CN110681334A - Continuous gas-liquid reaction device and continuous gas-liquid reaction system comprising same - Google Patents

Continuous gas-liquid reaction device and continuous gas-liquid reaction system comprising same Download PDF

Info

Publication number
CN110681334A
CN110681334A CN201910913234.8A CN201910913234A CN110681334A CN 110681334 A CN110681334 A CN 110681334A CN 201910913234 A CN201910913234 A CN 201910913234A CN 110681334 A CN110681334 A CN 110681334A
Authority
CN
China
Prior art keywords
reaction
continuous gas
main reactor
liquid
liquid reaction
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201910913234.8A
Other languages
Chinese (zh)
Other versions
CN110681334B (en
Inventor
洪浩
洪亮
陶建
郭金海
戴睿智
张岩
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kelleying Life Science And Technology (tianjin) Co Ltd
Asymchem Life Science Tianjin Co Ltd
Original Assignee
Kelleying Life Science And Technology (tianjin) Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Kelleying Life Science And Technology (tianjin) Co Ltd filed Critical Kelleying Life Science And Technology (tianjin) Co Ltd
Priority to CN201910913234.8A priority Critical patent/CN110681334B/en
Publication of CN110681334A publication Critical patent/CN110681334A/en
Application granted granted Critical
Publication of CN110681334B publication Critical patent/CN110681334B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • 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
    • B01J19/18Stationary reactors having moving elements inside
    • B01J19/1862Stationary reactors having moving elements inside placed in series
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006Controlling or regulating processes
    • B01J19/0013Controlling the temperature of the process
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details 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
    • B01J19/0053Details of the reactor
    • B01J19/0066Stirrers
    • 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
    • B01J19/18Stationary reactors having moving elements inside
    • B01J19/1806Stationary reactors having moving elements inside resulting in a turbulent flow of the reactants, such as in centrifugal-type reactors, or having a high Reynolds-number
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • B01J4/001Feed or outlet devices as such, e.g. feeding tubes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • B01J4/008Feed or outlet control devices
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • B01J4/02Feed or outlet devices; Feed or outlet control devices for feeding measured, i.e. prescribed quantities of reagents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2204/00Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
    • B01J2204/002Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the feeding side being of particular interest
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00054Controlling or regulating the heat exchange system
    • B01J2219/00056Controlling or regulating the heat exchange system involving measured parameters
    • B01J2219/00058Temperature measurement
    • B01J2219/00063Temperature measurement of the reactants
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00074Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00094Jackets
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00164Controlling or regulating processes controlling the flow

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The invention provides a continuous gas-liquid reaction device and a continuous gas-liquid reaction system containing the same. The continuous gas-liquid reaction device comprises: a main reactor, a stirring device and an oscillation source. The stirring device is arranged in the main reactor and extends along the length direction of the main reactor; the oscillation source is used for controlling the oscillation frequency of the main reactor. The continuous gas-liquid reaction device is simultaneously provided with the stirring device and the oscillation source, under the simultaneous action of the stirring device and the oscillation source, axial and radial complex vortexes can be formed in the main reactor, and the vortexes disappear continuously along with the oscillation. This makes the flow pattern in the main reactor more complex, strengthens the liquid-liquid mass transfer, and then makes the reaction more abundant, improves the heat transfer effect of the main reactor simultaneously. The existence of the oscillation source enables the system to be repeatedly washed between the wall of the reactor and the stirring device violently, so that the risk of bonding and blocking in the reaction process can be effectively inhibited.

