High-temperature cracking reaction device and method

Abstract

The invention relates to a high-temperature cracking reaction device and method. The device comprises a sample introduction unit, a reaction unit and a product separation and collection unit. The device can realize cracking reaction with the cracking temperature as high as 2000 DEG C and the reaction time of millisecond, and can be used for high-temperature cracking test research of hydrocarbon raw materials.

Description

Technical Field

[0001] The invention relates to the field of petrochemicals, and in particular to a high-temperature cracking reaction device and method. Background Art

[0002] In China, due to the reduction of crude oil reserves and the increase of environmental awareness, the availability of inferior oil and the increase of processing profits have reduced the market share of low-quality gasoline and diesel. At the same time, the increase in demand for high-quality gasoline and the economic slowdown have led to a structural surplus of diesel, and the diesel market share is decreasing. However, chemical raw materials such as low-carbon olefins and aromatics are still in short supply, and it is necessary to achieve the transformation of refining for development. Therefore, it is necessary to develop high-temperature cracking technology for producing chemical raw materials from inferior heavy oil, so as to realize the transformation from refining to chemical industry.

[0003] Acetylene is an important basic organic chemical raw material. The main industrial methods for producing acetylene are calcium carbide method, methane partial oxidation method and methane arc cracking method. Among them, the calcium carbide method acetylene process is mature and accounts for an absolute proportion in industrial production, but the pollution and energy consumption are relatively high. Plasma cracking of coal to acetylene is a new and promising direct chemical conversion route for coal. Related research began in the 1960s at the University of Sheffield in the UK: in the high-temperature, high-enthalpy, and highly reactive arc thermal plasma jet, the volatile matter and even fixed carbon of coal can be directly converted into acetylene. Since then, a large number of studies have been concentrated in countries such as the United Kingdom, the United States, Germany, India, and the Soviet Union. Since the 1990s, Chinese scholars and engineering and technical personnel have conducted a large number of basic and engineering research in this field. With the development of technology, some researchers have also used plasma in the production of acetylene from coal tar, asphaltene, oil slurry, etc., but there have been no industrial reports.

[0004] Carbon black raw materials are divided into three categories: coal tar, ethylene tar and catalytic cracking residue. Carbon black raw materials require high aromatic content, large BMCI value, low sulfur content and less asphaltene. Coal tar and its distillate oil (including anthracene oil, anti-corrosion oil, etc.) are ideal carbon black raw materials, but the supply of coal tar has reached its peak and is gradually falling; ethylene tar is produced by cracking naphtha, and its tar has a high aromatic content and a low sulfur content, which is ideal for carbon black production. However, when ethylene is produced by cracking hydrocarbon oil or crude diesel, its tar aromatic content is low and the asphaltene content is high, which is not conducive to the production of carbon black. Therefore, catalytic cracking residue is used in large quantities in the United States to produce carbon black. Carbon black technology mainly uses the oil furnace method to produce carbon black. The average scale of the factory is about 70,000 tons / year, and the highest is 240,000 tons / year. The production equipment and process of each enterprise are basically the same. In recent years, the production equipment and process of foreign carbon black companies are moving towards energy conservation and environmental protection. At present, some new technologies and processes are still in the development stage. For example, the exhaust gas passes through a water scrubber to keep the temperature at 40°C and remove excess water vapor, carbon black dust, etc., so as to achieve the ideal environmental protection effect. Secondly, the installation of exhaust gas desulfurization equipment can avoid the pollution of low-sulfur oxides to the environment. In addition, in terms of product packaging, powdered carbon black can be squeezed into blocks and then packaged in vacuum bags. During use, the whole bag of carbon black is placed in the grinding equipment, which can directly reduce dust pollution during transportation and use, and also avoid the problem of carbon black absorbing moisture.

