CN108160010B - Tube bundle reaction rectification integrated device - Google Patents

Tube bundle reaction rectification integrated device Download PDF

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Publication number
CN108160010B
CN108160010B CN201711472003.5A CN201711472003A CN108160010B CN 108160010 B CN108160010 B CN 108160010B CN 201711472003 A CN201711472003 A CN 201711472003A CN 108160010 B CN108160010 B CN 108160010B
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Prior art keywords
tube bundle
reaction
rectifying
rectification
reactive distillation
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CN108160010A (en
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顾正桂
曹晓艳
李硕
凌鸿钰
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Nanjing Normal University
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Nanjing Normal University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
    • B01J8/06—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds in tube reactors; the solid particles being arranged in tubes
    • B01J8/067—Heating or cooling the reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/42—Regulation; Control
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/001—Controlling catalytic processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00017—Controlling the temperature
    • B01J2208/00106—Controlling the temperature by indirect heat exchange
    • B01J2208/00168—Controlling the temperature by indirect heat exchange with heat exchange elements outside the bed of solid particles
    • B01J2208/00212—Plates; Jackets; Cylinders

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)

Abstract

The invention discloses a tube bundle reaction and rectification integrated device, which comprises a rectification device and a tube bundle reaction device which are integrally arranged up and down; the rectifying device sequentially comprises an internal reflux condenser, a rectifying section, a stripping section and a coil heater from top to bottom, and a first feeding hole is formed between the rectifying section and the stripping section; the upper end of the tube bundle reaction device is provided with a second feeding hole, the lower end of the tube bundle reaction device is provided with a second discharging hole, and the second discharging hole is communicated with the first feeding hole of the rectifying device through a lifting pipe. The tube bundle reaction and rectification integrated device has the advantages that the generated gas-phase material can be continuously and timely led out of the bottom of the tube bundle reaction device, does not need to be condensed and directly enters the rectification device for rectification, the phenomenon that the catalyst and the material are always in a high-temperature state and are coked and inactivated is avoided, secondary reaction is avoided, the generation of byproducts is reduced, the conversion rate of products and the selectivity of a reaction process are improved, and the device is simple in structure and convenient to operate.