Description

Continuous gas-liquid reaction device and continuous gas-liquid reaction system comprising same
Technical Field
The invention relates to the field of chemical reaction device manufacturing, in particular to a continuous gas-liquid reaction device and a continuous gas-liquid reaction system containing the same.
Background
The gas-liquid-solid three-phase reaction is widely applied in the field of pharmaceutical chemical industry, and can be divided into two types according to the properties of a bed layer: a fixed bed gas-liquid-solid three-phase reactor and a suspended bed gas-liquid-solid three-phase reactor. A fixed bed reactor is represented by a trickle bed. The advantage of the trickle bed is that the solid-liquid ratio (or liquid retention) of the gas under the action of plug flow is small, the influence of homogeneous reaction can be reduced, and flooding can not be formed on the flow pattern of the gas-liquid two-phase downward flow. However, the disadvantage is that the fixed bed reactor has a relatively high requirement for the particle size of the solid particles. If the solid particles are too small, the catalyst and the reaction system cannot be in uniform contact, so that the local temperature in the reactor is easily increased, a temperature runaway phenomenon is caused, and the whole reaction effect is influenced. In particular, fixed bed reactors are not very suitable for gas-liquid-solid three-phase reactions in which solids are formed.
In the suspension bed gas-liquid-solid three-phase reactor, the solid in the reaction system is in a suspension state in a gas-liquid mixture. According to the type of mechanical stirring, the suspension bed gas-liquid-solid three-phase reactor can be divided into a bubbling slurry reactor with mechanical stirring suspension and gas bubbling stirring, a three-phase fluidized bed reactor without stirring, in which gas-liquid flows upwards in parallel and solid is not taken out of the bed, a three-phase circulation reactor with a guide cylinder and the like. However, in some low-temperature continuous reaction processes, the reaction time is too long, the volume of the whole reactor is large easily after the suspension bed gas-liquid-solid three-phase reactor is used for scale-up production, and meanwhile, the reaction temperature needs to be ensured to be low. However, due to the low reaction temperature, the solubility of the product formed is not high, which leads to the reactants being easily separated out during the reaction process, resulting in the production of a large amount of solids in the reactor, whereas the solid beds in the reactors listed above mostly exist as catalysts and are mostly operated in batches.
It can be seen that the existing gas-liquid-solid three-phase reactor is usually a batch reaction, most of which can not meet the requirement of continuous production and can be blocked. And for the reaction with longer reaction time, in order to ensure the plug flow effect, huge reaction volume is needed to achieve the expected reaction effect. Meanwhile, the reactor has poor mass and heat transfer effects, greatly improves the risk of the amplification effect on the reaction, and needs to spend larger equipment investment cost.
On the basis, a continuous gas-liquid reaction device with good heat transfer effect and low cost is needed.
Disclosure of Invention
The invention mainly aims to provide a continuous gas-liquid reaction device and a continuous gas-liquid reaction system containing the same, and aims to solve the problems of discontinuous reaction and poor heat transfer effect caused by solid precipitation in the reaction of the conventional gas-liquid reaction device.
In order to achieve the above object, according to one aspect of the present invention, there is provided a continuous gas-liquid reaction apparatus comprising: a main reactor, a stirring device and an oscillation source. The stirring device is arranged in the main reactor and extends along the length direction of the main reactor; the oscillation source is used for controlling the oscillation frequency of the main reactor.
Further, the main reactor comprises: the reaction section is provided with a first feed inlet and a reaction product system outlet; the temperature-returning dissolving section is provided with a reaction product system inlet and a product outlet, and the reaction product system inlet is communicated with the reaction product system outlet through a reaction product system conveying pipeline; the temperature control unit is used for controlling the temperature of the main reactor.
Further, the main reactor also comprises a middle buffer section, the middle buffer section comprises a buffer solvent inlet, and the middle buffer section is arranged on the conveying pipeline of the reaction product system.
Further, the reaction section is also provided with a second feeding hole, and the level of the second feeding hole is lower than that of the first feeding hole.
Further, the temperature control unit includes: the first temperature control device is used for controlling the temperature of the reaction section; the second temperature control device is used for controlling the temperature of the middle buffer section; and the third temperature control device is used for controlling the temperature of the temperature returning dissolution section.
Further, the main reactor also comprises a product pool, and the inlet end of the product pool is communicated with the product outlet.
Another aspect of the present application also provides a continuous gas-liquid reaction system, comprising: the continuous gas-liquid reaction device and the premixing device. The continuous gas-liquid reaction device comprises a main reactor, and the main reactor is provided with a first feeding hole; the pre-mixing device is used for mixing at least part of reaction raw materials and then conveying the mixture to the continuous gas-liquid reaction device, the pre-mixing device is provided with a gas-phase raw material inlet, a solvent inlet and a pre-reaction product outlet, and the pre-reaction product outlet is communicated with the first feed inlet through a pre-reaction product conveying pipeline.