[0005] At present, the well-known conductive carbon black abroad includes Japan Lion's Ketjenblack series superconducting carbon black (Ketjenblack EC-300J and EC-600JD), the VXC series conductive carbon black of CABOT of the United States, PRINTEX XE2-B, PRINTEX L6, HIBLAXK 40B2 produced by Evonik Degussa, etc. The world's famous carbon black manufacturers, such as Cabot, Columbia, Akzo, etc., have invested a lot of manpower and material resources for a long time, committed to the development and production of conductive carbon black, and conducted special research on its application performance, forming conductive carbon black varieties suitable for different fields. The conductive carbon black products of these companies have the technical characteristics of large specific surface area, high oil absorption value, good conductivity and high purity. Europe, the United States and Japan have invested a lot of manpower, material and financial resources in the development of new energy vehicles, among which electric vehicles powered by lithium batteries are the main research objects, and their core technology is the technical development of lithium-ion batteries, and the core technology of lithium-ion batteries is the improvement of specific capacity, cycle life and safety. Conductive carbon black is an indispensable conductive agent in batteries. Its performance is directly related to the implementation of the core technology of the battery and the cost performance of the battery. Therefore, large foreign carbon black companies have targeted this market and invested a lot of effort in the development of conductive carbon black for power lithium-ion batteries or the improvement of existing products, and improved the conductivity of conductive carbon black products to meet the requirements of power batteries. The United States is the country with the largest carbon black production, and the sales volume of conductive carbon black produced by Cabot Corporation ranks among the top in the world. The Ketjen Black series superconducting carbon black of Lion of Japan is the best conductive carbon black, especially suitable for high-end conductive plastics, conductive rubber, etc. Other well-known foreign conductive carbon black research and development companies include Evonik Degussa, Nippon Electric Chemical Corporation and Swiss Termigo Co., Ltd.

[0006] Due to the limitations of heating methods, reactor types, and reactor materials, the reaction temperature of traditional oil refining test research equipment is generally below 700°C and the residence time is also relatively long. However, the production conditions of some high-end chemicals or chemical materials such as acetylene and carbon black have relatively strict requirements on reaction temperature and residence time. The current oil refining test equipment cannot meet the research needs. Summary of the invention

[0007] The purpose of the present invention is to provide an ultra-high temperature millisecond cracking reaction device, which can be used for experimental research on high-temperature cracking of hydrocarbon raw materials.

[0008] A first aspect of the present invention provides a high temperature cracking reaction device, the device comprising:

[0009] A sample injection unit, which includes a raw material feed pump, a raw material preheating furnace and a raw material purge gas preheating furnace;

[0010] A reaction unit comprising:

[0011] a first carrier gas preheating furnace, which is used to heat the carrier gas;

[0012] a second carrier gas preheating furnace, which is provided with a second carrier gas preheating inner tube and a second carrier gas preheating outer tube, and is used to further heat the carrier gas heated by the first carrier gas preheating furnace, the second carrier gas preheating furnace is heated by a first high-frequency electric induction heating device, and the first high-frequency electric induction heating device includes a first electromagnetic induction coil sleeved on the outer circumference of the second carrier gas preheating outer tube;

[0013] A reactor, which is provided with a reaction inner tube, a reaction inner sleeve and a reaction outer sleeve, and the reactor is also provided with a raw material inlet, the raw material inlet is connected to the raw material preheating furnace and the raw material purge gas preheating furnace of the sampling unit through a pipeline, and the reactor is heated by a second high-frequency electric induction heating device, and the second high-frequency electric induction heating device includes a second electromagnetic induction coil sleeved on the outer periphery of the reaction outer tube;

[0014] A product separation and collection unit, comprising:

[0015] a product cooler, which is provided with a cooling medium inlet, a cooling medium outlet and a product gas outlet, and the product cooler is connected to the outlet of the reactor through a pipeline;

[0016] A gas product collector is connected to the product gas outlet of the product cooler.

[0017] According to the device of the first aspect, the material of the second carrier gas preheating inner tube and / or the reaction inner tube is selected from one or more of the following: graphite, tungsten, molybdenum, tantalum, niobium, vanadium, chromium, titanium, zirconium, rare earth boride, rare earth carbide, rare earth nitride, rare earth silicide, rare earth phosphide, rare earth sulfide;

[0018] Wherein, the rare earth is selected from one or more of lanthanum, cerium, praseodymium and neodymium.

[0019] According to the device of the first aspect, the material of the reaction inner sleeve, the reaction outer sleeve and / or the carrier gas second preheating outer tube is selected from quartz and / or boron nitride.

[0020] The device according to the first aspect, wherein a filter is provided at the outlet connection of the reactor for filtering the product carbon black;

[0021] Preferably, the filter element is a quartz wool filter and / or a porous component;

[0022] More preferably, the mesh size of the quartz wool filter is 50-300 mesh; and / or the material of the porous component is selected from one or more of the following: tungsten, graphite, tungsten, molybdenum, tantalum, niobium, vanadium, chromium, titanium, zirconium, rare earth borides, rare earth carbides, rare earth nitrides, rare earth silicides, rare earth phosphides, and rare earth sulfides; wherein the rare earth is selected from one or more of lanthanum, cerium, praseodymium and neodymium.

