CN107519827B - High-efficiency energy-saving xylene separation process - Google Patents

High-efficiency energy-saving xylene separation process Download PDF

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CN107519827B
CN107519827B CN201610434437.5A CN201610434437A CN107519827B CN 107519827 B CN107519827 B CN 107519827B CN 201610434437 A CN201610434437 A CN 201610434437A CN 107519827 B CN107519827 B CN 107519827B
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reactor
guide cylinder
shell
guide
axis
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CN107519827A (en
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张英
薄德臣
高景山
陈建兵
高明
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China Petroleum and Chemical Corp
Sinopec Fushun Research Institute of Petroleum and Petrochemicals
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China Petroleum and Chemical Corp
Sinopec Fushun Research Institute of Petroleum and Petrochemicals
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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
    • B01J14/00Chemical processes in general for reacting liquids with liquids; Apparatus specially adapted therefor
    • 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
    • B01J19/0053Details of the reactor
    • 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
    • B01J19/26Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C15/00Cyclic hydrocarbons containing only six-membered aromatic rings as cyclic parts
    • C07C15/02Monocyclic hydrocarbons
    • C07C15/067C8H10 hydrocarbons
    • C07C15/08Xylenes
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00Purification; Separation; Use of additives
    • C07C7/14Purification; Separation; Use of additives by crystallisation; Purification or separation of the crystals
    • 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
    • B01J2219/00761Details of the reactor
    • 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
    • B01J2219/18Details relating to the spatial orientation of the reactor
    • B01J2219/182Details relating to the spatial orientation of the reactor horizontal

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Abstract

The invention discloses a process for separating and preparing high-purity m-xylene from carbon octaene. The invention uses an impinging stream reactor which is particularly suitable for the process, realizes fluid mixing by multiple times of impinging, has good micro-mixing effect, ensures that the mixed liquid flows horizontally outside an impinging zone, provides sufficient retention time for materials, realizes step reaction, and achieves the target conversion rate by flow channel and liquid flow rate design. The method overcomes the defect that the prior impinging stream reactor can not realize high conversion rate by a single reactor, simplifies the process flow, reduces the production cost and equipment investment, and ensures the long-term operation of equipment. The method has no waste liquid discharge in the production process, and is a green and environment-friendly process method.

Description

High-efficiency energy-saving xylene separation process
Technical Field
The invention belongs to the technical field of separation and purification of aromatic xylene, and particularly relates to a method for separating and extracting high-purity m-xylene from carbon octaene by using a high-efficiency impinging stream reactor.
Background
At present, mixed xylene separated from a toluene disproportionation device and carbon-octaarene obtained from reformed gasoline, pyrolysis gasoline and coal tar all contain four isomers, namely ortho-xylene, para-xylene, meta-xylene and ethylbenzene. Among the carbon octa-aromatics from these sources, the meta-xylene content is the greatest. Because the boiling points of the four carbon octa-aromatics are very close, especially the boiling points of the p-xylene and the m-xylene are the closest, the high-purity p-xylene and m-xylene products can not be economically obtained by adopting the conventional rectification technology. At present, the high-purity p-xylene is obtained industrially by adopting a mature adsorption separation process, and researches show that the separation of the high-purity m-xylene by adopting a complex reaction extraction technology is an effective separation method.
For the complex extraction separation process, the high-efficiency and rapid mixing contact between liquid and liquid phases is the most important factor influencing the separation effect and the separation efficiency. Impinging streams are a very effective way to achieve rapid mixing. Two high-speed fluids are impacted oppositely to form a highly turbulent impact area in the reactor, so that the external resistance in the transfer process can be effectively reduced, the mixing is promoted, and the mass transfer and heat transfer are enhanced. Impinging stream reactors have been widely used in extraction, mixing, absorption, crystallization and other chemical processes. The application of the high-efficiency impinging stream reaction to the reactive extraction process has become a research hotspot in recent years, and the impinging stream reactor used for the extraction and separation process has the advantages of greatly reducing the volume of equipment by fully utilizing the characteristic of good mixing effect and greatly improving the production efficiency and the processing capacity. The development of an efficient impinging stream reactor which is suitable for separating and obtaining high-purity meta-xylene by a complex extraction process is an effective means for improving the technical level of para-xylene production.
