CN109692646A - A kind of hot halogenation reactor - Google Patents

A kind of hot halogenation reactor Download PDF

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Publication number
CN109692646A
CN109692646A CN201910028998.9A CN201910028998A CN109692646A CN 109692646 A CN109692646 A CN 109692646A CN 201910028998 A CN201910028998 A CN 201910028998A CN 109692646 A CN109692646 A CN 109692646A
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CN
China
Prior art keywords
end socket
hot
reaction tube
halogenation reactor
flange
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Application number
CN201910028998.9A
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Chinese (zh)
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CN109692646B (en
Inventor
方治文
李芝保
王乐深
张峰
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Shandong Zhongshan Photoelectric Material Co Ltd
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Shandong Zhongshan Photoelectric Material Co Ltd
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Priority to CN201910028998.9A priority Critical patent/CN109692646B/en
Priority claimed from CN201910028998.9A external-priority patent/CN109692646B/en
Publication of CN109692646A publication Critical patent/CN109692646A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24Stationary reactors without moving elements inside
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor

Abstract

The present invention relates to chlorinations, the technical field of bromination equipment, and in particular to a kind of hot halogenation reactor, the reactor that will more specifically to react after chlorine, bromine high-temperature heating with organic matter.Hot halogenation reactor reaction zone of the invention good, clean surface the pure quartz glass material reactor using chlorine, bromine tolerance level under hot conditions, liner tetrafluoroethene, enamel is taken to be resistant to corrosive medium in the non-heated region such as non-reaction zone domain and end socket junction, end socket tyre cooling jacket, low in and high out.End socket inlet and outlet flange is connected with process pipe by liner tetrafluoro metal bellow, and liner tetrafluoro metal bellow joint flange one end is fixed, and one end uses lap joint flange, it is ensured that end socket connection and expanded by heating have certain freedom degree.

