WO2019149008A1 - 一种新型高温裂解反应装置 - Google Patents

一种新型高温裂解反应装置 Download PDF

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Publication number
WO2019149008A1
WO2019149008A1 PCT/CN2018/124679 CN2018124679W WO2019149008A1 WO 2019149008 A1 WO2019149008 A1 WO 2019149008A1 CN 2018124679 W CN2018124679 W CN 2018124679W WO 2019149008 A1 WO2019149008 A1 WO 2019149008A1
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condenser
atomizer
cracking reactor
cracking
temperature
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PCT/CN2018/124679
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English (en)
French (fr)
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聂勇
解庆龙
段莹
夏凡
卢美贞
于尚志
梁晓江
计建炳
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浙江工业大学
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Priority to US17/047,707 priority Critical patent/US11407948B2/en
Publication of WO2019149008A1 publication Critical patent/WO2019149008A1/zh

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006Controlling or regulating processes
    • B01J19/0013Controlling the temperature of the process
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24Stationary reactors without moving elements inside
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • B01J4/001Feed or outlet devices as such, e.g. feeding tubes
    • B01J4/002Nozzle-type elements
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • B01J4/008Feed or outlet control devices
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J6/00Heat treatments such as Calcining; Fusing ; Pyrolysis
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J6/00Heat treatments such as Calcining; Fusing ; Pyrolysis
    • B01J6/008Pyrolysis reactions
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G9/00Thermal non-catalytic cracking, in the absence of hydrogen, of hydrocarbon oils
    • C10G9/14Thermal non-catalytic cracking, in the absence of hydrogen, of hydrocarbon oils in pipes or coils with or without auxiliary means, e.g. digesters, soaking drums, expansion means
    • C10G9/18Apparatus
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00139Controlling the temperature using electromagnetic heating

Definitions

  • the invention relates to the field of chemical production, in particular to a novel high temperature cracking reaction device.
  • Pyrolysis is a chemical process that uses thermal energy to convert a substance into several other substances. Pyrolysis reactions are widely used in petrochemical production processes. High-temperature cracking methods are commonly used in industrial production to convert petroleum hydrocarbons into small molecules of olefins, alkynes and aromatic hydrocarbons, such as ethylene, propylene, butadiene, acetylene, benzene, toluene, etc., and then synthesize and produce other chemical products as raw materials. Pyrolysis reaction is often used in the oleochemical industry to produce fine chemicals with high added value.
  • methyl ricinoleate can be obtained by high temperature cracking to obtain methyl undecylenate, which can be further processed to produce nylon- 11 raw materials.
  • pyrolysis reaction is also widely used in other organic chemical production, such as pyrolysis of acetone to form ketene, which is an important intermediate for organic synthesis.
  • the pyrolysis reaction of liquids in the industry is often carried out by combustion cracking (Chinese patent CN 1751984A, CN 102951616A, CN 106744716A), and the gas and air are mixed and burned, and the heat released by the combustion is used to form a high temperature environment in the cracking furnace. .
  • the pyrolysis furnace in this high-temperature pyrolysis mode can only be controlled within a certain range, and is often used for waste liquid treatment. It is difficult to meet the requirements for high-temperature cracking reactions that require precise temperature control or high temperature influence.
  • the Chinese patent CN 104341298A uses microwave heating to carry out the high temperature cracking reaction of methyl ricinoleate. The processing amount of the raw material is easily limited by the power of the magnetron of the microwave generating device, which is difficult to achieve under the existing technical conditions. Larger capacity; and the need for absorbing materials as heating media increases costs.
  • Electromagnetic heating is widely used for its excellent heating performance (Chinese Patent CN 103561491A, CN 105025604A, CN 107477844A, CN 107339796A). Electromagnetic heating has the advantages of fast hot start, high thermal efficiency and good heating uniformity. In addition, the electromagnetic heating coil itself does not generate heat, the thermal block is small, and the thermal inertia is low, so that precise temperature control can be realized, and electromagnetic heating can easily realize amplification of the device and improvement of productivity. Spray technology can break up liquid materials to form uniform fine mist droplets, which can achieve efficient heat transfer. It is widely used in the fields of cooling, combustion, cracking, etc.
  • the object of the present invention is to overcome the deficiencies of the prior art and to provide a novel high temperature cracking reaction apparatus.