Since the 90 s of the 20 th century, research in the field of Impinging Streams has turned significantly to the focus of Liquid-continuous Impinging Streams (LIS). In patent CN 100364656C, two opposite guide cylinders are disposed in the reactor shell, and the liquid flows through the guide cylinders on both sides respectively by the driving action of the pump, and then opposite impacts occur at the center. Although the reactor has a simple structure, only the impact effect of the fluid of the guide flow cylinders at the two ends is emphasized, the flow condition of the fluid in the reactor after impact is not considered, and dead zones are easily formed at the two sides of the reactor. If solid phase catalyst exists in the two impact fluids, the catalyst is easy to settle and stay, and the reaction depth and the product quality are directly influenced. Patent CN 102989404A sets up the screw in the draft tube, utilizes the drive effect of two screws to make liquid take place to strike in the reactor in the center department, utilizes the effect of draft tube and guide vane simultaneously, has solved the problem of the outer mixture of striking district, the effectual blind spot of having eliminated. However, the improvement of the multi-emphasis impact effect of the current impact flow reactor is generally the improvement of the single-kettle mixing effect, and for the reaction which requires to reach a certain retention time and conversion rate, the improvement cannot meet the requirement of the retention time even if the reaction is extremely-to-reach the ideal state of the full-mixing flow reactor due to the limitation of the reactor form.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a process for separating and preparing high-purity m-xylene from carbon octaene.
The invention relates to a process for separating and preparing high-purity m-xylene from carbon octaene, which comprises the following steps:
the method comprises the steps of taking the C-octaarene as a raw material, taking an impinging stream reactor as a complex reaction extraction device, respectively introducing the arene raw material and an extracting agent into the impinging stream reactor through a conveying device for complex extraction reaction, discharging a reaction product out of the impinging stream reactor, carrying out liquid-liquid layering, and conventionally separating an extraction phase rich in m-xylene to obtain a high-purity m-xylene product.
Wherein, the conventional separation generally comprises operations such as rectification separation and the like. The extractant obtained by conventional separation can be recycled, and the raffinate phase can directly enter the next working procedure.
In the invention, the extracting agents are HF and BF3The mixed aqueous solution of (1) preferably contains 10 to 40 mass% of hydrogen fluoride and BF3The concentration by mass is preferably 10-40%;
in the invention, the temperature of the complex extraction reaction is 0-10 ℃, and preferably 0-5 ℃;
in the invention, the operating pressure of the system is in the range of 0.5-2 MPa, and the preferable pressure is 1-1.5 MPa.
In the present invention, the size of the impinging stream reactor can be determined depending on the throughput of the apparatus and the operating conditions. To enhance the mixing effect of the impinging stream reactor, a material circulation may be established between the outlet and the inlet of the impinging stream reactor. And (3) mixing a part of the obtained reaction product with the carbon octaarene raw material, and then circulating the mixture back to the impinging stream reactor, wherein the amount of the circulating material is 5-500% of the amount of the fresh feeding material.
In the invention, the impinging stream reactor for the m-xylene complex reaction extraction process adopts the following technical scheme:
an impinging stream reactor comprising a reactor shell and a draft tube; the reactor shell comprises a cylinder body and a sealing head; two opposite feed pipes are arranged at the center of the outer wall of the end socket; the first guide cylinder is connected with the feeding pipe in the reactor shell and consists of two truncated cone-shaped shells, the two shells are oppositely arranged, the axis of the first guide cylinder is superposed with the axis of the reactor, the thick end of the truncated cone-shaped shell is connected with the feeding pipe, and liquid entering through the feeding pipe is accelerated and then is impacted and mixed at the outlet of the thin end;
the outer side of the first guide cylinder is provided with a second guide cylinder which is cylindrical, a channel is reserved between the two ends of the second guide cylinder and the seal head, and the axis of the second guide cylinder is superposed with the axis of the reactor;
a third guide cylinder is arranged on the outer side of the second guide cylinder, the third guide cylinder is composed of two circular truncated cone-shaped shells, the two shells are oppositely arranged, the axis of the third guide cylinder is superposed with the axis of the reactor, the thick end of the third guide cylinder is connected with the end enclosure, and the outlet of the thin end is oppositely arranged;
and a fourth guide cylinder is arranged on the outer side of the third guide cylinder, the fourth guide cylinder is cylindrical, gaps are reserved between the two ends of the fourth guide cylinder and the end sockets, and the axis of the guide cylinder is superposed with the axis of the reactor.
