diesel has gradually decreased. However, the vacancies of chemical raw materials such as low-carbon olefins and aromatics still need to be supplemented to achieve the transformation of refining and further development. Therefore, it is necessary to develop high-temperature cracking technology for producing chemical materials from inferior heavy oil, so as to achieve a successful transformation from oil to chemical.

[0003] Carbon black is an important chemical raw material. As a reinforcing filler in the rubber industry, a colorant or toner for rubber compounds, it is widely used in many fields such as inks, coatings, leather making, chemical fibers, metallurgy, electronics, photosensitive materials, black agricultural films and packaging materials. The existing technology for producing carbon black includes furnace black, channel black, pyrolytic black and lampblack. Chinese patent (ZL89104111) provides a method for producing carbon black using natural gas as fuel and oxygen-rich gas as a combustion aid. This method improves the stability of furnace temperature and ensures heat supply, but does not solve the problem of carbon black yield and quality.

[0004] Conductive carbon black is generally obtained by producing carbon black as a byproduct of acetylene from natural gas. The main reaction process is that the raw natural gas and oxygen are heated to a certain temperature in the gas preheater and then mixed into the reactor. A part of the natural gas is burned to provide heat energy for the reaction, and the other part of the natural gas undergoes cracking reaction at about 1500℃ to produce acetylene. Acetylene is easily decomposed into carbon black and hydrogen at high temperatures, so the optimal reaction time at high temperatures is only a few thousandths of a second, and the reaction is terminated by quenching with water spray. Although the reaction time is extremely short, carbon black is still generated. Carbon black is a byproduct in this process.

[0005] CN110204930B A production method and feeding equipment for controlling the specific surface area of ​​conductive carbon black, belonging to the technical field of conductive carbon black preparation. The production method for controlling the specific surface area of ​​conductive carbon black comprises subjecting mixed acetylene and hydrocarbon raw materials to cracking reaction at 1300-1500°C; the hydrocarbon raw materials comprise a combination of one or more hydrocarbon compounds. The specific surface area of ​​the conductive carbon black obtained by introducing acetylene to cracking reaction at 1800°C is generally above 80m2 / g. CN112210233A The present invention relates to a method for preparing conductive carbon black, mainly to the problem of the lack of an effective regeneration method for carbon black produced as a by-product of acetylene production from natural gas. The present invention discloses a method for preparing conductive carbon black, which comprises the following steps: (a) acid treatment: the raw carbon black is treated with an acid solution to obtain a conductive carbon black intermediate product I; (b) alkali treatment: the conductive carbon black intermediate product I is treated with an alkali solution to obtain a conductive carbon black intermediate product II; (c) salt loading: the conductive carbon black intermediate product II is mixed with a salt-containing aqueous solution to obtain a conductive carbon black intermediate product III; (d) calcination: the conductive carbon black intermediate product III is calcined to obtain a conductive carbon black finished product. The technical solution solves the problem well and can be used in the recycling and utilization of carbon black produced as a byproduct of natural gas to acetylene in industrial devices. CN112210233A discloses a granular conductive carbon black and a method for preparing the same, which belongs to the field of conductive carbon black technology. The method for preparing the granular conductive carbon black comprises wetting the conductive carbon black raw material with water at a temperature of ≥80°C, wet granulation and drying in sequence. By using water with a temperature of ≥80°C to infiltrate the conductive carbon black raw material, the hydrophilicity of the conductive carbon black raw material is enhanced, and the water with a temperature of ≥80°C enters the microporous structure of the conductive carbon black raw material to achieve a good wetting effect. Further, granular conductive acetylene carbon black with uniform particle size distribution is obtained through wet granulation and drying. Summary of the invention

[0006] The object of the present invention is to provide a method for preparing conductive carbon black by catalyzing diesel.

