CN107890843B - Microreactor device and application thereof in preparation of benzene series sulfonation products - Google Patents

Microreactor device and application thereof in preparation of benzene series sulfonation products Download PDF

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Publication number
CN107890843B
CN107890843B CN201711137026.0A CN201711137026A CN107890843B CN 107890843 B CN107890843 B CN 107890843B CN 201711137026 A CN201711137026 A CN 201711137026A CN 107890843 B CN107890843 B CN 107890843B
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reaction
gas
micro
heat exchange
mixer
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CN107890843A (en
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郭凯
张东
万力
张锴
欧阳平凯
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Nanjing Tech University
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Nanjing Tech 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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
    • C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
    • C07C303/04—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups
    • C07C303/06—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups by reaction with sulfuric acid or sulfur trioxide
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00851—Additional features
    • B01J2219/00858—Aspects relating to the size of the reactor
    • B01J2219/00862—Dimensions of the reaction cavity itself
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00873—Heat exchange
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/0095—Control aspects
    • B01J2219/00952—Sensing operations
    • B01J2219/00954—Measured properties
    • B01J2219/00961—Temperature

Abstract

The invention discloses a micro-reaction device which comprises a liquid feeding pump, a gas feeding device, a mixer, a micro-reactor, a back pressure valve and a product collecting tank, wherein the liquid feeding pump and the gas feeding device are respectively connected with the mixer, the outlet of the mixer, the micro-reactor, the back pressure valve and the product collecting tank are connected in series, the micro-reactor comprises a reaction cavity and a heat exchange jacket, a reaction tube is arranged in the reaction cavity, the heat exchange jacket is arranged outside the reaction cavity, the upper part of the heat exchange jacket is provided with a heat exchange medium inlet, and the lower part of the heat exchange jacket is provided with a heat exchange medium outlet. The invention also discloses application of the micro-reaction device in preparation of sulfonated products of benzene series. The micro-reaction device is utilized to sulfonate benzene and the derivatives thereof, and the mass transfer and heat transfer are enhanced, so that the reaction can be carried out at a lower temperature, no amplification effect is generated, the investment and the operating cost of equipment are reduced, the production environment is safer and more efficient, and the micro-reaction device has good industrial application prospect.

Description

Microreactor device and application thereof in preparation of benzene series sulfonation products
Technical Field
The invention relates to chemical reaction equipment, in particular to a microreactor device and application thereof in preparation of sulfonated products of benzene series.
Background
The sulfonated products of benzene and derivatives thereof are important fine organic chemical raw materials, and are widely used for producing products such as sulfur dyes, detergents, ultraviolet curing coating photoinitiators, medical intermediates, pesticide intermediates and the like in industry. At present, benzene and the sulfonation of the derivatives thereof are all sulfonated by concentrated sulfuric acid or fuming sulfuric acid, the reaction temperature is high, a large amount of heat is released, the problems of more reaction byproducts, poor reaction selectivity and the like exist in the reaction process, and the yield and the quality of products are seriously influenced; and the waste acid after the reaction is difficult to treat and is easy to cause environmental pollution.
Disclosure of Invention
The purpose of the invention is as follows: in order to solve the problems of high reaction temperature and more byproducts when benzene and derivatives thereof are sulfonated in the prior art, the invention provides a micro-reaction device; the invention also provides application of the micro-reaction device in preparation of sulfonated products of benzene series.
The technical scheme is as follows: a micro-reaction device comprises a liquid feeding pump, a gas feeding device, a mixer, a micro-reactor, a back pressure valve and a product collecting tank, wherein the liquid feeding pump and the gas feeding device are respectively connected with the mixer, an outlet of the mixer, the micro-reactor, the back pressure valve and the product collecting tank are sequentially connected in series, the micro-reactor comprises a reaction cavity and a heat exchange jacket, a reaction tube is arranged in the reaction cavity, the heat exchange jacket is arranged outside the reaction cavity, a heat exchange medium inlet is arranged at the upper part of the heat exchange jacket, and a heat exchange medium outlet is arranged at the lower part of the heat exchange jacket; preferably, the heat exchange medium is water.
Furthermore, a sealing layer is arranged on the outer wall of the reaction cavity and used for isolating the reaction cavity from the heat exchange jacket.
