CN108993346A - A kind of anion bromination reactor and its application - Google Patents
A kind of anion bromination reactor and its application Download PDFInfo
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- CN108993346A CN108993346A CN201810908011.8A CN201810908011A CN108993346A CN 108993346 A CN108993346 A CN 108993346A CN 201810908011 A CN201810908011 A CN 201810908011A CN 108993346 A CN108993346 A CN 108993346A
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- anion
- bromine
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
- B01J19/088—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
Abstract
The present invention relates to a kind of anion bromination reactor and its application, anion bromination reactor includes voltage offer portion, bromine anion generator and reaction chamber;Make to form corona region in bromine anion generator by voltage offer portion, the bromine anion that bromine vapor generates in bromine anion generator, then bromine anion enters in reaction chamber, completes bromination reaction.The present invention, which has, reduces discharging of waste liquid, reaction temperature is low (room temperature or 100 DEG C or less carry out), the characteristics of reaction is easily realized, and reactor is without not only anticorrosive but also material resistant to high temperature, continuous reaction is realized simultaneously, 90% or more conversion ratio can be reached in a short time, product yield is up to 90% or more.
Description
Technical field
The present invention relates to organic synthesis fields, and in particular to a kind of reactor of anion bromination reaction and its application, more
More particularly to the reactor that will be reacted after bromine vapor negative ionization with organic matter.
Background technique
Many important organic intermediates containing bromo element, synthetic drug are obtained by bromination reaction.Bromination
Reaction is generally divided into two kinds: one is organic matter and reaction of hydrogen bromide, another kind is that organic matter is reacted with bromine simple substance.
Organic matter mainly carries out in a solvent with reacting for hydrogen bromide, and this method generates a large amount of waste liquid and waste material.Have
Machine object is reacted with bromine simple substance, is mostly used and is reacted under high temperature now, but 350 DEG C or more at a temperature of, there is no what materials
Material is resistant to the corrosion of bromine, but also to be resistant to certain pressure.
Summary of the invention
The purpose of the present invention is to provide a kind of anion bromination reactor and its application, anion bromination reaction of the present invention
Bromine can be converted to bromine anion and then participate in bromination reaction by device, which is not necessarily to carry out at high temperature, therefore to material
It is required that it is relatively low, bromination reaction can be realized.Technical solution of the present invention is as follows:
A kind of anion bromination reactor, including voltage offer portion, bromine anion generator and reaction chamber;Bromine anion generator
Including cylindrical shell body, it is close to outer housing inner wall and is equipped with insulation material layer, is close to insulation material layer inner wall and is being equipped with high voltage just
Pole material layer is connected with several spray points on high-voltage anode material layer, and spray point is directed toward outer housing center line, is close to high voltage
Positive electrode material layer inner wall is equipped with insulation liner material layer, and insulation liner material layer is equipped with aperture, and spray point is passed through out of aperture,
High voltage negative electrode material is located on the center line of outer housing, and the both ends of high voltage negative electrode material are fixed with collets, collets
It is connected on outer housing by support frame, the both ends of outer housing inner wall are equipped with dead ring, the internal diameter and insulation liner material of dead ring
The internal diameter of the bed of material is equal, and one end of outer housing is connect by flange with variable diameter conduit, and the other end is connect by flange with reaction chamber,
The other end of variable diameter conduit is bromine vapor entrance;
The input terminal of adjustable variable-pressure device is connect with alternating current 220V in voltage offer portion, the output end of adjustable transformer and rectification
Device connection, the output head anode of rectifier are connect with high-voltage anode material layer, and the negative pole of output end and high voltage of rectifier are negative
The connection of pole material, voltmeter are serially connected in the output end of rectifier, let out non-electricity protector and ammeter is connected on the output end of rectifier
Between anode and high-voltage anode material layer;
It is reaction chamber inside reaction chamber, the top of reaction chamber is end socket, and side wall is equipped with organic matter import and product exit.