Description

A kind of hot halogenation reactor
Technical field
The present invention relates to chlorinations, the technical field of bromination equipment, and in particular to a kind of hot halogenation reactor, more specifically Say the reactor for being related to reacting after chlorine, bromine high-temperature heating with organic matter.
Background technique
It is many it is important containing chlorine, the organic intermediate containing elements such as bromines, synthetic drug be all by hot halogenation It obtains.Halogenation is generally divided into two kinds: one is organic matters to react with hydrogen halides, and another kind is organic matter and halogen simple substance Reaction.
Organic matter mainly carries out in a solvent with reacting for hydrogen halides, and this method generates a large amount of waste liquid and waste material.Have Machine object is reacted with halogen simple substance, is mostly used and is reacted under high temperature now, but in 350 DEG C or more especially 500 DEG C or more of temperature Under degree, tolerance chlorine, the material of bromine are considerably less and expensive;Halogenated by-products can also cause product purity certain It influences, improves the difficulty of product separation, or even will limit the application range of high purity product.
Current halogenation device generally uses conventional metal material such as nickel, stainless steel etc., there are hot environment chlorine, Bromine gas tolerance level is poor, metallic material corrosion rate is fast, coefficient of thermal expansion is high, the proportion of goods damageds are high, service life is short, not high pressure resistant, by-product Impurity is more, influences the shortcomings that product quality;In addition, metal material is not easy to connect, can not use with nonmetallic materials quartz glass High-strength bolt compresses, sealing is poor, easily leakage;So that reaction unit utilization rate is low, service life is short, it is often necessary to stop Work.
Summary of the invention
The purpose of the present invention is to provide a kind of hot halogenation reactor, hot halogenation reactor reaction zone of the invention is using high Chlorine, bromine tolerance level be good under the conditions of temperature, pure quartz glass material reactor of clean surface, and non-reaction zone domain and end socket connect The place of connecing etc. takes in non-heated region liner tetrafluoroethene, enamel to be resistant to corrosive medium, and end socket tyre cooling jacket is low into height Out.End socket inlet and outlet flange is connected with process pipe by liner tetrafluoro metal bellow, liner tetrafluoro metal bellow Joint flange one end is fixed, and one end uses lap joint flange, it is ensured that end socket connection and expanded by heating have certain freedom degree.
The technical solution of the present invention is as follows:
A kind of hot halogenation reactor, including reaction tube, end socket, heater, outer insulation blocking cabinet, which is characterized in that end socket set It is connected to the port of reaction tube, seal member is set on the outside of the tube wall of end socket and reaction tube, is connect in the port of end socket and reaction tube Fluorubber pad is set between contacting surface, and the end of end socket is inlet and outlet flange, which passes through liner tetrafluoro wavy metal Hose with extraneous process pipe for connecting;Thermometer protective sleeve is arranged in end socket peripheral hardware cooling down collet, reaction tube inside, Temperature element is set in thermometer protective sleeve, and the temperature element is connected with temperature controller;The reaction tube is divided into non- Conversion zone and conversion zone, non-reaction zone domain are the part that end socket socket-connects, and rest part is conversion zone, in reaction tube Heating element is set at the corresponding outer wall of conversion zone.
The features of the present invention in addition,
The heating method of heating element is heat radiation, and heating element is electric furnace heating or electromagnetic heater.Wherein, electromagnetic heater It include: electromagnetic heating coil, immerging metal tube heater.Immerging metal tube heater be carbon steel, stainless steel, Meng Naier it is therein any one.
The reaction tube be ball mouth tubular quartz glass reaction tube, the material be quartz glass, have high temperature resistant, The features such as thermal expansion coefficient is low, resistance to heat shocks and electrical insulation capability are good.
The seal member is that labyrinth seal or polytetrafluoroethylene packing seal.
End socket is socketed on the port of reactor by end socket welded flange, and the end socket welded flange is reacted with being socketed on The reaction pipe flange of pipe outer wall is pre-tightened by flange bolt;Further preferably, the spiral shell between end socket welded flange and nut Spring is set on bolt.
Heat-insulating material is also set up between reaction tube wall and seal member.Chamber between end socket and quartz glass reaction pipe Intefused tetratiuorine airtight and watertight padding;Before filling filler, the first winding mica tape on the quartz glass reaction pipe more slightly longer than end socket size, The heat-insulating materials such as aluminosilicate fiber or lean ore object rock wool.
