CN208727464U - A loop reaction system for gas-liquid continuous production - Google Patents

Abstract

The utility model relates to a loop reaction system for gas-liquid continuous production, wherein a batching kettle is connected with a measuring tank, the measuring tank is connected with a loop reaction mechanism, the loop reaction mechanism is connected with a flash tank, and an outlet from the top of the flash tank is connected The gas port is connected with the receiving tank through the distillation condenser, and the waste liquid outlet at the bottom of the flash tank is connected with the buffer tank; the loop reaction mechanism in the utility model includes N-stage loop reactors connected in series in sequence, and the loop reactor includes a high-pressure reactor and a top The first-stage loop reactor is connected with the metering tank to enter the raw material liquid, the N-stage loop reactor is connected with the flash tank and the finished liquid is connected, and the upper-stage loop reactor introduces the reaction liquid into the next stage through the overflow pipeline. In the loop reactor, the loop reactors at all levels are respectively connected with external heat exchangers to exchange heat with the raw material liquid in the kettle. The reaction system of the utility model has high mass transfer coefficient, high reaction efficiency, and short reaction time. The continuous production of gas-liquid reaction is realized.

Description

A kind of circuit reaction system for gas-liquid continuous production

Technical field

The invention belongs to chemical production technical fields, and in particular to a kind of cost of investment is low, high conversion rate, using safe Circuit reaction system for gas-liquid continuous production.

Background technique

More mature high-effect reaction is circuit reaction in the gentle liquid-solid reaction of gas liquid reaction.Currently, external return Road reactor comparative maturity, is widely used in hydrogenation, oxidation reaction, alkylation, alkoxylate, amination, carbonylation, chlorine During the reaction process such as change.Since air-liquid adheres to different states of matters separately in gas liquid reaction system, in liquid phase reaction process, Component in gas phase, which has to enter into come into full contact with just to can be carried out with it in liquid phase, reacts, but gas and liquid in actual mechanical process Face contact is simultaneously unstable, and reaction rate is slow, therefore gas liquid reaction is required using dedicated gas liquid reaction kettle and corresponding machine Structure cooperatively forms special gas liquid reaction system and could effectively carry out.But due to gas liquid reaction to object be in contact degree require it is high, Reaction rate is slow, therefore current gas liquid reaction system can be only done intermittent reaction, and so reaction greatly reduces production Efficiency.

Traditional gas liquid reaction system capital equipment is autoclave stirred reactor, it is made of container and agitating device, container Middle setting coil pipe and collet are to meet the preheating of material and react the requirement of cooling.But this reaction system has the disadvantage in that 1, since system is there are mechanical stirring device, the ratio of height to diameter of reaction kettle is restricted, and increases equipment cost, and need in progress Because being influenced by the structures such as agitating device and internal coil baffle when portion is cleaned, rinse difficult；2, autoclave is stirred to react in system Device is because gas-liquid contact is insufficient, and mass tranfer coefficient is low to cause reaction efficiency low, and the reaction time is long；3, autoclave stirring is anti-in system Coil pipe and collet receptor size in device is answered to limit, exchange capability of heat is limited；4, in system autoclave stirred reactor from laboratory Industrial amplification process among to plant produced is considerably complicated and difficult；5, autoclave stirred reactor majority is used for interval in system And Semi-batch reaction, Yao Shixian continuous production difficulty are big.

Summary of the invention

The utility model provides a kind of circuit reaction system for gas-liquid continuous production, the reaction of the utility model System structure is reasonable, maintenance is convenient, and the mass tranfer coefficient inside loop reactor is high, and reaction efficiency is high, and the reaction time is short, generally The continuous production of gas liquid reaction is realized, relatively interval and Semi-batch reaction substantially increase production efficiency.