Further, the main reactor is provided with a product outlet, the continuous gas-liquid reaction system further comprises a product collecting device, the product collecting device is provided with a product collecting port, and the product collecting port is communicated with the product outlet through an overflow pipeline.
Further, the main reactor is further provided with a vent, the continuous gas-liquid reaction system further comprises an overflow pressure-balancing device, the overflow pressure-balancing device is provided with a first communicating port and a second communicating port, the first communicating port is communicated with an overflow pipeline, and the second communicating port is communicated with the vent through the overflow pressure-balancing pipeline.
Furthermore, the reaction section of the main reactor is also provided with a second feeding hole, the horizontal height of the second feeding hole is lower than that of the first feeding hole, and the first feeding hole is used for introducing liquid phase raw materials; the premixing device is provided with a solvent inlet, a gas phase raw material inlet and a mixed liquid outlet, and the mixed liquid outlet is communicated with the second feeding hole.
By applying the technical scheme of the invention, the continuous gas-liquid reaction device is simultaneously provided with the stirring device and the oscillation source, under the simultaneous action of the stirring device and the oscillation source, complex vortexes in the axial direction and the radial direction can be formed in the main reactor, and the vortexes continuously disappear along with the oscillation. This makes the flow pattern in the main reactor more complex, strengthens the liquid-liquid mass transfer, and then makes the reaction more abundant, improves the heat transfer effect of the main reactor simultaneously. In addition, the existence of the oscillation source enables the system to be repeatedly washed between the wall of the reactor and the stirring device vigorously to inhibit the risk of adhesion blockage during the reaction process. In summary, the continuous gas-liquid reaction device not only can realize continuous synthesis, but also can improve the mass transfer and heat transfer effects of reaction raw materials, and can effectively inhibit the risk of bonding and blocking.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 shows a schematic diagram of a continuous gas-liquid reaction apparatus provided in accordance with an exemplary embodiment of the present invention; and
fig. 2 is a schematic diagram showing the structure of a continuous gas-liquid reaction system according to a preferred embodiment of the present invention.
Wherein the figures include the following reference numerals:
100. a continuous gas-liquid reaction device;
110. a reaction section; 111. a first feed port; 112. a reaction product system outlet; 113. a vent port; 114. a second feed port; 115. a first temperature measuring port;
120. a middle buffer section; 121. a buffer solvent inlet; 122. a second temperature measuring port;
130. a temperature return dissolving section; 131. a reaction product system inlet; 132. a product outlet; 133. a third temperature measuring port;
140. a product pool;
151. a first temperature control jacket; 152. a first temperature control device; 153. a second temperature-control jacket; 154. a second temperature control device; 155. a third temperature control jacket; 156. a third temperature control device;
161. a motor; 162. a stirring shaft; 163. a stirring paddle; 170. an oscillation source; 180. a first weight control device; 190. a first delivery pump;
200. a premixing device; 210. a second weight control device; 220. a third weight control device; 230. a second delivery pump;
300. a product collection device; 400. an overflow pressure-balancing device; 410. and a fourth weight control device.
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 with reference to examples.
As described in the background art, the conventional gas-liquid reaction apparatus has problems in that the reaction is not continuous and the heat transfer effect is poor due to the precipitation of solids during the reaction. In order to solve the above technical problem, the present application provides a continuous gas-liquid reaction apparatus, as shown in fig. 1, comprising: a main reactor, a stirring device and a vibration source 170. The stirring device is disposed inside the main reactor and extends along the length direction of the main reactor, and the oscillation source 170 is used for controlling the oscillation frequency of the main reactor.
The continuous gas-liquid reaction device is simultaneously provided with the stirring device and the oscillation source 170, under the simultaneous action of the stirring device and the oscillation source, complex vortexes in the axial direction and the radial direction can be formed in the main reactor, and the vortexes disappear continuously along with the oscillation. This makes the flow pattern in the main reactor more complex, strengthens the liquid-liquid mass transfer, and then makes the reaction more abundant, improves the heat transfer effect of the main reactor simultaneously. In addition, the existence of the oscillation source 170 enables the system to be repeatedly washed between the wall of the system and the stirring device vigorously to inhibit the risk of adhesion blockage during the reaction process. In summary, the continuous gas-liquid reaction device not only can realize continuous synthesis, but also can improve the mass transfer and heat transfer effects of reaction raw materials, and can effectively inhibit the risk of bonding and blocking.