The micro-reactor is also provided with a thermometer, and a temperature probe of the thermometer is in contact with a reaction tube in the reaction cavity. Furthermore, a sealing ring is wrapped outside the thermometer, a thermometer probe is exposed, the thermometer is used for measuring the temperature of the reaction tube in the reaction cavity, and the sealing ring wrapped outside the thermometer is used for isolating the thermometer from the heat exchange jacket and the reaction cavity, so that the heat exchange jacket and the reaction cavity are prevented from influencing the accurate measurement of the temperature. Further, the temperature probe is a thermocouple.
The micro-reactor also comprises a heat exchange layer, and the heat exchange layer is arranged on the inner wall of the reaction cavity. The heat exchange layer is made of silicon carbide, stainless steel, titanium, hastelloy or a carbon fiber plate.
The tube shell of the heat exchange jacket is a metal tube shell, a ceramic tube shell or an engineering plastic tube shell.
The reaction tube in the reaction cavity is a spiral tube, the inner diameter of the reaction tube is 5-10 mm, and the volume of the reaction tube is 1000-2000 ml; furthermore, the reaction tube is made of quartz.
The gas feeding device comprises a device for providing nitrogen and a device for providing SO3Gas distribution tank, and apparatus for providing nitrogen gas and apparatus for providing SO3The gas device is respectively connected with a gas distribution tank, and the outlet of the gas distribution tank is connected with the mixer.
The method for providing N2In the clothesN comprising sequential connection2A steel cylinder, a pressure reducing valve, a first gas flow controller for providing SO3The gas device comprises SO connected in sequence3The system comprises a liquid feed pump, a steam generator and a second gas flow controller, wherein the steam generator is connected with the second gas flow controller through a heat insulation pipe, the first gas flow controller and the second gas flow controller are respectively connected with a gas distribution tank, and the gas distribution tank is used for distributing SO3Gas and N2Thorough mixing and control of SO3The gas distribution tank is connected with the mixer through a pressure reducing valve. Wherein the steam generator comprises a glass heating band and a thermocouple, the glass heating band is connected with SO3The outlet of the liquid feed pump is connected to heat the liquid SO3By the action of the gas, SO3The gas is introduced into the gas distribution tank through the heat preservation pipe and the second gas flow controller.
Wherein, the mixer is a T-shaped mixer.
The working principle is as follows: liquid SO3Gasifying the glass heating zone in the steam generator into gas, flowing into the gas distribution tank through the heat preservation pipe, and controlling SO by the second gas flow controller3The flow rate of (c). N is a radical of2As SO3Of the diluent gas of (2), controlling N by the first gas flow controller2Is introduced into the gas distribution tank by controlling SO3And N2The mixed gas of the gas flow regulating gas distribution tank is mixed with SO3The concentration of (c). The liquid benzene series is pumped into the mixer through the liquid feeding pump and is fully mixed with mixed gas in the mixer, then the mixed gas enters the micro-reactor to be subjected to continuous sulfonation reaction, the reaction temperature of the micro-reactor is controlled through the heat exchange jacket, the thermometer is used for monitoring in real time, reaction liquid flows into the back pressure valve to be buffered after the reaction is finished and then enters the product collecting tank, and residual gas is treated by the tail gas device, so that the sulfonation process is completed.
Wherein the reaction residence time may be determined by SO3The sample introduction speed, the size and the length of the inner diameter of the micro-channel quartz tube and N2Is controlled by the pressure level of (c). At a certain time of the inner diameter and length of the microchannel tube, N2The greater the pressure of (A), the greater the SO3Through a reaction tubeThe shorter the time of (A), due to SO3From N2Diluting with N2Load, therefore, N2The time of the gas flowing through the reaction tube is defined as SO3The residence time in the reaction tank. When N is present2、SO3When the flow rate is constant and the length of the quartz tube is constant, the larger the inner diameter of the quartz reaction tube is, the shorter the retention time is; otherwise when N is2、SO3The flow rate of (2) is constant and the inner diameter of the quartz tube is constant, the longer the tube is, the longer the reaction residence time is. The sample introduction speed is comprehensively controlled, the residence time of the reaction is controlled through the length of the reaction tube and the characteristic dimension of the channel, and the yield and the selectivity of the target product are further controlled.
The invention also provides application of the micro-reaction device in preparation of sulfonated products of benzene series, which comprises the following steps:
(1) for providing SO3SO provided by a device for gases3Mixing the gas and the nitrogen provided by the nitrogen providing device in a gas distribution tank to obtain mixed gas;
(2) mixing the liquid benzene series with the mixed gas obtained in the step (1) in a mixer through a liquid feeding pump, and pumping the mixed gas into a microreactor to perform sulfonation reaction to obtain reaction liquid;
(3) and (3) enabling the reaction liquid flow obtained in the step (2) to enter a product collecting tank through a back pressure valve, and thus obtaining the catalyst.