In order to realize above-mentioned technical goal, the utility model uses following technical scheme:

It is a kind of for gas-liquid continuous production circuit reaction system, including batching kettle, measuring tank, circuit reaction mechanism, External heat exchanger, flash vaporization kettle, receiving tank and buffer tank, the batching kettle are connect with measuring tank, and measuring tank is reacted with circuit Mechanism connection, circuit reaction mechanism are connect with flash vaporization kettle, and the gas outlet at the top of flash vaporization kettle connects through distiller condenser and receiving tank It connects, the waste liquid outlet of flash vaporization kettle bottom is connect with buffer tank；

The circuit reaction mechanism includes the N grades of loop reactors being sequentially connected in series, wherein N >=1, the circuit reaction Device includes autoclave, and the inside of autoclave is equipped with reaction chamber, and venturi reaction is equipped at the top of autoclave Device, the venturi reactor include Venturi tube, injection pipe and gas chamber, and the injection pipe protrudes into gas from the top of gas chamber Interior, and be connected in gas chamber with Venturi tube cooperation, the Venturi tube includes entrance, contraction section, venturi mixing section And diffuser, the inlet of injection pipe upper end stay in outside gas chamber, the nozzle of injection pipe lower end protrudes into Venturi tube through entrance And it is located at the upper at of venturi mixing section, gas entrainment channel is surrounded between the outer wall of injection pipe and the inner wall of contraction section；Gas chamber Side be equipped with gas circulation line, and the gas circulation line is connected to autoclave top gas phase space, literary mound In installing port at the top of outer wall and autoclave of the reactor through gas chamber bottom be tightly connected, the diffuser of Venturi tube lower end It extends downwardly into reaction chamber, the air inlet flowed into for reaction gas is equipped at the top of autoclave, the side of autoclave is set There is overflow port, overflow port is connected to overflow pipe, and the opening of Venturi tube diffuser most lower edge is higher than the position where overflow port It sets；Primary circuit reactor is connect into material liquid with measuring tank, and N grades of loop reactors connect out finished fluid with flash vaporization kettle, and upper one Grade loop reactor reaction solution is introduced into next stage loop reactor through overflow pipe, loop reactors at different levels respectively with it is external Formula heat exchanger connection exchange heat to the material liquid in kettle, wherein the inlet of loop reactor injection pipe upper end with accordingly it is external The liquid outlet of formula heat exchanger connects.

Through the above technical solutions, the circuit that the utility model provides a set of achievable gas liquid reaction continuous production is anti- Answer system, when this reaction system works, raw material initially enters batching kettle, is mixed to form raw material with catalyst etc. in batching kettle Then liquid is conveyed and is stored in measuring tank, material liquid reacts machine by being transported to circuit from measuring tank when starting reaction In structure, what the loop reactor that the circuit reaction mechanism of the utility model is sequentially connected in series by N grades formed, it is reacted in upper circuit While reacting progress in device, the semi-finished product for reacting part can be acted on by overflow and are sent into junior's loop reactor, progress Identical reaction is successively transmitted until the loop reactor of most end level-one is sent into semi-finished product overflow in part.According to requiring when use Product purity difference can increase or decrease concatenated loop reactor, and the series connection of loop reactors at different levels ensure that gas liquid reaction Abundant progress, realize the balance of product quality and efficiency.The finished fluid finally come out from most final stage loop reactor enters Flash vaporization kettle.It controls certain temperature and pressure and distiller condenser is entered by flash distillation by product, connect by being condensed into liquid inflow Closed cans is stored.Flashing remaining liquid delivers into surge tank simultaneously, keeps in surge tank.

