CN114516667A - Reaction device for fixed bed cracking of oily wastewater for laboratory - Google Patents
Reaction device for fixed bed cracking of oily wastewater for laboratory Download PDFInfo
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- CN114516667A CN114516667A CN202011315203.1A CN202011315203A CN114516667A CN 114516667 A CN114516667 A CN 114516667A CN 202011315203 A CN202011315203 A CN 202011315203A CN 114516667 A CN114516667 A CN 114516667A
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention provides a reaction device for fixed bed cracking of oily wastewater in a laboratory, which comprises: the air inlet control assembly is provided with an air inlet pipe and an air inlet outlet pipe, and the air inlet pipe is communicated with an air source; the liquid inlet control component is provided with a liquid inlet pipe and a liquid inlet outlet pipe, and the liquid inlet pipe is communicated with the reaction liquid; the bottom end, the bottom side face and the top end of the reaction heating component are respectively provided with a reaction gas inlet pipe, a reaction liquid inlet pipe and a reaction outlet pipe, the reaction gas inlet pipe is communicated with the gas inlet pipe, and the reaction liquid inlet pipe is communicated with the liquid inlet pipe; the condensation liquid-separating component is provided with a condensation inlet pipe and a condensation outlet pipe, and the condensation inlet pipe is communicated with the reaction outlet pipe; the air outlet control assembly is provided with an air outlet inlet pipe and an air outlet pipe, and the air outlet inlet pipe is communicated with the condensation outlet pipe. The invention solves the problem that the fixed bed reaction device in the prior art can not meet the experimental requirements.
Description
Technical Field
The invention relates to the technical field of petrochemical industry, and particularly relates to a reaction device for fixed bed cracking of oily wastewater in a laboratory.
Background
The oily sewage is the main wastewater generated in the processes of oil and gas field development, petroleum refining and processing, has complex composition, high Chemical Oxygen Demand (COD) content and more refractory substances such as hydrocarbons and derivatives thereof, needs to be treated to realize the recovery or removal of organic hydrocarbons and meets the requirements of recycling or discharging. In addition to the oily wastewater treatment mode of the traditional 'oil removal-air flotation-biochemical' process, the cracking of the oily wastewater by using surplus heat energy is also a treatment mode with potential advantages. The cracking of organic hydrocarbon and the interception and fixation of inorganic matters are realized through the contact heat exchange of the oily wastewater and a high-temperature medium, the treatment of the oily wastewater and the utilization of surplus heat energy can be realized together, and the clean production of enterprises is assisted.
The cracking of oily wastewater in high temperature catalyst can complete heat exchange and thermochemical reaction in a reactor in the form of a fixed bed. Compared with fluidized bed and moving bed, the fixed bed reactor is characterized in that the solid material filled in the equipment is fixed and becomes a bed layer, and gas or liquid as a mobile phase flows in the bed layer. Aiming at the needs of fixed bed cracking reaction and process research of oily wastewater, the device for laboratory research needs to meet the requirements of oily wastewater or simulation liquid controllable liquid inlet, full solid-liquid contact with a high-temperature catalyst, controllable reaction bed temperature, controllable reaction atmosphere and system pressure, online separation and collection of reaction products and the like. For example, CN205635520 discloses a fixed bed reactor for removing mercaptans from liquefied petroleum gas, which is provided with a condenser to cool and liquefy the reactants, so that the liquefied petroleum gas is in a pure liquid state and is powered by a feed pump, and enters a bed layer through the upper part of the fixed bed to realize a solid-liquid two-phase reaction; CN106753476 discloses a fast cooling fixed bed experimental apparatus and method for pyrolysis and gasification, which employs a carrier gas conduit extending from the upper part to the bottom part by the edge of the reactor for gas supply, and the carrier gas entrains the reaction product to be led out from the upper part gas outlet conduit during the reaction process. In addition, CN205731183 discloses a continuous hydrogenation reaction unit is used in laboratory, sets up the cavity formula mixing system who takes cooling function in the reactor, promotes the flash mixed and the high-efficient reaction of material.
However, in the process of carrying out the oil-containing wastewater cracking experiment, the oil-containing wastewater is used as a refrigerant (room temperature to 90 ℃) and needs to be in direct and good contact with a high-temperature catalyst solid porous material (350 to 480 ℃), and if the oil-containing wastewater enters from the upper part of a fixed bed by spraying, the instantaneous vaporization pressure is too high, so that unsmooth spraying is easily caused, and the implementation of the process is hindered. In the existing fixed bed reaction device and system, the problems of liquid backflow, poor solid-liquid contact and the like in the solid-liquid contact reaction process exist, the conditions of reaction liquid inlet, pressure stabilization, atmosphere and the like cannot be effectively controlled, and cracking products cannot be effectively collected, so that the device cannot meet the experimental requirements.
Disclosure of Invention
The invention mainly aims to provide a reaction device for fixed bed cracking of oily wastewater in a laboratory, which aims to solve the problem that a fixed bed reaction device in the prior art cannot meet the experimental requirements.