The benzene series refers to a general term of benzene and derivatives, and includes all aromatic compounds. Preferably, the benzene series is benzene.
SO in the mixed gas3The gas accounts for 6-8% of the mixed gas by volume percent, and SO in the mixed gas3The molar ratio of the gas to the benzene series is 1: 1.7-2.3.
The reaction temperature of the sulfonation reaction in the step (2) is 10-30 ℃, and the reaction residence time is 4-15 min.
And (3) the pressure of the back pressure valve is 1 MPa.
Has the advantages that: compared with the prior art, the invention has the following advantages:
(1) with SO3The new process of direct sulfonation of gas overcomes the defect of using concentrated sulfuric acid orThe method has the advantages that the method has the defect of high reaction temperature when toluene is sulfonated by fuming sulfuric acid, basically solves the pollution problem of waste acid, well controls the content of meta-isomer, and does not generate heavy components of tar;
(2) regulating SO by using gas flow controllers3The gas inflow of the gas is realized, the nitrogen is used for diluting the gas inflow concentration of the sulfur trioxide, the reaction product and the yield are controlled, the generation of non-target products is reduced, and the conversion rate of the product is improved;
(3) the micro-reaction device is utilized to sulfonate benzene and the derivatives thereof, and the mass transfer and heat transfer are enhanced, so that the reaction can be carried out at a lower temperature, no amplification effect is generated, the requirements on equipment materials are reduced, the investment and the operating cost of equipment are reduced, the production environment is safer and more efficient, and the micro-reaction device has a good industrial application prospect.
Drawings
FIG. 1 is a schematic structural view of a micro-reaction device according to the present invention;
FIG. 2 is a schematic diagram of the structure of a reaction tube in a microreactor.
Detailed Description
The invention is further described below with reference to the following figures and examples.
Wherein: 1-a liquid feed pump; 2-a gas feed means; 201-N2A steel cylinder; 202-a pressure relief valve; 203-a first gas flow controller; 204-SO3A liquid feed pump; 205-a steam generator; 206-a second gas flow controller; 207-insulating tube; 208-a gas distribution tank; 209-mixed gas pressure reducing valve; 3-a mixer; 4-a microreactor; 5-back pressure valve; 6-a product collection tank; 7-a reaction chamber; 8-heat exchange jacket; 9-a reaction tube; 10-a condensate inlet; 11-a condensate outlet; 12-a sealing layer; 13-a thermometer; 14-heat exchange layer; 15-lye tank.
Example 1
See fig. 1, a micro-reaction device, including liquid charge pump 1, gas feed arrangement 2, mixer 3, micro-reactor 4, back pressure valve 5 and result collecting tank 6, liquid charge pump 1, gas feed arrangement 2 links to each other with mixer 3 respectively, 3 exports of mixer, micro-reactor 4, back pressure valve 5, result collecting tank 6 and lye tank 15 are established ties, micro-reactor 4 includes reaction cavity 7 and heat transfer jacket 8, be equipped with reaction tube 9 in the reaction cavity 7, heat transfer jacket 8 establishes the outside at reaction cavity 7, heat transfer jacket 8 upper portion is equipped with comdenstion water import 10, heat transfer jacket 8 lower part is equipped with trades comdenstion water export 11. The outer wall of the reaction cavity 7 is provided with a sealing layer 12 for isolating the reaction cavity 7 and the heat exchange jacket 8 from each other.
The microreactor 4 is also provided with a thermometer 13, and a thermocouple carried by the thermometer 13 is in contact with the reaction tube 9 in the reaction chamber. The thermometer is externally wrapped with a sealing ring, a thermometer probe is exposed, the thermometer is used for measuring the temperature of the reaction tube 9 in the reaction cavity, and the thermometer 13 is isolated from the heat exchange jacket 8 and the reaction cavity 7 by wrapping the sealing ring outside the thermometer, so that the heat exchange jacket 8 and the reaction cavity 7 are prevented from influencing the accurate measurement of the temperature.
The microreactor further comprises a heat exchange layer 14, and the heat exchange layer 14 is arranged on the inner wall of the reaction cavity 7.
The reaction tube 9 in the reaction cavity is a spiral tube made of quartz, as shown in fig. 2, the inner diameter of the reaction tube 9 is 5-10 mm, and the volume of the reaction tube 9 is 1000 ml.