Bromine anion generating principle:
When being passed through bromine vapor in bromine anion generator, after electric power starting, is ionized in cathode area and generate free electron, in electric field
It is accelerated under power effect to anode and obtains enough energy, collided with molecular bromine, molecular bromine outer-shell electron is bombarded
Fall, then the free electron and cation fallen by bombardment will continuously emerge in electric field space.The lower freely electricity of part energy
Son is captured during colliding with other molecular bromines by molecular bromine, to form bromine anion.
Further, the material of variable diameter conduit and outer housing is selected from carbon steel, stainless steel, cupro-nickel titanium alloy or monel metal
In any one;The material of the insulation liner material layer is polytetrafluoroethylene (PTFE) or quartz glass;In the abutting outer housing
Insulation material layer and collets any one in ceramics, rubber material or polytetrafluoroethylene (PTFE) of material.The reaction
Any one of the material of chamber in 304 steel alloys, cupro-nickel titanium alloy, monel metal or stainless steel.
Further, the vertical range d of the spray point and high voltage negative electrode material is 20-30mm, this structure can be with
It generates corona but a breakdown cannot be generated.
The invention also includes application of the anion bromination reactor in bromination reaction, specifically: when bromine vapor passes through bromine
Steam inlet enters bromine anion generator;Voltage is risen into 3-10KV by adjustable variable-pressure device, forms one between positive and negative anodes
A powerful electric field will appear larger corona phenomenon at spray point, after bromine vapor passes through variable diameter conduit, so that bromine vapor enters
Positive and negative anodes opposed area, and make bromine vapor in the corona region residence time 0.5-1s of bromine anion generator, it is negative to generate bromine
Ion simultaneously enters in reaction chamber, and bromine anion is mixed with the organic matter from organic matter entrance and reacted, and it is logical to ultimately produce object
Cross product exit outflow;When reaction, bromine anion removes attack carbon atom, and nucleophilic substitution occurs.
Compared with the prior art, the present invention has the following advantages:
The present invention, which has, reduces discharging of waste liquid, and reaction temperature is low (room temperature or 100 DEG C or less carry out), and bromination reaction is safe, instead
The characteristics of should easily realizing, and reactor is without not only anticorrosive but also material resistant to high temperature, while realizing continuous reaction, Ke Yi
Reach 90% or more conversion ratio in short time, product yield is up to 90% or more.
Detailed description of the invention
To be illustrated more clearly that background technique or technical solution of the present invention, below to the prior art or specific embodiment
The attached drawing of middle combined use is briefly described;It should be evident that below in conjunction with the attached drawing side of being only for of specific embodiment
Just understand the embodiment of the present invention, for those of ordinary skill in the art, without creative efforts, may be used also
To obtain other drawings based on these drawings;
Fig. 1 is the structural schematic diagram of anion bromination reactor;
Fig. 2 is the topography of anion bromination reactor.
Symbol description:
1. electricity is let out in outer housing, 2. insulation material layers, 3. spray points, 4. insulation liner material layers, 5. ammeters, 6. voltmeters, 7.
Protector, 8. rectifiers, 9. adjustable variable-pressure devices, 10. bromine vapor entrances, 11. organic matter imports, 12. reaction chambers, 13. end sockets,
14. product exit, 15. collets, 16. dead rings, 17. high-voltage anode material layers, 18. high voltage negative electrode materials, 19. supports
Frame, 20. variable diameter conduits.
Specific embodiment
The invention will now be further described with reference to specific embodiments, the advantages and features of the present invention will be with description and
It is apparent.But examples are merely exemplary, and it is not intended to limit the scope of the present invention in any way.Those skilled in the art answer
It should be appreciated that without departing from the spirit and scope of the invention can details to technical solution of the present invention and form repair
Change or replace, but these modifications and replacement are fallen within the protection scope of the present invention.
