CN208727464U - A kind of circuit reaction system for gas-liquid continuous production - Google Patents

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

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Publication number
CN208727464U
CN208727464U CN201821400819.7U CN201821400819U CN208727464U CN 208727464 U CN208727464 U CN 208727464U CN 201821400819 U CN201821400819 U CN 201821400819U CN 208727464 U CN208727464 U CN 208727464U
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gas
reaction
connect
kettle
circuit
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丁龙
申志刚
张守兵
韩永志
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Weihai Xinyuan Chemical Machinery Co Ltd
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Weihai Xinyuan Chemical Machinery Co Ltd
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Abstract

The utility model relates to a kind of circuit reaction systems for gas-liquid continuous production, wherein batching kettle is connect with measuring tank, measuring tank is connect with circuit reaction mechanism, circuit reaction mechanism is connect with flash vaporization kettle, the gas outlet at the top of flash vaporization kettle is connect through distiller condenser with receiving tank, and the waste liquid outlet of flash vaporization kettle bottom is connect with buffer tank;Circuit reaction mechanism in the utility model includes the N grades of loop reactors being sequentially connected in series, loop reactor includes the venturi reactor at autoclave and top, primary circuit reactor is connect into material liquid with measuring tank, N grades of loop reactors connect out finished fluid with flash vaporization kettle, reaction solution is introduced into next stage loop reactor by upper level loop reactor through overflow pipe, loop reactors at different levels connect with external heat exchanger exchange heat to the material liquid in kettle respectively, mass tranfer coefficient inside the reaction system of utility model is high, reaction efficiency is high, reaction time is short, generally realize the continuous production of gas liquid reaction.

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 kind of circuit reaction system for gas-liquid continuous production, it is characterised in that: 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, measuring tank with The connection of circuit reaction mechanism, circuit reaction mechanism connect with flash vaporization kettle, the gas outlet at the top of flash vaporization kettle through distiller condenser and Receiving tank connection, the waste liquid outlet of flash vaporization kettle bottom are connect with buffer tank;
The circuit reaction mechanism includes the N grades of loop reactors being sequentially connected in series, wherein N >=1, the loop reactor packet Autoclave is included, the inside of autoclave is equipped with reaction chamber, is equipped with venturi reactor, institute at the top of autoclave The venturi reactor stated includes Venturi tube, injection pipe and gas chamber, and the injection pipe protrudes into gas chamber from the top of gas chamber, And be connected in gas chamber with Venturi tube cooperation, the Venturi tube includes entrance, contraction section, venturi mixing section and diffusion Section, the inlet of injection pipe upper end stay in outside gas chamber, and the nozzle of injection pipe lower end protrudes into Venturi tube and is located at through entrance At the upper edge of venturi mixing section, gas entrainment channel is surrounded between the outer wall of injection pipe and the inner wall of contraction section;The side of gas chamber Equipped with gas circulation line, and the gas circulation line is connected to autoclave top gas phase space, venturi reaction Installing port at the top of outer wall and autoclave of the device through gas chamber bottom is tightly connected, and the diffuser of Venturi tube lower end is stretched downwards Enter in reaction chamber, the air inlet flowed into for reaction gas is equipped at the top of autoclave, the side of autoclave is equipped with overflow Mouthful, 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;Level-one Loop 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 level circuit is anti- Answer device that reaction solution is introduced into next stage loop reactor through overflow pipe, loop reactors at different levels respectively with external heat exchanger Connection exchanges heat to the material liquid in kettle, wherein the inlet of loop reactor injection pipe upper end and corresponding external heat exchanger Liquid outlet connection.
2. a kind of circuit reaction system for gas-liquid continuous production according to claim 1, it is characterised in that: described Loop reactor be equipped with pressure detecting system and system for detecting temperature.
3. a kind of circuit reaction system for gas-liquid continuous production described in any claim according to claim 1 or in 2 System, it is characterised in that: be equipped with the sampling for detecting finished fluid qualification rate between most end level-one loop reactor and flash vaporization kettle and examine Survey mechanism.
4. a kind of circuit reaction system for gas-liquid continuous production described in any claim according to claim 1 or in 2 System, it is characterised in that: the buffer tank is connect with batching kettle.
5. a kind of circuit reaction system for gas-liquid continuous production according to claim 4, it is characterised in that: described Batching kettle and measuring tank between by dosing pump connect, between the measuring tank and circuit reaction mechanism by metering pump company It connects, caching pump connection, circuits at different levels is passed through by flash distillation pump connection, buffer tank and batching kettle between the flash vaporization kettle and buffer tank Material liquid in reactor is sent into corresponding external heat exchanger through circulating pump pressurization.
CN201821400819.7U 2018-08-29 2018-08-29 A kind of circuit reaction system for gas-liquid continuous production Active CN208727464U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110586000A (en) * 2019-09-30 2019-12-20 中国科学院上海应用物理研究所 Closed semi-continuous gas-liquid reaction system and method
CN114315612A (en) * 2021-12-27 2022-04-12 万华化学集团股份有限公司 Process for continuously producing isopropanolamine

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110586000A (en) * 2019-09-30 2019-12-20 中国科学院上海应用物理研究所 Closed semi-continuous gas-liquid reaction system and method
CN110586000B (en) * 2019-09-30 2021-11-12 中国科学院上海应用物理研究所 Closed semi-continuous gas-liquid reaction system and method
CN114315612A (en) * 2021-12-27 2022-04-12 万华化学集团股份有限公司 Process for continuously producing isopropanolamine
CN114315612B (en) * 2021-12-27 2024-02-02 万华化学集团股份有限公司 Process for continuously producing isopropanolamine

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PE01 Entry into force of the registration of the contract for pledge of patent right

Denomination of utility model: A loop reaction system for gas liquid continuous production

Effective date of registration: 20200918

Granted publication date: 20190412

Pledgee: Bank of China Limited Weihai Branch

Pledgor: WEIHAI XINYUAN CHEMICAL MACHINERY Co.,Ltd.

Registration number: Y2020980006219