In the invention, the impinging stream reactor can be vertical or horizontal. The shell cylinder of the reactor is cylindrical or rectangular, and the end enclosure is circular, oval, butterfly or flat cover.
The guide shell can be set to be more than 4, preferably 4-10. When the guide shell is in the shape of a circular truncated cone, the included angle (conical included angle) between the generatrix of the circular truncated cone and the axis is preferably 1-80 degrees.
In the invention, a discharge pipe is vertically arranged on the reactor shell at the center of the axis. The discharging pipe is generally arranged more than 2, preferably 2-6. The discharging pipes are symmetrically distributed along the axis of the reactor.
In the invention, the distance between the outlets of the thin ends of the two truncated cone-shaped shells of the first guide cylinder is 0.1-10 times of the diameter of the thin end, the distance between the two ends of the second guide cylinder and the end enclosure is equal and is 0.1-10 times of the diameter of the thin end of the truncated cone-shaped shell of the first guide cylinder, the distance between the outlets of the thin ends of the two truncated cone-shaped shells of the third guide cylinder is 0.1-10 times of the diameter of the thin end of the first guide cylinder, and the distance between the two ends of the fourth guide cylinder and the end enclosure is equal and is 0.1-10 times of the diameter of the thin end of the truncated.
In the invention, the guide shell is generally formed by rolling and welding steel plates. The guide shell and the end enclosure and the two guide shells are fixed by welding or riveting. The thick end of the circular truncated cone draft tube can be provided with a hole, so that materials can flow back under the suction effect, the mixing is enhanced, and the reaction conversion rate is improved. The reaction raw material flows in from the thick end of the circular truncated cone-shaped guide shell and flows to the thin end, the pressure potential energy of the fluid is converted into kinetic energy in the process, the kinetic energy reaches the maximum value at the outlet of the thin end and generates an impact action, the mixed fluid flows in a flat push way under the blocking and flow guiding actions of the circular truncated cone-shaped guide shell and the cylinder partition wall and is deflected to the next flat push flow channel after meeting the shell of the reactor, the flow channel has a structure similar to that of the previous flow channel, the fluid flows to the thin end from the thick end, the liquid is accelerated in the flow process and is subjected to impact mixing at the thin end, the reciprocating is carried out, and a plurality of flat push flow channels can be.
Compared with the prior art, the process has the following beneficial effects:
1. in the impinging stream liquid phase reactor adopted by the invention, the material flow is introduced through the guide shell and then is impacted in the impinging zone, and high-efficiency mixing is generated, and the zone can be regarded as a fully mixed flow reaction system. The single full mixed flow reactor is limited by the form, the residence time of partial materials is short, the reaction materials can not reach the required conversion rate in the period, the residence time of partial materials is too long, excessive reaction is caused, the volume of the reactor is occupied, and the volume utilization rate of the reactor is reduced. In the liquid-liquid impinging stream reactor, the material flow is introduced through the guide shell and then is impacted in an impinging zone, and efficient mixing is generated, and the zone can be regarded as a fully mixed flow reaction system. After the liquid after impact mixing flows out of an impact area, the isolation and the flow guiding of the guide shell generate horizontal push flow until secondary impact occurs, and the area can be regarded as a horizontal push flow reaction system. The reactor of the invention generates multiple times of impact mixing, thus strengthening the effects of mass transfer and heat transfer; the flow channel volume of the plug flow reaction system is high in occupied ratio, the material retention time is long, the target conversion rate can be achieved through design, and excessive reaction is eliminated.
2. The reactor used in the invention overcomes the defects of the traditional impinging stream reactor, so that the reaction is uniform and sufficient, the volume of the reactor is saved, the excessive reaction is reduced, the target conversion rate can be achieved through the design of the volume of the flow channel, the equipment investment is reduced, and the economic benefit is good. In addition, the guide cylinder has the functions of blocking fluid and guiding and conveying fluid, a special fluid distribution guide system is not required to be arranged in the reactor, and compared with the traditional guide system, the guide cylinder has the advantages of smooth liquid flow, small pressure drop and no dead zone.