The gas feed 2 comprises means for providing nitrogen, means for providing SO3Gas distribution tank, device for providing nitrogen, and device for providing SO3The gas device is respectively connected with the gas distribution tank 208, the outlet of the gas distribution tank is connected with the mixer, and the volume of the gas distribution tank is 1000 ml.
For providing N2The device comprises N connected in sequence2Cylinder 201, pressure reducing valve 202, first gas flow controller 203 for supplying SO3The gas device comprises SO connected in sequence3A liquid feed pump 204, a steam generator 205, a second gas flow controller 206, wherein the steam generator 205 and the second gas flow controller 206 are connected by a heat insulation pipe 207, the first gas flow controller and the second gas flow controller are respectively connected with a gas distribution tank 208, and the gas distribution tank 208 is used for SO3Gas and N2Thorough mixing and control of SO3The gas distribution tank 208 is connected to the mixer 3 via a pressure reducing valve 209. Wherein the steam generator 205 comprises a glass heating ribbon and a thermoelectricGlass heating tape and SO3The outlet of the liquid feed pump is connected to heat the liquid SO3By the action of the gas, SO3The gas is introduced into a gas distribution tank 208 through a heat preservation pipe 207 and a second gas flow controller 206.
The working principle is as follows: liquid SO3Gasifying the glass heating belt in the steam generator into gas, flowing into the gas distribution tank through the heat preservation pipe, and controlling SO by the second gas flow controller3The flow rate of (c). N is a radical of2As SO3Of the diluent gas of (2), controlling N by the first gas flow controller2Is introduced into the gas distribution tank by controlling SO3And N2The mixed gas of the gas flow regulating gas distribution tank is mixed with SO3The concentration of (c). The liquid benzene series is pumped into the mixer through the liquid feeding pump and is fully mixed with mixed gas in the mixer, then the mixed gas enters the micro-reactor to be subjected to continuous sulfonation reaction, the reaction temperature of the micro-reactor is controlled through the heat exchange jacket, the thermometer is used for monitoring in real time, reaction liquid flows into the back pressure valve to be buffered after the reaction is finished and then enters the product collecting tank, and residual gas is treated by the tail gas device, so that the sulfonation process is completed.
Wherein the reaction residence time may be determined by SO3The sample introduction speed, the size and the length of the inner diameter of the micro-channel quartz tube and N2Is controlled by the pressure level of (c). At a certain time of the inner diameter and length of the microchannel tube, N2The greater the pressure of (A), the greater the SO3The shorter the time for passing through the reaction tube, due to SO3From N2Diluting with N2Load, therefore, N2The time of the gas flowing through the reaction tube is defined as SO3The residence time in the reaction tank. When N is present2、SO3When the flow rate is constant and the length of the quartz tube is constant, the larger the inner diameter of the quartz reaction tube is, the shorter the retention time is; otherwise when N is2、SO3The flow rate of (2) is constant and the inner diameter of the quartz tube is constant, the longer the tube is, the longer the reaction residence time is. The sample introduction speed is comprehensively controlled, the residence time of the reaction is controlled through the length of the reaction tube and the characteristic dimension of the channel, and the yield and the selectivity of the target product are further controlled.
Example 2
Similar to example 1, the inner diameter of the microchannel reaction tube was 6mm, the total volume of the microchannel reaction tube was 1000ml, and SO was in the mixed gas3Was diluted to 6%, the benzene feed rate was 300ml, SO3The molar ratio of the benzene to the benzene is 1:1.7, the reaction residence time is 10min, the reaction temperature is 10 ℃, and the pressure of a back pressure valve is 1 MPa; the benzene conversion was 57.5% and the benzene sulfonic acid selectivity was 88.2%.
Example 3
Similar to example 1, the inner diameter of the microchannel reaction tube was 7mm, the total volume of the microchannel reaction tube was 1000ml, and SO was contained in the mixed gas3Was diluted to 6%, the benzene feed rate was 300ml, SO3The molar ratio of the benzene to the benzene is 1:1.7, the reaction residence time is 10min, the reaction temperature is 10 ℃, and the pressure of a back pressure valve is 1 MPa; the benzene conversion was 55.6% and the benzene sulfonic acid selectivity was 84.2%.
Example 4
The microchannel reaction apparatus was the same as in example 1, except that the inner diameter of the microchannel reaction tube was 8mm, the total volume of the microchannel reaction tube was 1000ml, and SO was contained in the mixed gas3Was diluted to 6%, the benzene feed rate was 300ml, SO3The molar ratio of the benzene to the benzene is 1:1.7, the reaction residence time is 10min, the reaction temperature is 10 ℃, and the pressure of a back pressure valve is 1 MPa; the benzene conversion was 54.9% and the benzene sulfonic acid selectivity was 82.2%.