In a preferred embodiment, as shown in fig. 1, the main reactor comprises: a reaction section 110, a temperature return dissolution section 130 and a temperature control unit. Wherein, the reaction section 110 is provided with a first feed port 111 and a reaction product system outlet 112; the temperature-return dissolving section 130 is provided with a reaction product system inlet 131 and a product outlet 132, and the reaction product system inlet 131 is communicated with the reaction product system outlet 112 through a reaction product system conveying pipeline; the temperature control unit is used for controlling the temperature of the main reactor.
Under the action of the temperature control unit, the reaction raw materials react in the reaction section 110 to obtain a desired reaction product, and then the reaction product is transferred to the temperature return dissolution section 130 through a reaction product system conveying pipeline. The vigorous turbulence of the gas-liquid phases in the tempering and dissolving section 130 enables the particle size of the solid product produced to be greatly reduced and facilitates the increase in the suspension time of the solid product in the tempering and dissolving section 130. This can intensify the solid dissolution and the dissolved gas precipitation in the temperature recovery dissolution section 130, and achieve the effects of dissolving the solid product and removing the gas phase raw material absorbed in the system, so that the subsequent material beating is more convenient.
Preferably, as shown in fig. 1, the reaction section 110 is further provided with a second feeding hole 114, the first feeding hole 111 is arranged at the top of the reaction section 110, and the level of the second feeding hole 114 is lower than the level of the first feeding hole 111. The plurality of feeding holes are arranged to ensure that the continuous gas-liquid reaction device has different feeding modes. For example, the reaction material without gas phase is introduced into the reaction section 110 through the first inlet 111, and the solvent with the gas phase raw material dissolved therein is introduced into the reaction section 110 through the second inlet 114.
In order to increase the utilization rate of the gas-phase raw material, it is preferable that the main reactor further includes an intermediate buffer section 120, as shown in fig. 1, the intermediate buffer section 120 includes a buffer solvent inlet 121, and the intermediate buffer section 120 is disposed on the conveying pipeline of the reaction product system. In order to inhibit adverse effects on the reaction such as convection formed by the temperature-returning dissolution section 130 on the reaction section 110 and the like, and the gas phase dissolved in the solvent can be re-precipitated due to temperature return, the intermediate buffer section 120 is arranged to re-dissolve and utilize the precipitated gas phase raw material, so that the raw material utilization rate is improved; in addition, the temperature-returning dissolving section also provides a place for the precipitation of solid products.
The intermediate buffer section 120 is disposed on the transportation pipeline of the reaction product system, and the buffer solvent is added into the intermediate buffer section 120 through the buffer solvent inlet 121, which is beneficial to make the unreacted gas-phase raw material in the reaction product system be absorbed by the buffer solvent again, and return to the reaction section 110 to participate in the reaction, thereby reducing the waste of the gas-phase raw material.
In order to more accurately monitor the temperature in the continuous gas-liquid reaction device, in a preferred embodiment, the continuous gas-liquid reaction device further comprises: the temperature measuring device comprises a first temperature measuring device, a second temperature measuring device and a third temperature measuring device. Wherein the first temperature measuring device is used for detecting the temperature of the reaction section 110, the second temperature measuring device is used for detecting the temperature of the middle buffer section 120, and the third temperature measuring device is used for detecting the temperature of the rewarming dissolution section 130. As shown in FIG. 1, the continuous gas-liquid reaction device is provided with a first temperature measuring port 115, a second temperature measuring port 122 and a third temperature measuring port 133, which correspond to the first temperature measuring device, the second temperature measuring device and the third temperature measuring device in sequence.
In order to better control the temperature of each section in the continuous gas-liquid reaction device, a sectional temperature control mode is adopted in the application. In a preferred embodiment, the temperature control unit comprises: the temperature control device comprises a first temperature control device, a second temperature control device and a third temperature control device; the first temperature control device is used for controlling the temperature of the reaction section 110, the second temperature control device is used for controlling the temperature of the intermediate buffer section 120, and the third temperature control device is used for controlling the temperature of the rewarming dissolution section 130.