3. The invention strengthens the impact effect of the reactor through multiple impact designs, greatly enhances the micro-mixing effect of the reactor, greatly shortens the mixing time, improves the production efficiency, avoids the existence of dead zones through a good flat push flow channel design, improves the synchronism of chemical reactions at each position of the reactor space, and is beneficial to improving the product quality; the reactor has simple structure, no need of adding other diversion distribution systems, small equipment processing difficulty, low equipment investment cost and good economic benefit.
4. The invention utilizes the characteristic that the molecular alkalinity of the intermediate xylene of the carbon octaarene is far higher than that of other three components, and adopts HF and BF3The composite solvent has high selectivity to m-xylene as an extracting agent, and the high-efficiency impinging stream reactor is used as extraction equipment, so that the production efficiency is greatly improved, the equipment volume is reduced, and the key technical problems of low extraction efficiency and low production efficiency caused by poor mixing effect of the traditional extraction equipment are solved. In addition, the invention also has the characteristic of high purity of the m-xylene product, and the purity of the m-xylene product can reach more than 99.5 percent.
5. The method and the special extraction equipment greatly improve the efficiency of extracting the high-purity m-xylene from the carbon octaarene, remarkably reduce the volume of the equipment, simplify the process flow, reduce the production cost and the equipment investment and ensure the long-period operation of the equipment. No waste liquid is discharged in the production process, and the method is a green and environment-friendly process method.
Drawings
FIG. 1 is a schematic view of the structure of a reactor according to the present invention.
FIG. 2 is a process flow diagram of the present invention.
FIG. 3 is a schematic diagram of the structure of a conventional impinging stream reactor.
Detailed Description
The structure of an impinging stream reactor for liquid-liquid reactive extraction process according to the present invention is described in more detail below with reference to the accompanying drawings.
The liquid phase impinging stream reactor of the present invention is described in more detail below with reference to the specific figures.
As shown in figure 1, the liquid phase impinging stream reactor for liquid-liquid multiple-effect mixing of the invention comprises two parts, namely a reactor shell and a guide shell. The reactor shell consists of a cylinder body 12 and a seal head 15. Two opposite feed pipes 16 are arranged in the center of the outer wall of a reactor shell end enclosure 15, first guide cylinders 3 and 14 are connected with the feed pipes on the inner side of the reactor shell, the first guide cylinders 3 and 14 are respectively truncated cone-shaped shells, the two truncated cone-shaped shells are arranged oppositely, and the axis of the first guide cylinder (the truncated cone-shaped shell) is superposed with the axis of the reactor. The thick end of the circular truncated cone-shaped shell is connected with a feeding pipe, and liquid is accelerated and then is impacted and mixed at the outlet of the thin end. Outside the first guide shell 3 and 14 is the second guide shell 4. The second guide cylinder 4 is cylindrical, and a gap is reserved between the second guide cylinder and the end enclosure 15 to provide a fluid flow channel. The second guide shell 4 can be fixedly connected with the end socket 15 or the first guide shells 3 and 14 through a support. The axis of the second guide cylinder 4 is coincident with the axis of the reactor. And third guide cylinders 5 and 13 are arranged on the outer side of the second guide cylinder 4, the third guide cylinder is a circular truncated cone-shaped shell, and the two shells are arranged oppositely. The axis of the third guide cylinder coincides with the axis of the reactor, the thick end of the truncated cone-shaped shell is hermetically connected with the seal head 15, and the outlet of the thin end is oppositely arranged. And a fourth guide cylinder 6 is arranged outside the third guide cylinders 5 and 13 and is cylindrical, and the axis of the fourth guide cylinder coincides with the axis of the reactor. A channel (gap) is reserved between the two ends of the fourth guide cylinder and the end enclosure 15 to provide a channel for fluid to flow. The fourth guide cylinder 6 can be fixedly connected with the end socket 15, the cylinder 12 or the third guide cylinders 5 and 13 through supports. The tapping pipes 8 are arranged on the vertical outer shell in the center of the reactor axis, and the tapping pipes 8 are generally arranged in more than two, preferably 2 to 6. The several tapping pipes are generally distributed symmetrically along the reactor axis.