  • the novel pyrolysis reaction device mainly comprises a feed pump, a flow meter, an atomizer, a cracking reactor, an electromagnetic coil, an electromagnetic heating power source, a temperature sensor, and a temperature control.
  • the instrument, the condenser, the product tank, the feed pump are connected with a flow meter, the flow meter is connected with the atomizer inlet of the atomizer, the atomizer is placed in the cracking reactor, and the lower part of the cracking reactor has a cracking reactor lower mouth.
  • the cracking reactor of the cracking reactor is connected with a condenser, and the condenser is connected with the product tank.
  • the outer wall of the cracking reactor is wound with an electromagnetic coil, the electromagnetic coil is connected with the electromagnetic heating power source, and a temperature sensor is placed between the cracking reactor and the electromagnetic coil.
  • the temperature sensor is connected to a temperature controller.
  • the cleavage reactor is provided with an upper mouth of the cleavage reactor, and the upper position of the cleavage reactor is located at the upper part of the cleavage reactor, and the cleavage reactor is composed of stainless steel, carbon steel, iron and other materials with high temperature resistance and good magnetic permeability. .
  • the atomizer is placed in the middle of the cracking reactor cavity, the atomizer is nozzle type or centrifugal type, and the nozzle atomizer head is single, single layer and multiple layers, nozzle atomizer
  • the nozzle is fixed and rotated by an intermediate vertical feed tube.
  • the atomizer is made of stainless steel, copper and other materials with high temperature resistance and poor magnetic permeability.
  • the temperature sensor is a thermocouple and a thermistor, and the temperature sensor temperature measuring point is set in the middle of the electromagnetic coil.
  • the material fed by the feed pump is a liquid, slurryed fluid.
  • the condenser is provided with one condenser, two condensers, three condensers and four condensers.
  • the product tank has one product tank, two product tanks, three product tanks, and one condenser is connected to the upper end of the cracking reactor.
  • the condenser is connected to the product tank.
  • the invention adopts the process of the novel high temperature cracking reaction device, and the specific steps are as follows:
  • the cracking raw material is transported through the feed pump, and after being metered by the flow meter, it is atomized into fine droplets by the atomizer, and the droplets are sprayed on the inner wall of the cracking reactor to be cracked.
  • the cracking feedstock is rapidly cracked at a set temperature to form a gaseous cracked product, and the cracked gas is introduced into the condenser through the discharge pipe to be condensed into the product tank.
  • the electromagnetic heating process of the invention adopts internal heat heating mode, has fast hot start, high thermal efficiency, low thermal inertia, good heating uniformity, and can provide a uniform and stable high temperature reaction place. Electromagnetic heating is easy to achieve amplification of the device and increase in productivity.
  • the spraying technology of the invention eliminates the contact thermal resistance between the spray medium and the high temperature surface, realizes rapid temperature cracking of the material, shortens the reaction time, improves the reaction efficiency, and improves the target product yield.
  • FIG. 1 is a schematic flow chart and structure of the present invention (atomizer nozzle atomizer).
  • the atomizer is a centrifugal atomizer.
  • FIG 3 is a schematic view showing the distribution of the nozzles of the multi-nozzle nozzle atomizer of the present invention.
  • the new high-temperature cracking reaction device mainly includes a feed pump 1, a flow meter 2, an atomizer 3, a cracking reactor 4, an electromagnetic coil 5, an electromagnetic heating power source 6, a temperature sensor 7, and temperature control.
  • the lower portion of the reactor 4 has a cracking reactor lower port 42.
  • the cracking reactor upper port 41 of the cracking reactor 4 is connected with a condenser 9, and the condenser 9 is connected to the product tank 10.
  • the outer wall of the cracking reactor 4 is wound with an electromagnetic coil 5, The electromagnetic coil 5 is connected to the electromagnetic heating power source 6, a temperature sensor 7 is placed between the cracking reactor 4 and the electromagnetic coil 5, and the temperature sensor 7 is connected to the temperature controller 8.
  • the cracking reactor 4 is provided with a cracking reactor upper port 41, and the cracking reactor upper port 41 is located at the upper portion of the cracking reactor 4, and the cracking reactor 4 is made of stainless steel, carbon steel, iron and other high temperature resistant Made of magnetic material.