Wherein loop reactor is the core of this reaction system, and the loop reactor of this reaction system mainly has anti-by high pressure Kettle, venturi reactor, external heat exchanger composition are answered, principle is that volume is mutually gone to inhale other phases using flow at high speed, makes each phase Close contact, then evenly dispersed in reaction kettle or suspension, and complete to react.Venturi reactor at the top of loop reactor It is a kind of high performance Liqiud-gas mixing device.It is made of Venturi tube, injection pipe, gas chamber and gas circulation line.Match in advance After the material liquid set enters autoclave, and it is transported into heat exchange in external heat exchanger, gone out from external heat exchanger The material liquid come enters venturi reactor, and the injection stream of high speed is formed by the nozzle of venturi reactor, and injection stream is passed through When gas chamber, gas indoor gas is carried channel secretly by gas and is taken away by liquid, forms negative pressure, under pressure reaction chamber top gas Reaction gas in phase space is again introduced into gas chamber by gas circulation line and forms gas circulation.Liquid carries gas and impacts Energy consumption is formed on tube wall, creates strong mixing vibration area herein, in this each region, fierce turbulent flow makes foam Good spreading.Impact the unusual minor diameter of gas bubble generated between 30 ~ 70 μm, and simultaneously gas liquid ratio reached 0.5 ~ More than 2.0.So this is the ideal initially main dispersal device that loop reactor carries out gas liquid reaction, reach initial Most important mass transfer function, then, gas-fluid two-phase mixture are injected into the liquid storage in loop reactor.It is anti-by venturi The two-phase mixture for answering device spouting, which is ejected into loop reactor, causes second of fierce mixing, has realized again Mass transfer performance.Current mass transfer is completed by the minute bubbles in reaction kettle, and the diameter of minute bubbles is between 0.2 ~ 0.7mm, this bubble Diameter is greater than the bubble in venturi injection gas, this is because bubble has occurred in the minute bubbles in venturi-type eductors at this time Polymerization.

It is worth noting that, can be connect respectively with external heat exchanger pair in the utility model using loop reactors at different levels Material liquid in kettle exchanges heat, and the material liquid in the reaction kettle of circuit is pressurized to be sent into external heat exchanger, external heat exchanger It, can be according to chemical reaction heat transfer requirements system instead of collet, coil pipe or the built-in heat exchanger of traditional autoclave stirred reactor Make, compared with previous structure, size is not limited by autoclave volume.External heat exchanger can full heat exchange area Work, or even in the case where reducing working volume (such as semi-batch operation or half kettle material reaction).

Further, loop reactor described in the utility model is equipped with pressure detecting system and system for detecting temperature.

Further, it is equipped between the utility model most end level-one loop reactor and flash vaporization kettle for detecting finished fluid qualification The sample detection mechanism of rate.

Further, buffer tank described in the utility model is connect with batching kettle

Through the above technical solutions, buffer tank is connect by the reaction system of the utility model with batching kettle, it can be to buffer tank It is sent into batching kettle after the amount of the liquid of middle collection requirement to be achieved and carries out preparation raw material liquid again, so makes having arrived sufficiently for raw material The utilization of circulation, while also saving the use of solvent catalyst.

Further, it is connected between batching kettle and measuring tank described in the utility model by dosing pump, the measuring tank It is connect between the reaction mechanism of circuit by metering pump, passes through flash distillation pump connection, buffer tank between the flash vaporization kettle and buffer tank Pass through caching pump connection with batching kettle；Material liquid in loop reactors at different levels is sent into corresponding external through circulating pump pressurization and is changed In hot device.

Through the above technical solutions, the utility model conveys object using force (forcing) pump or metering pump etc. between each reaction vessel Material ensure that the accuracy of reaction and going on smoothly for reaction, and especially the material liquid in loop reactors at different levels is by following Ring pump pressurization is sent into external heat exchanger, and the circulating pump of the utility model can convey high air content (volume ratio reaches 30%) High solids (volume ratio reaches 15%) reaction liquid, circulating pump continue working while alloing gas bubble with reaction solution Body enters circulation loop, and dynamical circulating pump, which can directly transport gas-liquid two-phase and a small amount of solid catalyst, carries out circuit Circulation, enhances gas-liquid mixed effect and void fraction, enhances mass-transfer efficiency, and making gas-liquid, persistently mixing passes in entire circuit Matter, reaction effect have significant enhancing than conventional circuit reactor.