A kind of anion bromination reactor of embodiment 1
As illustrated in fig. 1 and 2, reactor includes voltage offer portion, bromine anion generator and reaction chamber;Bromine anion generator packet
Cylindrical shell body 1 is included, is close to 1 inner wall of outer housing and is equipped with insulation material layer 2, is close to 2 inner wall of insulation material layer and is equipped with high voltage
Positive electrode material layer 17 is connected with several spray points 3 on high-voltage anode material layer 17, and spray point 3 is directed toward 1 center line of outer housing,
It is close to 17 inner wall of high-voltage anode material layer and is equipped with insulation liner material layer 4, insulation liner material layer 4 is equipped with aperture, electric discharge
Needle 3 is passed through out of aperture, and high voltage negative electrode material 18 is located on the center line of outer housing 1, the both ends of high voltage negative electrode material 18
Collets 15 are fixed with, collets 15 are connected on outer housing 1 by support frame 19, and the both ends of 1 inner wall of outer housing are equipped with exhausted
The internal diameter of edge ring 16, dead ring 16 is equal with the internal diameter of insulation liner material layer 4, and one end of outer housing 1 passes through flange and variable diameter
Conduit 20 connects, and the other end is connect by flange with reaction chamber, and the other end of variable diameter conduit 20 is bromine vapor entrance 10;
The input terminal of adjustable variable-pressure device 9 is connect with alternating current 220V in voltage offer portion, the output end of adjustable transformer 9 with it is whole
It flows device 8 to connect, the output head anode of rectifier 8 is connect with high-voltage anode material layer 17, the negative pole of output end and height of rectifier 8
Voltage negative electrode material 18 connects, and voltmeter 6 is serially connected in the output end of rectifier 8, let out non-electricity protector 7 and ammeter 5 be connected on it is whole
Between the output head anode and high-voltage anode material layer 17 for flowing device 8;
It is reaction chamber 12 inside reaction chamber, the top of reaction chamber is end socket 13, and side wall is equipped with organic matter import 11 and product goes out
Mouth 14;
The material of the variable diameter conduit and outer housing is stainless steel;The material of insulation liner material layer is quartz glass;Insulation material
The material of the bed of material and collets is ceramics;The material of reaction chamber is 304 steel alloys;The spray point is vertical with high voltage cathode
Distance d is 25mm.
Embodiment 2 prepares bromotrifluoromethane using anion bromination reactor of the present invention
Reactant: bromine, fluoroform, product: bromotrifluoromethane
Bromine is heated to 58.8 DEG C of gasifications, and continues to be heated to 70 DEG C or so, it is logical with the speed speed of 2m/s to control bromine vapor
The bromine vapor entrance for crossing bromine anion generator enters;Opening power supply will be in bromide ion generator by adjustable transformer
The voltage of positive and negative interpolar is in 8KV or so, so that powerful electric field is formed between positive and negative anodes, so that spray point is formed about corona and shows
As;After bromine vapor passes through variable diameter conduit, so that bromine vapor enters positive and negative anodes opposed area, and stop bromine vapor in corona region
Time is 0.5-1s, generates bromine anion and enters in reaction chamber;Fluoroform gas enters reaction chamber by organic matter entrance
It is interior;Two kinds of reactants mix and are reacted in reaction chamber;Last bromotrifluoromethane passes through product exit outflow reactor.
Through detecting, the conversion ratio of end reaction is 95%, and the yield of product is 92%.
Embodiment 3 prepares vinyl bromide using anion bromination reactor of the present invention
Reactant: bromine, ethylene, product: vinyl bromide
Bromine is heated to 58.8 DEG C of gasifications, and continues to be heated to 70 DEG C or so, it is logical with the speed speed of 2m/s to control bromine vapor
The bromine vapor entrance for crossing bromine anion generator enters;Power supply is opened, by transformer, by interpolar positive and negative in bromide ion generator
Voltage in 5KV or so so that form powerful electric field between positive and negative anodes, so that nearby there is corona phenomenon in spray point;Bromine steams
After vapour passes through variable diameter conduit, so that bromine vapor enters positive and negative anodes opposed area, and make bromine vapor in the corona region residence time
0.5-1s generates bromine anion and enters in reaction chamber;Ethylene gas is entered in reaction chamber by organic matter entrance;In reaction chamber
Interior two kinds of reactants carry out mixing and react;Last vinyl bromide passes through product exit outflow reactor.