  • the atomizer 3 is placed in the middle of the cavity of the cracking reactor 4, the atomizer 3 is nozzle type or centrifugal type, and the nozzles of the nozzle atomizer are single, single layer multiple and multiple layers, nozzle type fog
  • the nozzle of the chemical device is fixed or rotated by an intermediate vertical feeding tube.
  • the atomizer 3 is made of stainless steel, copper and other materials with high temperature resistance and poor magnetic permeability.
  • the temperature sensor 7 is a thermocouple and a thermistor, and the temperature measuring point of the temperature sensor 7 is provided in the middle of the electromagnetic coil 5.
  • the feed material of the feed pump 1 is a liquid, slurryed fluid.
  • the condenser 9 is provided with a condenser one port 91, a condenser two ports 92, a condenser three ports 93, and a condenser four ports 94.
  • the product tank 10 has a product tank one 101, a product tank two 102, a product tank three 103, and condensation.
  • a port 91 is connected to the upper port 41 of the cracking reactor, and a condenser port 92 is connected to the product tank 101.
  • the invention adopts the process of the novel high temperature cracking reaction device, and the specific steps are as follows:
  • the cracked raw material is transported through the feed pump 1, and after being metered by the flow meter 2, it is atomized into fine droplets by the atomizer 3, and the droplets are sprayed on the inner wall of the cracking reactor 4 to be cracked.
  • the cracking feedstock is rapidly cracked at a set temperature to form a gaseous cracked product, and the cracked gas is introduced into the condenser 9 through the discharge pipe and condensed into the product tank 10.
  • Example 1 High-purity ricinoleic acid methyl ester (purity greater than 99%) was used as a raw material for pyrolysis to obtain methyl undecylenate.
  • the atomizer 3 used was a four-nozzle fixed nozzle atomizer, and atomized.
  • the nozzle distribution of the device 3 is as shown in FIG.
  • the electromagnetic coil 5 was uniformly wound around the outer wall of the chamber of the cracking reactor 4, and the reaction temperature of the electromagnetic coil 5 was set at 500 °C.
  • the nozzle atomizer 3 is placed in the middle of the chamber of the cracking reactor 4, the feed tube is connected to the inlet A of the nozzle atomizer 3, and the discharge tube is connected to the outlet B of the cracking reactor 4, and is connected to the condenser.
  • the condenser three ports 93 are chilled water inlets, and the condenser four ports 94 are chilled water outlets.
  • the electromagnetic heating power source 6 to start the energization of the electromagnetic coil 5
  • the cracking reactor 4 starts to heat up, and after the temperature reaches the set value and stabilizes for a period of time, the raw material (high-purity ricinoleic acid methyl ester) is transported and flowed through the feed pump 1.
  • the meter 2 is metered at a flow rate of 20 kg/h through the atomizer inlet 31 of the nozzle atomizer 3 and atomized into fine droplets by the nozzle atomizer 3, and the droplets are sprayed on the inner wall of the cracking reactor 4 to be lysed. reaction.
  • the raw material is rapidly cracked at a set temperature to form a product methyl undecylenate and heptaldehyde gas, and a gas is introduced into the cracking reactor upper port 41 of the condenser 9 through the outlet B, and the resulting liquid obtained by condensation is condensed from the condenser 9.
  • the two ports 92 are discharged and enter the product tank 10 through the product tank 101.
  • the product tank 10 of the product tank 10 can be evacuated to provide a vacuum operating condition for the cracking system.
  • a small amount of the cleavage residue in the cleavage reactor 4 is discharged through the cleavage reactor lower port 42.
  • the cleavage product is separated and purified by a downstream rectification device to obtain methyl undecylenate, which is acidified by saponification to obtain undecylenic acid.
  • the results of the examples are as follows: the yield of electromagnetic heating pyrolysis solution is 90%, the yield of undecylenic acid is 73%, and the yield of the conventional electric heating process reported by Chinese patent CN101289383A is 34 to 38%, in contrast, this The yield of the undecylenic acid of the invention can be increased by about 1 time.
  • Example 2 High-purity ricinoleic acid methyl ester (purity greater than 99%) was used as a raw material for pyrolysis to obtain methyl undecylenate.
  • the atomizer 3 used was a centrifugal atomizer. As shown in Fig. 2, the electromagnetic coil 5 was uniformly wound around the outer wall of the chamber of the cracking reactor 4, and the reaction temperature of the electromagnetic coil 5 was set at 500 °C.