[0023] According to the device of the first aspect, a gas-solid separator is provided at the bottom of the reaction jacket of the reactor;

[0024] Preferably, the separation method of the gas-solid separator is cyclone separation and / or sedimentation separation;

[0025] More preferably, the gas-solid separator is further connected to a filter, and the filter is preferably a metal sintered filter element or a container filled with a washing liquid.

[0026] The device according to the first aspect, wherein the device further comprises a temperature measuring instrument for testing the temperature of the reactor;

[0027] Preferably, the thermometer is a non-contact infrared thermometer.

[0028] The device according to the first aspect, wherein an injection port for injecting a cooling medium is provided in the middle and upper part of the product cooler; and / or

[0029] The product cooler is in an inverted cone shape.

[0030] The second aspect of the present invention provides an ultra-high temperature millisecond pyrolysis method, wherein the method uses the device described in the first aspect to perform pyrolysis, and comprises the following steps:

[0031] (1) introducing a carrier gas into the device to replace the air in the device;

[0032] (2) heating the feedstock oil, feedstock purge gas and carrier gas to a first preheating temperature respectively, introducing the carrier gas into a second carrier gas preheating furnace and further heating it to a second preheating temperature before entering the reactor, and purging the feedstock oil through a feedstock inlet on the reactor under the action of the feedstock purge gas into the reactor to undergo a cracking reaction;

[0033] (3) The carbon black product is collected in the reactor, and the cracking gas product is introduced into the product cooler. After being cooled by the cooling medium spray, the gas product enters the gas product collector for collection.

[0034] According to the method of the second aspect, wherein the first preheating temperature of the feedstock oil is 100-300°C;

[0035] The first preheating temperature of the raw material purge gas is 150-350°C;

[0036] The first preheating temperature of the carrier gas is 200-500° C.; and / or

[0037] The second preheating temperature of the carrier gas is 1000-2000°C.

[0038] According to the method of the second aspect, the purge gas and / or carrier gas is selected from one or more of the following: nitrogen, helium, argon, methane, C2-C4 light hydrocarbons; and / or

[0039] The raw oil is selected from one or more of the following: gasoline, diesel, heavy oil, slurry oil, dry gas, waste plastic oil, and tire oil.

[0040] According to the method of the second aspect, the cracking reaction conditions in the reactor are:

[0041] Temperature is 500-3000℃;

[0042] The response time is 3 milliseconds to 2 seconds;

[0043] The feed ratio of carrier gas to cracked crude oil per unit time is 1-15 liters / gram; and / or

[0044] The carrier gas flow rate is 0.05-30 L / min, preferably 0.1-10 L / min.

[0045] According to the method of the second aspect, the cooling medium is selected from one or more of the following: water, argon, nitrogen, preferably water.

[0046] The advantages of the present invention are:

[0047] (1) The electromagnetic induction coil heats the high-temperature cracking reactor, which can achieve rapid heating of the high-temperature cracking reactor, and the reaction temperature control is simple and the operation is stable.

[0048] (2) It can provide ultra-high temperature and millisecond residence time to achieve direct cracking of hydrocarbon feedstocks with high acetylene, hydrogen and carbon black yields.

[0049] (3) The flow rate of the carrier gas introduced through the carrier gas inlet controls the reaction linear velocity, thereby adjusting the rate at which the cracking raw materials pass through the reaction inner tube to control the reaction residence time.

[0050] (4) The type of inner sleeve provided can avoid direct contact between the inner tube of the reaction and the product, and can also realize electromagnetic induction heating control, thereby protecting the inner tube of the reaction, and can especially effectively prevent oxidation of the reaction tube and avoid contamination of the product carbon black.

[0051] (5) A filter component is provided at the lower part of the inner reaction tube, which can effectively filter out the carbon black produced by the reaction and prevent the carbon black from clogging the subsequent pipelines. BRIEF DESCRIPTION OF THE DRAWINGS

[0052] The accompanying drawings are used to provide a further understanding of the present invention and constitute a part of the specification. Together with the following specific embodiments, they are used to explain the present invention but do not constitute a limitation of the present invention. In the accompanying drawings:

[0053] Figure 1 A schematic diagram of the structure and flow of a specific implementation of the system of the present invention is shown.

[0054] Figure 2 The schematic diagram of the structure of the reactor of the present invention is shown.

