CN208082482U - A kind of spraying cycle reactor - Google Patents

A kind of spraying cycle reactor Download PDF

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Publication number
CN208082482U
CN208082482U CN201721773016.1U CN201721773016U CN208082482U CN 208082482 U CN208082482 U CN 208082482U CN 201721773016 U CN201721773016 U CN 201721773016U CN 208082482 U CN208082482 U CN 208082482U
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China
Prior art keywords
diameter
reaction kettle
injector
reaction
gas
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Expired - Fee Related
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CN201721773016.1U
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Chinese (zh)
Inventor
马建军
李晓明
毛志红
边祥成
滕志君
蒙鸿飞
陶春霞
王萍
白卫兵
陈其宝
任若飞
张建强
赵伟
王迎军
田正义
刘锦民
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Gansu Yinguang Juyin Chemical Industry Co Ltd
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Gansu Yinguang Juyin Chemical Industry Co Ltd
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Priority to CN201721773016.1U priority Critical patent/CN208082482U/en
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Abstract

The utility model provides a kind of spraying cycle reactor, by being optimized to inside reactor structure, organic amine and solvent mixture, hydrogen chloride or the phosgene efficient hybrid reaction in injector, then it is sprayed by injector nozzle, it is reacted by continuous spraying cycle, realizes that organic amine compound reaction completely is isocyanate products.