The head lining polytetrafluoroethylene (PTFE) or the corrosion-resistant medium of enamel.
Fixed bracket is set in end socket lower end, fixed bracket is set in heating element lower end.
Refractory material cushion block is placed between reaction tube and heating element, further preferably, which is arc Formula refractory material cushion block.
Two glass vision panels are arranged in the outer insulation blocking cabinet, and top setting cabinet ventilation import, cabinet are taken a breath out Mouthful, transportable fresh air to the space, and the pernicious gas of generation is pumped to purified treatment process.
The material of the thermometer protective sleeve is quartz glass, protrudes into the thermometer protective sleeve of inside reactor as envelope Close cecum.
First reaction tube flange sleeve is entered before the installation of quartz glass reaction pipe, passes through flanged joint with the flange of end socket welding It is bolted;One, bolt has spring, adjusts and compress end socket and quartzy glass by slowly fastening the nut being pressed on spring Seal member between glass plays reinforcement sealing and each bolt strained effect of distributed equalization.
The course of work of hot halogenation reactor:
The material that molar ratio premix is completed enters the non-reaction near end socket and end socket by liner tetrafluoro metal bellow Region, the corrosion-resistant material of liner which has heat-insulating material and cooling jacket cooling measure resistant to high temperature to guarantee end socket In its permission operating temperature range.Further, material enters residence time initiation region i.e. reaction tube conversion zone.Heating Mode is heated using electric furnace or electromagnetism casing heating method, heater, is arranged by power adjustable formula temperature controller Heating target temperature observes and records chamber of the reactor's actual temperature.As the temperature rises, raw material starts to react and generates mesh Product is marked, flows into reaction tube other end non-reaction zone domain in the form of plug flow in reaction tube.Both ends non-reaction zone domain structure, Pattern, material selection are consistent.
Hot halogenation reactor of the invention, providing heat source by heating element makes to reach 300-1000 DEG C inside reaction tube Reaction temperature, halogen (chlorine, bromine) complete halogenation with reactant in reaction tube, synthesize target product.
Compared with the prior art, the present invention has the following advantages:
Hot halogenation reactor of the invention has high temperature chlorine, bromine tolerance good, overcomes ordinary metallic material corrosion rate Fastly, service life is short, and by-product impurity is more, influences the shortcomings that product quality;For quartz glass method blue brittleness big, quartz flange with Between metal flange gasket can not be compressed using high-strength bolt, the big difficult point of leakage rate, Creative Design end socket and former The structural shape that process pipe flange is attached ensure that the sealing reliability of equipment;Non-reaction zone domain end socket part and stone Used between English glass reaction tube labyrinth seal or polytetrafluoroethylene packing sealing structure, it is ensured that equipment sealing performance and The low leakage rate of technique, optimizes the connection of conventional quartz glass reaction tube ball mouth or horn mouth connects the high disadvantage of slip, Significantly improve operating environment and the occupational health health of operator;The heat-insulating material and low in and high out that end socket part uses Cooling down measure then solves the liners media such as resistance to chlorine, the nonmetallic materials polytetrafluoroethylene (PTFE) of bromine erosion, enamel also The difficult point of non-refractory.Meanwhile entire reaction tube portion is built in outer insulation blocking cabinet, has been effectively isolated due to reaction tube The high-temperature technology medium that the emergency situations such as rupture generate has prevented the secondary injury of unexpected situation generation.
The structural shape of hot halogenation effectively reduces reaction accident rate, provides good air-proof condition, greatly Operating environment is improved, solves the disadvantages of high temperature halogenation downtime ratio is not high, easy to operate, environment is poor difficult point, the company of realizing Continuous metaplasia produces, and avoids and reduces downtime ratio, reduce industrial time cost, energy consumption cost, the cost of overhaul, thus Productive profit is improved, can simultaneously be effectively by the unified collection of the hazardous medium of uncontrollable discharge, purified treatment, is greatly changed It has been apt to production environment, has prevented the discharge of hazardous gas.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of hot halogenation reactor;
Fig. 2 is the end socket topography of hot halogenation reactor;
Fig. 3 is the ball mouth flange main view of hot halogenation reactor;
Fig. 4 is the ball mouth flange cross-sectional view of hot halogenation reactor.