[0055] Description of reference numerals:

[0056] 1. Preheating carrier gas pipeline; 2. Raw material purge gas pipeline; 3. Raw material oil pipeline; 4. Product gas pipeline I; 5. Product gas pipeline II; 6. Cooling medium inlet pipeline; 7. Cooling medium outlet pipeline; 8. Electromagnetic induction coil I; 9. Electromagnetic induction coil II; 101. Raw material preheating furnace; 102. Raw material purge gas preheating furnace; 103. Raw material inlet; 201. Thermometer; 202. Reactor; 203. Second carrier gas preheating furnace; 204. High-frequency electric induction heating device I; 205. High-frequency electric induction heating device II; 206. First carrier gas preheating furnace; 221. Reaction inner tube; 222. Reaction inner sleeve; 223. Reaction outer sleeve; 224. Inner sleeve seal; 225. Filter component; 226. Porous component; 301. Product cooler; 302. Gas product collector. DETAILED DESCRIPTION

[0057] 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.

[0058] 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.

[0059] 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.

[0060] The present invention provides a high temperature cracking reaction device, the device comprising:

[0061] A sample injection unit, which includes a raw material feed pump, a raw material preheating furnace and a raw material purge gas preheating furnace;

[0062] A reaction unit comprising:

[0063] a first carrier gas preheating furnace, which is used to heat the carrier gas;

[0064] a second carrier gas preheating furnace, which is provided with a second carrier gas preheating inner tube and a second carrier gas preheating outer tube, and is used to further heat the carrier gas heated by the first carrier gas preheating furnace, the second carrier gas preheating furnace is heated by a first high-frequency electric induction heating device, and the first high-frequency electric induction heating device includes a first electromagnetic induction coil sleeved on the outer circumference of the second carrier gas preheating outer tube;

[0065] A reactor, which is provided with a reaction inner tube, a reaction inner sleeve and a reaction outer sleeve, and the reactor is also provided with a raw material inlet, the raw material inlet is connected to the raw material preheating furnace and the raw material purge gas preheating furnace of the sampling unit through a pipeline, and the reactor is heated by a second high-frequency electric induction heating device, and the second high-frequency electric induction heating device includes a second electromagnetic induction coil sleeved on the outer periphery of the reaction outer tube;

[0066] A product separation and collection unit, comprising:

[0067] a product cooler, which is provided with a cooling medium inlet, a cooling medium outlet and a product gas outlet, and the product cooler is connected to the outlet of the reactor through a pipeline;

[0068] A gas product collector is connected to the product gas outlet of the product cooler.

[0069] 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.

[0070] like Figure 1 As shown, the present invention provides an ultra-high temperature millisecond cracking reaction device, which includes a sampling unit (including a raw material preheating furnace 101, a raw material purge gas preheating furnace 102 and a raw material inlet 103), a reaction unit (including a temperature meter 201, a reactor 202, a carrier gas second preheating furnace 203, a high-frequency electric induction heating device I 204 and a high-frequency electric induction heating device II 205), and a product separation and collection system (a product cooler 301 and a gas product collector 302).

[0071] The ultra-high temperature millisecond cracking device sampling system includes a raw material preheating furnace 101, a raw material purge gas preheating furnace 102 and a raw material sampling port 103. The raw material is introduced into the raw material preheating furnace through a raw material oil pump, introduced into the raw material sampling port through a raw material oil pipeline, and introduced into the reactor 202 through the preheated purge gas. At the same time, a large flow of carrier gas is preheated in the first carrier gas preheating furnace 206 and then introduced into the second carrier gas preheating furnace 203, and then enters the reactor 202. The reaction raw material undergoes a cracking reaction from top to bottom, and the reaction product gas is filtered through a filter component located at the bottom of the reactor 202 to filter the carbon black. The cracked gas enters the product cooler 301 through pipeline 4, is rapidly cooled by a quenching medium, and then enters the gas collection tank through pipeline 5.

[0072] The electromagnetic induction coil I8 is connected to the high-frequency electric induction heating device I204 for carrier gas heating.

[0073] The electromagnetic induction coil II9 is ​​connected to the high-frequency induction heating device II205 for heating the reactor.

[0074] In one embodiment, the material of the second carrier gas preheating inner tube and / or the reaction inner tube is selected from one or more of the following: graphite, tungsten, molybdenum, tantalum, niobium, vanadium, chromium, titanium, zirconium, rare earth boride, rare earth carbide, rare earth nitride, rare earth silicide, rare earth phosphide, rare earth sulfide;

[0075] Wherein, the rare earth is selected from one or more of lanthanum, cerium, praseodymium and neodymium.

[0076] In one embodiment, the material of the reaction inner sleeve, the reaction outer sleeve and / or the carrier gas second preheating outer tube is selected from quartz and / or boron nitride.