In order to further increase the conversion rate of the reaction, as shown in fig. 1, more preferably, the first temperature control device comprises a first temperature control jacket 151 and a first temperature control device 152, wherein the first temperature control jacket 151 is provided with a first temperature control medium inlet and a first temperature control medium outlet, and the first temperature control device 152 is communicated with the first temperature control medium inlet and is used for providing a temperature control medium into the first temperature control jacket 151; the second temperature control device comprises a second temperature control jacket 153 and a second temperature control device 154, wherein the second temperature control jacket 153 is provided with a second temperature control medium inlet and a second temperature control medium outlet, and the second temperature control device 154 is communicated with the second temperature control medium inlet and is used for providing a temperature control medium for the second temperature control jacket 153; the third temperature control device comprises a third temperature control jacket 155 and a third temperature control device 156, wherein the third temperature control jacket 155 is provided with a third temperature control medium inlet and a third temperature control medium outlet, and the third temperature control device 156 is communicated with the third temperature control medium inlet and is used for providing a temperature control medium for the third temperature control jacket 155.
The stirring device may be of the kind commonly used in the art. Preferably, as shown in fig. 1, the stirring device includes a motor 161, a stirring shaft 162 and a stirring paddle 163 sequentially connected, the stirring shaft 162 extends along the length direction of the continuous gas-liquid reaction device, and the motor 161 is used for driving the stirring shaft 162 to drive the stirring paddle 163 to stir the material. The stirring device may be made of materials commonly used in the art, including but not limited to enamel, stainless steel, teflon, etc. The stirring shape of the stirring device includes, but is not limited to, propeller type, disk type, plate and frame type, etc.
In a preferred embodiment, as shown in FIG. 1, the main reactor further comprises a product tank 140, and the inlet end of the product tank 140 is in communication with the product outlet 132. The product tank 140 is configured to provide a location for overflow of the product system passing through the tempering dissolving section 130.
Preferably, the material of the main reactor includes but is not limited to glass or stainless steel, etc., and enamel or teflon spray coating can be adopted for the highly corrosive materials.
It should be noted that the above-mentioned main reactor segment connection (such as flange connection, quick-opening connection or screw connection) provided in the present application can also be integrally formed.
Another aspect of the present application also provides a continuous gas-liquid reaction system, as shown in fig. 1 and 2, comprising: the continuous gas-liquid reaction apparatus 100 and the premixing apparatus 200 described above. The continuous gas-liquid reaction device 100 comprises a main reactor, the main reactor is provided with a first feeding hole 111, the premixing device 200 is used for mixing at least part of reaction raw materials and then conveying the mixture to the continuous gas-liquid reaction device 100, the premixing device 200 is provided with a gas-phase raw material inlet, a solvent inlet and a pre-reaction product outlet, and the pre-reaction product outlet is communicated with the first feeding hole 111 through a pre-reaction product conveying pipeline.
The continuous gas-liquid reaction device 100 not only can realize continuous synthesis, but also can improve the mass transfer and heat transfer effects of reaction raw materials and effectively inhibit the risk of bonding and blocking. The pre-mixing device 200 can increase the absorption rate of the solvent to the gas-phase raw material, increase the contact area between the gas-phase raw material and the liquid-phase raw material, and increase the conversion rate of the reaction raw material. Therefore, the continuous gas-liquid reaction system has the advantages of high mass transfer and heat transfer efficiency, difficult blockage, high reaction conversion rate and the like.
In order to facilitate the collection of the product, as shown in fig. 2, preferably, the main reactor is further provided with a product outlet 132, and the continuous gas-liquid reaction system further comprises a product collecting device 300, wherein the product collecting device 300 is provided with a product collecting port, and the product collecting port is communicated with the product outlet 132 through an overflow pipeline.
In a preferred embodiment, as shown in FIG. 2, the main reactor is further provided with a vent 113, the continuous gas-liquid reaction system further comprises an overflow pressure-balancing device 400, the overflow pressure-balancing device 400 is provided with a first communicating port and a second communicating port, the first communicating port is communicated with the overflow pipeline, and the second communicating port is communicated with the vent 113 through the overflow pressure-balancing pipeline. The overflow pressure-balancing device 400 is communicated with the main reactor through an overflow pressure-balancing pipeline and is communicated with the product collecting device through an overflow pipeline, so that the arrangement of the overflow pressure-balancing device 400 can balance the pressure in the overflow pipeline and the main reactor, and the overflow is ensured to be generated.
The premixing device 200 may be a mixing device commonly used in the art, and preferably, as shown in fig. 2, the main reactor is further provided with a second feed port 114, the level of the second feed port 114 is lower than that of the first feed port 111, and the first feed port 111 is used for feeding the liquid-phase raw material; the premixing device 200 is provided with a solvent inlet, a gas-phase raw material inlet, and a mixed liquid outlet, which is communicated with the second feed port 114.
