CN205368184U - Adopt reaction system of synthetic adipic acid of loop reactor - Google Patents
Adopt reaction system of synthetic adipic acid of loop reactor Download PDFInfo
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- CN205368184U CN205368184U CN201620085037.3U CN201620085037U CN205368184U CN 205368184 U CN205368184 U CN 205368184U CN 201620085037 U CN201620085037 U CN 201620085037U CN 205368184 U CN205368184 U CN 205368184U
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Abstract
The utility model relates to an adopt reaction system of synthetic adipic acid of loop reactor, this loop reactor mainly includes the retort, the circulating pump, external heat exchanger and venturi sprayer, be provided with venturi sprayer 4 in the retort, the venturi sprayer is under the narrow width's splayed setting, the jet setting of venturi sprayer is below the liquid level, systemic circulation through the material, utilize the venturi sprayer to form the negative pressure, the oxide isolation inhale and with the reaction material intensive mixing, the dispersion, and spout in the retort, the bottom of retort 1 is connected with the input of circulating pump, and the output of circulating pump is connected with the top of retort through external heat exchanger, is equipped with refrigerant import, refrigerant outlet and steam inlet on the external heat exchanger, and condenser discharge tail gas is passed through to the retort, the retort is connected with the import of protection gas, oxygen mouth, feed inlet and discharge gate.
Description
Technical field
This utility model belongs to chemical industry equipment and method, particularly relates to a kind of response system adopting loop reactor synthesizing adipic acid.
Background technology
Adipic acid is the important intermediate of nylon66 fiber and polyurethane.Producing adipic acid at present and be generally adopted two step nitrate methods productions, the first step adopts hexamethylene air oxidation, production Ketohexamethylene and cyclohexanol mixture (being called for short KA oil), second step employing nitric acid oxidation, generates adipic acid, but there is N in cost height and tail gasxThe severe contamination problem of O gas.
Report according to domestic and international open source literature, there are the process routes that metallic compound is catalyst oxidation step oxidizing ethyle alkyl adipic acid such as use ferrum, manganese, cobalt, chromium, but owing to oxygen participates in reaction, there is the possibility of blast, heavy industrialization application that so far there are no, the high efficiency dispersion of simultaneous reactions gas phase has no and identical structure of the present utility model so far.
The safety interlocking how improved during oxide isolation particularly spreads completely with oxygen and reacts in reaction system controls to be an engineering roadblock.Such as Zhejiang Shu Yang Chemical Co., Ltd. have developed a kind of technique adopting pipe reaction One-step production adipic acid.This technique produced problem has: 1. Matter Transfer problem, and owing to pipeline adopts parallel way, uneven phenomenon occurs in the sample introduction of many pipelines, causes that the reaction of each pipeline is uneven, and reaction is difficult to control to；2., owing to winter temperature is relatively low, the temperature of pipeline is also relatively low, and adipic acid easily precipitates out at low temperatures, it is easy to cause line clogging；3. owing to reaction is gas liquid reaction, gas inlet pipe road reacts with liquid, need certain time of staying and enough contacts area, and owing to the diffusion velocity of gas/liquid two is different, the catalytic action of catalyst and the Absorption of liquid phase can only being relied in pipeline to absorb gas react, reaction efficiency is low, and unreacted oxygen easily gathers on reactor top, reach explosion limit, form potential safety hazard.
Owing to response system belongs to core process in adipic acid production process, the factors such as the exploitation of its reactor, improvement, perfect production capacity, stability and the safety being important to pay close attention to, mostly adopt the reactor of still reaction or other forms, all have that mass-transfer efficiency is low, temperature control is difficult or the shortcoming such as easy blast.
Utility model content
The purpose of this utility model is in that the deficiency overcoming prior art to exist, and provides a kind of response system adopting loop reactor synthesizing adipic acid.
The purpose of this utility model completes by following technical solution.The response system of this employing loop reactor synthesizing adipic acid, this loop reactor mainly includes retort, circulating pump, outer heat exchanger and venturi-type eductors, retort is provided with venturi-type eductors 4, the splayed that venturi-type eductors is up-narrow and down-wide is arranged, the jet of venturi-type eductors is arranged on below liquid level, by the systemic circulation of material, venturi-type eductors is utilized to form negative pressure, oxide isolation sucked and is sufficiently mixed with reaction mass, disperses, and being injected in retort；The bottom of retort 1 is connected with the input of circulating pump, circulation delivery side of pump is connected with the top of retort by outer heat exchanger, outer heat exchanger is provided with coolant import, refrigerant exit and steam inlet, and retort discharges tail gas by condenser；Retort is connected with protection gas import, oxygen port, charging aperture and discharging opening.