[0077] According to the present invention, Figure 1 As shown, the reaction device includes a first carrier gas preheating furnace 206 and a second carrier gas preheating furnace 203; the carrier gas preheating furnace is provided with a carrier gas inlet and a preheated carrier gas outlet, and the preheated material outlet of the first carrier gas preheating furnace is connected to the inlet of the second carrier gas preheating furnace 203 through a pipeline 1; the second carrier gas preheating furnace is provided with a carrier gas inlet and a preheated material outlet, and the preheated material outlet of the second carrier gas preheating furnace is connected to the reactor 202. The reaction device also includes a raw material preheating furnace 101, which is provided with a raw material inlet and a preheated raw material outlet, and the outlet of the raw material preheating furnace is connected to the raw material inlet 103 of the reactor 202 through a pipeline 3. The reaction device also includes a raw material purge gas preheating furnace 102, which is provided with a gas inlet and a preheated material outlet, and the outlet of the raw material purge gas preheating furnace is connected to the raw material inlet 103 of the reactor 202 through a pipeline 2. Preheating the cracking raw material and the carrier gas can enable the cracking raw material and the carrier gas to quickly reach the reaction temperature in the high-temperature cracking reactor and improve the cracking yield.

[0078] The present invention adopts electromagnetic induction heating to heat the high-temperature cracking reactor, so that the high-temperature cracking reactor can be heated quickly and the temperature is stable. Compared with the plasma reactor, the equipment is simple, easy to implement, convenient to operate, and the volume of the equipment is greatly reduced, which is conducive to the construction of laboratory equipment. Moreover, the acetylene and hydrogen yields can reach the level of plasma reactor cracking.

[0079] The electromagnetic induction coil is sleeved on the outer circumference of the outer sleeve to heat the inner reaction tube through the alternating magnetic field generated by the electromagnetic induction coil. High-frequency electric induction heating equipment is well known to those skilled in the art. On the one hand, it can power the electromagnetic induction coil, and on the other hand, it can be provided with an electromagnetic heating controller to control the frequency of the alternating current input into the electromagnetic induction coil. The electromagnetic heating controller is well known to those skilled in the art, and the present invention will not be described in detail.

[0080] In one embodiment, a filter is provided at the outlet connection of the reactor to filter the product carbon black;

[0081] Preferably, the filter element is a quartz wool filter and / or a porous component;

[0082] More preferably, the mesh size of the quartz wool filter is 50-300 mesh; and / or the material of the porous component is selected from one or more of the following: tungsten, graphite, tungsten, molybdenum, tantalum, niobium, vanadium, chromium, titanium, zirconium, rare earth borides, rare earth carbides, rare earth nitrides, rare earth silicides, rare earth phosphides, and rare earth sulfides; wherein the rare earth is selected from one or more of lanthanum, cerium, praseodymium and neodymium.

[0083] like Figure 2 As shown, the reactor 202 includes a reaction inner tube 221, a reaction inner sleeve 222, and a reaction outer sleeve 223. One end of the reaction inner sleeve 222 is closed, and the open end is inserted into the reaction inner tube 221 and sealed with an inner sleeve seal 224. The outlet end of the reaction outer sleeve 223 is also provided with a filter component 225 and a porous component 226.

[0084] Among them, the inner reaction tube is used for electromagnetic induction heating, the inner reaction tube and the inner tube seal can avoid direct contact between the inner reaction tube and the product, and can realize electromagnetic induction heating control, so as to protect the inner reaction tube, especially effectively prevent the oxidation of the inner reaction tube, and avoid contamination of the product carbon black. The outer reaction tube is the place where the cracking reaction occurs, and the filter component and the porous component are used to filter out the carbon black produced by the reaction to prevent the carbon black from clogging the subsequent pipeline, and the porous component supports the filter component.

[0085] In one embodiment, a gas-solid separator is provided at the bottom of the reaction jacket of the reactor;

[0086] Preferably, the separation method of the gas-solid separator is cyclone separation and / or sedimentation separation;

[0087] More preferably, the gas-solid separator is further connected to a filter, and the filter is preferably a metal sintered filter element or a container filled with a washing liquid.

[0088] In one embodiment, an injection port for injecting cooling medium is provided in the upper middle portion of the product cooler; and / or

[0089] The product cooler is in an inverted cone shape.

[0090] According to the present invention, in order to further purify and collect gas products, the system also includes a gas product collector 302 and an optional gas-solid separator and / or filter. The gas-solid separator is arranged at the bottom of the outer sleeve of the reactor 202. The gas-solid separator is used to perform coarse separation of the reaction products, which can be cyclone separation, sedimentation separation, etc. The filter further separates the gas products separated by the gas-solid separator, and can be a metal sintered filter element or a container filled with washing liquid. The filtration accuracy of the metal sintered filter element can be less than 5 microns. The gas product collector 302 can be a container such as a gas tank or an air bag.