The liquid phase impinging stream reactor of the present invention may be in the form of a vertical or horizontal structure. The shell cylinder of the reactor is cylindrical or rectangular, and the end socket 15 is generally circular, oval, butterfly or flat cover. The number of the draft tubes can be more than 4, preferably 4 to 10. When the guide cylinder is in the shape of a circular truncated cone, the included angle between the generatrix of the circular truncated cone and the axis is generally 1-80 degrees. In the first guide cylinders 3 and 14, the distance between the outlets of the thin ends of the two truncated cone-shaped shells is 0.1-10 times of the diameter of the outlets of the thin ends. The distance between the two ends of the second guide cylinder 4 and the end socket is equal, and the distance is generally 0.1-10 times of the diameter of the outlet of the thin end of the circular truncated cone shell of the first guide cylinder. In the third guide cylinders 5 and 13, the distance between the outlets of the thin ends of the two truncated cone-shaped shells is 0.1-10 times of the diameter of the thin end (outlet) of the first guide cylinder. The distances between the two ends of the fourth guide cylinder 6 and the end socket are equal, and are generally 0.1-10 times of the diameter of the outlet of the thin end of the truncated cone-shaped shell of the first guide cylinder.
The guide shell is generally formed by rolling and welding steel plates. The guide shell and the end enclosure 15, and the adjacent two guide shells are generally fixed by welding or riveting 7. The thick end of the circular truncated cone draft tube can be provided with a plurality of holes to enable materials to flow back under the suction effect, so that the mixing is enhanced, and the reaction conversion rate is improved.
With reference to fig. 1, the working principle or working process of the liquid phase impinging stream reactor of the present invention is as follows: the reaction feed 1 is pressurized by a raw material pump 2, flows in from the thick end of the first guide cylinder 3 and 14, flows to the thin end, in the process, the pressure potential of the fluid is converted into kinetic energy, and the kinetic energy reaches the maximum value at the outlet of the thin end and generates an impact action to form a first impact surface 11. The mixed fluid flows in a horizontal pushing mode along the flow channel (formed by the first guide cylinder and the second guide cylinder at intervals) under the blocking and flow guiding effects of the first guide cylinder 3 and the second guide cylinder 14 and the second guide cylinder 4, and is deflected to a next horizontal pushing flow channel after encountering the end socket 15, the flow channel is similar to the structure of the previous flow channel and is formed by the second guide cylinder 4 and the third guide cylinder 5 and 13 at intervals, the fluid flows from a thick end section to a thin end section, and the liquid is accelerated and is subjected to impact mixing at the thin end in the flowing process to form an impact surface 10. The impacted fluid flows in the flow channels formed by the third guide cylinders 5 and 13 and the fourth guide cylinder 6 at intervals, is baffled after meeting the end socket 15, enters the flow channels formed by the fourth guide cylinder 6 and the cylinder 12 at intervals, and is impacted at the outlet to form an impact surface 9. The impinged fluid exits the reactor through outlet 8.
Compared with the impinging stream reactor in the prior art, the impinging stream reactor adopted by the invention adopts multiple-effect impingement, so that the impinging mixing effect is enhanced, the micro-mixing effect of the reactor is greatly enhanced, the mixing time is greatly shortened, and the production efficiency is improved; in addition, through the design of a horizontal push flow channel, the retention time of materials in the reactor is prolonged, the target conversion rate can be achieved by using a single impinging stream reactor, the back mixing is reduced, the reaction is uniform, and the space utilization rate of the reactor is improved; the reactor has the advantages of simple structure, small processing difficulty, low equipment investment and good economic benefit due to good flow channel design without additionally arranging an additional diversion distribution system.
The process flow of the present invention is described in more detail below with reference to the accompanying drawings.
As shown in figure 2, according to the metering ratio, the carbon-octaarene mixture 17 and the extracting agent 18 are respectively input into a buffer tank 19 by a pump or other liquid conveying equipment for premixing, then input into feed inlets 20 and 21 of an impinging stream reactor 22 by the pump or other liquid conveying equipment, raw material flows flow to the center of the vessel at high speed through a guide shell under the action of pressure and are impinged in opposite directions at the center, the impinged materials flow out of the reactor from an outlet 23, and the pressure of the reactor is controlled by a pressure regulator 24. The reaction material discharged from the pressure regulator 24 directly enters a phase separation tank 25 for cooling, standing and layering, the upper layer is a raffinate phase 27 after reaction, the raffinate phase can directly enter the next procedure, the lower layer is an extract phase 26 rich in m-xylene, the extract phase can be separated conventionally to obtain a high-purity m-xylene product, and the extractant can be recycled. Wherein material circulation can be established between the outlet and the inlet of the impinging stream reactor as desired.
