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CN111672421B - High temperature and high pressure reactor - Google Patents

High temperature and high pressure reactor Download PDF

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Publication number
CN111672421B
CN111672421B CN202010685417.1A CN202010685417A CN111672421B CN 111672421 B CN111672421 B CN 111672421B CN 202010685417 A CN202010685417 A CN 202010685417A CN 111672421 B CN111672421 B CN 111672421B
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China
Prior art keywords
reactor
pressure
temperature
tubular
circular ring
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CN202010685417.1A
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Chinese (zh)
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CN111672421A (en
Inventor
高明山
王钰
申畅
刘彦君
丁振杰
马旭武
赵世乾
袁源
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Ningxia Ink Technology Co ltd
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Ningxia Ink Technology Co ltd
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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
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/04Pressure vessels, e.g. autoclaves
    • B01J3/042Pressure vessels, e.g. autoclaves in the form of a tube
    • 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
    • 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
    • B01J19/2415Tubular reactors
    • B01J19/242Tubular reactors in series
    • 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
    • B01J2219/00074Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00094Jackets
    • 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
    • B01J2219/00132Controlling the temperature using electric heating or cooling elements
    • B01J2219/00135Electric resistance heaters

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)

Abstract

The high-temperature high-pressure reactor comprises a plurality of tubular reactors, wherein the tubular reactors comprise pipe bodies for transporting powder materials, the pipe body of each tubular reactor is connected with the pipe bodies of the adjacent tubular reactors, the outlet of the gathering structure of each tubular reactor is communicated with the pipe bodies of the adjacent tubular reactors, the high-temperature high-pressure reactor further comprises a material conveying pipe, the material conveying pipe extends upwards into the pipe bodies of the tubular reactors from the opening at the bottom of the pipe bodies of the tubular reactors at the bottom layer, and the bottom of the material conveying pipe is provided with a high-pressure gas interface and a material inlet for blowing materials into the pipe bodies through high-pressure gas. According to the high-temperature and high-pressure reactor, the powder materials are fully dispersed and gradually heated in the reactor in a mode of combining pulse gas blowing and multi-temperature-zone heating, so that the purposes of fully heating and purifying the powder materials are finally achieved, continuous production can be realized, and the production efficiency is improved.