[0007] A first aspect of the present invention provides a method for preparing conductive carbon black from LCO, comprising:

[0008] (1) cutting LCO into aromatic components and non-aromatic components, wherein the LCO cutting temperature is 210-260° C., the non-aromatic components are fractions having a distillation range less than the cutting temperature, and the aromatic components are fractions having a distillation range greater than the cutting temperature;

[0009] (2) introducing the non-aromatic component into the first cracking reactor to undergo cracking reaction, and the obtained first cracking product enters the second cracking reactor under the action of the carrier gas to merge with the aromatic component and continue to undergo cracking reaction to obtain a second cracking product containing conductive carbon black and cracking gas;

[0010] (3) The second cracking product enters the carbon black collector, where it is quenched and cooled to separate the solid product, conductive carbon black. The gas product is further washed and filtered before entering the cracking gas collector for collection.

[0011] According to the method of the first aspect, the reaction temperature of the first cracking reactor is 1800-2000°C;

[0012] The reaction time of the first cracking reactor is 2 milliseconds to 30 milliseconds;

[0013] The reaction temperature of the second cracking reactor is 1100-1800°C, preferably 1200-1500°C; and / or

[0014] The reaction time of the second cracking reactor is 2 milliseconds to 5 seconds, preferably 40 milliseconds to 2 seconds.

[0015] According to the method of the first aspect, wherein the carrier gas is selected from one or more of the following: methane, nitrogen, dry gas, helium, argon, C2-C4 light hydrocarbons;

[0016] Preferably, the carrier gas enters the first cracking reactor after being preheated, and the preheating temperature is 800-2500°C, more preferably 1500-2300°C.

[0017] According to the method of the first aspect, the aromatic components and non-aromatic components are introduced into the first cracking reactor and the second cracking reactor respectively after preheating, and the preheating temperature is 200-600°C, preferably 230-250°C.

[0018] According to the method of the first aspect, the feed ratio of carrier gas to LCO per unit time is 0.5-200 liters / gram, preferably 1-40 liters / gram.

[0019] According to the method of the first aspect, the cooling rate of the quenching is 50-1000°C / millisecond, preferably 50-500°C / millisecond; and / or

[0020] The temperature of the product after quenching is 100-900°C, preferably 200-500°C;

[0021] Preferably, the second cracking product is quenched and cooled using a quenching medium, wherein the quenching medium is selected from one or more of the following: water, nitrogen, argon, and more preferably liquid nitrogen.

[0022] A second aspect of the present invention provides a system for preparing conductive carbon black from LCO, comprising:

[0023] A raw material cutting device, which is provided with an LCO inlet, an aromatic component outlet and a non-aromatic component outlet, and is used to cut the LCO into aromatic components and non-aromatic components;

[0024] A carrier gas preheating unit, comprising one or more carrier gas preheating furnaces connected in series, preferably, the carrier gas preheating unit comprises two carrier gas preheating furnaces;

[0025] A reaction unit comprising:

[0026] A first cracking reactor, used for cracking non-aromatic components, wherein the first cracking reactor is respectively connected to the non-aromatic component outlet of the raw material cutting device and the carrier gas outlet of the carrier gas preheating unit;

[0027] A second cracking reactor, used for cracking the aromatic component and the first cracking product obtained by the first cracking reactor, wherein the second cracking reactor is connected to the aromatic component outlet of the raw material cutting device and the first cracking product outlet of the first cracking reactor respectively;

[0028] Product collection unit, including

[0029] A carbon black collector, which is provided with a quenching medium inlet and a gas product outlet, and is used to cool the second cracking product obtained by the second cracking reactor and collect the conductive carbon black, and the carbon black collector is connected to the second cracking product outlet of the second cracking reactor;

[0030] one or more gas scrubbers and carbon black filters for scrubbing and filtering the gaseous products exiting the carbon black collector;

[0031] The cracking gas collector is used to collect the cracking gas products after gas washing and carbon black filter washing and filtering.