In order to achieve the above object, the present invention provides a reaction apparatus for fixed bed cracking of oily wastewater in a laboratory, comprising: the air inlet control assembly is provided with an air inlet pipe and an air inlet outlet pipe, and the air inlet pipe is communicated with an air source through a metal hose; the liquid inlet control component is provided with a liquid inlet pipe and a liquid inlet outlet pipe, and the liquid inlet pipe is communicated with the reaction liquid through a metal hose; the bottom end, the bottom side face and the top end of the reaction heating component are respectively provided with a reaction air inlet pipe, a reaction liquid inlet pipe and a reaction outlet pipe, the reaction air inlet pipe is communicated with the air inlet pipe through a metal hose, and the reaction liquid inlet pipe is communicated with the liquid inlet pipe through a metal hose; the condensation liquid-separating component is provided with a condensation inlet pipe and a condensation outlet pipe, and the condensation inlet pipe is communicated with the reaction outlet pipe through a metal hose; the air outlet control assembly is provided with an air outlet inlet pipe and an air outlet pipe, and the air outlet inlet pipe is communicated with the condensation outlet pipe through a metal hose.
Furthermore, the air inlet control assembly comprises a first air inlet branch and a second air inlet branch, the first air inlet branch and the second air inlet branch are respectively provided with an air inlet pipe, and the first air inlet branch and the second air inlet branch share the same air inlet outlet pipe through an air inlet multi-way.
Further, the intake control assembly further includes: a plurality of intake control valves; a plurality of mass flowmeters and totalizers; the air inlet control valves, the mass flow meters, the integrating meters and the air inlet one-way valves are arranged on the first air inlet branch and the second air inlet branch, and the air inlet control valves, the mass flow meters, the integrating meters and the air inlet one-way valves are sequentially arranged from the air inlet pipe to the air inlet outlet pipe.
Furthermore, the air inlet control assembly further comprises a bypass pipeline, the bypass pipeline is connected with the first air inlet branch in parallel, and an air inlet control valve is arranged on the bypass pipeline.
Further, the intake control assembly further includes: an air intake control valve; the air inlet check valve, the air inlet control valve and the air inlet check valve are positioned on the air inlet outlet pipe, and the air inlet control valve is close to the air inlet multi-way; and the air inlet pressure gauge is communicated with the air inlet manifold.
Further, the feed control assembly comprises: the liquid inlet pump is communicated with the liquid inlet pipe and the liquid inlet outlet pipe; a liquid inlet control valve; the liquid inlet one-way valve, the liquid inlet control valve and the liquid inlet one-way valve are arranged between the liquid inlet pump and the liquid inlet outlet pipe, and the liquid inlet control valve is close to the liquid inlet pump.
Further, the reaction heating assembly includes: the height position of the heating furnace can be adjusted; a reactor for holding reaction solid material, the reactor sets up in the heating furnace, and the heating furnace can heat reactor to predetermined temperature, and bottom, bottom side and the top of reactor are provided with reaction intake pipe, reaction feed liquor pipe and reaction outlet pipe respectively.
Furthermore, one end of the reaction air inlet pipe extending into the reactor is provided with an inverted U-shaped structure, and one end of the reaction liquid inlet pipe extending into the reactor is positioned below the inverted U-shaped structure.
Further, the reactor comprises: a tube body in which reaction solid materials are contained; the two ends of the tube body are respectively provided with a sealing cap; the galvanic couple sleeves penetrate through the tube body, and at least two galvanic couple sleeves extend into different heights in the tube body.
Further, the condensation divides liquid subassembly to include: the cold trap cylinder is provided with an inner shell and an outer shell, an interlayer is formed between the inner shell and the outer shell, the circulating cold trap is communicated with the interlayer, and a refrigerant can be introduced into the interlayer; the cold trap cover body is arranged on the cold trap cylinder body in a covering mode, and the condensation inlet pipe and the condensation outlet pipe penetrate through the cold trap cover body and extend into the cold trap cylinder body.
Furthermore, the air outlet control assembly comprises a first air outlet branch and a second air outlet branch, the first air outlet branch and the second air outlet branch share the same air outlet inlet pipe through air outlet multiple ways, air outlet pipes are respectively arranged on the first air outlet branch and the second air outlet branch, and air outlet control valves are respectively arranged on the first air outlet branch and the second air outlet branch.
Furthermore, the air outlet control assembly also comprises a filter, an air outlet one-way valve, an air outlet control valve and a back pressure valve which are sequentially arranged from the air outlet inlet pipe to the air outlet pipe, and the air outlet control assembly also comprises an air outlet pressure gauge which is arranged between the air outlet one-way valve and the air outlet control valve.