Description

High-temperature high-pressure reactor
Technical Field
The invention relates to the technical field of micro-chemical industry, in particular to a high-temperature and high-pressure reactor.
Background
Purified powder materials are of substantial and wide demand in both raw material selection processes, production processes and final product forms of industrial processes. In the actual production process, powder purification is often realized by adopting a high-temperature calcination process.
The high-temperature high-pressure reactor is an important reaction device in the chemical process, and has important value in a plurality of reactions such as catalytic reaction, synthesis reaction, hydrogenation reaction and the like.
The reactor is a very important device in the powder purification process, and is mainly used in kettle reactors, tubular reactors and the like at present, and although a stirring system is additionally arranged in the reactors, the condition that powder materials are heated unevenly locally still easily occurs in the actual operation process, and in addition, the reactors are difficult to realize continuous production such as cooling, material taking, reheating, new reaction and the like, so that the production efficiency is influenced.
Disclosure of Invention
The invention aims to solve the technical problem of providing a high-temperature and high-pressure reactor for purifying powder materials, which can uniformly heat the materials.
The high-temperature high-pressure reactor comprises a plurality of tubular reactors which are vertically arranged and sequentially connected in series, wherein the tubular reactors comprise pipe bodies for transporting powder materials, the pipe body of each tubular reactor is connected with the pipe bodies of the adjacent tubular reactors, the top of the pipe body of each tubular reactor is provided with a gathering structure for collecting materials, the outlet of the gathering structure of each tubular reactor is communicated with the pipe bodies of the adjacent tubular reactors, the high-temperature high-pressure reactor further comprises a material conveying pipe, the material conveying pipe extends into the pipe bodies of the tubular reactors upwards from the opening at the bottom of the pipe bodies of the tubular reactors at the bottom layer, and the bottom of the material conveying pipe is provided with a high-pressure gas interface and a material inlet for blowing materials into the pipe bodies through high-pressure gas.
The high-temperature high-pressure reactor comprises a plurality of layers of refractory ceramics, wherein the outer part of a tube body of each tube reactor is wrapped with two layers of refractory ceramics, and an electric heating wire for heating is arranged between the two layers of refractory ceramics.
The invention relates to a high-temperature high-pressure reactor, wherein the gathering structure comprises a truncated cone-shaped truncated cone with a small upper part and a large lower part, the diameters of the upper bottom surface and the lower bottom surface of the truncated cone are smaller than the inner diameter of a tubular body of a tubular reactor, the truncated cone is connected with an upper circular ring and a lower circular ring, the outer diameters of the upper circular ring and the lower circular ring are equal to the inner diameter of the tubular body of the reactor, the lower circular ring is welded with the lower bottom surface of the truncated cone, the upper circular ring is welded with the side surface of the truncated cone, air holes for air circulation are distributed on the surface of the upper circular ring, a cavity is formed between the upper circular ring and the lower circular ring, and one side of the cavity is connected with a supplementary air interface for pulse air circulation and is used for supplementing air flow and blowing residual materials scattered around the gathering structure.
The high-temperature high-pressure reactor is characterized in that a shell is arranged outside a tube body of the tube reactor, a water jacket is arranged outside the shell, and heat-insulating cotton is used for filling between the shell and the tube body.
The high-temperature high-pressure reactor is characterized in that each tubular reactor is internally connected with a thermocouple and a pressure sensor.
The high-temperature high-pressure reactor is characterized in that a high-pressure gas transmission pipeline is connected to a material inlet and used for discharging materials in a pipe body of the pipe reactor after the reaction is finished.
The high-temperature high-pressure reactor provided by the invention is characterized in that the two ends of each tubular reactor are sealed by using high-temperature high-pressure sealing rings.
The high-temperature high-pressure reactor disclosed by the invention is provided with the plurality of tubular reactors, the plurality of tubular reactors form a plurality of temperature areas, continuous production can be realized, and materials in the reaction process are heated uniformly.
According to the high-temperature and high-pressure reactor, the powder materials are fully dispersed and gradually heated in the reactor in a mode of combining pulse gas blowing and multi-temperature-zone heating, so that the purposes of fully heating and purifying the powder materials are finally achieved, continuous production can be realized, and the production efficiency is improved.
Drawings
FIG. 1 is a front view showing a schematic structure of a high temperature and high pressure reactor according to the present invention;
FIG. 2 is a front view of a schematic structural view of a tubular reactor;
FIG. 3 is a front view of a schematic structural view of a material gathering structure;
fig. 4 is a schematic structural view of a ring plate on a gathering structure.
In the figure, the mark is 1, an electric heating wire; 2, refractory ceramics, 3, heat insulation cotton, 4, a cooling water jacket, 5, a water inlet, 6, a water outlet, 9, a heating wire binding post, 10, a high-pressure gas interface, 11, a material inlet, 12, a pulse gas interface, 13, a gathering structure, 15, a material output device, 16, a supplementary gas interface, 17, an air hole, 20, a tubular reactor, 21, a pipe body, 22, a material conveying pipe, 25, a round table, 26, an upper round ring, 27, a lower round ring and 30, and a shell.
Detailed Description
As shown in fig. 1, 2, 3 and 4, the high-temperature and high-pressure reactor of the invention comprises a plurality of tubular reactors 20, wherein the tubular reactors are vertically arranged and sequentially connected in series, each tubular reactor comprises a pipe body 21 for transporting powder materials, the pipe body of each tubular reactor is connected with the pipe body of the adjacent tubular reactor, the top of the pipe body of each tubular reactor is provided with a gathering structure 13 for collecting materials, the outlet of the gathering structure of each tubular reactor is communicated with the pipe body of the adjacent tubular reactor, the high-temperature and high-pressure reactor further comprises a material conveying pipe 22, the material conveying pipe extends into the inside of the pipe body of the tubular reactor from the opening at the bottom of the pipe body of the tubular reactor at the bottom, and the bottom of the material conveying pipe is provided with a high-pressure gas interface 10 and a material inlet 11 for blowing materials into the pipe body through high-pressure gas.
The high-temperature high-pressure reactor comprises two layers of refractory ceramics 2 wrapped outside a tube body of each tube reactor, and an electric heating wire 1 for heating is arranged between the two layers of refractory ceramics.