[0032] The system according to the second aspect, wherein the first cleavage reactor and / or the second cleavage reactor is a tubular reactor;

[0033] Preferably, the material of the tubular reactor is selected from one or more of the following: tungsten, molybdenum, tantalum, niobium, vanadium, chromium, titanium, zirconium, rare earth metal borides, rare earth metal carbides, rare earth metal nitrides, rare earth metal silicides, rare earth metal phosphides and rare earth metal sulfides, wherein the rare earth metal is selected from one or more of lanthanum, cerium, praseodymium and neodymium.

[0034] According to the system of the second aspect, the outer circumference of the first cracking reactor and / or the second cracking reactor is sheathed with an electromagnetic induction coil for heating.

[0035] The system according to the second aspect, wherein the first cracking reactor is arranged vertically or horizontally, preferably vertically; and / or

[0036] The second cracking reactor is arranged horizontally.

[0037] Through the above technical solution, the advantages of the present invention are:

[0038] (1) The electromagnetic induction coil heats the cracking reactor, which can achieve rapid temperature rise of the cracking reactor, and the reaction temperature control is simple and the operation is stable;

[0039] (2) By rationally utilizing the components in catalytic cracking diesel (LCO), catalytic cracking diesel (LCO) is subjected to high-temperature cracking in different reaction zones according to the properties of the fractions, which not only increases the yield of carbon black, but also improves the effective utilization rate of catalytic cracking diesel (LCO).

[0040] (3) The method for producing carbon black of the present invention can prepare conductive carbon black simply and efficiently, and the yield of carbon black is high. BRIEF DESCRIPTION OF THE DRAWINGS

[0041] Figure 1 The present invention shows a process flow and structural schematic diagram of a specific implementation method of the method for producing conductive carbon black.

[0042] Figure 2 The test results of the battery capacity of the conductive carbon black prepared in Example 1 of the present invention as a conductive agent for lithium batteries are shown.

[0043] Figure 3 The charge and discharge curves of the conductive carbon black material prepared in Example 1 at different rates are shown.

[0044] Figure 4 The TEM image of the conductive carbon black prepared in Example 1 is shown.

[0045] Description of reference numerals:

[0046] 1. LCO sampling pipeline; 2. carrier gas sampling pipeline; 3-7, 9, 11-13, pipelines; 8. quenching medium inlet pipeline; 14. LCO raw material cutting device; 15. carrier gas preheating furnace I; 16. carrier gas preheating furnace II; 17. cracking reactor I; 18. cracking reactor II; 19. carbon black collector; 20. gas washing and carbon black filter I; 21. gas washing and carbon black filter II; 22. gas collector. DETAILED DESCRIPTION

[0047] The present application is further described in detail below through the accompanying drawings and embodiments. Through these descriptions, the characteristics and advantages of the present application will become clearer and more specific.

[0048] The word "exemplary" is used exclusively 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 shown in the drawings, the drawings are not necessarily drawn to scale unless otherwise noted.

[0049] In addition, the technical features involved in different embodiments of the present application described below can be combined with each other as long as they do not conflict with each other.

[0050] Before describing the technical solution of the present invention, the terms used in this article are defined as follows:

[0051] The term "LCO" refers to: light cycle oil, that is, catalytic cracking diesel.

[0052] The term "aromatic component" refers to a heavy fraction rich in aromatics after LCO is cut.

[0053] The term "non-aromatic component" refers to the light fraction that is not rich in aromatics after LCO is cut.

[0054] The present invention provides a method for preparing conductive carbon black from LCO, comprising:

[0055] (1) cutting LCO into aromatic components and non-aromatic components, wherein the LCO cutting temperature is 210-260° C., the non-aromatic components are fractions having a distillation range less than the cutting temperature, and the aromatic components are fractions having a distillation range greater than the cutting temperature;

[0056] (2) introducing the non-aromatic component into the first cracking reactor to undergo cracking reaction, and the obtained first cracking product enters the second cracking reactor under the action of the carrier gas to merge with the aromatic component and continue to undergo cracking reaction to obtain a second cracking product containing conductive carbon black and cracking gas;

[0057] (3) The second cracking product enters the carbon black collector, where it is quenched and cooled to separate the solid product, conductive carbon black. The gas product is further washed and filtered before entering the cracking gas collector for collection.