  • the centrifugal atomizer 3 is placed in the middle of the chamber of the cracking reactor 4, and the feed tube is connected to the inlet tube A of the centrifugal atomizer 3, and the discharge tube is connected to the outlet B of the cracking reactor 4, and connected
  • the condenser three ports 93 are chilled water inlets
  • the condenser four ports 94 are chilled water outlets.
  • the liquid is atomized into fine droplets, and the droplets are sprayed in the cracking reactor A cracking reaction occurred on the inner wall of 4.
  • the raw material is rapidly cracked at a set temperature to form a product methyl undecylenate and heptaldehyde gas, and the generated gas is introduced into the condenser 91 of the condenser 9 through the upper port 41 of the cracking reactor, and the resulting liquid is condensed from the condenser 9
  • the condenser two ports 92 are discharged and enter the product tank 10 through the product tank 101.
  • the product tank 10 of the product tank 10 can be evacuated to provide a vacuum operating condition for the cracking system.
  • a small amount of the cleavage residue in the cleavage reactor 4 is discharged through the cleavage reactor lower port 42.
  • the cleavage product is separated and purified by a downstream rectification device to obtain methyl undecylenate, which can be obtained by saponification and acidification to obtain undecylenic acid.
  • the yield of electromagnetic heating pyrolysis solution is 92%
  • the yield of undecylenic acid is 70%
  • the yield of the conventional electric heating process reported by Chinese patent CN101289383A is 34 to 38%, in contrast, this
  • the yield of the undecylenic acid of the invention can be increased by about 1 time.
  • the product tank two ports 102 are vented or evacuated to provide a vacuum operating condition for the cracking system.

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Abstract