1. reaction tube, 2. heating elements, 3. flange bolts, 4. springs, 5. end sockets, 6. cooling down collets, 7. fluorine Rubber pad, 8. inlet and outlet flanges, 9. temperature controllers, 10. fixed brackets, 11. refractory material cushion blocks, 13. protecting jacket for thermometer Pipe, 14. liner tetrafluoro metal bellows, 15. outer insulation blocking cabinets, 16. forms, 17. cabinets ventilation outlet, 18. cabinets Ventilation import, 19- polytetrafluoroethylene packing, 20- heat-insulating material, 21- temperature element, 22- end socket welded flange, 23- reaction tube Flange.
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 hot halogenation reactor of embodiment 1
As shown in Figure 1, Figure 2 and Figure 3, reactor includes ball mouth tubular quartz glass reaction tube 1, end socket 5, heater 2, outer isolation Protect cabinet 15.End socket 5 is socketed on the port of reaction tube 1, using poly- between ball mouth tubular quartz glass reaction tube 1 and end socket 5 Tetrafluoroethene filler 19 uses fluorubber pad 7 in the port contact face of end socket and reaction tube;End socket welded flange and reaction tube method Orchid is pre-tightened by flange bolt 3, is pressed and sealed component, plays the role of reinforcing sealing.End socket welded flange 22 and nut Between bolt on spring 4, the stress of dispersion and balanced bolt are set.5 inner liner polytetrafluoroethylene of end socket or enamel corrosion resistant Lose medium, corresponding reactor length part wound insulation material 20.5 peripheral hardware cooling down collet 6 of end socket, is passed through cooling cycle Water cools down to the non-reaction zone domain.Thermometer protective sleeve 13 is arranged in inside reactor conversion zone, and material is quartz glass, will Temperature element 21 protrudes into the region and surveys internal chamber temperature.The temperature signal that temperature element 21 measures is inputed into power adjustable formula Temperature controller 9 is completed the adjustment of 2 input power of heating element by power adjustable formula temperature controller 9, to maintain technique institute Need the stability of temperature.End socket 5 keeps its stability using fixed bracket 10.If tube length of reaction tube is longer, at interval of 1 meter, Refractory material cushion block 11 can be placed between quartz glass reaction pipe and heating element.Heating element also uses fixed bracket 10, Keep the heat radiation gap that 5-50mm is maintained between heating element and reaction tube.
Thermometer protective sleeve 13 uses comb-tooth-type sealing ring or tetrafluoroethene band and high temperature resistant on end socket 5 Gluing closes sealing, and length, which stretches within reaction heating zone, to be advisable.
The refractory material cushion block 11 is arc formula refractory material cushion block.
End socket 5 is imported and exported flange and is connect with extraneous process pipe by liner tetrafluoro metal bellow 14.Liner tetrafluoro Metal bellow 14 has certain flexibility and freedom degree, prevents pipeline and equipment stress shock reaction device.
The outer insulation blocking cabinet 15 of equipment, as buffering insulating space of the reaction tube under burst accident state, outer isolation Protect cabinet 15 using splicing removably installation.Two glass vision panels 16 are arranged in outer insulation blocking cabinet 15, convenient for observation Inner case, outlet 18 that cabinet ventilation import 17 is arranged in top, cabinet is taken a breath, transportable fresh air to the space, and will production Raw pernicious gas is pumped to purified treatment process.
A kind of hot halogenation reactor of embodiment 2
Unlike the first embodiment, in the present embodiment, comb teeth is used between ball mouth tubular quartz glass reaction tube 1 and end socket 5 Sealing.
The groove of setting and reaction tube ball mouth units specification in end socket, guarantees the concentricity of reaction tube and end socket.End socket with Connector is liner tetrafluoro metal bellow between process metal pipeline, it is ensured that certain move freely surplus, release reaction The stress that pipe heating expansion generates.
Reaction tube both ends are ball mouth, are divided into conversion zone and non-reaction zone domain.The stop of material is calculated according to process flow meter Time and reaction pipe size, residence time corresponding specification region are conversion zone, other regions are non-reaction zone domain.
5 side of end socket is material import and export flange 8, and the other side is welded as the end socket welding that reactor ball mouth specification matches Flange 22.The matched aluminum reaction tube flange of reaction tube ball mouth is packed on reaction tube in advance, measures the depth of end socket, and according to Heat-insulating material is wrapped on reactor outer wall by this size, with a thickness of 2-5mm;It reuses tetrafluoro packing and is wrapped in heat-insulating material Except.Fluorubber pad through over cure is built in inside end socket, is slowly covered end socket on reaction tube, chamber between the two is filled out Full polytetrafluoroethylene packing 19.After the completion of above-mentioned work, aluminum reacts half a month ring built in pipe flange, is carried out by bolt and end socket Connection.Bolt is in the two side portions of flange, and one end string upper spring 4, the other end is nut.By tightening nut and spring stress, Ensure that the uniform force of circumferential flange is consistent.