Through detecting, the conversion ratio of end reaction is 90%, and the yield of product is 95%.
Claims (8)
1. a kind of anion bromination reactor, which is characterized in that anion bromination reactor includes voltage offer portion, bromine anion
Generator and reaction chamber;Bromine anion generator includes cylindrical shell body, is close to outer housing inner wall and is equipped with insulation material layer, tightly
It pastes insulation material layer inner wall and is equipped with high-voltage anode material layer, be connected with several spray points on high-voltage anode material layer, discharge
Needle is directed toward outer housing center line, is close to high-voltage anode material layer inner wall and is equipped with insulation liner material layer, insulation liner material layer
It is equipped with aperture, spray point is passed through out of aperture, and high voltage negative electrode material is located on the center line of outer housing, high voltage cathode material
The both ends of material are fixed with collets, and collets are connected on outer housing by support frame, and the both ends of outer housing inner wall are equipped with exhausted
The internal diameter of edge ring, dead ring is equal with the internal diameter of insulation liner material layer, and one end of outer housing is connected by flange and variable diameter conduit
It connects, the other end is connect by flange with reaction chamber, and the other end of variable diameter conduit is bromine vapor entrance;
The input terminal of adjustable variable-pressure device is connect with alternating current 220V in voltage offer portion, the output end of adjustable transformer and rectification
Device connection, the output head anode of rectifier are connect with high-voltage anode material layer, and the negative pole of output end and high voltage of rectifier are negative
The connection of pole material, voltmeter are serially connected in the output end of rectifier, let out non-electricity protector and ammeter is connected on the output end of rectifier
Between anode and high-voltage anode material layer;
It is reaction chamber inside reaction chamber, the top of reaction chamber is end socket, and side wall is equipped with organic matter import and product exit.
2. anion bromination reactor according to claim 1, which is characterized in that the material of the variable diameter conduit and outer housing
Any one of matter in carbon steel, stainless steel, cupro-nickel titanium alloy or monel metal.
3. anion bromination reactor according to claim 1, which is characterized in that the material of the insulation liner material layer
For polytetrafluoroethylene (PTFE) or quartz glass.
4. anion bromination reactor according to claim 1, which is characterized in that the intracorporal insulation material of the abutting shell
Any one of the material of the bed of material and collets in ceramics, rubber material or polytetrafluoroethylene (PTFE).
5. anion bromination reactor according to claim 1, which is characterized in that the material of the reaction chamber is selected from 304
Any one in steel alloy, cupro-nickel titanium alloy, monel metal or stainless steel.
6. anion bromination reactor according to claim 1, which is characterized in that the spray point and high voltage cathode material
The vertical range d of material is 20-30mm.
7. application of the anion bromination reactor in bromination reaction as described in claim any one of 1-6.
8. application of the anion bromination reactor in bromination reaction as described in claim any one of 1-6, which is characterized in that tool
Steps are as follows for body:
When bromine vapor enters bromine anion generator by bromine vapor entrance, voltage is risen to by 3- by adjustable variable-pressure device
10KV, bromine vapor residence time in bromine anion generator is 0.5-1s, and the bromine anion of generation enters in reaction chamber, and bromine is negative
Ion is mixed with the organic matter from organic matter entrance and is reacted, and is ultimately produced object and is flowed out by product exit.
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CN201810908011.8A CN108993346A (en) | 2018-08-10 | 2018-08-10 | A kind of anion bromination reactor and its application |
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Cited By (1)
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CN109692646A (en) * | 2019-01-12 | 2019-04-30 | 山东重山光电材料股份有限公司 | A kind of hot halogenation reactor |
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