By applying the technical scheme of the invention, the reaction heating component feeds liquid from the bottom end through mutual matching of the components, so that the overall height of a bed layer can be fully utilized, and in the process of vaporizing and ascending sewage, the porous medium realizes the pyrolysis of macromolecules and the interception of inorganic substances, further the cracking reaction is carried out, and the aim of effectively removing organic hydrocarbons in the oily wastewater is fulfilled; the air inlet control assembly and the liquid inlet control assembly are respectively used for controlling air inlet and liquid inlet, and the air outlet control assembly is used for controlling air outlet, so that conditions such as reaction liquid inlet, pressure stabilization and atmosphere can be controlled. The condensation liquid-separating component separates out condensable parts in the cracked waste gas, and the reaction products are quickly condensed, separated and collected. The above arrangement mode solves the problems of liquid backflow, poor solid-liquid contact and the like, satisfies the control of conditions such as reaction temperature, reaction process pressure, reaction atmosphere, liquid sampling rate and the like, realizes the rapid condensation separation and collection of reaction products, and satisfies the relevant experimental requirements of the oil-containing wastewater cracking reaction in a laboratory. In addition, each subassembly of this embodiment is connected through metal collapsible tube, and the equipment of being convenient for is dismantled, can increase and decrease system configuration according to the function needs, improves the practicality and the suitability of device greatly.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate embodiment(s) of the invention and together with the description serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic view showing the construction of a reaction apparatus for fixed bed cracking of oily wastewater for a laboratory according to the present invention;
FIG. 2 shows a practical layout of the reaction apparatus of FIG. 1;
FIG. 3 is a schematic diagram showing the structure of an intake control assembly of the reaction apparatus of FIG. 1;
FIG. 4 shows a schematic diagram of a faceplate for the intake control assembly of FIG. 3;
FIG. 5 shows a schematic diagram of the liquid inlet control module of the reaction device in FIG. 1;
FIG. 6 shows a schematic diagram of a panel of the liquid inlet control module of FIG. 5;
FIG. 7 shows a schematic view of the reaction heating assembly of the reaction apparatus of FIG. 1;
FIG. 8 shows a schematic structural view of a reactor of the reaction heating assembly of FIG. 7;
FIG. 9 shows a schematic of a faceplate of the reaction heating assembly of FIG. 7;
FIG. 10 shows a schematic diagram of the condensed liquid-separating component of the reaction apparatus in FIG. 1;
FIG. 11 is a schematic diagram showing the structure of the gas outlet control module of the reaction apparatus in FIG. 1;
fig. 12 is a schematic diagram of a panel of the air outlet control assembly of fig. 3.
Wherein the figures include the following reference numerals:
10. an air intake control assembly; 11. an air inlet pipe; 12. an inlet outlet pipe; 13. a first air intake branch; 14. a second air intake branch; 15. an air intake control valve; 16. a mass flow meter and an integrating meter; 17. an air inlet check valve; 18. a bypass line; 19. an intake pressure gauge; 20. a liquid inlet control component; 21. a liquid inlet pipe; 22. a liquid inlet and outlet pipe; 23. a liquid inlet pump; 24. a liquid inlet control valve; 25. a liquid inlet check valve; 30. a reaction heating assembly; 31. a reaction air inlet pipe; 32. a reaction liquid inlet pipe; 33. a reaction outlet pipe; 34. a heating furnace; 35. a reactor; 351. a pipe body; 352. a sealing cap; 353. a galvanic couple casing; 40. a condensation liquid-separating component; 41. a condensation inlet pipe; 42. a condensation outlet pipe; 43. a cold trap cylinder; 44. a cold trap cover body; 50. an air outlet control component; 51. an air outlet inlet pipe; 52. an air outlet pipe; 53. a first air outlet branch; 54. a second air outlet branch; 55. an air outlet control valve; 56. a filter; 57. an air outlet one-way valve; 58. a back pressure valve; 59. an air outlet pressure gauge; 60. a gas source; 70. reaction solution; 80. an air switch; 90. power switch and indication; 100. temperature indicating or controlling instruments.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
It is noted that, unless otherwise indicated, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
In the present invention, unless specified to the contrary, use of the terms of orientation such as "upper, lower, top, bottom" or the like, generally refer to the orientation as shown in the drawings, or to the component itself in a vertical, perpendicular, or gravitational orientation; likewise, for ease of understanding and description, "inner and outer" refer to the inner and outer relative to the profile of the components themselves, but the above directional words are not intended to limit the invention.
The invention provides a reaction device for fixed bed cracking of oily wastewater in a laboratory, aiming at solving the problem that a fixed bed reaction device in the prior art cannot meet the experimental requirements.
The reaction device for the fixed bed cracking of the oily wastewater in the laboratory, as shown in fig. 1 to fig. 12, comprises an air inlet control component 10, an air inlet control component 20, a reaction heating component 30, a condensation liquid separation component 40 and an air outlet control component 50, wherein the air inlet control component 10 is provided with an air inlet pipe 11 and an air inlet outlet pipe 12, and the air inlet pipe 11 is communicated with an air source 60 through a metal hose; the liquid inlet control module 20 is provided with a liquid inlet pipe 21 and a liquid outlet pipe 22, and the liquid inlet pipe 21 is communicated with the reaction liquid 70 through a metal hose; the bottom, the bottom side and the top of the reaction heating component 30 are respectively provided with a reaction air inlet pipe 31, a reaction liquid inlet pipe 32 and a reaction outlet pipe 33, the reaction air inlet pipe 31 is communicated with the air inlet outlet pipe 12 through a metal hose, and the reaction liquid inlet pipe 32 is communicated with the liquid inlet outlet pipe 22 through a metal hose; the condensation liquid separation component 40 is provided with a condensation inlet pipe 41 and a condensation outlet pipe 42, and the condensation inlet pipe 41 is communicated with the reaction outlet pipe 33 through a metal hose; the air outlet control member 50 has an air outlet inlet pipe 51 and an air outlet pipe 52, and the air outlet inlet pipe 51 and the condensation outlet pipe 42 are communicated through a metal hose.