The high-temperature high-pressure reactor comprises a gathering structure 13, wherein the gathering structure comprises a truncated cone-shaped round platform 25 with a small upper part and a large lower part, the diameters of the upper bottom surface and the lower bottom surface of the round platform are smaller than the inner diameter of a tubular body of the tubular reactor, an upper circular ring 26 and a lower circular ring 27 are connected to the round platform, the outer diameters of the upper circular ring and the lower circular ring are equal to the inner diameter of the tubular body of the reactor, the lower circular ring is welded with the lower bottom surface of the round platform, the upper circular ring is welded with the side surface of the round platform, air holes 17 for air circulation are distributed on the surface of the upper circular ring, a cavity is formed between the upper circular ring and the lower circular ring, and a supplementary air interface 16 for pulse air circulation is connected to one side of the cavity and used for supplementing air flow and blowing residual materials scattered around the gathering structure.
The high-temperature high-pressure reactor is characterized in that a shell 30 is arranged outside a tube body of the tube reactor, a cooling water jacket 4 is arranged outside the shell, and heat insulation cotton 3 is used for filling between the shell and the tube body.
The high-temperature high-pressure reactor is characterized in that each tubular reactor is internally connected with a thermocouple and a pressure sensor.
The high-temperature high-pressure reactor is characterized in that a high-pressure gas transmission pipeline is connected to a material inlet and used for discharging materials in a pipe body of the pipe reactor after the reaction is finished.
The high-temperature high-pressure reactor provided by the invention is characterized in that the two ends of each tubular reactor are sealed by using high-temperature high-pressure sealing rings.
The high-temperature high-pressure reactor disclosed by the invention is provided with the plurality of tubular reactors, the plurality of tubular reactors form a plurality of temperature areas, continuous production can be realized, and materials in the reaction process are heated uniformly.
According to the high-temperature and high-pressure reactor, the powder materials are fully dispersed and gradually heated in the reactor in a mode of combining pulse gas blowing and multi-temperature-zone heating, so that the purposes of fully heating and purifying the powder materials are finally achieved, continuous production can be realized, and the production efficiency is improved.
The high-temperature high-pressure reactor is formed by connecting a plurality of tubular reactors in series, wherein each tubular reactor comprises a tube body for transporting powder materials, one end of the tube body is provided with a gathering structure 13 for gathering materials and gathering air flow, two layers of refractory ceramics 2 are wrapped outside the tube body of each tubular reactor, and an electric heating wire 1 for heating is fixed and wound between the two layers of refractory ceramics.
The gathering structure comprises a hollow truncated cone-shaped round platform 25, the round platform 25 is made of heat-resistant metal, the diameters of the upper bottom surface and the lower bottom surface are smaller than the inner diameter of the tubular reactor body, and two circular rings (an upper circular ring 26 and a lower circular ring 27) which are equal in size to the inner diameter of the tubular reactor body are welded together with the hollow round platform.
According to the high-temperature high-pressure reactor, each tubular reactor is internally connected with the thermocouple and the pressure sensor, each thermocouple and each pressure sensor are connected with the controller, and the temperature transition of a plurality of temperature areas inside the reactor can be realized through the controller.
The high-temperature high-pressure reactor also comprises a pulse gas interface 12 for entering pulse gas, and the pulse gas interface is used for the up-and-down movement of materials in the reactor in the reaction process so as to achieve the purpose of fully dispersing the materials.
The high-temperature high-pressure reactor is characterized in that a high-pressure gas transmission interface 10 is connected to a material inlet 11 and is used for discharging materials in a tube body after the reaction is finished.
According to the high-temperature high-pressure reactor, the two ends of each tubular reactor are sealed by using the high-temperature high-pressure sealing rings.
The working process of the high-temperature high-pressure reactor is as follows:
Before the operation, the external cooling water jacket 4 is firstly subjected to water feeding operation, cooling water continuously flows in from the water inlet 5 and flows out from the water outlet 6, then the reactor is preheated, the electric heating wires 1 connected with the electric heating wire binding posts 9 are heated and warmed, when different temperature ranges respectively reach preset temperatures T1, T2, T3 and T4, materials are pushed into the reactor through the material inlet 11 by external air flow, the materials are heated in different temperature ranges in the process of being conveyed in the cavity, gradually reach the optimal reaction temperature T4, and in addition, pulse gas is continuously pushed into the reactor through the pulse gas interface 12, so that the materials are continuously subjected to upward thrust of the gas in the reactor cavity, and the materials are subjected to up-down reciprocating motion in the reactor cavity under the action of gravity when the pulse gas is intermittent, so that the materials are heated uniformly in the heating process.
The gathering structure 13 is beneficial to gathering and transporting materials on one hand, and increases the airflow speed and the material transporting speed of the gap area covered by the heating wire on the other hand, and a small amount of materials inevitably fall on an upper circular plate of the gathering structure in the process of reciprocating up and down, at this time, through the supplementary gas interface 16, gas enters a cavity between the upper circular plate and the lower circular plate, and scattered materials are pushed up and down through the air holes of the upper circular plate.
After the reaction is finished, the materials in the pipeline are all pushed upwards by the high-pressure gas introduced through the high-pressure gas inlet 10, the materials in the pipeline are discharged in a high-pressure environment in a pressure release mode by the material output device 15 at the top end of the reactor, and after the materials in the pipeline are all transported and output, the high-pressure gas is closed, the material output device is closed, and then the reaction process of the next batch of materials is started.
Compared with the prior art, the high-temperature high-pressure reactor has the following technical points:
1. The high-temperature high-pressure reactor of the invention uses the pulse gas to continuously process the materials in the reactor in a reciprocating way up and down, so that the distribution of the materials in the reactor is more uniform.
2. According to the high-temperature high-pressure reactor, the multiple temperature areas are heated gradually, so that the material heating process in the reactor is sufficient, and the situation of uneven local heating is avoided.
3. The high-temperature high-pressure reactor has simple and effective structural design, can ensure the continuity of industrial production and increases the production efficiency.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.

