CN204107483U - Double-sided cooled concentric locking collar tubular sulfonator - Google Patents

Double-sided cooled concentric locking collar tubular sulfonator Download PDF

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Publication number
CN204107483U
CN204107483U CN201420489866.9U CN201420489866U CN204107483U CN 204107483 U CN204107483 U CN 204107483U CN 201420489866 U CN201420489866 U CN 201420489866U CN 204107483 U CN204107483 U CN 204107483U
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China
Prior art keywords
reaction
pipe
cooling
spiral
sulfonator
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Expired - Fee Related
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CN201420489866.9U
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Chinese (zh)
Inventor
王宗勇
孟辉波
吴剑华
张春梅
田瑞
朱军
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Shenyang University of Chemical Technology
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Shenyang University of Chemical Technology
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Abstract

Double-sided cooled concentric locking collar tubular sulfonator, relate to a kind of double-sided cooled concentric locking collar tubular sulfonator, double-sided cooled concentric locking collar tubular sulfonator comprises pipe (1) in cooling, reaction sleeve pipe (2), cooling collar (3), spiral jet pipe (4), spiral flow deflector (5), turbulence columns (6), cooling collar outlet (7), reaction cannula exit pipe (8), cooling collar inlet tube (9) and reaction sleeve pipe inlet tube (10) etc.Pipe, reaction sleeve pipe and cooling collar three pipe arranged concentric in cooling, form a reaction cavity and two heat exchange cavitys, simultaneously in two kinds of cavitys, assemble spiral jet pipe and spiral flow deflector respectively, ensure that reaction mass and cooling agent can helical flow, mass transfer and heat transfer are synchronously strengthened.The utility model heat transfer rate is fast, reacts safe and reliable, is specially adapted to the continuous sulfonating reaction process that employing liquid phase sulfur trioxide is sulfonating agent.