The whole temperature is controlled and the solvent dissolved with gas phase is continuously fed from the second feeding port 114 at the lower part of the reaction section 110. The other reactant is fed from the first feed port 111 at the top of the reaction section 110, and the two are in countercurrent contact, and the mass transfer effect of the reaction is increased under the stirring and stirring action of the incompletely absorbed gas bubbles in the premixing device 200. And along with the process that the system is gradually pushed to the temperature returning dissolving section 130, the solid precipitate which is sensitive to the temperature is dissolved back to the system, and the gas which is not reacted is separated out again along with the temperature rise and floats to the reaction section 110 to participate in the reaction again. Finally, the system is received by the overflow pressure balancing device 400 in an overflow mode. Preferably, the overflow line is a U-shaped overflow line, so as to ensure pressure balance in the whole reactor, thereby ensuring reaction time and preventing unstable system overflow caused by pressure unbalance. More preferably, the continuous gas-liquid reaction system further comprises a fourth temperature control device for controlling the temperature of the material in the overflow pipeline.
An exemplary embodiment of the present application also provides a continuous gas-liquid reaction process, which is performed by using the apparatus shown in fig. 1 and 2, and comprises the following steps:
the liquid phase raw material is transferred to the reaction section 110 through the first feed port 111 by the first transfer pump 190, and the amount of the liquid phase raw material added is controlled by the first weight control device 180. The gas-phase raw material is delivered by the second delivery pump 230, and is delivered to the premixing device 200 together with the gas-phase raw material to be mixed, and then the mixture is delivered to the reaction section 110 through the second feed port 114, in the process, the ratio of the gas-phase material to the solvent is controlled by the second weight control device 210 and the third weight control device 220. Gases generated during the reaction and excess gas-phase raw materials are discharged from the vent 113.
After the reaction raw material enters the reaction section 110, the stirring paddle 163 and the stirring shaft 162 are stirred under the action of the motor, and the oscillation source 170 is turned on. The refrigerant in the first temperature control device 152 (refrigerator) is transported to the first temperature control jacket 151 to control the temperature of the reaction section 110. Meanwhile, a first temperature measuring device is inserted into the first temperature measuring port 115 to monitor the reaction temperature.
The reaction product system obtained after the reaction is completed is transported to the intermediate buffer section 120 through the reaction product system outlet 112. Buffer solvent is added to the intermediate buffer stage 120 via buffer solvent inlet 121. Unreacted gas in the reaction product system is absorbed and dissolved after contacting with the buffer solvent. The refrigerant in the second temperature control device 154 (refrigerator) is delivered to the second temperature control jacket 153 to control the temperature of the middle buffer section 120. Meanwhile, a second temperature measuring device is inserted into the second temperature measuring port 122 to monitor the temperature in the middle buffer section 120.
The reaction product system is then transported to the rewarming dissolution zone 130 via product outlet 132. The temperature control medium in the third temperature control device 156 (water bath device) is fed into the third temperature control jacket 155 to control the temperature of the rewarming dissolution section 130. Meanwhile, a third temperature measuring device is inserted into the third temperature measuring port 133 to monitor the temperature in the rewarming and dissolving section 130. Since the temperature of the temperature-returning dissolution section 130 is higher than the temperatures of the intermediate buffer section 120 and the reaction section 110, the solid in the reaction product system can be re-dissolved, and at the same time, the residual gas-phase raw material can be removed.
The product overflowing from the temperature-returning dissolution section 130 enters the overflow pressure-balancing device 400 through the product pool 140 and subsequent overflow lines, and finally enters the product collection device 300. While a fourth weight control 410 is provided on the overflow line. Furthermore, the overflow pressure-balancing device 400 is also in communication with the vent 113 via an overflow pressure-balancing line, which enables regulation of the pressure in the main reactor and the product collection device 300 during the reaction.
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects:
the continuous gas-liquid reaction device has the advantage of high integration level, and particularly integrates gas dissolution, gas-liquid reaction, solid phase dissolution, gas phase raw material recycling and system degassing. This ensures that the reaction is completed in the reactor all at once. The number of times of unit operation is saved, the labor intensity and the investment on equipment are reduced, and compared with a batch device, the device is safer, more practical and more efficient. The continuous process of the reaction with the solid product precipitation is successfully realized through the segmented temperature control, compared with the intermittent batch reaction operation, the segmented temperature control continuous reaction has the advantages of high reaction speed, high raw material conversion rate and product yield, high product purity, and higher safety and practicability.
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 (10)