[0058] According to the property analysis of catalytic cracking diesel (LCO), most of the aromatic compounds in catalytic cracking diesel (LCO) are concentrated in the heavy fraction. Studies have found that aromatic compounds are precursors for carbon black production and are more conducive to improving the yield of carbon black. By studying the formation mechanism of acetylene, it is found that straight-chain hydrocarbons are more conducive to the formation of acetylene. Therefore, the present invention reasonably utilizes the components in catalytic cracking diesel (LCO), performs high-temperature cracking reactions in different reaction zones according to the fraction properties to obtain acetylene and carbon black products respectively, thereby improving the yield of acetylene and carbon black and the effective utilization rate of catalytic cracking diesel (LCO).

[0059] The present invention will be further described below through specific implementation modes in conjunction with the accompanying drawings, but the present invention is not limited thereby.

[0060] like Figure 1As shown, LCO is cut into aromatic components and non-aromatic components in the LCO raw material cutting device 14 according to its properties, the carrier gas is introduced into the carrier gas preheating furnace I15 and the carrier gas preheating furnace II 16 through the carrier gas injection pipeline 2 to increase the temperature, the non-aromatic components are introduced into the cracking reactor I17 from top to bottom through the pipeline 5, and the aromatic components are introduced into the cracking reactor II 18 through the pipeline 6, the gas product of the cracking reactor I17 and the raw material of the cracking reactor II 18 are combined as the raw material of the cracking reactor II 18 and cracked in the cracking reactor II 18, the cracking product enters the carbon black collector 19, the quenching water entering the carbon black collector 19 through the quenching medium inlet pipeline 8 quenches the product to terminate the reaction, and then enters the gas washing and carbon black filter I 20 and the gas washing and carbon black filter II 21 in sequence, and enters the subsequent separation system to obtain conductive carbon black, and the gas product is collected in the gas collector 22.

[0061] The present invention adopts electromagnetic induction heating pyrolysis reactor, which can realize rapid temperature rise of pyrolysis reactor and stable temperature. Compared with plasma reactor, the equipment is simpler, smaller in size, and easy to implement and operate. The present invention combines the technical scheme of electromagnetic induction heating pyrolysis reactor for pyrolysis reaction with controlling the temperature drop rate of rapid cooling within a specific range, so as to produce more high-quality conductive carbon black.

[0062] According to the present invention, the cracking reaction is completed at an ultra-high temperature and in a very short time. Compared with a plasma reactor, the cracking reactor of the present invention has a simple structure, an easy-to-control cracking process and low energy consumption.

[0063] In one embodiment, the reaction temperature of the first cracking reactor is 1800-2000°C;

[0064] The reaction time of the first cracking reactor is 2 milliseconds to 30 milliseconds;

[0065] The reaction temperature of the second cracking reactor is 1100-1800°C, preferably 1200-1500°C; and / or

[0066] The reaction time of the second cracking reactor is 2 milliseconds to 5 seconds, preferably 40 milliseconds to 2 seconds, and more preferably 40 milliseconds to 1 second.

[0067] According to the present invention, the method of the present invention may further include: preheating the cracking raw material and the carrier gas before feeding them into the cracking reactor, so that the cracking raw material and the carrier gas quickly reach the reaction temperature in the cracking reactor. The temperature of the preheated cracking raw material and the carrier gas can vary within a large range. The carrier gas is used to control the reaction time on the one hand, so that the cracking raw material passes through the cracking reactor quickly, and on the other hand, to provide a high-temperature reaction gas environment for the cracking of the raw material.