Example 5
The microchannel reaction apparatus was the same as in example 1, except that the inner diameter of the microchannel reaction tube was 9mm, the total volume of the microchannel reaction tube was 1000ml, and SO was contained in the mixed gas3Was diluted to 6%, the benzene feed rate was 300ml, SO3The molar ratio of the benzene to the benzene is 1:1.7, the reaction residence time is 10min, the reaction temperature is 10 ℃, and the pressure of a back pressure valve is 1 MPa; the benzene conversion was 41.2% and the benzene sulfonic acid selectivity was 79.3%.
Example 6
The microchannel reaction apparatus was the same as in example 1, except that the inner diameter of the microchannel reaction tube was 9mm, the total volume of the microchannel reaction tube was 1000ml, and SO was contained in the mixed gas3The concentration of (A) is diluted to 8%, the feeding amount of benzene is 300ml, and benzene and SO3At a molar ratio of 1:2.3, a reaction residence time of 10min and a reaction temperatureThe pressure of the backpressure valve is 1MPa at 10 ℃; the benzene conversion was 47.3% and the benzene sulfonic acid selectivity was 85.4%.
Example 7
The procedure is as in example 2, except that the reaction temperature is 10 ℃ and the reaction residence time is 4 min.
Example 8
The procedure is as in example 2, except that the reaction temperature is 10 ℃ and the reaction residence time is 15 min.
Example 9
The procedure is as in example 2, except that the reaction temperature is 30 ℃ and the reaction residence time is 15 min.

Claims (6)

1. A micro-reaction device is characterized by comprising a liquid feed pump, a gas feed device, a mixer, a micro-reactor, a back pressure valve and a product collecting tank, wherein the liquid feed pump and the gas feed device are respectively connected with the mixer, and an outlet of the mixer, the micro-reactor, the back pressure valve and the product collecting tank are sequentially connected in series; the micro-reactor comprises a reaction cavity and a heat exchange jacket, wherein a reaction tube is arranged in the reaction cavity, the heat exchange jacket is arranged outside the reaction cavity, the upper part of the heat exchange jacket is provided with a heat exchange medium inlet, the lower part of the heat exchange jacket is provided with a heat exchange medium outlet, the micro-reactor also comprises a heat exchange layer, and the heat exchange layer is arranged on the inner wall of the reaction cavity;
the micro-reactor is also provided with a thermometer, and a temperature probe of the thermometer is contacted with a reaction tube in the reaction cavity;
the reaction tube in the reaction cavity is a spiral tube, the inner diameter of the reaction tube is 5-10 mm, and the volume of the reaction tube is 1000-2000 ml;
the gas feeding device comprises a device for providing nitrogen and a device for providing SO3Gas distribution tank, and apparatus for providing nitrogen gas and apparatus for providing SO3The gas device is respectively connected with a gas distribution tank, and the outlet of the gas distribution tank is connected with the mixer.
2. Use of the micro-reaction device according to claim 1 for the preparation of sulfonated products of benzene series.
3. Use according to claim 2, characterized in that it comprises the following steps:
(1) for providing SO3SO provided by a device for gases3Mixing the gas and the nitrogen provided by the device for providing the nitrogen in the gas distribution tank to obtain mixed gas;
(2) mixing the liquid benzene series with the mixed gas obtained in the step (1) in a mixer through a liquid feeding pump, and pumping the mixed gas into a microreactor to perform sulfonation reaction to obtain reaction liquid;
(3) and (3) enabling the reaction liquid flow obtained in the step (2) to enter a product collecting tank through a back pressure valve, and thus obtaining the catalyst.
4. Use according to claim 3, wherein SO is present in the mixed gas3The gas accounts for 6-8% of the mixed gas by volume percent, and SO in the mixed gas3The molar ratio of the gas to the benzene series is 1: 1.7-2.3.
5. The use of claim 3, wherein the reaction temperature of the sulfonation reaction in the step (2) is 10-30 ℃ and the reaction residence time is 4-15 min.
6. Use according to claim 3, wherein the pressure of the back pressure valve of step (3) is 1 MPa.
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CN113896660A (en) * 2021-11-30 2022-01-07 湖北师范大学 Micro-channel continuous sulfonation synthesis method of ultraviolet absorbent BP-4
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