Example 1
The concentration of raw material carbon octa-arene and xylene is 20wt%, and HF and BF are in extracting agent3The concentrations were all 20 wt%.
The feeding ratio of the extracting agent to the carbon octaarene is 2:1 (volume ratio), the extracting agent and the carbon octaarene are respectively pumped into the impinging stream reactor and are rapidly mixed with the circulating material in the impinging stream reactor to generate a complex reaction extraction process, and the speed of the circulating material is 200% of the feeding amount. The operation temperature is controlled to be 3 ℃, the retention time is 10 min, and the reaction pressure is 1.5 MPa.
The experimental result shows that the recovery rate of the m-xylene is 88wt%, and the purity of the obtained m-xylene is 99.6 wt%.
Example 2
The procedure of example 1 was followed except that the operating temperature was changed to 10 ℃.
The experimental result shows that the recovery rate of the m-xylene is 83 wt%, and the purity of the obtained m-xylene is 99.5 wt%.
Example 3
The procedure of example 1 was followed except that the residence time was changed to 5 min.
The experimental result shows that the recovery rate of the m-xylene is 86 wt%, and the purity of the obtained m-xylene is 99.7 wt%.
Example 4
The procedure of example 1 was followed except that the residence time was changed to 15 min.
The experimental result shows that the recovery rate of the m-xylene is 90 wt%, and the purity of the obtained m-xylene is 99.8 wt%.
Comparative example 1
For comparison with the process of the present invention, comparative experiments were conducted using a conventional impinging stream reactor. A conventional impinging stream reaction structure is shown in fig. 3. The working process is briefly described as follows: two guide cylinders C1, C2 which are symmetrically arranged at the middle part of the container 22 near two ends respectively and are sunk in the material, and two feeding pipes 20, 21 which are coaxially and symmetrically arranged in the two guide cylinders respectively. The materials in the guide shell flow to the center of the container 22 from two ends through the guide shell C1 and C2 under the push of the materials in the two feeding pipes, and impact oppositely at the center to form an impact area around the impact surface. The intense relative motion between the fluid masses from different directions in this zone allows for efficient contact and mixing between the fluid masses and the liquid phase. After impact, the fluid returns to both ends through the annular chamber between the inner walls of the container 22, and is then conveyed by the material in the feed pipes 20 and 21 through the guide cylinders C1 and C2 to the center of the container 22 and impacted again, and the circulation is repeated, and the fluid is discharged through the outlet 23.
The operating conditions and process parameters were the same as in example 1.
The experimental result shows that the recovery rate of the m-xylene is 67.5 percent, and the purity of the obtained m-xylene is 99.5 percent.

Claims (18)

1. A process for separating and preparing high-purity meta-xylene from carbon octaarene comprises the following steps:
taking carbon octa-arene as a raw material, adopting an impinging stream reactor as a complex reaction extraction device, respectively introducing the arene raw material and an extracting agent into the impinging stream reactor through a conveying device for complex extraction reaction, discharging a reaction product out of the impinging stream reactor, and then carrying out liquid-liquid layering, wherein an extraction phase rich in m-xylene can be subjected to conventional separation to obtain a high-purity m-xylene product;
the impinging stream reactor comprises a reactor shell and a guide shell, wherein the reactor shell comprises a cylinder body and an end enclosure; the center of the outer wall of the end socket is provided with two opposite feeding pipes, the inner side of the reactor shell is connected with the feeding pipes and is provided with a first guide cylinder, the first guide cylinder consists of two truncated cone-shaped shells, the two shells are oppositely arranged, the axis of the truncated cone-shaped shell is superposed with the axis of the reactor, and the thick end of the truncated cone-shaped shell is connected with the feeding pipes; a second guide cylinder is arranged on the outer side of the first guide cylinder, the second guide cylinder is cylindrical, gaps are reserved between two ends of the second guide cylinder and the end socket, and the axis of the second guide cylinder is superposed with the axis of the reactor; a third guide cylinder is arranged on the outer side of the second guide cylinder, the third guide cylinder is composed of two circular truncated cone-shaped shells, the two shells are oppositely arranged, the axis of the guide cylinder is superposed with the axis of the reactor, the thick end of the third guide cylinder is connected with the end enclosure, and the outlets of the thin ends are oppositely arranged; and a fourth guide cylinder is arranged on the outer side of the third guide cylinder, the fourth guide cylinder is cylindrical, a channel is reserved between the two ends of the fourth guide cylinder and the seal head, and the axis of the fourth guide cylinder is superposed with the axis of the reactor.