一种新型高温裂解反应装置,主要包括进料泵(1)、流量计(2)、雾化器(3)、裂解反应器(4)、电磁线圈(5)、电磁加热电源(6)、温度传感器(7)、温控仪(8)、冷凝器(9)、产品罐(10),进料泵(1)连有流量计(2),流量计(2)与雾化器(3)的雾化器进口(31)相连,雾化器(3)置于裂解反应器(4)中,裂解反应器(4)下部有裂解反应器下口(42),裂解反应器(4)的裂解反应器上口(41)连有冷凝器(9),冷凝器(9)与产品罐(10)相连,裂解反应器(4)的外壁绕有电磁线圈(5),电磁线圈(5)与电磁加热电源(6)连接,裂解反应器(4)与电磁线圈(5)之间放置温度传感器(7),温度传感器(7)连有温控仪(8)。消除了喷雾介质与高温表面之间的接触热阻,实现了物料的快速升温裂解,缩短了反应时间,提高了反应效率,提高了目标产物收率。

Description

一种新型高温裂解反应装置 技术领域
本发明涉及化工生产的领域,具体涉及一种新型高温裂解反应装置。
背景技术
高温裂解是指利用热能将一种物质转变成另外几种物质的化学过程。高温裂解反应在石油化工生产过程中有着广泛应用。工业生产中常用高温裂解的方法将石油烃转变成小分子的烯烃、炔烃和芳香烃,如乙烯、丙烯、丁二烯、乙炔、苯、甲苯等,进而作为原料合成和生产其他化工产品。高温裂解反应在油脂化工中常用于生产具有高附加值的精细化学品,例如蓖麻油酸甲酯经高温裂解后可以得到十一碳烯酸甲酯,后者经进一步处理后可作生产尼龙-11的原料。另外,高温裂解反应在其它有机化工生产中也有着广泛应用,比如丙酮高温裂解可生成乙烯酮,是有机合成的重要中间体。
目前工业上液体的高温裂解反应常采用燃烧裂解的方式(中国专利CN 1751984A,CN 102951616A,CN 106744716A),将燃气和空气进行混合燃烧,利用燃烧释放的热量在裂解炉内形成所需的高温环境。这种高温裂解方式的裂解炉内温度往往只能控制在一定的区间范围内,常用于废液处理,对于需要精确控温或受温度影响较大的高温裂解反应则很难达到要求。中国专利CN 104341298A采用微波加热的方式进行蓖麻油酸甲酯的高温裂解反应,采用该方法原料的处理量很容易受微波发生装置磁控管功率的限制,在现有技术条件下很难做到较大产能;且需要吸波材料作为加热介质,增加了成本。
电磁加热以其优良的加热性能而被广泛应用(中国专利CN 103561491A,CN 105025604A,CN 107477844A,CN 107339796A)。电磁加热具有热启动快、热效率高、加热均匀性好等优点。另外,电磁加热线圈本身不发热,热阻滞小、热惯性低,从而可以实现温度的精确控制,而且电磁加热很容易实现装置的放大和产能的提高。喷雾技术可以将液体物料破碎形成均匀的微细雾状液滴,进而可实现高效传热,被广泛应用于冷却、燃烧、裂解等领域(中国专利CN 102951616A,CN 103740904A,CN 104061797A,CN 106744716A,CN 106987691A)。将喷雾技术用于传热的优点主要体现为喷雾介质与传热表面之间没有接触热阻,对喷雾介质而言实现了高效快速传热。将喷雾技术用于高温裂解反应时可实现物料的快速升温裂解。将电磁加热耦合喷雾技术用于高温裂解反应,国内外鲜有报道。
发明内容
本发明的目的在于克服现有技术存在的不足,而提供一种新型高温裂解反应装置。
本发明的目的是通过如下技术方案来完成的:这种新型高温裂解反应装置,主要包括进料泵、流量计、雾化器、裂解反应器、电磁线圈、电磁加热电源、温度传感器、温控仪、冷凝器、产品罐,进料泵连有流量计,流量计与雾化器的雾化器进口相连,雾化器置于裂解反应器中,裂解反应器下部有裂解反应器下口,裂解反应器的裂解反应器上口连有冷凝器,冷凝器与产品罐相连,裂解反应器的外壁绕有电磁线圈,电磁线圈与电磁加热电源连接,裂解 反应器与电磁线圈之间放置温度传感器,温度传感器连有温控仪。
所述裂解反应器设有裂解反应器上口,裂解反应器上口位置设在裂解反应器的上部,裂解反应器由不锈铁、碳钢、铁及其它耐高温且导磁性好的材质组成。
所述雾化器置于裂解反应器腔体中部,雾化器采用喷嘴式或离心式,喷嘴式雾化器的喷头为单个、单层多个和多层多个,喷嘴式雾化器的喷头采用固定式和以中间垂直进料管为轴旋转,雾化器由不锈钢、铜及其他耐高温且导磁性差的材质组成。
所述温度传感器为热电偶和热敏电阻,温度传感器测温点设在电磁线圈的中部。