The utility model beneficial effect is: in the reaction system of 1. the utility model, in loop reactors at different levels not There are mechanical stirring device, the ratio of height to diameter of reaction kettle is unrestricted, therefore can increase ratio of height to diameter reduction equipment cost, especially high The circuit reaction kettle equipment cost reduction of pressure is more obvious, and inside does not have the structures such as coil pipe, baffle in the reaction kettle of circuit, into It is rinsed simply, thoroughly when row internal washing.2. in the reaction system of the utility model, the mass tranfer coefficient of loop reactor is high, instead It answers high-efficient, needs the reaction time short.3. in the reaction system of the utility model, the technique heat exchange of circuit reaction kettle can lead to External heat exchanger realization is crossed, not by reaction vessel effect of structural dimension, can accomplish full heat exchange area work.4. practical new In the reaction system of type, chemical reaction process is only being controlled by kinetics in loop reactor, from laboratory to factory It produces in intermediate industrial amplification process and greatly reduces difficulty.5. the reaction system of the utility model realizes continuous metaplasia It produces, relatively interval and Semi-batch reaction greatly improve efficiency.

Detailed description of the invention

Fig. 1 is the overall flow figure of the utility model reaction system.

Fig. 2 is the structural schematic diagram of the utility model loop reactor.

Specific embodiment

The invention will be further described with reference to the accompanying drawing.

As shown in Figure 1, a kind of circuit reaction system for gas-liquid continuous production, including batching kettle 1-1, measuring tank 2- 1, circuit reaction mechanism, external heat exchanger, flash vaporization kettle 4-1, receiving tank 5-1 and buffer tank 6-1, the batching kettle 1-1 with It is connected between measuring tank 2-1 by dosing pump 1-2, is connected between measuring tank 2-1 and circuit reaction mechanism by metering pump 2-2, Circuit reaction mechanism is connect with flash vaporization kettle 4-1, and the gas outlet at the top of flash vaporization kettle 4-1 is through distiller condenser 7-1 and receiving tank 5-1 Connection will flash remaining liquid by flash distillation pump 4-2 connection between the waste liquid outlet and buffer tank 6-1 of the bottom flash vaporization kettle 4-1 It is conveyed into buffer tank 6-1 and keeps in, buffer tank 6-1 is also connect with batching kettle 1-1 by caching pump 6-2 simultaneously, in buffer tank 6-1 Liquid requirement to be achieved amount after, be fed again into batching kettle 1-1 and carry out preparation raw material liquid again.

The circuit reaction mechanism in the present embodiment includes loop reactor 3-1,3-2 and 3- that three-level is sequentially connected in series 3, as shown in Fig. 2, loop reactor 3-1 includes autoclave 3-1a, autoclave 3- by taking loop reactor 3-1 as an example 1a is equipped with pressure detecting system 3-1m and system for detecting temperature 3-1n.The inside of autoclave is equipped with reaction chamber, and high pressure is anti- It answers and venturi reactor 3-1b is installed at the top of kettle, the venturi reactor includes Venturi tube, injection pipe and gas chamber, The injection pipe is protruded into from the top of gas chamber in gas chamber 3-1c, and is connected in gas chamber with Venturi tube cooperation, the text Venturi includes entrance A, contraction section B, venturi mixing section C and diffuser D, and the inlet 3-1d of injection pipe upper end stays in gas chamber Outside, the nozzle 3-1e of injection pipe lower end is protruded into through entrance A in Venturi tube and positioned at the upper at of venturi mixing section C, injection Gas entrainment channel is surrounded between the outer wall of pipe and the inner wall of contraction section B；The side of gas chamber is equipped with gas circulation line 3-1f, and The gas circulation line is connected to autoclave top gas phase space, outer wall of the venturi reactor through gas chamber bottom with Installing port at the top of autoclave is tightly connected, and the diffuser D of Venturi tube lower end is extended downwardly into reaction chamber, reaction under high pressure Kettle top portion is equipped with the air inlet that flows into for reaction gas, and the side of autoclave is equipped with overflow port 3-1h, overflow port 3-1h and Overflow pipe connection, the opening of Venturi tube diffuser most lower edge are higher than the position where overflow port；Primary circuit reactor 3-1 is connect into material liquid with measuring tank 2-1, and three-level loop reactor 3-3 connect out finished fluid with flash vaporization kettle 4-1, and three-level is returned The sample detection mechanism 8-1 for detecting finished fluid qualification rate is equipped between road reactor 3-3 and flash vaporization kettle 4-1, such as Fig. 1 institute Show, reaction solution is introduced into next stage loop reactor by upper level loop reactor through overflow pipe, and the position of overflow port is under The liquid level difference of grade circuit reaction kettle, adjusts and controls by calculating when being applied particularly to a certain gas liquid reaction.At different levels times Road reactor is pressurizeed in the corresponding external heat exchanger of 3-1B, 3-2B and 3-3B feeding by circulating pump respectively and external heat exchanger Device 3-1A, 3-2A and 3-3A, which are connected, exchanges heat to the material liquid in kettle, wherein the inlet of loop reactor injection pipe upper end It is connect with the liquid outlet of corresponding external heat exchanger.