[0068] In one embodiment, the carrier gas is selected from one or more of the following: methane, nitrogen, dry gas, helium, argon, C2-C4 light hydrocarbons;

[0069] Preferably, the carrier gas enters the first cracking reactor after being preheated, and the preheating temperature is 800-2500°C, more preferably 1500-2300°C.

[0070] In one embodiment, the aromatic component and the non-aromatic component are introduced into the first cracking reactor and the second cracking reactor respectively after being preheated, and the preheating temperature is 200-600°C, preferably 230-250°C.

[0071] In one embodiment, the feed ratio of carrier gas to LCO per unit time is 0.5-200 L / g, preferably 1-40 L / g.

[0072] In one embodiment, the carrier gas to non-aromatic component feed ratio is 0.5-200 liters / gram, preferably 1-40 liters / gram; and / or

[0073] The feed ratio of carrier gas to aromatic component raw material per unit time is 0.1-50 liters / gram, preferably 0.5-10 liters / gram.

[0074] According to the present invention, rapid cooling is used to rapidly cool the reaction product to terminate the reaction and generate a product with a specific composition. The quenching medium used in rapid cooling is a medium well known to those skilled in the art.

[0075] In one embodiment, the cooling rate of the quenching is 50-1000°C / millisecond, preferably 50-500°C / millisecond; and / or

[0076] The temperature of the product after quenching is 100-900°C, preferably 200-500°C;

[0077] Preferably, the second cracking product is quenched and cooled using a quenching medium, wherein the quenching medium is selected from one or more of the following: water, nitrogen, argon, and more preferably liquid nitrogen.

[0078] The present invention also provides a system for preparing conductive carbon black from LCO, comprising:

[0079] A raw material cutting device, which is provided with an LCO inlet, an aromatic component outlet and a non-aromatic component outlet, and is used to cut the LCO into aromatic components and non-aromatic components;

[0080] A carrier gas preheating unit, comprising one or more carrier gas preheating furnaces connected in series, preferably, the carrier gas preheating unit comprises two carrier gas preheating furnaces;

[0081] A reaction unit comprising:

[0082] A first cracking reactor, used for cracking non-aromatic components, wherein the first cracking reactor is respectively connected to the non-aromatic component outlet of the raw material cutting device and the carrier gas outlet of the carrier gas preheating unit;

[0083] A second cracking reactor, used for cracking the aromatic component and the first cracking product obtained by the first cracking reactor, wherein the second cracking reactor is connected to the aromatic component outlet of the raw material cutting device and the first cracking product outlet of the first cracking reactor respectively;

[0084] Product collection unit, including

[0085] A carbon black collector, which is provided with a quenching medium inlet and a gas product outlet, and is used to cool the second cracking product obtained by the second cracking reactor and collect the conductive carbon black, and the carbon black collector is connected to the second cracking product outlet of the second cracking reactor;

[0086] one or more gas scrubbers and carbon black filters for scrubbing and filtering the gaseous products exiting the carbon black collector;

[0087] The cracking gas collector is used to collect the cracking gas products after gas washing and carbon black filter washing and filtering.

[0088] In one embodiment, the first cleavage reactor and / or the second cleavage reactor is a tubular reactor;

[0089] Preferably, the material of the tubular reactor is selected from one or more of the following: tungsten, molybdenum, tantalum, niobium, vanadium, chromium, titanium, zirconium, rare earth metal borides, rare earth metal carbides, rare earth metal nitrides, rare earth metal silicides, rare earth metal phosphides and rare earth metal sulfides, wherein the rare earth metal is selected from one or more of lanthanum, cerium, praseodymium and neodymium.

[0090] In one embodiment, the first cracking reactor and / or the second cracking reactor is / are sheathed with an electromagnetic induction coil for heating.