1. A continuous gas-liquid reaction apparatus, comprising:
a main reactor;
the stirring device is arranged in the main reactor and extends along the length direction of the main reactor; and
an oscillation source (170), the oscillation source (170) for controlling an oscillation frequency of the main reactor.
2. The continuous gas-liquid reaction device according to claim 1, wherein the main reactor comprises:
a reaction section (110), wherein the reaction section (110) is provided with a first feed inlet (111) and a reaction product system outlet (112);
the system comprises a temperature-return dissolving section (130), wherein the temperature-return dissolving section (130) is provided with a reaction product system inlet (131) and a product outlet (132), and the reaction product system inlet (131) is communicated with the reaction product system outlet (112) through a reaction product system conveying pipeline;
and the temperature control unit is used for controlling the temperature of the main reactor.
3. The continuous gas-liquid reaction device according to claim 2, wherein the main reactor further comprises an intermediate buffer section (120), the intermediate buffer section (120) comprising a buffer solvent inlet (121), the intermediate buffer section (120) being arranged on the reaction product system transfer line.
4. The continuous gas-liquid reaction device according to claim 2 or 3, characterized in that the reaction section (110) is further provided with a second feed opening (114), and the level of the second feed opening (114) is lower than the level of the first feed opening (111).
5. The continuous gas-liquid reaction device according to claim 3, the temperature control unit comprising:
a first temperature control device for controlling the temperature of the reaction section (110);
a second temperature control device for controlling the temperature of the intermediate buffer section (120); and
a third temperature control device for controlling the temperature of the rewarming dissolution section (130).
6. The continuous gas liquid reaction device according to claim 5, characterized in that the main reactor further comprises a product reservoir (140), an inlet end of the product reservoir (140) being in communication with the product outlet (132).
7. A continuous gas-liquid reaction system, comprising:
the continuous gas-liquid reaction device (100) according to any one of claims 2 to 6, the continuous gas-liquid reaction device (100) comprising a main reactor, and the main reactor being provided with a first inlet opening (111);
the pre-mixing device (200) is used for mixing at least part of reaction raw materials and then conveying the mixture into the continuous gas-liquid reaction device (100), the pre-mixing device (200) is provided with a gas-phase raw material inlet, a solvent inlet and a pre-reaction product outlet, and the pre-reaction product outlet is communicated with the first feed inlet (111) through a pre-reaction product conveying pipeline.
8. The continuous gas-liquid reaction system according to claim 7, wherein the main reactor is further provided with a product outlet (132), the continuous gas-liquid reaction system further comprising a product collecting device (300), the product collecting device (300) being provided with a product collecting port, the product collecting port being in communication with the product outlet (132) via an overflow line.
9. The continuous gas-liquid reaction system according to claim 8, wherein the main reactor is further provided with a vent (113), the continuous gas-liquid reaction system further comprises an overflow pressure-balancing device (400), the overflow pressure-balancing device (400) is provided with a first communication port and a second communication port, the first communication port is communicated with the overflow pipeline, and the second communication port is communicated with the vent (113) through the overflow pressure-balancing pipeline.
10. The continuous gas liquid reaction system according to claim 7, wherein the main reactor is further provided with a second inlet (114), and the level of the second inlet (114) is lower than the level of the first inlet (111), the first inlet (111) being for feeding a liquid phase feedstock;
the premixing device (200) is provided with a solvent inlet, a gas-phase raw material inlet and a mixed liquid outlet, and the mixed liquid outlet is communicated with the second feeding hole (114).
CN201910913234.8A 2019-09-25 2019-09-25 Continuous gas-liquid reaction device and continuous gas-liquid reaction system comprising same Active CN110681334B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910913234.8A CN110681334B (en) 2019-09-25 2019-09-25 Continuous gas-liquid reaction device and continuous gas-liquid reaction system comprising same