Description

A kind of spraying cycle reactor
Technical field
The utility model belongs to organic chemical industry field, and in particular to a kind of spraying cycle reactor for continuous operation.
Background technology
Isocyanates has non-as a kind of important organic chemical industry's intermediate in industry, agricultural, medical and health everyway Normal extensive purposes.Such compound is widely used in polyisocyanate, polyurethanes, polyureas, superpolymer adhesive, desinsection The synthesis of agent, herbicide etc..Existing mainstream technology is to react to prepare isocyanates in atent solvent with phosgene using organic amine, Phosgenation is divided into direct method and salt forming method, and direct method is by the way that isocyanates is directly made in amine and phosgene;Salt forming method is then first Corresponding amine and sour gas such as hydrogen chloride, carbon dioxide etc. are reacted, amine salt is made, then generates amine salt and phosgene reaction Isocyanates.Such reaction is that gas-liquid two-phase reacts, and phosgene needs excess in reaction, in order to reduce the excessive ratio of phosgene, it is necessary to have Mass transfer, heat transfer are reinforced in strong stirring, and making phosgene and heat, dispersion in liquid phase, accelerates reaction rate very well, reduce by-product The generation of object improves reaction yield.
Patent CN206404772U reports a kind of synthesizing isocyanate reaction kettle, which sets on inner chamber body top After having blending tank, reaction raw materials to be reacted first in the blending tank, the reaction was continued for reaction solution overflow to cavity lower part;The reaction kettle Reinforce mixing by being respectively equipped with blender with cavity lower part in blending tank, improves combined coefficient.The patent and tradition are anti- It answers kettle to compare, the mixing efficiency of phosgene and amine is improved by two level stirring, but phosgene reacts with organic amine and still falls within boundary Face is reacted, and is reacted after not reaching intermolecular and being sufficiently mixed, and it is excessively bigger to eventually lead to phosgene, generates by-product More, phosgene utilization rate is not high.
Patent CN103357363A reports a kind of reaction kettle synthesizing isocyanate of bottom reflux phosgene, which will Phosgene condensation reflux liquid pipeline enters from reactor bottom, and adds a non-return valve, the liquid phase phosgene of condensation whole in inlet location Reaction solution system is flowed back into from reactor bottom through non-return valve, the patent by excess phosgene gas by condensing reuse, effectively Improve the utilization rate of phosgene, but blender used to reinforce the mixing of organic amine and phosgene, this kind of mode be equally phosgene with The interfacial reaction of organic amine reaction, reacts after not reaching intermolecular and being sufficiently mixed, and it is more to lead to generate by-product, Reduce the yield of isocyanates.
From above-mentioned example can be seen that light phosgenation synthesizing isocyanate use equipment mainly pass through Multi-stage stirring To reinforce mass transfer, heat transfer;On the other hand, by phosgene back flow reaction kettle, improving the utilization rate of phosgene, but no matter which uses Kind mode, the reaction of phosgene and organic amine belong to interfacial reaction, do not reach intermolecular hybrid reaction, do not make phosgene Fairly evenly disperse in liquid phase, to eventually lead to that side reaction product increases or phosgene utilization rate is inadequate with heat.Therefore, it is necessary to Finding one kind makes phosgene reach intermolecular hybrid reaction, technique continuous operation with organic amine, and can reduce phosgene excess Than, reduce side reaction occur equipment.
Invention content
The purpose of the utility model is to provide a kind of spraying cycle reactor, organic amine and solvent mixture, hydrogen chloride Or phosgene in injector quick hybrid reaction then spray, reacted by continuous spraying cycle, until the reaction is complete until, The practical efficiency of hydrogen chloride or phosgene is improved, phosgene excess ratio is reduced, shortens the reaction time, effectively reduces the hair of side reaction It is raw, further increase the yield of organic amine hydrochloride or isocyanates.
To achieve the above object, the technical scheme adopted by the utility model is that:A kind of spraying cycle reactor, the reactor It is made of injector 1 and reaction kettle 5 and circulating pump 6, injector 1 is connect with reaction kettle 5 and circulating pump 6 by pipeline, injector 1 Inside 5 open top intercalation reaction kettle 5 of reaction kettle, 5 bottom line of reaction kettle is connect with circulating pump 6,6 outlet of circulating pump Line is connect with 1 suction line of injector;Injector 1 is expanded by injector nozzle 8, fluerics 9, gas-liquid mixed impact zone 10, gas-liquid Dissipate area 11, draft tube 12 is constituted, the respectively composition element coaxial connection of injector 1;Reaction kettle 5 is by reacting kettle jacketing 3,4 structure of guide shell At guide shell 4 is located inside reaction kettle 5, by fixing bracket that guide shell 4 is equidistant on 5 inner horizontal section of reaction kettle Distribution;Raw material ingress pipe 2, inside 5 open top intercalation reaction kettle 5 of reaction kettle, gas outlet pipe 7 is connected to reaction kettle 5 Top;Organic amine is entered in reaction kettle for N4 mouthfuls with solvent mixture by reaction raw materials entrance, and 6 outlet of circulating pump is then passed through Line, N1 mouthfuls of active inflow entrance enter in injector 1, and hydrogen chloride or phosgene are entered by passive inflow entrance N2 mouthfuls in injector 1, Then quick hybrid reaction in injector 1 exports N3 mouthfuls of ejections, by continuously spraying by injector nozzle 8, intermediate product Circular response, until the reaction is complete until, pass through N5 mouthfuls of the reacting product outlet discharge isocyanate products that the reaction was complete;Do not join The hydrogen chloride or phosgene for adding reaction export N6 mouthfuls of discharges by unreacting gas.