Description

Tube bundle reaction rectification integrated device
Technical Field
The invention belongs to the field of chemical reaction and separation equipment, and particularly relates to a tube bundle reaction and rectification integrated device.
Background
The traditional chemical preparation process comprises reaction and refining units, wherein reaction equipment mostly adopts a high-pressure reaction kettle, a fixed bed reactor, a fluidized bed reactor, a tubular reactor and the like, and the refining process usually adopts units such as distillation, rectification, azeotropic rectification or extractive rectification and the like. In order to simplify the production process and save energy consumption, two units of reaction and refining are integrated in the current production, and the preparation of chemicals is realized in the same device. The kettle type reaction rectification is a common device, the process is simple in process, convenient to operate and intuitive in phenomenon, and is generally used in industrial production, but the equipment has some problems, mainly the raw materials and the catalyst in the reaction process are always in a high-temperature state, the raw materials and the catalyst are not uniformly mixed, the catalyst is easy to coke and deactivate, and meanwhile, by using the equipment, the generated product is difficult to timely move out in the reaction process, secondary reaction is easy to occur, the difficulty is brought to refining, and the product quality and the yield are influenced. Through research and analysis, the problems are caused by defects of the reaction equipment.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide an integrated device which can continuously catalyze reaction and simultaneously refine so as to improve the conversion rate of products and the selectivity of the reaction process and reduce the generation of byproducts.
The technical scheme is as follows: the invention relates to a tube bundle reaction and rectification integrated device, which comprises a rectification device and a tube bundle reaction device which are integrally arranged up and down; the rectifying device sequentially comprises an internal reflux condenser, a rectifying section, a stripping section and a coil heater from top to bottom, and a first feeding hole is formed between the rectifying section and the stripping section; the upper end of the tube bundle reaction device is provided with a second feeding hole, the lower end of the tube bundle reaction device is provided with a second discharging hole, and the second discharging hole is communicated with the first feeding hole of the rectifying device through a lifting pipe.
The device realizes the integration of tube bundle reaction and refining, has simple structure and convenient operation, obviously improves the conversion rate and selectivity of products and reduces the generation of byproducts. Furthermore, the rectifying device is provided with a first thermocouple and a second thermocouple respectively, and the lower end of the rectifying device is provided with a first discharge hole. The rectifying device also comprises an outer condenser connected with the inner reflux condenser pipe and a collecting tank connected with the outer condenser.
Still further, the tube bundle reaction device comprises a shell, a plurality of reaction tubes arranged in the shell and a distributor arranged at the upper ends of the reaction tubes. The upper end of the tube bundle reaction device is provided with a heat medium discharge hole, the lower end of the tube bundle reaction device is provided with a heat medium feed hole, and the heat medium provides reaction temperature for the reaction tubes. The reaction tube is internally provided with a catalyst, glass wool, a tray for supporting the catalyst and the glass wool and a support ring for supporting the tray in sequence from top to bottom. The second feed inlet end of the tube bundle reaction device is provided with a preheater for preheating the raw materials. And the upper end and the lower end of the tube bundle reaction device are respectively provided with a third thermocouple and a fourth thermocouple.
Furthermore, the diameter ratio of the opening diameter of the distributor to the reaction tube is 1: 5-10. With this range of diameter ratios, the feed can be evenly distributed.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages: this tube bank reaction rectification integrated device can make the gaseous phase material that generates export tube bank reaction unit bottom in succession, in time, need not the condensation, directly gets into the rectifier unit and rectifies, avoids catalyst and material to be in high temperature state and coking deactivation all the time, avoids the emergence of secondary reaction, has reduced the production of accessory substance, improves the conversion rate of product and reaction process's selectivity, and simple structure, convenient operation.
Drawings
FIG. 1 is a schematic structural diagram of a tube bundle reaction rectification integrated device of the invention;
FIG. 2 is a schematic view showing the internal structure of a reaction tube;
FIG. 3 is a top view of the distributor;
fig. 4 is a side view of the distributor.
Detailed Description
As shown in figure 1, the tube bundle reaction and rectification integrated device comprises a rectification device 1 and a tube bundle reaction device 2 which are integrally arranged up and down.
The rectifying device 1 sequentially comprises an inner reflux condenser 3, a rectifying section 4, a stripping section 5 and a coil heater 6 from top to bottom, the inner reflux condenser 3 is also connected with an outer condenser 12 and a collecting tank 13 connected with the outer condenser 12, and the inner reflux condenser 3 and the outer condenser 12 are controlled in temperature by adopting cooling media. The whole rectification device 1 is supplemented with heat and controlled in temperature by a coil heater 6. The upper end and the lower end of the rectifying device 1 are respectively provided with a first thermocouple 14 and a second thermocouple 15 for measuring temperature. A first feed inlet 7 is arranged between the rectifying section 4 and the stripping section 5, and a first discharge outlet 11 is arranged at the lower end of the rectifying device 1.
The tube bundle reaction device 2 comprises a shell 16, a plurality of reaction tubes 17 with the same specification arranged in the shell 16, and a distributor 18 arranged at the upper ends of the reaction tubes 17. The reaction tube 17 is provided with a catalyst 21, glass wool 22, a tray 23 for supporting the catalyst 21 and the glass wool 22, and a support ring 24 for supporting the tray 23 in sequence from top to bottom, as shown in fig. 2. The upper end of the tube bundle reaction device 2 is provided with a second feeding hole 8 and a heat medium discharging hole 19, the lower end is provided with a second discharging hole 9 and a heat medium feeding hole 20, a heating medium is added into the heat medium feeding hole 20, and the reaction temperature is provided for the reaction tube 17 through a jacket and is stably controlled. The second inlet 8 is provided with a preheater 25 for preheating the raw material and a valve 28 for controlling the feeding amount and maintaining the residence time of the material in the reaction tube 17. The second discharge hole 9 is communicated with the first feed inlet 7 of the rectifying device 1 through a riser 10. The upper end and the lower end of the tube bundle reaction device 2 are respectively provided with a third thermocouple 26 and a fourth thermocouple 27 for temperature measurement.
Wherein, the number of the reaction tubes 17 can be 5-37, the ratio of the outer diameter to the length can be 1: 30-60, and the ratio of the diameter of the opening of the distributor 18 to the diameter of the reaction tubes 17 can be 1: 5-10, as shown in fig. 3 and 4. The outer diameter of the tube bundle reaction device 2 is the same as that of the rectification device 1, and the ratio of the diameter to the length of the preheater 25 is 1: 5-8. The height of the packing filled in the rectifying section 4 and the height of the packing filled in the stripping section 5 are determined according to the difference of the boiling points of the synthetic materials. The catalyst 21 may be SO4 2-/ZrO2A solid acid catalyst.
The working principle is as follows: the rectifying apparatus 1 is flange-connected to the upper end of the tube bundle reaction apparatus 2, the temperature of the tube bundle reaction apparatus 2 and the preheater 25 is controlled by feeding a heating medium from the heating medium feed port 20, and the temperature of the inner reflux condenser 3 and the outer condenser 12 is controlled by a cooling medium.
The composition and proportion of the raw materials are adjusted, the preheated raw materials are added into a reaction tube 17 from a second feeding hole 8 through a distributor 18 for reaction, and the generated gas-phase product is lifted to a first feeding hole 7 through a lifting tube 10 for rectification. When the bottom liquid level of the rectifying device is higher than that of the coil heater 6, the coil heater 6 is opened, and the temperature of the rectifying device 1 is controlled, so that the low-boiling-point components partially reflux through the condensation part of the internal reflux condenser 3, the reflux quantity of the internal reflux condenser 3 can be adjusted, the rest part is condensed through the external condenser 12, the materials are discharged to the collecting tank 13, and the high-boiling-point fractions flow out from the first discharge port 11 at the lower end of the rectifying device 1 to finish the rectification.