The beneficial effects of the utility model are: this utility model make use of venturi-type eductors as the feature of high-performance air and liquid mixer, make oxygen fully dispersed, and the oxygen having neither part nor lot in reaction is re-dispersed in reactant liquor, mass-transfer efficiency is greatly improved, improve response speed, reaction controlling is more prone to, and autoclave need not arrange baffle plate and be equipped with stirring, it is static device, it is provided with gas phase oxygen content automatically to detect and a series of safety measures such as chain regulation and control system and solidifying exhaust emissions simultaneously, improve the safety of device of knowing clearly, it it is a kind of most suitable reactor.
Accompanying drawing explanation
Fig. 1 is structural representation of the present utility model.
Detailed description of the invention
Below in conjunction with accompanying drawing, this utility model done detailed introduction:
As shown in Figure 1, the response system of this employing loop reactor synthesizing adipic acid, this loop reactor mainly includes retort 1, circulating pump 2, outer heat exchanger 3 and venturi-type eductors 4, retort 1 is provided with venturi-type eductors 4, the splayed that venturi-type eductors 4 is up-narrow and down-wide is arranged, the jet of venturi-type eductors 4 is arranged on below liquid level, by the systemic circulation of material, venturi-type eductors is utilized to form negative pressure, oxide isolation sucked and is sufficiently mixed with reaction mass, disperses, and being injected in retort 1；This negative pressure can also unreacted for high-pressure reactor inner top oxygen and the N shielded2Or CO2Deng in noble gas again sucting reaction medium, react safely under a series of security interlocking protections control.The bottom of retort 1 is connected with the input of circulating pump 2, the outfan of circulating pump 2 is connected by the top of outer heat exchanger 3 with retort 1, outer heat exchanger 3 is provided with coolant import 3-1, refrigerant exit 3-2 and steam inlet 3-3, and retort 1 discharges tail gas by condenser 5；Retort 1 is connected with protection gas import 6, oxygen port 7, charging aperture 8 and discharging opening 9.
This reaction unit is equally applicable to a class reaction of the oxidation of the gaseous oxidant such as hexamethylene, Ketohexamethylene, Hexalin, cyclohexene, gas-liquid two-phase reaction.
The method is to adopt loop reactor, first by hexamethylene, KA oil or both mixture, catalyst addition loop reactor, start to play circulation with circulating pump, after being preheated to 80-180 DEG C, oxygen is passed into continuously from air inlet, the negative pressure utilizing Matter Transfer to be formed at the venturi-type eductors mouth of pipe, makes oxygen uniformly pass into and fine dispersion, controls reaction temperature at 120～200 DEG C with coolant in course of reaction.The intake of hexamethylene and oxygen continuous uniform in proportion passes into, and finished product is continuously withdrawn from pipeline opening, enters rear portion separation, crystallization procedure, and unreacted hexamethylene returns head tank.In course of reaction, in retort, pass into N continuously2Or CO2Protect Deng noble gas, control gas phase oxygen content in safety range, control reaction temperature by coolant.
Adopt loop reactor as the dominant response device of synthesizing adipic acid; comprise several systems such as the inert gas protection system such as charging system, nitrogen, temperature control system, control pressurer system in proportion; automatic control can realizing the operation of device stable and continuous, the advantage of this device is in that: the venturi-type eductors (replacing gas distributor or other gas spreading systems) in loop reactor is a kind of high performance Liqiud-gas mixing device.It is made up of four parts, turbulent flow nozzle, air chamber, and gas circulation line and pipe form.Pumping liquid is formed by nozzle and quickly sprays stream to take gas indoor gas spouting, and hydraulic shock forms energy expenditure to tube wall.This creating strong mixing vibrations district, in this each region, fierce turbulent flow makes the good spreading of foam.The gas foam that impact produces little (30～70 μm) very, and gas liquid ratio has reached more than 0.5～2.0 simultaneously.So the desirable initial main dispersal device of this to be loop reactor carry out gas liquid reaction, reach initial topmost mass transfer function.And this device nozzle is positioned at below liquid level, the oxygen-containing material ejected has impacted with the existing material in autoclave, serves the effect of secondary mixing.
Due to the negative pressure that ejector porch is formed, it is also possible to unreacted for autoclave top gas weight sucting reaction medium, carry out secondary response.At reactor upper gaseous phase position, under the noble gas control oxygen protections such as noble gas, better ensure that safety.Fixed gas discharge and the cold bright recovery system of raw material it is provided with, it is ensured that proceeding smoothly of reaction in reactor upper end.
Autoclave need not arrange baffle plate, compare autoclave stirred reactor, it generally has a big ratio of height to diameter, the two-phase mixture that venturi-type eductors is spouting be ejected in autoclave and cause the fierce mixing of second time, the mass transfer realized again performance.
It is can make according to chemical reaction heat transfer requirements that external heat exchanger (replaces coil pipe or built-in heat exchanger), and compared with conventional built-in heat exchanger, its size is not by the volumetric constraint of reaction vessel (reactor).External heat exchanger can work by heat exchange area entirely, even at when reducing working volume, for instance semi-batch operation or half still material reaction.