Claims (6)

1. The high-temperature high-pressure reactor is characterized by comprising a plurality of tubular reactors which are vertically arranged and sequentially connected in series, wherein the tubular reactors comprise pipe bodies for transporting powder materials, the pipe body of each tubular reactor is connected with the pipe body of the adjacent tubular reactor, the top of the pipe body of each tubular reactor is provided with a gathering structure for collecting materials, the outlet of the gathering structure of each tubular reactor is communicated with the pipe body of the adjacent tubular reactor, the high-temperature high-pressure reactor also comprises a material conveying pipe, the material conveying pipe extends into the pipe body of the tubular reactor upwards from the opening at the bottom of the pipe body of the tubular reactor at the bottom layer, the bottom of the material conveying pipe is provided with a high-pressure gas interface and a material inlet, the device comprises a tube body, a gathering structure, a tubular reactor, a pulse gas inlet, a pulse gas outlet, a pulse gas inlet and a pulse gas outlet, wherein the tube body is internally blown with materials through high-pressure gas, the gathering structure comprises a truncated cone-shaped truncated cone, the diameter of the upper bottom surface and the diameter of the lower bottom surface of the truncated cone are smaller than the inner diameter of the tubular reactor tube body, the truncated cone is connected with an upper circular ring and a lower circular ring, the outer diameter of the upper circular ring and the outer diameter of the lower circular ring are equal to the inner diameter of the tubular reactor tube body, the lower circular ring is welded with the lower bottom surface of the truncated cone, the upper circular ring is welded with the side surface of the truncated cone, air holes for gas circulation are distributed on the surface of the upper circular ring, a cavity is formed between the upper circular ring and the lower circular ring, and one side of the cavity is connected with a supplementary gas interface for pulse gas circulation and is used for supplementing and blowing residual materials scattered around the gathering structure.
2. The high temperature and high pressure reactor according to claim 1, wherein the outside of the tube body of each tube reactor is wrapped with two layers of refractory ceramics, and an electric heating wire for heating is arranged between the two layers of refractory ceramics.
3. The high-temperature and high-pressure reactor according to claim 2, wherein a shell is arranged outside a tube body of the tube reactor, a water jacket is arranged outside the shell, and heat-insulating cotton is used for filling between the shell and the tube body.
4. A high temperature, high pressure reactor according to claim 3, wherein each tubular reactor is connected with a thermocouple and a pressure sensor.
5. The high-temperature and high-pressure reactor according to claim 4, wherein a high-pressure gas pipeline is connected to the material inlet for discharging the material in the tube body of the tube reactor after the reaction is finished.
6. The high-temperature and high-pressure reactor according to claim 5, wherein both ends of each tubular reactor are sealed by using high-temperature and high-pressure sealing rings.
CN202010685417.1A 2020-07-16 2020-07-16 High temperature and high pressure reactor Active CN111672421B (en)

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CN111672421B true CN111672421B (en) 2024-12-27

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Publication number Priority date Publication date Assignee Title
CN114984898B (en) * 2022-07-15 2022-10-25 常州市明珠干燥设备有限公司 Temperature-controllable reaction kettle for lithium battery material

Citations (3)

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CN202527151U (en) * 2012-01-18 2012-11-14 浙江大学 Oscillatory flow tubular reaction crystallizer
CN108501250A (en) * 2018-04-16 2018-09-07 四川大学 Air-flow spheroidization reactor and its method for preparing polymer matrix spherical powder material
CN212263189U (en) * 2020-07-16 2021-01-01 宁夏墨工科技有限公司 High temperature and high pressure reactor

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CN201959798U (en) * 2011-01-19 2011-09-07 颜建平 Tubular polymerization reactor
WO2017194494A1 (en) * 2016-05-10 2017-11-16 Basell Polyolefine Gmbh High-pressure polymerization process of ethylenically unsaturated monomers in a production line having flanges covered by a chimney construction
CN109970507B (en) * 2019-04-30 2022-09-27 山东道可化学有限公司 A kind of continuous production method and continuous production equipment of 3,4-dichlorotrifluorotoluene

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Publication number Priority date Publication date Assignee Title
CN202527151U (en) * 2012-01-18 2012-11-14 浙江大学 Oscillatory flow tubular reaction crystallizer
CN108501250A (en) * 2018-04-16 2018-09-07 四川大学 Air-flow spheroidization reactor and its method for preparing polymer matrix spherical powder material
CN212263189U (en) * 2020-07-16 2021-01-01 宁夏墨工科技有限公司 High temperature and high pressure reactor

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