[0091] In one embodiment, the first cracking reactor is arranged vertically or horizontally, preferably vertically; and / or

[0092] The second cracking reactor is arranged horizontally.

[0093] According to the present invention, the cracking reactor of the present invention is a reactor that can be heated by electromagnetic induction, for example, it can be a metal tubular reactor arranged horizontally. There is no specific restriction on the way of introducing the cracking raw material and the carrier gas into the metal tubular reactor. In a specific embodiment, the cracking raw material and the carrier gas are introduced into the metal tubular reactor from the front of the metal tubular reactor, the reaction product is led out of the metal tubular reactor from the rear of the metal tubular reactor, and the quenching medium is introduced into the carbon black collector from the pipeline 8 through the nozzle, and the reaction product coming out of the reactor outlet is quenched and cooled. The outer periphery of the metal tubular reactor can be provided with an electromagnetic induction coil to heat the reactor by the alternating magnetic field generated by the electromagnetic induction coil.

[0094] The present invention is further illustrated by the following examples, but the present invention is not limited thereto.

[0095] like Figure 1 As shown, LCO is cut into non-aromatic components and aromatic components in the LCO raw material cutting device 14. The non-aromatic components pass through pipeline 5, carrier gas preheating furnace I15, and carrier gas preheating furnace II16 preheated to 500-2000°C and enter the cracking reactor I17 through pipeline 4 for cracking reaction. The aromatic components cut from the LCO raw material cutting device 14 and the products from the cracking reactor I17 enter the cracking reactor II18 through pipeline 6 and pipeline 7 for cracking reaction. The products enter the carbon black collector 19 and are quenched by the quenching medium entering through pipeline 8. The products are rapidly cooled (the cooling rate of the reaction products during rapid cooling is 100°C / millisecond) to 200-500°C. The quenching medium from pipeline 8 is sprayed into the bottom of the carbon black collector 19 through the quenching medium inlet at the bottom of the carbon black collector 19 to further cool the gas product and separate the gas and solid. Among them, the gas product containing acetylene enters the gas washing and carbon black filter I20 and the gas washing and carbon black filter II21 in sequence from the gas outlet of the carbon black collector 19, and the obtained product gas enters the gas collector 22 through pipeline 13.

[0096] Example 1

[0097] This embodiment Figure 1In the system shown, LCO with properties as described in Table 1 is used as the cracking raw material, the cutting temperature is 260°C, the fraction below 260°C is the non-aromatic component, and the fraction above 260°C is the aromatic component; the carrier gas is nitrogen, the first preheating temperature of the carrier gas preheating furnace I is 500°C, and the second preheating temperature of the carrier gas preheating furnace II is 1500°C. The quartz tube is used as the reactor, and the graphite tube is used as the heating medium. The quartz tube of the first cracking reactor is vertically arranged along the length direction, with an inner diameter of 10mm and a length of 38mm. The outer periphery of the quartz tube is sheathed with an electromagnetic induction coil. The quartz tube of the second cracking reactor is horizontally arranged along the axial direction, with an inner diameter of 20mm and a length of 50mm. The outer periphery of the quartz tube is sheathed with an electromagnetic induction coil. Water is introduced into the carbon black collector 19 from the quenching medium inlet at the bottom thereof as the quenching medium, and the water flow rate is 4 liters / minute. The cooling rate of the reaction product is controlled to be 100°C / millisecond, so that its temperature is reduced to about 250°C. The gas product containing acetylene enters the gas washing and carbon black filter I20 and the washing and carbon black filter II21 from the gas outlet of the carbon black collector 19, and the obtained product gas enters the gas collector 22 through the pipeline 13. The carbon black product is separated and dried to obtain a conductive carbon black product. The quality of catalytic cracking diesel is shown in Table 1.