所述进料泵所进物料为液体、浆态化的流体。
所述冷凝器设有冷凝器一口、冷凝器二口、冷凝器三口、冷凝器四口,产品罐有产品罐一口、产品罐二口、产品罐三口,冷凝器一口连接裂解反应器上口,冷凝器二口连接产品罐一口。
本发明采用新型高温裂解反应装置的工艺,具体步骤如下:
1、设置电磁线圈的裂解反应温度,接通电磁加热电源,开始升温。
2、将裂解原料通过进料泵输送,经流量计计量后通过雾化器雾化成微细液滴,液滴喷在裂解反应器的内壁发生裂解。
3、裂解原料在设定温度下快速裂解生成气态的裂解产物,裂解气通过出料管导入冷凝器中冷凝进入产品罐。
本发明的有益效果为:
1、本发明的电磁加热过程,采用内热加热方式,热启动快,热效率高,热惯性低,加热均匀性好,可提供均匀稳定的高温反应场所。电磁加热容易实现装置的放大和产能的提高。
2、本发明的喷雾技术,消除了喷雾介质与高温表面之间的接触热阻,实现了物料的快速升温裂解,缩短了反应时间,提高了反应效率,提高了目标产物收率。
附图说明
图1为本发明的流程及结构示意图(雾化器喷嘴式雾化器)。
图2为本发明的流程及结构示意图(雾化器为离心式雾化器)。
图3为本发明的多喷头喷嘴式雾化器的喷头分布示意图。
附图标记说明:进料泵1、流量计2、雾化器3、裂解反应器4、电磁线圈5、电磁加热电源6、温度传感器7、温控仪8、冷凝器9、产品罐10、雾化器进口31、裂解反应器上口41、裂解反应器下口42、冷凝器一口91、冷凝器二口92、冷凝器三口93、冷凝器四口94、产品罐一口101、产品罐二口102、产品罐三口103。
具体实施方式
下面将结合附图对本发明做详细的介绍:
如附图所示,这种新型高温裂解反应装置,主要包括进料泵1、流量计2、雾化器3、裂解反应器4、电磁线圈5、电磁加热电源6、温度传感器7、温控仪8、冷凝器9、产品罐10, 进料泵1连有流量计2,流量计2与雾化器3的雾化器进口31相连,雾化器3置于裂解反应器4中,裂解反应器4下部有裂解反应器下口42,裂解反应器4的裂解反应器上口41连有冷凝器9,冷凝器9与产品罐10相连,裂解反应器4的外壁绕有电磁线圈5,电磁线圈5与电磁加热电源6连接,裂解反应器4与电磁线圈5之间放置温度传感器7,温度传感器7连有温控仪8。
所述裂解反应器4设有裂解反应器上口41,裂解反应器上口41位置设在裂解反应器4的上部,裂解反应器4由不锈铁、碳钢、铁及其它耐高温且导磁性好的材质组成。
所述雾化器3置于裂解反应器4腔体中部,雾化器3采用喷嘴式或离心式,喷嘴式雾化器的喷头为单个、单层多个和多层多个,喷嘴式雾化器的喷头采用固定式或以中间垂直进料管为轴旋转,雾化器3由不锈钢、铜及其他耐高温且导磁性差的材质组成。
所述温度传感器7为热电偶和热敏电阻,温度传感器7测温点设在电磁线圈5的中部。
所述进料泵1所进物料为液体、浆态化的流体。
所述冷凝器9设有冷凝器一口91、冷凝器二口92、冷凝器三口93、冷凝器四口94,产品罐10有产品罐一口101、产品罐二口102、产品罐三口103,冷凝器一口91连接裂解反应器上口41,冷凝器二口92连接产品罐一口101。
本发明采用新型高温裂解反应装置的工艺,具体步骤如下:
1、设置电磁线圈5的裂解反应温度,接通电磁加热电源6,开始升温。
2、将裂解原料通过进料泵1输送,经流量计2计量后通过雾化器3雾化成微细液滴,液滴喷在裂解反应器4的内壁发生裂解。
3、裂解原料在设定温度下快速裂解生成气态的裂解产物,裂解气通过出料管导入冷凝器9中冷凝进入产品罐10。
实施例1:以高纯蓖麻油酸甲酯(纯度大于99%)为原料进行高温裂解制取十一碳烯酸甲酯,所用雾化器3为四喷头固定喷嘴式雾化器,雾化器3的喷头分布如图3所示。如图1所示,将电磁线圈5均匀缠绕在裂解反应器4腔体的外壁,将电磁线圈5的反应温度设定在500°C。将喷嘴式雾化器3放置在裂解反应器4腔体中部,将进料管与喷嘴式雾化器3的进口A连接,出料管与裂解反应器4出口B连接,并连接到冷凝器9上,冷凝器9上冷凝器三口93为冷冻水进口,冷凝器四口94为冷冻水出口。接通电磁加热电源6使电磁线圈5开始通电,裂解反应器4开始升温,待温度达到设定值并稳定一段时间后,原料(高纯蓖麻油酸甲酯)经进料泵1输送、流量计2计量,以20kg/h的流量经喷嘴式雾化器3的雾化器进口31进入并被喷嘴式雾化器3雾化成微细液滴,液滴喷在裂解反应器4的内壁发生裂解反应。原料在设定温度下快速裂解生成产物十一碳烯酸甲酯和庚醛气体,生成气通过出口B导入冷凝器9的裂解反应器上口41,冷凝得到的生成液从冷凝器9的冷凝器二口92排出,通过产品罐一口101进入产品罐10。产品罐10的产品罐二口102处可抽真空,为裂解系统提供负压操作条件。裂解反应器4中少量裂解残液通过裂解反应器下口42排出。裂解生成液经下游精馏装置分离 纯化得到十一碳烯酸甲酯,经皂化酸化可制得十一碳烯酸。实施例结果如下:电磁加热高温裂解生成液得率90%,十一碳烯酸收率73%,而中国专利CN101289383A所报道的传统电加热工艺收率34~38%,相比之下,本发明十一碳烯酸收率可提高1倍左右。