[0091] In one embodiment, the device further comprises a temperature measuring instrument for testing the temperature of the reactor;

[0092] Preferably, the thermometer is a non-contact infrared thermometer.

[0093] In order to control and monitor the reaction temperature, such as Figure 1 As shown, the reaction system may further include a thermometer 201, which is preferably a non-contact infrared high temperature thermometer. The temperature near the outlet of the reaction inner tube can be measured by the thermometer, and the heating power of the heat source can be adjusted according to the temperature, preferably by a PID controller in a closed-loop control mode to adjust the heating power of the heat source according to the temperature measured by the thermometer.

[0094] The present invention also provides an ultra-high temperature millisecond cracking method, which uses the above device to perform cracking, and comprises the following steps:

[0095] (1) introducing a carrier gas into the device to replace the air in the device;

[0096] (2) heating the feedstock oil, feedstock purge gas and carrier gas to a first preheating temperature respectively, introducing the carrier gas into a second carrier gas preheating furnace and further heating it to a second preheating temperature before entering the reactor, and purging the feedstock oil through a feedstock inlet on the reactor under the action of the feedstock purge gas into the reactor to undergo a cracking reaction;

[0097] (3) The carbon black product is collected in the reactor, and the cracking gas product is introduced into the product cooler. After being cooled by the cooling medium spray, the gas product enters the gas product collector for collection.

[0098] In one embodiment, the first preheating temperature of the feedstock oil is 100-300°C;

[0099] The first preheating temperature of the raw material purge gas is 150-350°C;

[0100] The first preheating temperature of the carrier gas is 200-500° C.; and / or

[0101] The second preheating temperature of the carrier gas is 1000-2000°C.

[0102] In one embodiment, the purge gas and / or carrier gas is selected from one or more of the following: nitrogen, helium, argon, methane, C2-C4 light hydrocarbons; and / or

[0103] The raw oil is selected from one or more of the following: gasoline, diesel, heavy oil, slurry oil, dry gas, waste plastic oil, and tire oil.

[0104] In one embodiment, the cleavage reaction conditions in the reactor are:

[0105] Temperature is 500-3000℃;

[0106] The response time is 3 milliseconds to 2 seconds;

[0107] The feed ratio of carrier gas to cracked crude oil per unit time is 1-15 liters / gram; and / or

[0108] The carrier gas flow rate is 0.05-30 L / min, preferably 0.1-10 L / min.

[0109] In one embodiment, the cooling medium is selected from one or more of the following: water, liquid nitrogen, nitrogen gas, preferably water.

[0110] Specifically, the steps of performing a high temperature cracking reaction in the high temperature cracking device provided by the present invention are as follows:

[0111] (1) After the reaction inner tube 221 is installed into the reactor inner sleeve 222, it is sealed with the inner sleeve seal 224. The reactor inner sleeve 222 is installed into the reaction outer sleeve 223. Quartz wool is installed at the bottom of the reaction outer sleeve as a filter element 225 and a porous element 226 is used as a support for the filter element. The outer sleeve outlet is sealed and connected to the product quench tank. The air tightness of the device is checked. The carrier gas flow is turned on to replace the air in the reaction system.

[0112] (2) open heating switch, stock oil is preheated by stock oil preheating furnace, carrier gas is preheated by carrier gas first preheating furnace, purge gas is preheated through purge gas preheating furnace, treat that temperature reaches set value, by electromagnetic induction coil 8, carrier gas second preheating furnace 203 is warming up to preset high temperature carrier gas preheating temperature, then the cracking raw material preheated by raw material preheating furnace 101 is introduced into reactor 202 from cracking raw material entrance, under the high temperature effect of high temperature preheating carrier gas outlet high temperature preheating carrier gas and reactor, cracking raw material is gasified and carries out cracking reaction, now by the flow velocity of the carrier gas such as the nitrogen that enters from the carrier gas pipeline 1 can control the reaction residence time of cracking raw material in the reaction interior tube, and then optimize the cracking reaction product distribution, the flow of carrier gas can be adjusted as required in a larger range, for example, is 50-10000 ml / minute.From reactor 202 cracking gained cracking reaction product is introduced into product cooler 301 by pipeline 4 from reactor 202 bottoms after separating carbon black, and described product cooler 301 is preferably product chilling tank. After being cooled by the spraying of the quenching medium, it enters the gas product collector 302.

[0113] The present invention is further illustrated by the following examples, but the present invention is not limited thereto.