Owing to it has These characteristics, it is possible to make oxidant and hexamethylene, KA wet goods raw material effectively disperse；Reaction temperature is effectively shifted and is controlled；Unreacted oxygen can reaction system secondary response in time, it is ensured that the safety of reaction.
Embodiment 1
By 5000g hexamethylene and 900g solvent (acetic acid), and add catalyst with being pumped into loop reactor, it is ensured that ON cycle pump also circulates, and opens heat exchanger steam valve, start to be heated material to reaction temperature.Passing into inert gas shielding in reactor, the pressure maintained in reaction by still top on-condensible gas drain valve is 1.0MPa, and passes into oxygen in gas feed, starts reaction.Controlling reaction temperature with coolant in course of reaction is 150 DEG C.Continuously raw material is sent into loop reactor according to the speed of 100ml/min continuously, it is ensured that material is 25min in the time of staying of reactor.The analysis of gas chromatogram and liquid chromatograph is it is shown that a conversion ratio of hexamethylene is 8%, and the selective conversion rate of end product adipic acid is 85%.
Embodiment 2
By 5000g hexamethylene and catalyst with being pumped into loop reactor, it is ensured that ON cycle pump also circulates, and opens heat exchanger steam valve and fixed gas drain valve, starts to be heated material to reaction temperature.Pass into inert gas shielding in reactor, and pass into oxygen in gas feed, start reaction.Controlling reaction temperature with coolant in course of reaction is 160 DEG C.Continuously raw material is sent into loop reactor according to the speed of 100ml/min continuously, it is ensured that material is 18min in the time of staying of reactor.The analysis of gas chromatogram and liquid chromatograph is it is shown that a conversion ratio of hexamethylene is 9%, and the selective conversion rate of end product adipic acid is 80%.
Embodiment 3
By 5000gKA oil, catalyst and 1000g diluent with being pumped into loop reactor, it is ensured that ON cycle pump also circulates, and opens heat exchanger steam valve and still top fixed gas drain valve, starts to be heated material to reaction temperature.Pass into inert gas shielding in reactor, and pass into air in gas feed, start reaction.Controlling reaction temperature with coolant in course of reaction is 90 DEG C.Continuously raw material is sent into loop reactor according to the speed of 110ml/min continuously, it is ensured that material is 25min in the time of staying of reactor.The analysis of gas chromatogram and liquid chromatograph is it is shown that a conversion ratio of hexamethylene is 4%, and the selective conversion rate of end product adipic acid is 73%.
This utility model is not limited to above-mentioned embodiment, no matter making any change, every employing structural design provided by the utility model on its shape or material are constituted, being all a kind of deformation of the present utility model, being all considered as within this utility model protection domain.
Claims (1)
1. the response system adopting loop reactor synthesizing adipic acid, it is characterized in that: this loop reactor mainly includes retort (1), circulating pump (2), outer heat exchanger (3) and venturi-type eductors (4), retort (1) is provided with venturi-type eductors (4), venturi-type eductors (4) is arranged for up-narrow and down-wide splayed, the jet of venturi-type eductors (4) is arranged on below liquid level, by the systemic circulation of material, venturi-type eductors is utilized to form negative pressure, oxide isolation is sucked and is sufficiently mixed with reaction mass, dispersion, and be injected in retort (1)；The bottom of retort (1) is connected with the input of circulating pump (2), the outfan of circulating pump (2) is connected by the top of outer heat exchanger (3) with retort (1), outer heat exchanger (3) is provided with coolant import (3-1), refrigerant exit (3-2) and steam inlet (3-3), and retort (1) discharges tail gas by condenser (5)；Retort (1) is connected with protection gas import (6), oxygen port (7), charging aperture (8) and discharging opening (9).
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| CN201620085037.3U CN205368184U (en) | 2016-01-28 | 2016-01-28 | Adopt reaction system of synthetic adipic acid of loop reactor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105503568A (en) * | 2016-01-28 | 2016-04-20 | 杭州海虹精细化工有限公司 | Reaction system and method for compounding adipic acid by adopting loop reactor |
| CN112979437A (en) * | 2021-03-05 | 2021-06-18 | 江苏诺盟化工有限公司 | Preparation method of benzaldehyde and special reactor |
-
2016
- 2016-01-28 CN CN201620085037.3U patent/CN205368184U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105503568A (en) * | 2016-01-28 | 2016-04-20 | 杭州海虹精细化工有限公司 | Reaction system and method for compounding adipic acid by adopting loop reactor |
| CN112979437A (en) * | 2021-03-05 | 2021-06-18 | 江苏诺盟化工有限公司 | Preparation method of benzaldehyde and special reactor |
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