Wherein, be set forth in spraying cycle reactor injector nozzle inside diameter is 5-30mm;Fluerics entrance is straight Diameter is 25-30 times of nozzle interior diameter, and outlet diameter is 15-20 times of nozzle interior diameter, fluerics duct length be into 2-3 times of mouth diameter;Gas-liquid mixed impact zone pipe diameter is equal with fluerics pipe outlet diameter, and length is 2-3 times of diameter; Gas-liquid diffusion region entrance diameter is equal with gas-liquid mixed impact zone pipe diameter, and outlet diameter is the 1.5-2 of inlet diameter Times, length is 2-3 times of diameter;Suction pipe diameter is equal with gas-liquid diffusion region pipe outlet diameter, and length is the 2-3 of diameter Times.
The upper equidistant 4-8 guide shell of arrangement in reaction kettle inner horizontal section;Guide shell internal diameter 15-30mm;Its length It is total 0.3-0.4 times high for reaction kettle;Each guide shell layering is radial to be provided with 15-30 aperture;Small aperture is 3-5mm.
It is 15-30mm that raw material, which imports bore,;Gas outlet pipe internal diameter is 20-50mm.
The utility model has the beneficial effects that:
By being optimized to inside reactor structure, organic amine is being sprayed with solvent mixture, hydrogen chloride or phosgene Efficient hybrid reaction, is then sprayed by injector nozzle in emitter, is reacted by continuous spraying cycle, make corresponding amine and Hydrogen chloride or phosgene are quickly mixed, are reacted, and improve the practical efficiency of hydrogen chloride or phosgene, realize that organic amine compound is complete Reaction is isocyanate products.
Description of the drawings
Fig. 1 injector main view installation diagrams.
Fig. 2 spraying cycle reactor main view installation diagrams.
Fig. 3 spraying cycle reactor I-I cutaway view Amplified images.
Fig. 4 guide shell partial elevational elevation views.
Fig. 5 guide shell partly enlarged top views.
Code name explanation in figure:1. injector;2. raw material ingress pipe;3. reacting kettle jacketing;4. guide shell;5. reaction kettle; 6. Circulating pump;7. gas outlet pipe;8. injector nozzle;9. fluerics;10. gas-liquid mixed impact zone;11. gas-liquid diffusion region;12. Draft tube;N1- active inflow entrances;The passive inflow entrances of N2-;N3- intermediate products export;N4- reaction raw materials entrances;N5- reaction productions Object exports;N6- unreacting gas exports
Specific implementation mode
A kind of spraying cycle reactor provided by the utility model, the reactor is by injector 1 and reaction kettle 5 and circulating pump 6 compositions, injector 1 are connect with reaction kettle 5 and circulating pump 6 by pipeline, and injector 1 is inserted into anti-by 5 open top of reaction kettle It answers inside kettle 5,5 bottom line of reaction kettle is connect with circulating pump 6, and 6 outlet line of circulating pump is connect with 1 suction line of injector; Injector 1 is made of injector nozzle 8, fluerics 9, gas-liquid mixed impact zone 10, gas-liquid diffusion region 11, draft tube 12, injection The respectively composition element coaxial connection of device 1;Reaction kettle 5 is made of reacting kettle jacketing 3, guide shell 4, and guide shell 4 is located in reaction kettle 5 Portion, by fixing bracket by guide shell 4 equidistantly distributed on 5 inner horizontal section of reaction kettle;Raw material ingress pipe 2, by anti- It answers inside 5 open top intercalation reaction kettle 5 of kettle, gas outlet pipe 7 is connected to 5 top of reaction kettle;Organic amine and solvent mixture Entered in reaction kettle for N4 mouthfuls by reaction raw materials entrance, spray is then entered by 6 outlet line of circulating pump, N1 mouthfuls of active inflow entrance In emitter 1, hydrogen chloride or phosgene are entered by passive inflow entrance N2 mouthfuls in injector 1, the quick hybrid reaction in injector 1, Then N3 mouthfuls of ejections are exported by injector nozzle 8, intermediate product, is reacted by continuous spraying cycle, until the reaction is complete Until, pass through N5 mouthfuls of discharge isocyanate products that the reaction was complete of reacting product outlet;The hydrogen chloride or phosgene of reaction are not participated in N6 mouthfuls of discharges are exported by unreacting gas.
Wherein, the spraying cycle reactor injector nozzle inside diameter is 5-30mm;Fluerics entrance diameter It it is 25-30 times of nozzle interior diameter, outlet diameter is 15-20 times of nozzle interior diameter, and fluerics duct length is entrance 2-3 times of diameter;Gas-liquid mixed impact zone pipe diameter is equal with fluerics pipe outlet diameter, and length is 2-3 times of diameter;Gas Liquid diffusion region entrance diameter is equal with gas-liquid mixed impact zone pipe diameter, and outlet diameter is 1.5-2 times of inlet diameter, Length is 2-3 times of diameter;Suction pipe diameter is equal with gas-liquid diffusion region pipe outlet diameter, and length is 2-3 times of diameter.
Reaction kettle inner horizontal equidistantly arranges 4-8 guide shell on section;Guide shell internal diameter 15-30mm;It is the length of Reaction kettle is total 0.3-0.4 times high;Each guide shell layering is radial to be provided with 15-30 aperture;Small aperture is 3-5mm.
It is 15-30mm that raw material, which imports bore,;Gas outlet pipe internal diameter is 20-50mm.
The internal structure parameter of injection reactor see the table below in each embodiment.