[0098] Table 1 Properties of catalytic cracking diesel

[0099]

[0100]

[0101] The specific conditions of Example 1 are as follows: the first reaction temperature is 1800°C, the second reaction temperature is 1500°C, nitrogen is used as the carrier gas, the carrier gas flow rate is 4L / min, the LCO feed rate is 1.0 g / min, the oil feeding time is 4 minutes, the first reaction time is 25 milliseconds, the second reaction time is 50 milliseconds, the cooling rate is 100°C / millisecond, the product temperature is 200°C, and the gas product composition is as follows: gas yield 10.58%, carbon black yield 89.42%, wherein the gas contains 0.73% hydrogen, 4.86% methane, and 1.71% acetylene. It can be seen that segmented feeding can better convert raw materials into carbon black and improve the yield of carbon black. The property analysis of carbon black is shown in the attached Figure 2-4 shown.

[0102] Electrochemical performance test

[0103] The conductive carbon black prepared in Example 1 was assembled into a battery with lithium iron phosphate. The assembled battery was allowed to stand at 25°C for 5 hours before the electrochemical performance test was performed. In the experiment, the battery charge and discharge performance test was performed on a blue electric system with a test voltage of 2.0 to 3.9V. The test items were the battery's charge and discharge specific capacity, cycle performance, rate performance, etc. The battery's cyclic voltammetry test (CV) was performed on an electrochemical analyzer.

[0104] (1) Charge and discharge performance test

[0105] The test is mainly to obtain the battery's first charge and discharge, cycle stability and rate performance data. The test system used is the blue electric test system, the test conditions are 25℃, 2.0~3.9V, and the current density is 160mAh / g. Before the test, the assembled battery is left to stand at 25℃ for 5h before subsequent testing.

[0106] (2) Cyclic voltammetry (CV)

[0107] Cyclic voltammetry tests analyze the electrochemical performance of batteries by studying the redox process occurring on the electrodes. The test instrument used is Shanghai Chenhua CHI electrochemical analyzer, and the test conditions are: test temperature is room temperature, test voltage is 2.5~4V, and scan rate is 0.2mV / s.

[0108] from Figure 2 From the battery capacity test curve, when the rate increases from a small rate, the discharge capacity slightly decays, and when the rate returns to the initial rate from a large rate, the discharge capacity returns to the initial state, indicating that the battery capacity is good and relatively stable. Figure 3 It can be seen that the prepared conductive carbon black has a good charge and discharge voltage platform stability and has good charge and discharge performance.

[0109] from Figure 4 From the TEM image, it can be seen that the carbon black produced by the present invention is approximately spherical particles, a part of which is connected end to end to form a chain-like agglomerate, and the other part is overlapped; the particle size is generally less than 100nm; the end to end is connected to form a chain-like aggregate. It can be seen that the method and system of the present invention can be used to prepare conductive carbon black, and the prepared conductive carbon black has good conductive properties.

[0110] In the description of this application, it should be noted that, unless otherwise clearly specified and limited, the terms "install", "connect" and "connect" should be understood in a broad sense. For ordinary technicians in this field, the specific meanings of the above terms in this application can be understood according to specific circumstances.

[0111] The present application has been described above in conjunction with preferred embodiments, but these embodiments are only exemplary and serve only as an illustration. On this basis, various replacements and improvements may be made to the present application, all of which fall within the scope of protection of the present application.

Claims

1. A method for preparing conductive carbon black from LCO, comprising: (1) cutting LCO into aromatic components and non-aromatic components, wherein the LCO cutting temperature is 210-260° C., the non-aromatic components are fractions with a distillation range less than the cutting temperature, and the aromatic components are fractions with a distillation range greater than the cutting temperature; (2) introducing the non-aromatic component into the first cracking reactor to undergo cracking reaction, and the obtained first cracking product enters the second cracking reactor under the action of the carrier gas to merge with the aromatic component and continue to undergo cracking reaction to obtain a second cracking product containing conductive carbon black and cracking gas; (3) The second cracking product enters the carbon black collector, where it is quenched and cooled to separate the solid product, conductive carbon black. The gas product is further washed and filtered before entering the cracking gas collector for collection.