In the embodiment, through the mutual matching of the components, the reaction heating component 30 enters liquid from the bottom end, so that the overall height of a bed layer can be fully utilized, and in the process of vaporizing and ascending sewage, the porous medium realizes the cracking of macromolecules and the interception of inorganic substances, further the cracking reaction is carried out, and the purpose of effectively removing organic hydrocarbons in the oily wastewater is realized; the air inlet control component 10 and the liquid inlet control component 20 are respectively used for controlling air inlet and liquid inlet, and the air outlet control component 50 is used for controlling air outlet, so that conditions such as reaction liquid inlet, pressure stabilization, atmosphere and the like can be controlled. The condensation liquid-separating component 40 separates condensable parts in the cracked waste gas, so as to realize rapid condensation separation and collection of reaction products. The above arrangement mode solves the problems of liquid backflow, poor solid-liquid contact and the like, satisfies the control of conditions such as reaction temperature, reaction process pressure, reaction atmosphere, liquid sampling rate and the like, realizes the rapid condensation separation and collection of reaction products, and satisfies the relevant experimental requirements of the oil-containing wastewater cracking reaction in a laboratory. In addition, each subassembly of this embodiment is connected through metal collapsible tube, and the equipment of being convenient for is dismantled, can increase and decrease system configuration according to the function needs, improves the practicality and the suitability of device greatly.
As shown in fig. 3, the air inlet control assembly 10 includes a first air inlet branch 13 and a second air inlet branch 14, the first air inlet branch 13 and the second air inlet branch 14 are respectively provided with an air inlet pipe 11, and the two can independently inlet air, according to the experimental requirement, the air source 60 includes two types of reaction air sources and carrier air sources, and therefore two branches of the first air inlet branch 13 and the second air inlet branch 14 are provided, the first air inlet branch 13 of the embodiment is communicated with the carrier air source, and the second air inlet branch 14 is communicated with the reaction air source, so as to realize independent air inlet of the two types of air sources 60. And, the first and second branch air intake ducts 13 and 14 share the same air intake outlet duct 12 through the intake manifold.
The intake control assembly 10 of the present embodiment further includes a plurality of intake control valves 15, a plurality of mass flow meters and integrators 16, and a plurality of intake check valves 17, the intake control valves 15, the mass flow meters and the integrators 16, and the intake check valves 17 are provided on the first intake branch 13 and the second intake branch 14, respectively, and the intake control valves 15, the mass flow meters and the integrators 16, and the intake check valves 17 are provided in this order from the intake inlet pipe 11 toward the intake outlet pipe 12. Therefore, the on-off, air inflow, airflow direction and the like of the first air inlet branch 13 and the second air inlet branch 14 can be effectively controlled respectively, so that the pressure and flow parameters of the reaction gas and the carrier gas meet the experimental requirements.
Preferably, the intake control assembly 10 further comprises a bypass line 18, since the first intake branch 13 of the present embodiment is communicated with the carrier gas source, the bypass line 18 is connected in parallel with the first intake branch 13, the bypass line 18 is also provided with an intake control valve 15, and the highest pressure in the reactor 35 can be controlled in advance through the bypass line 18 by controlling the intake control valve 15 on the bypass line 18. In this way, through the arrangement of the first air inlet branch 13, the second air inlet branch 14 and the bypass pipeline 18, the air inlet control assembly 10 integrally forms three branches of the first air inlet branch 13, the second air inlet branch 14 and the bypass pipeline 18 and one main branch of the air inlet outlet pipe 12 communicated with the three branches.
In the present embodiment, the intake control assembly 10 further includes an intake control valve 15, an intake check valve 17, and an intake pressure gauge 19, the intake control valve 15 and the intake check valve 17 are both located on a line trunk where the intake outlet pipe 12 is located, and the intake control valve 15 is close to the intake multi-port; the intake pressure gauge 19 communicates with the intake manifold. The air inlet control assembly 10 of the embodiment adopts four-way integrated air inlet channels, the air inlet control valve 15 on the air inlet outlet pipe 12 controls the air supply of the whole air inlet control assembly 10 to the subsequent system to be switched on and off, and the air inlet check valve 17 prevents the subsequent air from flowing back to the air inlet control assembly 10. The whole air inlet control assembly 10 realizes the functions of monitoring and controlling the air inlet pressure and the flow of at least two gases and preventing backflow.
As shown in fig. 5, the liquid inlet control assembly 20 includes a liquid inlet pump 23, a liquid inlet control valve 24 and a liquid inlet check valve 25, wherein the liquid inlet pump 23 is communicated with a liquid inlet pipe 21 and a liquid inlet outlet pipe 22; the liquid inlet control valve 24 and the liquid inlet check valve 25 are provided between the liquid inlet pump 23 and the liquid inlet outlet pipe 22, and the liquid inlet control valve 24 is close to the liquid inlet pump 23, thereby controlling the liquid inlet of the reaction liquid 70.
As shown in fig. 7, the reaction heating unit 30 includes a heating furnace 34 and a reactor 35 for containing the reaction solid materials, and the height position of the heating furnace 34 is adjustably set so that the reaction heating unit 30 can be installed at a suitable height position as required; the reactor 35 is disposed in the heating furnace 34, the heating furnace 34 is provided with a temperature control system, and the heating furnace 34 can heat the reactor 35 to a predetermined temperature, so as to better perform the cracking reaction. The bottom end, the bottom side and the top end of the reactor 35 are respectively provided with a reaction gas inlet pipe 31, a reaction liquid inlet pipe 32 and a reaction outlet pipe 33. The heating furnace 34 of this embodiment has openable and closable furnace doors at the top and bottom, and a channel at the side, the reaction inlet pipe 31 and the reaction outlet pipe 33 respectively penetrate through the top and bottom of the heating furnace 34, and the reaction inlet pipe 32 penetrates through the channel at the side.