Claims (4)

1. a kind of spraying cycle reactor, it is characterised in that:The reactor is by injector (1) and reaction kettle (5) and circulating pump (6) Composition, injector (1) are connect with reaction kettle (5) and circulating pump (6) by pipeline, and injector (1) at the top of reaction kettle (5) by opening Mouth intercalation reaction kettle (5) is internal, and reaction kettle (5) bottom line is connect with circulating pump (6), circulating pump (6) outlet line and injection Device (1) suction line connects;Injector (1) is by injector nozzle (8), fluerics (9), gas-liquid mixed impact zone (10), gas-liquid Diffusion region (11), draft tube (12) are constituted, injector (1) respectively composition element coaxial connection;Reaction kettle (5) is by reacting kettle jacketing (3), guide shell (4) is constituted, and guide shell (4) is located at reaction kettle (5) inside, by fixing bracket by guide shell (4) in reaction kettle (5) equidistantly distributed on inner horizontal section;Raw material ingress pipe (2) passes through reaction kettle (5) open top intercalation reaction kettle (5) Inside, gas outlet pipe (6) are connected at the top of reaction kettle (5).Organic amine passes through reaction raw materials entrance (N4) with solvent mixture Into in reaction kettle, then by circulating pump (6) outlet line, active inflow entrance (N1) enter injector (1) in, hydrogen chloride or Phosgene is entered by passive inflow entrance (N2) in injector (1), and the quick hybrid reaction in injector (1) then passes through injection Device nozzle (8), intermediate product outlet (N3) spray, reacted by continuous spraying cycle, until the reaction is complete until, by anti- Answer product exit (N5) the discharge isocyanate products that the reaction was complete;The hydrogen chloride or phosgene for not participating in reaction pass through unreacting gas Body exports (N6) discharge.
2. a kind of spraying cycle reactor according to claim 1, it is characterised in that the spraying cycle reactor nozzle Inside diameter is 5-30mm;25-30 times of a diameter of nozzle interior diameter of fluerics entrance, outlet diameter is nozzle interior 15-20 times of diameter, fluerics duct length are 2-3 times of inlet diameter;Gas-liquid mixed impact zone pipe diameter and fluerics Pipe outlet diameter is equal, and length is 2-3 times of diameter;Gas-liquid diffusion region entrance diameter and gas-liquid mixed impact zone pipeline are straight Diameter is equal, and outlet diameter is 1.5-2 times of inlet diameter, and length is 2-3 times of diameter;Pipe diameter is sucked out to manage with gas-liquid diffusion region Road outlet diameter is equal, and length is 2-3 times of diameter.
3. a kind of spraying cycle reactor according to claim 1, it is characterised in that reaction kettle inner horizontal section Upper equidistantly 4-8 guide shell of arrangement;Guide shell internal diameter 15-30mm;The length of reaction kettle is total 0.3-0.4 times high;Each Guide shell layering is radial to be provided with 15-30 aperture;Small aperture is 3-5mm.
4. a kind of spraying cycle reactor according to claim 1, it is characterised in that it is 15- that the raw material, which imports bore, 30mm;Gas outlet pipe internal diameter is 20-50mm.
CN201721773016.1U 2017-12-18 2017-12-18 A kind of spraying cycle reactor Expired - Fee Related CN208082482U (en)

Priority Applications (1)

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CN201721773016.1U CN208082482U (en) 2017-12-18 2017-12-18 A kind of spraying cycle reactor

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Application Number Priority Date Filing Date Title
CN201721773016.1U CN208082482U (en) 2017-12-18 2017-12-18 A kind of spraying cycle reactor

Publications (1)

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CN208082482U true CN208082482U (en) 2018-11-13

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107899531A (en) * 2017-12-18 2018-04-13 甘肃银光聚银化工有限公司 A kind of spraying cycle reactor and the method for being synthesized by isocyanates
CN109810024A (en) * 2019-03-28 2019-05-28 南京工业大学 A kind of spray circuits reactor being used to prepare penta diisocyanate and its application method
CN110075779A (en) * 2019-05-31 2019-08-02 昆明理工大学 A kind of injection reactor and calcium monohydrogen phosphate, nanometer or micro-powder synthetic method for powder body material synthesis
CN113024416A (en) * 2021-04-26 2021-06-25 上海交通大学 Reaction system for preparing isocyanate by organic amine phosgenation

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107899531A (en) * 2017-12-18 2018-04-13 甘肃银光聚银化工有限公司 A kind of spraying cycle reactor and the method for being synthesized by isocyanates
CN109810024A (en) * 2019-03-28 2019-05-28 南京工业大学 A kind of spray circuits reactor being used to prepare penta diisocyanate and its application method
CN110075779A (en) * 2019-05-31 2019-08-02 昆明理工大学 A kind of injection reactor and calcium monohydrogen phosphate, nanometer or micro-powder synthetic method for powder body material synthesis
CN110075779B (en) * 2019-05-31 2024-02-09 昆明理工大学 Jet reactor for powder material synthesis and powder synthesis method
CN113024416A (en) * 2021-04-26 2021-06-25 上海交通大学 Reaction system for preparing isocyanate by organic amine phosgenation

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CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20181113

Termination date: 20191218