Description

Double-sided cooled concentric locking collar tubular sulfonator
Technical field
The utility model relates to a kind of double tube reactor, particularly relates to a kind of double-sided cooled concentric locking collar tubular sulfonator.
Background technology
The sulfonating reaction being sulfonating agent with liquid phase sulfur trioxide normally drips mode with autoclave and carries out, namely first will be sulfonated thing (as nitrobenzene) renders in reactor, again sulfur trioxide is slowly added drop-wise in reactor by bottom insert canal, by stirring, mixing of materials is even, material generation vigorous reaction, releases a large amount of reaction heat simultaneously.Reaction heat is shifted out by the cooling agent in reacting kettle jacketing, to keep suitable reaction temperature.There is many defects that self cannot overcome in this reactive mode: first, and reactor heat transfer area is little, and it is slow that reaction heat shifts out speed, and then cause sulfonating agent to drip slowly, and the production cycle is long; Secondly, sulfonating agent is added drop-wise in still continuously, sulfur trioxide and product continuous contact, and cause early reaction product to occur in-depth reaction, accessory substance increases; In addition, there is huge potential safety hazard in this kind of course of reaction, once reaction midway cuts off the water, power-off or stirring system break down, reaction heat cannot shift out in time will cause temperature control, and security incident occurs.
For the deficiency that autoclave dropwise reaction exists, occurred a kind of continuous pipe type sulfonating reaction process in recent years, the two kinds of materials namely participating in reacting enter tubular reactor simultaneously, complete course of reaction while both synchronously flowings.But find through great many of experiments, this reaction process is often difficult to control, reason is exactly that two kinds of materials of participation reaction are close to theoretical rate of charge, the reaction of reaction unit initial reaction section is very violent, reactor with common cooling collar cannot shift out reaction heat fast, cause temperature control, reaction cannot proceed.As can be seen here, developing a kind of reactor that can realize efficient flash heat transfer is the key realizing continuous pipe type sulfonating reaction process.
Summary of the invention
The purpose of this utility model is to provide a kind of double-sided cooled concentric locking collar tubular sulfonator, this reactor has inside and outside two heat transfer walls, the helical flow of cooling agent and reaction mass can be realized, heat transfer area is large, heat transfer coefficient is high, and reaction mass contact fully, mixes, byproduct of reaction is few, ensures that course of reaction safety is controlled.
The purpose of this utility model is achieved through the following technical solutions:
Double-sided cooled concentric locking collar tubular sulfonator, described reactor comprises pipe in cooling, reaction sleeve pipe, cooling collar, spiral jet pipe, spiral flow deflector, turbulence columns, cooling collar outlet, reaction cannula exit pipe, cooling collar inlet tube and reaction sleeve pipe inlet tube; Annular housing between cooling outer wall of inner tube and reaction internal surface of sleeve pipe is material reaction space, and this space is separated into a helical flow path by spiral jet pipe, participates in material hybrid reaction in helical flow path of reaction; The tube wall of spiral jet pipe has jet orifice along reactor axis direction, and jet orifice is axial and circumferential uniform along helix tube, and jet orifice diameter is determined by the mass flow transitivity in spiral jet pipe; The diameter of spiral jet pipe equals annular reaction spatial radial width, and reaction mass is complete or substantially flow along helical flow path direction; The pitch of spiral jet pipe determines reaction mass circulation sectional area, and its size is determined according to reactor for treatment amount and reaction time; Spiral flow deflector is assemblied in cooling collar and the annular space that formed of reaction sleeve pipe, and this annular space is divided into a spiral flow channel, cooling medium flows at runner inside spin; Spiral flow deflector width equals cooling collar and the annular space distance that formed of reaction sleeve pipe; The negate of spiral flow deflector pitch answers 0.2 ~ 0.8 times of casing diameter.
Described double-sided cooled concentric locking collar tubular sulfonator, described turbulence columns is welded on reaction sleeve outer wall, is distributed in the middle of the helical flow path that spiral flow deflector formed along hand of helix.
Described double-sided cooled concentric locking collar tubular sulfonator, described pin-fin diameter gets 1/6 ~ 1/3 of runner axial width; Turbulence columns height gets 0.5 ~ 1 times of spiral flow deflector width.
Described double-sided cooled concentric locking collar tubular sulfonator, pipe is contrary with the overall flow direction of the cooling medium in cooling collar in described cooling, and on guarantee reactor length direction, homogeneous temperature is everywhere consistent.
Advantage of the present utility model and effect are:
1. the utility model has inside and outside two heat transfer space, can realize the helical flow of cooling agent, and heat transfer area is large, and heat transfer coefficient is high, and it is fast that reaction heat shifts out speed;
2. the utility model can the eddy flow of realization response material and jet synchronized mixes, without flow blind angle, without short circuit, can not react excessively and reaction shortcoming phenomenon;
3. the utility model bearing capacity is strong, and mixed pipe diameters is less, can bear higher pressure medium, can be applied to high pressure operating mode;
4. the utility model is safe and reliable, is convenient to temperature and controls, be applicable to strong exothermal reaction operating mode;
5. the utility model compact conformation, is convenient to connect, saves space.
6. the alternative tank reactor of the utility model, the serialization of realization response process.
Accompanying drawing explanation
Fig. 1 is assembly structure figure of the present utility model;
Fig. 2 is the assembly structure figure of reaction sleeve pipe and spiral flow deflector and turbulence columns;
Fig. 3 is the assembly structure figure of pipe and spiral jet pipe in cooling;
Fig. 4 is that (wherein, solid single arrow represents sulfonating agent to utility model works principle schematic; Hollow single arrow representative is sulfonated thing; Solid double-head arrow represents cooling agent; Hollow solid double-head arrow represents product).
Detailed description of the invention
With reference to the accompanying drawings the utility model is described in detail.
Double-sided cooled concentric locking collar tubular sulfonator, comprise pipe 1 in cooling, reaction sleeve pipe 2, cooling collar 3, spiral jet pipe 4, spiral flow deflector 5, turbulence columns 6, cooling collar outlet 7, reaction cannula exit pipe 8, cooling collar inlet tube 9 and reaction sleeve pipe inlet tube 10 etc., as shown in Figure 1.Pipe 1 in cooling, reaction sleeve pipe 2 and cooling collar 3 arranged concentric successively from inside to outside, spiral jet pipe and spiral flow deflector lay respectively in two annular spaces that three pipes are formed.