Claims (5)

1. a loop reaction system for gas-liquid continuous production is characterized in that: comprising batching still, metering tank, loop reaction mechanism, external heat exchanger, flash still, receiving tank and buffer tank, the described The batching kettle is connected with the metering tank, the metering tank is connected with the loop reaction mechanism, the loop reaction mechanism is connected with the flash tank, the air outlet at the top of the flash tank is connected with the receiving tank through the distillation condenser, and the waste liquid outlet at the bottom of the flash tank is connected with the receiving tank. cache tank connection; The loop reaction mechanism includes N-stage loop reactors connected in series in sequence, wherein N≥1, the loop reactor includes a high-pressure reactor, a reaction chamber is arranged inside the high-pressure reactor, and a venturi is installed on the top of the high-pressure reactor. The venturi reactor includes a venturi tube, a jet tube and a gas chamber, and the jet tube extends into the gas chamber from the top of the gas chamber, and communicates with the venturi tube in the gas chamber. The Venturi tube includes an inlet section, a constriction section, a throat mixing section and a diffusion section. The liquid inlet at the upper end of the jet tube is left outside the gas chamber, and the nozzle at the lower end of the jet tube extends into the Venturi tube through the inlet section and is located in the throat mixing section. At the upper edge of the injection pipe, a gas entrainment channel is formed between the outer wall of the injection pipe and the inner wall of the constricted section; the side of the gas chamber is provided with a gas circulation pipeline, and the gas circulation pipeline is communicated with the gas phase space at the top of the high pressure reactor, The venturi reactor is sealedly connected with the installation port on the top of the high pressure reactor through the outer wall of the bottom of the gas chamber, the diffusion section at the lower end of the venturi tube extends downward into the reaction chamber, and the top of the high pressure reactor is provided with an air inlet for the inflow of the reaction gas , there is an overflow port on one side of the high pressure reactor, the overflow port is connected with the overflow pipe, and the opening of the bottom edge of the diffusion section of the venturi tube is higher than the position of the overflow port; the primary loop reactor is connected with the metering tank It is connected to the raw material liquid, the N-stage loop reactor and the flash tank are connected to the finished liquid, and the upper-stage loop reactor introduces the reaction liquid into the next-stage loop reactor through the overflow pipeline. The heat exchanger is connected to exchange heat with the raw material liquid in the kettle, wherein the liquid inlet at the upper end of the injection pipe of the loop reactor is connected with the liquid outlet of the corresponding external heat exchanger. 2 . The loop reaction system for gas-liquid continuous production according to claim 1 , wherein the loop reactor is provided with a pressure detection system and a temperature detection system. 3 . 3. a kind of loop reaction system for gas-liquid continuous production according to any one of claim 1 or 2, is characterized in that: between the last stage loop reactor and the flash tank, there is a Sampling and testing organization for testing the qualified rate of finished liquid. 4. A loop reaction system for gas-liquid continuous production according to any one of claims 1 or 2, wherein the buffer tank is connected to the batching kettle. 5. A kind of loop reaction system for gas-liquid continuous production according to claim 4, is characterized in that: described batching kettle and measuring tank are connected by batching pump, and described measuring tank reacts with loop The mechanisms are connected by a metering pump, the flash tank and the buffer tank are connected by a flash pump, the buffer tank and the batching kettle are connected by a buffer pump, and the raw material liquid in the loop reactors at all levels is pressurized and sent to the circulating pump. in the corresponding external heat exchanger.