One end that this embodiment stretched into in reactor 35 at reaction intake pipe 31 is provided with the structure of falling the U-shaped, and the one end that reaction feed liquor pipe 32 stretched into in reactor 35 is located the below of the structure of falling the U-shaped to can prevent that liquid from flowing backward to the gas circuit in, guarantee the whole normal work of device.
As shown in fig. 8, the reactor 35 comprises a tubular body 351, a sealing cap 352 and a plurality of galvanic sleeves 353, the reaction solid material being contained inside the tubular body 351; sealing caps 352 are respectively provided at both ends of the tube body 351 to seal the tube body 351; this embodiment is provided with three galvanic couple sleeve 353, and one of them galvanic couple sleeve 353 is worn to establish by the sealing cap 352 of body 351 top and is stretched into to the body 351 in, and two galvanic couple sleeve 353 are worn to establish by the sealing cap 352 of body 351 bottom and are stretched into to the body 351 in addition, and two galvanic couple sleeve 353 that set up at the bottom stretch into the different height departments in the body 351 to can monitor the intraformational temperature of bed more comprehensively.
As shown in fig. 10, the condensation liquid-separating assembly 40 includes a cold trap cylinder 43 and a cold trap cover 44, the cold trap cylinder 43 has an inner shell and an outer shell, an interlayer is formed between the inner shell and the outer shell, a refrigerant outlet is formed at the top of the interlayer, a refrigerant inlet is formed at the bottom of the interlayer, the circulating cold trap is communicated with the interlayer through the refrigerant inlet and the refrigerant outlet, and a refrigerant can be introduced into the interlayer, so as to condense the volatile gas product entering the cold trap cylinder 43; the cold trap cover body 44 covers the cold trap cylinder body 43, the condensation inlet pipe 41 and the condensation outlet pipe 42 penetrate through the cold trap cover body 44 and extend into the cold trap cylinder body 43, condensed water obtained by condensation is stored in the cold trap cylinder body 43, and non-condensed gas can be discharged into subsequent collecting devices such as an air collecting bag through the condensation outlet pipe 42.
As shown in fig. 11, the air outlet control component 50 is similar to the air inlet control component 10 and includes a first air outlet branch 53 and a second air outlet branch 54, the first air outlet branch 53 and the second air outlet branch 54 share the same air outlet inlet pipe 51 through multiple air outlets, and the first air outlet branch 53 and the second air outlet branch 54 are respectively provided with an air outlet pipe 52, so that an air receiving bag is arranged behind the first air outlet branch 53 for collecting air, and a carafe is arranged behind the second air outlet branch 54 for performing the tightness detection. And air outlet control valves 55 are provided on both the first air outlet branch 53 and the second air outlet branch 54 to control the on/off of each branch.
In the present embodiment, outlet control module 50 further includes a filter 56, an outlet check valve 57, an outlet control valve 55, and a back pressure valve 58, all of which are disposed on the trunk, and are sequentially disposed from outlet inlet pipe 51 toward outlet pipe 52. The air outlet control assembly 50 further comprises an air outlet pressure gauge 59, a three-way valve is arranged between the air outlet check valve 57 and the air outlet control valve 55, and the air outlet pressure gauge 59 is connected with the three-way valve so as to monitor the air outlet pressure.
The above components of the present embodiment form respective control panels on the outer side of the device, and the components of the components that need to be operated or observed are exposed out of the instrument panel for convenient operation and monitoring. In addition to the respective components, components such as the air switch 80, the power switch, and the indicator 90 may be added as necessary. Specifically, as shown in fig. 4, each intake control valve 15, the mass flow meter 16, and the intake pressure gauge 19 of the intake control module 10 of the present embodiment are provided on an instrument panel, and an air switch 80, a power switch, and an instruction 90 are provided to protect the circuit and control the on/off of the circuit; as shown in fig. 6, the liquid inlet control valve 24 of the liquid inlet control module 20 is disposed on the instrument panel, and an air switch 80, a power switch and an indicator 90 are also disposed; as shown in fig. 9, the reaction heating assembly 30 includes, in addition to the air switch 80, the power switch and the indicator 90, a temperature indicator or control instrument 100 for monitoring and controlling parameters such as the heating temperature of the reactor 35, wherein the three components of the reaction heating assembly 30 are disposed on instrument panels; as shown in fig. 12, the outlet control valve 55, the outlet pressure gauge 59, and the back pressure valve 58 of the outlet control module 50 are provided on the instrument panel. Of course, in addition to the above arrangement, the number of components may be increased or decreased as necessary.
Optionally, all the control valves of the present embodiment are ball valves, and the carrier gas is nitrogen.
The operation of the reactor of this example is as follows:
assembling device before experiment:
all control valves remain closed, the back pressure valve 58 remains closed, and the power supply remains closed. A source of nitrogen gas is connected to the inlet gas inlet pipe 11. The liquid inlet pump 23 is connected with the reaction liquid 70 and is filled with the pump.