2. The process as claimed in claim 1, wherein the tapping pipe is provided on a casing which is vertically disposed at the center of the axis of the reactor.
3. The process according to claim 2, wherein the number of the discharge pipes is 2 to 6, and the discharge pipes are symmetrically distributed along the axis of the reactor.
4. The process of claim 1, wherein the reactor is in the form of a vertical or horizontal configuration.
5. The process as claimed in claim 1, wherein the reactor shell cylinder is cylindrical or rectangular and the head is circular, elliptical, butterfly or flat cover shaped.
6. The process according to claim 1, wherein the number of the guide shell is 4-10.
7. The process according to claim 1, wherein the included angle between the generatrix of the circular truncated cone and the axis is 1-80 °.
8. The process according to claim 1, wherein the distance between the outlets of the thin ends of the two truncated cone-shaped shells of the first guide shell is 0.1 to 10 times the diameter of the outlets of the thin ends.
9. The process according to claim 1, wherein the distance between the two ends of the second guide cylinder and the end socket is equal to 0.1-10 times of the diameter of the thin end of the circular truncated cone shell of the first guide cylinder.
10. The process as claimed in claim 1, wherein the distance between the outlets of the thin ends of the two truncated cone-shaped shells of the third guide shell is 0.1-10 times of the diameter of the thin end of the first guide shell.
11. The process according to claim 1, wherein the distance between the two ends of the fourth guide cylinder and the end socket is equal to 0.1-10 times of the diameter of the thin end of the circular truncated cone shell of the first guide cylinder.
12. The process according to claim 1, wherein the guide shell and the end enclosure, and the adjacent guide shells are fixed by welding or riveting.
13. The process of claim 1, wherein the truncated cone-shaped shell of the first guide shell and the third guide shell is provided with a plurality of holes at the thick end.
14. The process of claim 1, wherein said conventional separation comprises a rectification separation.
15. The process according to claim 1, wherein the extractant obtained by conventional separation is recycled, and the raffinate phase obtained is directly fed to the next step.
16. The process of claim 1 wherein said extractive agents are HF and BF3The mixed aqueous solution of (1) has a hydrogen fluoride mass concentration of 10-40% and BF3The mass concentration of (A) is 10-40%.
17. The process according to claim 1, wherein the temperature of the complex extraction reaction is 0 ℃ to 10 ℃ and the operating pressure is 0.5 MPa to 2 MPa.
18. The process of claim 1, wherein a portion of the reaction product obtained is recycled to the impinging stream reactor after mixing with the carbon octaarene feedstock, wherein the amount of recycled material is from 5% to 500% of the fresh feed.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1814344A (en) * 2005-02-05 2006-08-09 中国石油化工股份有限公司 Impact flow reactor for liquid-phase reaction
CN103203213A (en) * 2012-01-16 2013-07-17 清华大学 Liquid phase impinging stream reactor with controllable acidity
CN103848481A (en) * 2012-11-30 2014-06-11 沈阳工业大学 Rotating cylinder type cavitation impinging stream micro-electrolysis reactor
CN204352850U (en) * 2014-11-24 2015-05-27 沈阳化工大学 A kind of multicomponent laminar submergence impact flow reactor

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101804317B (en) * 2010-04-02 2012-10-17 南京大学 Multiphase catalysis tower type collision current reactor

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1814344A (en) * 2005-02-05 2006-08-09 中国石油化工股份有限公司 Impact flow reactor for liquid-phase reaction
CN103203213A (en) * 2012-01-16 2013-07-17 清华大学 Liquid phase impinging stream reactor with controllable acidity
CN103848481A (en) * 2012-11-30 2014-06-11 沈阳工业大学 Rotating cylinder type cavitation impinging stream micro-electrolysis reactor
CN204352850U (en) * 2014-11-24 2015-05-27 沈阳化工大学 A kind of multicomponent laminar submergence impact flow reactor

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
间二甲苯的分离和利用;顾文华;《江苏化工》;19800930;第8卷(第3期);第42,49-53页 *

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