[0114] In the embodiments and comparative examples:

[0115] The reaction temperature refers to the temperature in the middle of the reaction tube covered by the electromagnetic induction coil;

[0116] Reaction time = length of inner reaction tube / flow rate of reaction material in inner reaction tube;

[0117] Product yield = product weight / cracking raw material weight × 100%;

[0118] The gaseous reaction products were determined by gas chromatography.

[0119] Example 1 - Example 2

[0120] Embodiments 1 and 2 are respectively Figure 1 The device shown uses catalytic diesel with properties as described in Table 1 as cracking raw material according to the process of the above-mentioned specific implementation method, the raw material preheating temperature is 250°C, the purge gas preheating temperature is 250°C, the carrier gas is nitrogen, the first carrier gas preheating furnace temperature is 500°C, and the second carrier gas preheating furnace temperature is 1200°C. Figure 2The schematic diagram of the structure of the reactor of the present invention is shown, wherein the total height of the reactor is H, and the height of the raw material injection port is h. In this embodiment, tungsten tubes are used as the inner reaction tubes, the number is 5, the inner diameter is 2 mm, the outer diameter is 3 mm, and the height is 90 mm. The inner reaction sleeve is a quartz tube with one end closed, the inner diameter is 4 mm, the outer diameter is 5 mm, and the height is 110 mm. The open end of the inner reaction sleeve is filled with the inner reaction tube and sealed with quartz wool; the outer reaction sleeve is a quartz tube with an inner diameter of 14 mm, an outer diameter of 22 mm, and a height of H of 270 mm. The height h of the raw material injection port is 250 mm. The top of the inner reaction sleeve is located at the raw material injection port. 5mm below the mouth, the outer periphery of the reaction outer sleeve is covered with an electromagnetic induction coil, the inner diameter of the electromagnetic induction coil is 25mm, and the upper and lower ends of the electromagnetic induction coil are respectively about 5mm lower than the upper and lower ends of the reaction inner sleeve; the porous component is a tungsten plate, the porous component is 10mm away from the bottom of the tungsten tube, the opening rate is 32.45%, and the pore size is 0.053mm; the filter component is a quartz wool filter, the quartz wool filter is 10mm away from the bottom of the tungsten tube, and the mesh size is 60 mesh; the porous component supports the filter component. Water is used as the quenching medium, and the gas collector is a gas collection bag. The specific reaction conditions and reaction results are shown in Table 2.

[0121] It can be seen from the results in Table 2 that the device can achieve high-temperature, millisecond-level cracking reactions, and the device has good material balance and parallelism.

[0122] Table 1

[0123] Raw material name Catalytic diesel <![CDATA[Density (20 °C) / (g / cm 3 )]]> 0.8965 Refractive index (20℃) 1.5579 Sulfur content / (weight %) 0.231 Nitrogen content / (μg / g) 548 Carbon content / weight% 89.23 Hydrogen content / weight% 10.32 Hydrocarbon composition / ℃ Paraffins, weight % 16.9 Cycloalkanes, weight % 6.0 Monocyclic aromatic hydrocarbons, weight % 56.0 Bicyclic aromatic hydrocarbons, weight % 21.1 Tricyclic aromatic hydrocarbons, weight % 0.0 Total aromatics, weight % 77.1 Gel, weight% 0.0

[0124] Table 2

[0125] Example 1 Example 2 Cracking raw materials Catalytic diesel Catalytic diesel Reaction temperature, °C 1450 1450 Carrier gas flow rate, L / min 4 4 Oil inlet speed, g / min 0.5 0.5 Oil inlet time, minutes 2 2 Response time, milliseconds 19.06 20.78 Gas product yield, weight % 18.12 18.49 Acetylene yield, weight % 12.34 12.56 Hydrogen yield, weight % 6.89 6.76 Carbon black yield, weight % 78.52 78.25 Total, weight % 96.64 96.74 Loss, weight % 3.36 3.26

[0126] 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.