Screwing the tube 351 of the reactor 35 and the sealing cap 352 at the bottom, placing the reaction solid material at a proper height in the reactor 35 to form a solid reaction bed layer, and screwing the tube 351 and the sealing cap 352 at the top to complete the filling of the solid material.
The reaction feed pipe 32 is inserted into a passage in the side of the heating furnace 34, and the reactor 35 filled with the materials is placed in the heating furnace 34. The pipe 351 is connected with one end of the reaction liquid inlet pipe 32, the other end of the reaction liquid inlet pipe 32 is connected with the liquid inlet outlet pipe 22 of the liquid inlet control component 20, and the reaction air inlet pipe 31 at the bottom of the reactor 35 is connected with the air inlet outlet pipe 12 of the air inlet control component 10.
The cold trap cover 44 and the cold trap cylinder 43 are locked by bolts in a sealing way, and the cold trap cylinder 43 is filled with a refrigerant with the temperature of 15 ℃ below zero for cooling and circulation and is limited on the platform. The reaction outlet pipe 33 of the reaction heating component 30 is connected with the condensation inlet pipe 41 of the condensation liquid-separating component 40 by a stainless steel metal hose, and a heat-insulating sleeve is arranged. The condensation outlet pipe 42 is connected with an outlet inlet pipe 51 of the outlet control component 50 by a stainless steel metal hose, an outlet pipe 52 of a first outlet branch 53 of the outlet control component 50 is externally connected with a gas collecting bag, and an outlet pipe 52 of a second outlet branch 54 is externally connected with a metal hose and extends to a glass water bottle liquid seal. The door of the temperature-controlled oven 34 is closed.
After the assembly is completed, the experiment is carried out:
and opening a nitrogen gas source to adjust the pressure to be 0.7MPa, opening the air inlet control valve 15 on the air inlet bypass pipeline 18, observing that the pressure of the air inlet pressure gauge 19 reaches 0.7MPa, opening the air inlet control valve 15 on the trunk of the air inlet control assembly 10 and the air outlet control valve 55 on the trunk of the air outlet control assembly 50, and observing whether the air outlet pressure gauge 59 has a reading or not until the pressure is stable and unchanged. And then closing the air inlet control valve 15 on the bypass pipeline 18, and observing the pressure readings of the air inlet pressure gauge 19 and the air outlet pressure gauge 59 to keep unchanged for 5min, thereby proving that the system is tightly connected and has no air leakage.
And (3) turning on a power supply of the mass flow meter and the integrating meter 16, opening the air inlet control valve 15 on the first air inlet branch 13 and the air outlet control valve 55 on the second air outlet branch 54, slowly opening the backpressure valve 58, observing the bubbling condition of an external metal hose on the second air outlet branch 54 in the glass bottle, releasing the pressure of the device until the reading of the air inlet pressure gauge 19 is 0.5MPa, then adjusting the backpressure valve 58 until the bubbles are blown out at a constant speed, and establishing the pressure balance of the whole system.
Keeping the previous state for 10-15 min, and discharging other gases in the system by using nitrogen. Then, the power supply of the heating furnace 34 was turned on, and the heating temperature was set to 450 ℃. After the temperature reaches 450 ℃ and is constant, the heating furnace 34 is closed, the air outlet control valve 55 on the second air outlet branch 54 is closed, the air outlet control valve 55 and the liquid inlet control valve 24 on the first air outlet branch 53 are opened, the liquid inlet pump 23 is opened, liquid is infused into the reaction liquid inlet pipe 32 from the liquid inlet outlet pipe 22 according to the set flow rate, the liquid reacts with hot materials after entering the reactor 35, heat exchange is carried out between the liquid and the materials by utilizing the temperature of the materials, the reaction is carried out, the bed temperature change is monitored by utilizing the thermocouple of the thermocouple sleeve 353, and the bed temperature change is fed back to a user by the temperature indicating or controlling instrument 100. If two gases are required to be introduced simultaneously for reaction, the air inlet control valve 15 on the second air inlet branch 14 can be opened or closed according to actual requirements.
The generated volatile products enter the cold trap cylinder 43 through the reaction outlet pipe 33 and the condensation inlet pipe 41, the volatile is cooled, the condensed liquid is stored in the cold trap cylinder 43, and the non-condensable gas enters the gas outlet control component 50 through the condensation outlet pipe 42. In the air outlet control component 50, the non-condensable gas passes through a filter 56, an air outlet one-way valve 57, a back pressure valve 58 and an air outlet control valve 55 on the first air outlet branch 53 in sequence, and enters the air bag from the first air outlet branch 53 to be collected.
After the temperature of the material in the reaction bed of the reactor 35 is reduced to 250 ℃, the liquid inlet pump 23 stops feeding liquid, and the liquid inlet control valve 24 is closed. And (3) when the temperature of the materials in the reaction bed layer is reduced to be below 100 ℃, closing the air inlet control valve 15 on the trunk line of the air inlet control component 10, the air inlet control valve 15 on the first air inlet branch 13 and the air outlet control valve 55 on the first air outlet branch 53, stopping gas collection, closing the power supply of the mass flow meter and the integrating instrument 16, opening the air outlet control valve 55 on the second air outlet branch 54, and slowly opening the backpressure valve 58 to be maximum so as to reduce the pressure in the system to be zero. And opening the heating furnace 34, naturally cooling to room temperature, sequentially disassembling the reaction heating assembly 30, the air inlet control assembly 10, the liquid inlet control assembly 20 and the metal hoses for connecting the condensation liquid separation assembly 40, taking out the reactor 35, opening the sealing cap 352 at the top, and taking out the solid material. And (3) disassembling the metal connecting hose of the condensation liquid-separating assembly 40 and the air outlet control assembly 50, disassembling the bolt between the cold trap cover body 44 and the cold trap cylinder body 43, opening the cold trap, and taking out the liquid product.