Annular space cavity in cooling between pipe 1 outer wall and reaction sleeve pipe 2 inwall is the reaction compartment of reaction mass, the flow regime of material in this space and distribution character determine reaction effect, in order to improve the less turbulence of fluid, the Radial Flow of strengthening fluid, a spiral jet pipe 4 is inserted in the reaction compartment of ring-type, this jet pipe is lucky and cool outer wall of inner tube 1 and react sleeve pipe 2 contact internal walls, thus be that the cylindrical shape reaction compartment of ring-type is divided into a cross section to be approximate rectangular helical flow path by original cross section, as shown in Figure 3.The pitch of spiral jet pipe 4 hdetermine the circulation area of helical flow path, its size should be determined according to reactor for treatment amount and reaction time.Reaction mass flows in helical flow path, and not only flow path increases, and fluid can form secondary vortex flow under the effect of spiral flow centrifugal force, and the Radial Flow effect of fluid is strengthened, and mixing is more abundant, and reaction effect is better.
Spiral jet pipe 4, except having the effect of formation helical flow path, also plays the effect of sulfonating agent conduit and jet pipe.The tube wall of spiral jet pipe 4 has through hole along reactor axis direction, and this hole is sulfur trioxide jet orifice.Jet orifice is uniform along helix circumferencial direction, and interval angles is generally 90 ° or 180 °, as shown in Figure 3.The diameter of jet orifice drelevant with jet pipe mass flow and material characteristic, be generally 0.5 ~ 1 times of helix tube diameter, determine that principle ensures that jet flow core area fluid axial length is a helix tube pitch.Spiral jet pipe 4 end flat board is shut, and ensures that all sulfonating agents all flow out from jet orifice.Reacting fluid in helical flow path under multiple jet effect, achieve entrainment, disperse, the forms of motion such as merging, two kinds of reacting fluids mixing are more fully, evenly.
The concentric toroidal shell that reaction sleeve pipe 2 and cooling collar 3 are formed is the flowing space of cooling medium, and cooling medium determines the size of convective heat-transfer coefficient in the flow regime in this space.Traditional heat exchange jacket is a toroidal cavity, the inlet/outlet pipe of cooling agent is arranged symmetrically with at axial two ends, cooling agent along the diagonal overall flow of inlet/outlet pipe, thus causes two ends to there is larger flow dead, and heat transfer area reduces, simultaneously because actual internal area is larger, coolant flow speed is comparatively slow, and heat transfer coefficient is lower, and above two kinds of unfavorable factors combine and cause heat-transfer effect poor, not in time, reaction temperature is easily out of control in heat exchange.In order to change this situation, the utility model adds a water conservancy diversion flight 5 in traditional annular cooling space, and this flow deflector and inside and outside circle tube wall surface close contact, be transformed into a square-section helical flow path, as shown in Figure 2 by original annular channel.Rectangular coil runner eliminates flow dead, improves fluid-flow rate, enhances fluid Radial Flow, is thinned heat transfer boundary layer, thus significantly improve convective heat-transfer coefficient.In addition, spiral flow deflector 5 is welded and fixed with reaction sleeve pipe 2 outer wall, plays " fin " effect, is equivalent to extend heat transfer wall, increases heat transfer area.
For the heat-transfer effect of further enhanced reactor, in the multiple turbulence columns 6 of the uniform welding of helical flow path inner periphery of the outer wall of reaction sleeve pipe 2, turbulence columns 6 is positioned at the centre position of the helical flow path that water conservancy diversion flight is formed, as shown in Figure 2.Cooling agent in helical flow path is subject to the barrier effect of turbulence columns 6, can form eddy current in its rear, and eddy current further increases the less turbulence of cooling agent.The effect of turbulence columns 6 augmentation of heat transfer when coolant flow speed is lower is more obvious.Turbulence columns 6 diameter gets 1/6 ~ 1/3 of width of flow path.Turbulence columns 6 highly gets 0.5 ~ 1 times of spiral flow deflector width.
Double-sided cooled concentric locking collar tubular sulfonator, except having an annular outside cooling space, also has cooling space inside a cylindrical shape, namely cools the cooling space that inner core is formed.For ensureing homogeneous temperature distribution on reactor length direction, in cooling, pipe is contrary with the overall flow direction of the cooling medium in cooling collar.In cooling, pipe is according to the needs of heat transfer conditions, can add the convection heat transfer' heat-transfer by convection that the elements such as twisted blade come in enhanced tube.
For ensureing that this reactor has good corrosion resistance, its all parts all adopt stainless steel material, and as S30408, in cooling, pipe and reaction sleeve pipe are under the prerequisite meeting pressure medium, and wall thickness should be thin as far as possible, to improve heat-conducting effect, usually gets 2 ~ 4mm.
Spiral flow deflector and the corresponding tube wall laminating of spiral jet Guan Yingyu, maximal clearance should control within 2mm, ensures that fluid does not occur short circuit phenomenon.Spiral jet pipe can adopt circular section pipe, rectangular section tube or be made up of a pair flight.Spiral flow deflector and corresponding with it the respectively pipeline outer wall of spiral jet pipe adopt the mode firm welding of sequential welding or intermittent weld, and assembly relation is shown in Fig. 2 and Fig. 3.
Adopt Circular Plate as cooling collar and the end socket reacting sleeve pipe, reduce the length difference between three concentric tubes to greatest extent, ensure that heat transfer area is enough large.Turbulence columns adopts solid steel pole or steel pipe to make, and ensures itself and reaction sleeve outer wall firm welding.
The utility model can be arranged vertically, horizontally disposed, be in tilted layout; Or vertical, level, inclination combination layout; Can single use also can use by serial or parallel connection, can adopt docking when serial or parallel connection uses or adopt tube connector to connect, connected mode can adopt welding or Flange joint.
The course of work, is shown in Fig. 4: first, by cooling agent, as refrigerated brine, enters into cooling cavities by pipe 1 import in cooling collar inlet tube 9 and cooling simultaneously, after its flowing and temperature plateau, makes to be sulfonated thing, nitrobenzene through what measure; Flowed in reaction sleeve pipe 2 by reaction sleeve pipe inlet tube 10, guarantee that nitrobenzene is full of whole reaction cavity and flowing is steady; Then, the liquid phase sulfur trioxide through metering is transported in spiral jet pipe 4, utilizes piston pump or pressurized tank; Be ejected in the nitrobenzene of eddy flow by each jet orifice, mixing limit, two kinds of reaction mass limits is reacted; Finally, regulate the flow of cooling agent, reaction temperature is controlled at about 90 DEG C.
Embodiment
The present embodiment is the application example of the utility model at the SO 3 sulfonated m-nitro of liquid phase.
By three double-sided cooled concentric locking collar tubular sulfonators, reaction casing diameter DN25, effecting reaction length 1.2m; Be cascaded and form sulfonation initial reactor, the SK type static mixer of 8 DN20 that then connected again, single pipe range 1.2m; As maintenance reactor.In experimentation, reaction temperature controls at 90 DEG C ± 5 DEG C, and m-nitro flow is 200L/h, and sulfur trioxide flow is 100L/h, and it is 96.5% that experiment obtains liquid m-nitrobenzene sulfonic acid content, nitro sulfone mass content 2.5%.
Experimental result shows that this reactor can shift out reaction heat fast, and reaction temperature controls sensitive, and conversion rate of products is high, can the serialization of realization response process safely.