[0127] 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 high temperature cracking reaction device, characterized in that: The device comprises: A sample injection unit, which includes a raw material feed pump, a raw material preheating furnace and a raw material purge gas preheating furnace; A reaction unit comprising: a first carrier gas preheating furnace, which is used to heat the carrier gas; a second carrier gas preheating furnace, which is provided with a second carrier gas preheating inner tube and a second carrier gas preheating outer tube, and is used to further heat the carrier gas heated by the first carrier gas preheating furnace, the second carrier gas preheating furnace is heated by a first high-frequency electric induction heating device, and the first high-frequency electric induction heating device includes a first electromagnetic induction coil sleeved on the outer circumference of the second carrier gas preheating outer tube; A reactor, which is provided with a reaction inner tube, a reaction inner sleeve and a reaction outer sleeve, and the reactor is also provided with a raw material inlet, the raw material inlet is connected to the raw material preheating furnace and the raw material purge gas preheating furnace of the sampling unit through a pipeline, and the reactor is heated by a second high-frequency electric induction heating device, and the second high-frequency electric induction heating device includes a second electromagnetic induction coil sleeved on the outer periphery of the reaction outer tube; A product separation and collection unit, comprising: a product cooler, which is provided with a cooling medium inlet, a cooling medium outlet and a product gas outlet, and the product cooler is connected to the outlet of the reactor through a pipeline; A gas product collector is connected to the product gas outlet of the product cooler.

2. The device according to claim 1, characterized in that The material of the second carrier gas preheating inner tube and / or the reaction inner tube is selected from one or more of the following: graphite, tungsten, molybdenum, tantalum, niobium, vanadium, chromium, titanium, zirconium, rare earth boride, rare earth carbide, rare earth nitride, rare earth silicide, rare earth phosphide, rare earth sulfide; Wherein, the rare earth is selected from one or more of lanthanum, cerium, praseodymium and neodymium.

3. The device according to claim 1, characterized in that The material of the inner reaction tube, the outer reaction tube and / or the second carrier gas preheating outer tube is selected from quartz and / or boron nitride.

4. The device according to claim 1, characterized in that A filter is provided at the outlet connection of the reactor to filter the product carbon black; Preferably, the filter element is a quartz wool filter and / or a porous component; More preferably, the mesh size of the quartz wool filter is 50-300 mesh; and / or the material of the porous component is selected from one or more of the following: tungsten, graphite, tungsten, molybdenum, tantalum, niobium, vanadium, chromium, titanium, zirconium, rare earth borides, rare earth carbides, rare earth nitrides, rare earth silicides, rare earth phosphides, and rare earth sulfides; wherein the rare earth is selected from one or more of lanthanum, cerium, praseodymium and neodymium.

5. The device according to claim 1, characterized in that A gas-solid separator is provided at the bottom of the reaction jacket of the reactor; Preferably, the separation method of the gas-solid separator is cyclone separation and / or sedimentation separation; More preferably, the gas-solid separator is further connected to a filter, and the filter is preferably a metal sintered filter element or a container filled with a washing liquid.

6. The device according to claim 1, characterized in that The device also includes a temperature measuring instrument for testing the temperature of the reactor; Preferably, the thermometer is a non-contact infrared thermometer.

7. The device according to claim 1, characterized in that The product cooler is provided with an injection port for injecting cooling medium in the middle and upper part; and / or The product cooler is in an inverted cone shape.

8. An ultra-high temperature millisecond pyrolysis method, characterized in that: The method uses the device according to any one of claims 1 to 7 for lysis, comprising the following steps: (1) introducing a carrier gas into the device to replace the air in the device; (2) heating the feedstock oil, feedstock purge gas and carrier gas to a first preheating temperature respectively, introducing the carrier gas into a second carrier gas preheating furnace and further heating it to a second preheating temperature before entering the reactor, and purging the feedstock oil through a feedstock inlet on the reactor under the action of the feedstock purge gas into the reactor to undergo a cracking reaction; (3) The carbon black product is collected in the reactor, and the cracking gas product is introduced into the product cooler. After being cooled by the cooling medium spray, the gas product enters the gas product collector for collection.

9. The method according to claim 8, characterized in that The first preheating temperature of the raw oil is 100-300°C; The first preheating temperature of the raw material purge gas is 150-350°C; The first preheating temperature of the carrier gas is 200-500° C.; and / or The second preheating temperature of the carrier gas is 1000-2000°C.

10. The method according to claim 8, characterized in that The purge gas and / or carrier gas is selected from one or more of the following: nitrogen, helium, argon, methane, C2-C4 light hydrocarbons; and / or The raw oil is selected from one or more of the following: gasoline, diesel, heavy oil, slurry oil, dry gas, waste plastic oil, and tire oil.

11. The method according to claim 8, characterized in that The cracking reaction conditions in the reactor are: Temperature is 500-3000℃; The response time is 3 milliseconds to 2 seconds; The feed ratio of carrier gas to cracked crude oil per unit time is 1-15 liters / gram; and / or The carrier gas flow rate is 0.05-30 L / min, preferably 0.1-10 L / min.

12. The method according to claim 8, characterized in that The cooling medium is selected from one or more of the following: water, argon, nitrogen, preferably water.

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