It should be noted that, a plurality in the above embodiments means at least two.
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects:
1. the problem that a fixed bed reaction device in the prior art cannot meet experimental requirements is solved;
2. the problems of liquid backflow, poor solid-liquid contact and the like are solved;
3. the control of the gas circuit and the liquid circuit is optimized, the control of conditions such as reaction temperature, reaction process pressure, reaction atmosphere, liquid sampling rate and the like is met, and the controllability of the whole experiment system is improved;
4. the reaction product is quickly condensed, separated and collected;
5. the components are connected through metal hoses, so that the assembly and disassembly are convenient, the system configuration can be increased or decreased according to the function requirement, and the practicability and the applicability of the device are greatly improved;
6. the inverted U-shaped structure of the reaction liquid inlet pipe can ensure that gas is fully contacted with materials and liquid can be prevented from entering the gas circuit.
It is to be understood that the above-described embodiments are only a few, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular is intended to include the plural unless the context clearly dictates otherwise, and it should be further understood that the terms "comprises" and/or "comprising," when used in this specification, specify the presence of features, steps, operations, devices, components, and/or combinations thereof.
It should be noted that the terms "first," "second," and the like in the description and claims of this application and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the application described herein are capable of operation in sequences other than those illustrated or described herein.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (12)
1. The utility model provides a reaction unit with oily waste water fixed bed cracking is used in laboratory which characterized in that includes:
the air inlet control assembly (10), the air inlet control assembly (10) is provided with an air inlet pipe (11) and an air inlet outlet pipe (12), and the air inlet pipe (11) is communicated with an air source (60) through a metal hose;
the liquid inlet control assembly (20), the liquid inlet control assembly (20) is provided with a liquid inlet pipe (21) and a liquid outlet pipe (22), and the liquid inlet pipe (21) is communicated with the reaction liquid (70) through a metal hose;
the reaction heating assembly (30) is provided with a reaction air inlet pipe (31), a reaction liquid inlet pipe (32) and a reaction outlet pipe (33) at the bottom end, the bottom side face and the top end of the reaction heating assembly (30) respectively, the reaction air inlet pipe (31) is communicated with the air inlet pipe (12) through a metal hose, and the reaction liquid inlet pipe (32) is communicated with the liquid inlet pipe (22) through a metal hose;
the condensation liquid separation component (40), the condensation liquid separation component (40) is provided with a condensation inlet pipe (41) and a condensation outlet pipe (42), and the condensation inlet pipe (41) is communicated with the reaction outlet pipe (33) through a metal hose;
an air outlet control component (50), wherein the air outlet control component (50) is provided with an air outlet inlet pipe (51) and an air outlet pipe (52), and the air outlet inlet pipe (51) is communicated with the condensation outlet pipe (42) through a metal hose.
2. The reactor according to claim 1, characterized in that the inlet control assembly (10) comprises a first inlet branch (13) and a second inlet branch (14), the first inlet branch (13) and the second inlet branch (14) are respectively provided with the inlet pipe (11), and the first inlet branch (13) and the second inlet branch (14) share the same inlet outlet pipe (12) through an inlet manifold.
3. A reactor device as claimed in claim 2, wherein the inlet control assembly (10) further comprises:
a plurality of intake control valves (15);
a plurality of mass flow meters and integrators (16);
the air inlet control valve (15), the mass flow meter and the integrating meter (16) and the air inlet check valve (17) are arranged on each of the first air inlet branch (13) and the second air inlet branch (14), and the air inlet control valve (15), the mass flow meter and the integrating meter (16) and the air inlet check valve (17) are arranged in sequence from the air inlet pipe (11) to the air inlet outlet pipe (12).
4. The reactor apparatus according to claim 2, wherein the intake control assembly (10) further comprises a bypass line (18), the bypass line (18) being disposed in parallel with the first intake branch (13), the bypass line (18) being provided with an intake control valve (15).
5. A reactor device as claimed in claim 2, wherein the inlet control assembly (10) further comprises:
an intake control valve (15);
the air inlet check valve (17), the air inlet control valve (15) and the air inlet check valve (17) are both positioned on the air inlet outlet pipe (12), and the air inlet control valve (15) is close to the air inlet multi-way;
and the air inlet pressure gauge (19) is communicated with the air inlet multi-way, and the air inlet pressure gauge (19) is communicated with the air inlet multi-way.
6. A reactor device as claimed in claim 1, wherein said inlet control means (20) comprises:
the liquid inlet pump (23), the liquid inlet pump (23) is communicated with the liquid inlet pipe (21) and the liquid inlet outlet pipe (22);
a liquid inlet control valve (24);
liquid inlet check valve (25), advance liquid control valve (24) with liquid inlet check valve (25) set up liquid inlet pump (23) with between liquid inlet outlet pipe (22), just it is close to advance liquid control valve (24) liquid inlet pump (23).