2. The method according to claim 1, characterized in that The reaction temperature of the first cracking reactor is 1800-2000°C; The reaction time of the first cracking reactor is 2 milliseconds to 30 milliseconds; The reaction temperature of the second cracking reactor is 1100-1800°C, preferably 1200-1500°C; and / or The reaction time of the second cracking reactor is 2 milliseconds to 5 seconds, preferably 40 milliseconds to 2 seconds.

3. The method according to claim 1, characterized in that The carrier gas is selected from one or more of the following: methane, nitrogen, dry gas, helium, argon, C2-C4 light hydrocarbons; Preferably, the carrier gas enters the first cracking reactor after being preheated, and the preheating temperature is 800-2500°C, more preferably 1500-2300°C.

4. The method according to claim 1, characterized in that: The aromatic components and non-aromatic components are introduced into the first cracking reactor and the second cracking reactor respectively after being preheated, and the preheating temperature is 200-600°C, preferably 230-250°C.

5. The method according to claim 1, characterized in that The feed ratio of carrier gas to LCO per unit time is 0.5-200 L / g, preferably 1-40 L / g.

6. The method according to claim 1, characterized in that The cooling rate of the quenching is 50-1000°C / millisecond, preferably 50-500°C / millisecond; and / or The temperature of the product after quenching is 100-900°C, preferably 200-500°C; Preferably, the second cracking product is quenched and cooled using a quenching medium, wherein the quenching medium is selected from one or more of the following: water, nitrogen, argon, and more preferably liquid nitrogen.

7. A system for preparing conductive carbon black from LCO, comprising: A raw material cutting device, which is provided with an LCO inlet, an aromatic component outlet and a non-aromatic component outlet, and is used to cut the LCO into aromatic components and non-aromatic components; A carrier gas preheating unit, comprising one or more carrier gas preheating furnaces connected in series, preferably, the carrier gas preheating unit comprises two carrier gas preheating furnaces; A reaction unit comprising: A first cracking reactor, used for cracking non-aromatic components, wherein the first cracking reactor is respectively connected to the non-aromatic component outlet of the raw material cutting device and the carrier gas outlet of the carrier gas preheating unit; A second cracking reactor, used for cracking the aromatic component and the first cracking product obtained by the first cracking reactor, wherein the second cracking reactor is connected to the aromatic component outlet of the raw material cutting device and the first cracking product outlet of the first cracking reactor respectively; Product collection unit, including A carbon black collector, which is provided with a quenching medium inlet and a gas product outlet, and is used to cool the second cracking product obtained by the second cracking reactor and collect the conductive carbon black, and the carbon black collector is connected to the second cracking product outlet of the second cracking reactor; one or more gas scrubbers and carbon black filters for scrubbing and filtering the gaseous products exiting the carbon black collector; The cracking gas collector is used to collect the cracking gas products after gas washing and carbon black filter washing and filtering.

8. The system according to claim 7, characterized in that The first cleavage reactor and / or the second cleavage reactor are tubular reactors; Preferably, the material of the tubular reactor is selected from one or more of the following: tungsten, molybdenum, tantalum, niobium, vanadium, chromium, titanium, zirconium, rare earth metal borides, rare earth metal carbides, rare earth metal nitrides, rare earth metal silicides, rare earth metal phosphides and rare earth metal sulfides, wherein the rare earth metal is selected from one or more of lanthanum, cerium, praseodymium and neodymium.

9. The system according to claim 7, characterized in that The outer circumference of the first cracking reactor and / or the second cracking reactor is sheathed with an electromagnetic induction coil for heating.

10. The system according to claim 7, characterized in that The first cracking reactor is arranged vertically or horizontally, preferably vertically; and / or The second cracking reactor is arranged horizontally.

Citation Information

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