Claims (10)

1. a kind of hot halogenation reactor, including reaction tube, end socket, heater, outer insulation blocking cabinet, which is characterized in that end socket It is socketed on the port of reaction tube, seal member is set on the outside of the tube wall of end socket and reaction tube, in the port of end socket and reaction tube Fluorubber pad is set between contact surface, and the end of end socket is inlet and outlet flange, which passes through liner tetrafluoro metal wave Line hose with extraneous process pipe for connecting;Protecting jacket for thermometer is arranged in end socket peripheral hardware cooling down collet, reaction tube inside Pipe, is arranged temperature element, the temperature element is connected with temperature controller in thermometer protective sleeve;The reaction tube is divided into Non-reaction zone domain and conversion zone, non-reaction zone domain are the part that end socket socket-connects, and rest part is conversion zone, in reaction tube The corresponding outer wall of conversion zone at be arranged heating element.
2. hot halogenation reactor according to claim 1, which is characterized in that the heating method of heating element is heat radiation, The heating element is electric furnace heating or electromagnetic heater.
3. hot halogenation reactor according to claim 1, which is characterized in that the reaction tube is ball mouth tubular quartz glass Glass reaction tube.
4. hot halogenation reactor according to claim 1, which is characterized in that the seal member is labyrinth seal or gathers Tetrafluoroethene packing seal.
5. hot halogenation reactor according to claim 1, which is characterized in that end socket is socketed on instead by end socket welded flange Answer the port of device, the end socket welded flange with to be socketed on the reaction pipe flange for reacting pipe outer wall pre- by flange bolt Tightly;Further preferably, spring is set on the bolt between end socket welded flange and nut.
6. hot halogenation reactor according to claim 1, which is characterized in that between reaction tube wall and seal member also Heat-insulating material, any one of the heat-insulating material in mica tape, aluminosilicate fiber or lean ore object rock wool are set.
7. hot halogenation reactor according to claim 1, which is characterized in that the head lining polytetrafluoroethylene (PTFE) or The corrosion-resistant medium of enamel.
8. hot halogenation reactor according to claim 1, which is characterized in that fixed bracket is arranged in end socket lower end, is adding Fixed bracket is arranged in thermal part lower end;Further preferably, refractory material cushion block is placed between reaction tube and heating element, into one Preferably, which is arc formula refractory material cushion block to step.
9. hot halogenation reactor according to claim 1, which is characterized in that the material of the thermometer protective sleeve is stone English glass protrudes into the thermometer protective sleeve of inside reactor as closing cecum.
10. hot halogenation reactor according to claim 1, which is characterized in that the outer insulation blocking cabinet setting two Cabinet ventilation import, cabinet ventilation outlet is arranged in a glass vision panel, top.
CN201910028998.9A 2019-01-12 Thermal halogenation reactor Active CN109692646B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910028998.9A CN109692646B (en) 2019-01-12 Thermal halogenation reactor

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910028998.9A CN109692646B (en) 2019-01-12 Thermal halogenation reactor

Publications (2)

Publication Number Publication Date
CN109692646A true CN109692646A (en) 2019-04-30
CN109692646B CN109692646B (en) 2024-04-26

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101537327A (en) * 2009-04-29 2009-09-23 太原理工大学 Fixed bed reactor
CN201701925U (en) * 2010-06-13 2011-01-12 大连四方佳特流体设备有限公司 Temperature-control parallel reactor
US20130105378A1 (en) * 2010-10-15 2013-05-02 Xi'an Jiaotong University Countercurrent tank type supercritical water reactor with a sacrificial lining
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
CN210009969U (en) * 2019-01-12 2020-02-04 山东重山光电材料股份有限公司 Thermal halogenation reactor

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101537327A (en) * 2009-04-29 2009-09-23 太原理工大学 Fixed bed reactor
CN201701925U (en) * 2010-06-13 2011-01-12 大连四方佳特流体设备有限公司 Temperature-control parallel reactor
US20130105378A1 (en) * 2010-10-15 2013-05-02 Xi'an Jiaotong University Countercurrent tank type supercritical water reactor with a sacrificial lining
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
CN210009969U (en) * 2019-01-12 2020-02-04 山东重山光电材料股份有限公司 Thermal halogenation reactor

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