Claims (8)

1. A tube bundle reaction rectification integrated device is characterized in that: comprises a rectifying device (1) and a tube bundle reaction device (2) which are integrally arranged up and down; the rectifying device (1) sequentially comprises an internal reflux condenser (3), a rectifying section (4), a stripping section (5) and a coil heater (6) from top to bottom, a first feeding hole (7) is formed between the rectifying section (4) and the stripping section (5), and a first discharging hole (11) is formed in the lower end of the rectifying device (1); the upper end of the tube bundle reaction device (2) is provided with a second feeding hole (8), the lower end of the tube bundle reaction device is provided with a second discharging hole (9), and the second discharging hole (9) is communicated with the first feeding hole (7) of the rectifying device (1) through a lifting pipe (10); the tube bundle reaction device (2) comprises a shell (16), a plurality of reaction tubes (17) arranged in the shell (16) and a distributor (18) arranged at the upper ends of the reaction tubes (17).
2. The tube bundle reactive distillation integrated apparatus of claim 1, wherein: the rectifying device (1) also comprises an outer condenser (12) connected with the inner reflux condenser (3) and a collecting tank (13) connected with the outer condenser (12).
3. The tube bundle reactive distillation integrated apparatus of claim 1, wherein: the rectifying device (1) is provided with a first thermocouple (14) and a second thermocouple (15) respectively.
4. The tube bundle reactive distillation integrated apparatus of claim 1, wherein: the upper end of the tube bundle reaction device (2) is provided with a heat medium discharge hole (19), the lower end of the tube bundle reaction device is provided with a heat medium feed hole (20), and the heat medium provides reaction temperature for the reaction tubes (17).
5. The tube bundle reactive distillation integrated apparatus of claim 1, wherein: and a catalyst (21), glass wool (22), a tray (23) for supporting the catalyst (21) and the glass wool (22) and a support ring (24) for supporting the tray (23) are sequentially arranged in the reaction tube (17) from top to bottom.
6. The tube bundle reactive distillation integrated apparatus of claim 1, wherein: and a preheater (25) for preheating the raw materials is arranged at the end of the second feed port (8).
7. The tube bundle reactive distillation integrated apparatus of claim 1, wherein: the upper end and the lower end of the tube bundle reaction device (2) are respectively provided with a third thermocouple (26) and a fourth thermocouple (27).
8. The tube bundle reactive distillation integrated apparatus of claim 1, wherein: the diameter ratio of the opening diameter of the distributor (18) to the diameter of the reaction tube (17) is 1: 5-10.
CN201711472003.5A 2017-12-29 2017-12-29 Tube bundle reaction rectification integrated device Active CN108160010B (en)

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CN108160010B true CN108160010B (en) 2020-05-19

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101480591A (en) * 2008-01-11 2009-07-15 山东科技大学 Tubular reaction fractionating tower
CN202169099U (en) * 2011-08-08 2012-03-21 江苏沿江化工资源开发研究院有限公司 Plate type and packing combined reactive distillation device with continuous external circulation

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101480591A (en) * 2008-01-11 2009-07-15 山东科技大学 Tubular reaction fractionating tower
CN202169099U (en) * 2011-08-08 2012-03-21 江苏沿江化工资源开发研究院有限公司 Plate type and packing combined reactive distillation device with continuous external circulation

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