实施例2:以高纯蓖麻油酸甲酯(纯度大于99%)为原料进行高温裂解制取十一碳烯酸甲酯,所用雾化器3为离心式雾化器。如图2所示,将电磁线圈5均匀缠绕在裂解反应器4腔体的外壁,将电磁线圈5的反应温度设定在500℃。将离心式雾化器3放置在裂解反应器4腔体中部,将进料管与离心式雾化器3的进料管进口A连接,出料管与裂解反应器4出口B连接,并连接到冷凝器9上,冷凝器9上冷凝器三口93为冷冻水进口,冷凝器四口94为冷冻水出口。接通电磁加热电源6使电磁线圈5开始通电,裂解反应器4开始升温,待温度达到设定值并稳定一段时间后,原料(高纯蓖麻油酸甲酯)经进料泵1输送、流量计2计量,以50kg/h的流量经离心式雾化器3进料管的雾化器进口31进入高速旋转的喷雾盘中,料液被雾化成微细液滴,液滴喷在裂解反应器4的内壁发生裂解反应。原料在设定温度下快速裂解生成产物十一碳烯酸甲酯和庚醛气体,生成气通过裂解反应器上口41导入冷凝器9的冷凝器一口91,冷凝得到的生成液从冷凝器9的冷凝器二口92排出,通过产品罐一口101进入产品罐10。产品罐10的产品罐二口102处可抽真空,为裂解系统提供负压操作条件。裂解反应器4中少量裂解残液通过裂解反应器下口42排出。裂解生成液经下游精馏装置分离纯化得到十一碳烯酸甲酯,经皂化酸化可制得十一碳烯酸。实施例结果如下:电磁加热高温裂解生成液得率92%,十一碳烯酸收率70%,而中国专利CN101289383A所报道的传统电加热工艺收率34~38%,相比之下,本发明十一碳烯酸收率可提高1倍左右。
作为优选,所述产品罐二口102处放空或抽真空,为裂解系统提供负压操作条件。
可以理解的是,对本领域技术人员来说,对本发明的技术方案及发明构思加以等同替换或改变都应属于本发明所附的权利要求的保护范围。

Claims (6)

  1. 一种新型高温裂解反应装置,其特征在于:主要包括进料泵(1)、流量计(2)、雾化器(3)、裂解反应器(4)、电磁线圈(5)、电磁加热电源(6)、温度传感器(7)、温控仪(8)、冷凝器(9)、产品罐(10),进料泵(1)连有流量计(2),流量计(2)与雾化器(3)的雾化器进口(31)相连,雾化器(3)置于裂解反应器(4)中,裂解反应器(4)下部有裂解反应器下口(42),裂解反应器(4)的裂解反应器上口(41)连有冷凝器(9),冷凝器(9)与产品罐(10)相连,裂解反应器(4)的外壁绕有电磁线圈(5),电磁线圈(5)与电磁加热电源(6)连接,裂解反应器(4)与电磁线圈(5)之间放置温度传感器(7),温度传感器(7)连有温控仪(8)。
  2. 根据权利要求1所述的新型高温裂解反应装置,其特征在于:所述裂解反应器(4)设有裂解反应器上口(41),裂解反应器上口(41)位置设在裂解反应器(4)的上部,裂解反应器(4)由不锈铁、碳钢、铁及其它耐高温且导磁性好的材质组成。
  3. 根据权利要求1所述的新型高温裂解反应装置,其特征在于:所述雾化器(3)置于裂解反应器(4)腔体中部,雾化器(3)采用喷嘴式或离心式,喷嘴式雾化器的喷头为单个、单层多个和多层多个,喷嘴式雾化器的喷头采用固定式或以中间垂直进料管为轴旋转。
  4. 根据权利要求1所述的新型高温裂解反应装置,其特征在于:所述温度传感器(7)为热电偶和热敏电阻,温度传感器(7)测温点设在电磁线圈(5)的中部。
  5. 根据权利要求1所述的新型高温裂解反应装置,其特征在于:所述进料泵(1)所进物料为液体、浆态化的流体。
  6. 根据权利要求1所述的新型高温裂解反应装置,其特征在于:所述冷凝器(9)设有冷凝器一口(91)、冷凝器二口(92)、冷凝器三口(93)、冷凝器四口(94),产品罐(10)有产品罐一口(101)、产品罐二口(102)、产品罐三口(103),冷凝器一口(91)连接裂解反应器上口(41),冷凝器二口(92)连接产品罐一口(101)。
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