7. The reaction device according to claim 1, wherein the reaction heating assembly (30) comprises:
the height position of the heating furnace (34) can be adjusted and set;
a reactor (35) for holding reaction solid material, reactor (35) set up in heating furnace (34), heating furnace (34) can heat reactor (35) is to predetermined temperature, the bottom of reactor (35), bottom side and top are provided with respectively reaction intake pipe (31), reaction feed liquor pipe (32) and reaction outlet pipe (33).
8. The reactor according to claim 7, characterized in that the end of the reaction gas inlet pipe (31) extending into the reactor (35) is provided with an inverted U-shaped structure, and the end of the reaction liquid inlet pipe (32) extending into the reactor (35) is positioned below the inverted U-shaped structure.
9. The reactor device according to claim 7, characterized in that the reactor (35) comprises:
a tube (351) in which the reaction solid material is contained;
the sealing caps (352) are respectively arranged at two ends of the tube body (351);
the electric coupling sleeve comprises a plurality of electric coupling sleeves (353), wherein the electric coupling sleeves (353) penetrate through the pipe body (351), and at least two electric coupling sleeves (353) extend into different heights of the pipe body (351).
10. The reaction device according to claim 1, wherein the condensation and separation assembly (40) comprises:
the cold trap cylinder (43) is provided with an inner shell and an outer shell, an interlayer is formed between the inner shell and the outer shell, the circulating cold trap is communicated with the interlayer, and a refrigerant can be introduced into the interlayer;
the cold trap cover body (44) is covered on the cold trap cylinder body (43), and the condensation inlet pipe (41) and the condensation outlet pipe (42) penetrate through the cold trap cover body (44) and extend into the cold trap cylinder body (43).
11. The reaction device according to claim 1, wherein the gas outlet control component (50) comprises a first gas outlet branch (53) and a second gas outlet branch (54), the first gas outlet branch (53) and the second gas outlet branch (54) share the same gas outlet inlet pipe (51) through a gas outlet manifold, the gas outlet pipes (52) are respectively arranged on the first gas outlet branch (53) and the second gas outlet branch (54), and gas outlet control valves (55) are respectively arranged on the first gas outlet branch (53) and the second gas outlet branch (54).
12. The reaction apparatus according to claim 11, wherein the gas outlet control unit (50) further comprises a filter (56), a gas outlet check valve (57), a gas outlet control valve (55), and a back pressure valve (58) which are sequentially disposed from the gas outlet inlet pipe (51) toward the gas outlet pipe (52), and the gas outlet control unit (50) further comprises a gas outlet pressure gauge (59), and the gas outlet pressure gauge (59) is disposed between the gas outlet check valve (57) and the gas outlet control valve (55).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202011315203.1A CN114516667A (en) | 2020-11-20 | 2020-11-20 | Reaction device for fixed bed cracking of oily wastewater for laboratory |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011315203.1A CN114516667A (en) | 2020-11-20 | 2020-11-20 | Reaction device for fixed bed cracking of oily wastewater for laboratory |
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| CN114516667A true CN114516667A (en) | 2022-05-20 |
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| CN202011315203.1A Pending CN114516667A (en) | 2020-11-20 | 2020-11-20 | Reaction device for fixed bed cracking of oily wastewater for laboratory |
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| GB812648A (en) * | 1956-12-03 | 1959-04-29 | Universal Oil Prod Co | Improvements in or relating to the purification of waste waters from petroleum hydrocarbon processing |
| CN1958731A (en) * | 2005-10-31 | 2007-05-09 | 中国石油化工股份有限公司 | Method for producing olefin through catalytic cracking |
| CN101825548A (en) * | 2010-04-28 | 2010-09-08 | 辽宁科技大学 | Detection method and device of coke reactivity and post-reaction heat-treatability |
| CN103566837A (en) * | 2013-11-13 | 2014-02-12 | 山西大学 | External circular reaction device suitable for hydrogenation exothermic reaction |
| CN109279575A (en) * | 2017-07-21 | 2019-01-29 | 盐城科莱特电热机械有限公司 | Methanol low-temperature decomposing device |
| CN210229907U (en) * | 2019-07-18 | 2020-04-03 | 北京拓川科研设备股份有限公司 | Fixed bed reaction device |
| CN211179829U (en) * | 2019-11-23 | 2020-08-04 | 青岛汇鑫混凝土有限公司 | Cement boiling box |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB812648A (en) * | 1956-12-03 | 1959-04-29 | Universal Oil Prod Co | Improvements in or relating to the purification of waste waters from petroleum hydrocarbon processing |
| CN1958731A (en) * | 2005-10-31 | 2007-05-09 | 中国石油化工股份有限公司 | Method for producing olefin through catalytic cracking |
| CN101825548A (en) * | 2010-04-28 | 2010-09-08 | 辽宁科技大学 | Detection method and device of coke reactivity and post-reaction heat-treatability |
| CN103566837A (en) * | 2013-11-13 | 2014-02-12 | 山西大学 | External circular reaction device suitable for hydrogenation exothermic reaction |
| CN109279575A (en) * | 2017-07-21 | 2019-01-29 | 盐城科莱特电热机械有限公司 | Methanol low-temperature decomposing device |
| CN210229907U (en) * | 2019-07-18 | 2020-04-03 | 北京拓川科研设备股份有限公司 | Fixed bed reaction device |
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