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910913234.8A CN110681334B (en) 2019-09-25 2019-09-25 Continuous gas-liquid reaction device and continuous gas-liquid reaction system comprising same

Publications (2)

Publication Number Publication Date
CN110681334A true CN110681334A (en) 2020-01-14
CN110681334B CN110681334B (en) 2021-09-07

Family

ID=69110285

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910913234.8A Active CN110681334B (en) 2019-09-25 2019-09-25 Continuous gas-liquid reaction device and continuous gas-liquid reaction system comprising same

Country Status (1)

Country Link
CN (1) CN110681334B (en)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006297379A (en) * 2005-03-25 2006-11-02 Asahi Kasei Chemicals Corp Ultrasonic reactor apparatus
CN202527151U (en) * 2012-01-18 2012-11-14 浙江大学 Oscillatory flow tubular reaction crystallizer
CN206424927U (en) * 2017-01-05 2017-08-22 恒力石化(大连)有限公司 A kind of chemical gas-liquid mixed reaction unit
CN208661150U (en) * 2018-06-29 2019-03-29 福建科宏生物工程股份有限公司 A kind of segmented Oscillatory Flow Reactor
CN109876747A (en) * 2019-04-02 2019-06-14 吉林凯莱英医药化学有限公司 Pillar flow reactor and pillar continuous reaction system
CN110183480A (en) * 2019-06-21 2019-08-30 辽宁凯莱英医药化学有限公司 Trimethyl silicane ethyl-acetylene is continuously synthesizing to system and is continuously synthesizing to method

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006297379A (en) * 2005-03-25 2006-11-02 Asahi Kasei Chemicals Corp Ultrasonic reactor apparatus
CN202527151U (en) * 2012-01-18 2012-11-14 浙江大学 Oscillatory flow tubular reaction crystallizer
CN206424927U (en) * 2017-01-05 2017-08-22 恒力石化(大连)有限公司 A kind of chemical gas-liquid mixed reaction unit
CN208661150U (en) * 2018-06-29 2019-03-29 福建科宏生物工程股份有限公司 A kind of segmented Oscillatory Flow Reactor
CN109876747A (en) * 2019-04-02 2019-06-14 吉林凯莱英医药化学有限公司 Pillar flow reactor and pillar continuous reaction system
CN110183480A (en) * 2019-06-21 2019-08-30 辽宁凯莱英医药化学有限公司 Trimethyl silicane ethyl-acetylene is continuously synthesizing to system and is continuously synthesizing to method

Also Published As

Publication number Publication date
CN110681334B (en) 2021-09-07

Similar Documents

Publication Publication Date Title
KR101187181B1 (en) Stirring device and process for carrying out a gas-liquid reaction
JP4891480B2 (en) Reactor for continuous gas-liquid reaction, liquid-liquid reaction, or gas-liquid-solid reaction
KR100349476B1 (en) Two stage reactor for continuous three phase slurry hydrogenation and method of operation
US4699740A (en) Stirring system and method for introducing gases to liquids
Patwardhan et al. Design of gas-inducing reactors
US10449509B2 (en) Synthesis of organic peroxydes using an oscillatory flow mixing reactor
CN101247886A (en) Method and apparatus for fluid-liquid reactions
JP2008255091A (en) Method for producing polymethylene-polyphenyl-polyamine
JP2002502310A (en) Equipment for mixing and dissolving solid granules in liquid for the production of phosphorus nitrogen fertilizer
CN110681334B (en) Continuous gas-liquid reaction device and continuous gas-liquid reaction system comprising same
CN100393688C (en) Method for producing terephthalic acid and terephthalic acid
CN212595615U (en) Reaction unit and system for synthesizing acetic acid by methanol carbonyl
WO2021056272A1 (en) Continuous gas-liquid reaction device and continuous gas-liquid reaction system including same
CN213348863U (en) Resin reaction kettle
WO2012005519A2 (en) Method for polymerizing alpha-olefins with utilizing three-phase system, using three-phase fluidized-bed reactor
US6403729B1 (en) Process for heterophase reactions in a liquid or supercritical dispersion medium
TWI782337B (en) Continuous stirred tank reactor for aldol condensation reaction
RU196107U1 (en) Hydroxylamine Sulfate Reactor
CN214051628U (en) Hydrogenation reaction kettle capable of automatically calculating hydrogen consumption
Leng et al. Industrial mixing technology
Karthik et al. Enabling Process Innovations via Mastering Multiphase Flows: Gas–Liquid and Gas–Liquid–Solid Processes
CN110302688A (en) Material dissolution device and method
CN211886852U (en) Continuous production equipment for free radical polymerization
CN217450144U (en) Gas-liquid continuous reaction device
CN220835474U (en) Two-stage oximation device

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant