CN208878547U - A kind of anion bromination reactor - Google Patents

A kind of anion bromination reactor Download PDF

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Publication number
CN208878547U
CN208878547U CN201821288464.7U CN201821288464U CN208878547U CN 208878547 U CN208878547 U CN 208878547U CN 201821288464 U CN201821288464 U CN 201821288464U CN 208878547 U CN208878547 U CN 208878547U
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material layer
anion
reaction chamber
outer housing
bromine
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CN201821288464.7U
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方治文
李芝保
王乐深
刘传江
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Shandong Zhongshan Photoelectric Material Co Ltd
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Shandong Zhongshan Photoelectric Material Co Ltd
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Abstract

The utility model relates to a kind of anion bromination reactors, including voltage offer portion, bromine anion generator and reaction chamber;Bromine anion generator is followed successively by outer housing, insulation material layer, positive electrode material layer and insulation liner material layer from outside to inside, several spray points are connected on positive electrode material layer, the both ends of outer housing inner wall are equipped with dead ring, the internal diameter of dead ring is equal with the internal diameter of insulation liner material layer, one end of outer housing is connect by flange with variable diameter conduit, the other end is connect by flange with reaction chamber, and the other end of variable diameter conduit is bromine vapor entrance;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.The utility model, which has, reduces discharging of waste liquid, and reaction temperature is low, reacts the characteristics of easily realizing, and reactor is without not only anticorrosive but also material resistant to high temperature, while realizing continuous reaction.

Description

A kind of anion bromination reactor
Technical field
The present invention relates to organic synthesis fields, and in particular to a kind of reactor of anion bromination reaction, in particular It is related 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 is raw It grows up to be a useful person including cylindrical shell body, is close to outer housing inner wall and is equipped with insulation material layer, be close to insulation material layer inner wall and be equipped with high electricity Positive electrode material layer is pressed, several spray points are connected on high-voltage anode material layer, spray point is directed toward outer housing center line, is close to high Positive polarity material layer inner wall is equipped with insulation liner material layer, and insulation liner material layer is equipped with aperture, and spray point is out of aperture It passes through, 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, absolutely Edge block is connected on outer housing by support frame, and the both ends of outer housing inner wall are equipped with dead ring, and the internal diameter and liner of dead ring are exhausted The internal diameter of edge material layer is equal, and one end of outer housing is connect by flange with variable diameter conduit, and the other end passes through flange and reaction chamber Connection, the other end of variable diameter conduit are 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 with Rectifier connection, the output head anode of rectifier are connect with high-voltage anode material layer, negative pole of output end and the height electricity of rectifier Negative electrode material connection is pressed, voltmeter is serially connected in the output end of rectifier, lets out non-electricity protector and ammeter is connected on the defeated of rectifier Between outlet 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, It is accelerated under electric field force effect to anode and obtains enough energy, collided with molecular bromine, by molecular bromine outer-shell electron Bombardment is fallen, then the free electron and cation fallen by bombardment will continuously emerge in electric field space.Part energy is lower certainly It is captured during being collided with other molecular bromines by molecular bromine by electronics, 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 pacified Entirely, the characteristics of reaction is easily realized, and reactor is without not only anticorrosive but also material resistant to high temperature, while realizing continuous reaction, 90% or more conversion ratio can be reached in a 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. outer housing, 2. insulation material layers, 3. spray points, 4. insulation liner material layers, 5. ammeters, 6. voltmeters, 7. Let out non-electricity protector, 8. rectifiers, 9. adjustable variable-pressure devices, 10. bromine vapor entrances, 11. organic matter imports, 12. reaction chambers, 13. End socket, 14. product exits, 15. collets, 16. dead rings, 17. high-voltage anode material layers, 18. high voltage negative electrode materials, 19. support 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 generates Device includes cylindrical shell body 1, 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 height Positive polarity material layer 17, several spray points 3 are connected on high-voltage anode material layer 17, and spray point 3 is directed toward 1 center of outer housing Line is close to 17 inner wall of high-voltage anode material layer and is equipped with insulation liner material layer 4, and insulation liner material layer 4 is equipped with aperture, puts Acusector 3 is passed through out of aperture, and high voltage negative electrode material 18 is located on the center line of outer housing 1, and the two of high voltage negative electrode material 18 End is fixed with collets 15, and 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 The internal diameter of dead ring 16, dead ring 16 is equal with the internal diameter of insulation liner material layer 4, and one end of outer housing 1 by flange and becomes Diametered duct 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 It is connect with rectifier 8, the output head anode of rectifier 8 is connect with high-voltage anode material layer 17, the negative pole of output end of rectifier 8 It is connect with high voltage negative electrode material 18, voltmeter 6 is serially connected in the output end of rectifier 8, lets out non-electricity protector 7 and ammeter 5 is connected Between the output head anode and high-voltage anode material layer 17 of rectifier 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 produces Object outlet 14;
The material of the variable diameter conduit and outer housing is stainless steel;The material of insulation liner material layer is quartz glass;Absolutely Edge material layer and the material of collets are ceramics;The material of reaction chamber is 304 steel alloys;The spray point and high voltage cathode Vertical range 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, controls bromine vapor with the speed speed of 2m/s Degree is entered by the bromine vapor entrance of bromine anion generator;Power supply is opened bromide ion occurs by adjustable transformer The voltage of positive and negative interpolar is in 8KV or so in device, so that powerful electric field is formed between positive and negative anodes, so that spray point is formed about electricity Dizzy phenomenon;After bromine vapor passes through variable diameter conduit, so that bromine vapor enters positive and negative anodes opposed area, and make bromine vapor in corona region Residence time is 0.5-1s, generates bromine anion and enters in reaction chamber;Fluoroform gas is entered anti-by organic matter entrance Answer interior;Two kinds of reactants mix and are reacted in reaction chamber;Last bromotrifluoromethane is flowed out anti-by product exit Answer device.
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, controls bromine vapor with the speed speed of 2m/s Degree is entered by the bromine vapor entrance of bromine anion generator;Opening power supply will be positive and negative in bromide ion generator by transformer The voltage of interpolar is in 5KV or so, so that powerful electric field is formed between positive and negative anodes, so that corona phenomenon nearby occurs in 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 when corona region stops Between be 0.5-1s, generate bromine anion simultaneously enter reaction chamber in;Ethylene gas is entered in reaction chamber by organic matter entrance;Anti- It answers indoor two kinds of reactants to carry out mixing to 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 (7)

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. 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 25mm.
CN201821288464.7U 2018-08-10 2018-08-10 A kind of anion bromination reactor Active CN208878547U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108993346A (en) * 2018-08-10 2018-12-14 山东重山光电材料股份有限公司 A kind of anion bromination reactor and its application

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108993346A (en) * 2018-08-10 2018-12-14 山东重山光电材料股份有限公司 A kind of anion bromination reactor and its application

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