Claims (3)

1. double-sided cooled concentric locking collar tubular sulfonator, it is characterized in that, described reactor comprises pipe (1) in cooling, reaction sleeve pipe (2), cooling collar (3), spiral jet pipe (4), spiral flow deflector (5), turbulence columns (6), cooling collar outlet (7), reaction cannula exit pipe (8), cooling collar inlet tube (9) and reaction sleeve pipe inlet tube (10); Annular housing in cooling between pipe (1) outer wall and reaction sleeve pipe (2) inwall is material reaction space, and this space is separated into a helical flow path by spiral jet pipe (4); The tube wall of spiral jet pipe (4) has jet orifice along reactor axis direction, and jet orifice is axial and circumferential uniform along helix tube, and jet orifice diameter is determined by the mass flow transitivity in spiral jet pipe; The diameter of spiral jet pipe (4) equals annular reaction spatial radial width; The pitch of spiral jet pipe (4) determines reaction mass circulation sectional area, and its size is determined according to reactor for treatment amount and reaction time; Spiral flow deflector (5) is assemblied in cooling collar and the annular space that formed of reaction sleeve pipe, this annular space is divided into a spiral flow channel; Spiral flow deflector (5) width equals cooling collar and the annular space distance that formed of reaction sleeve pipe; Spiral flow deflector (5) pitch negate answers 0.2 ~ 0.8 times of casing diameter.
2. double-sided cooled concentric locking collar tubular sulfonator according to claim 1, is characterized in that, described turbulence columns (6) is welded on reaction sleeve outer wall, is distributed in the middle of the helical flow path that spiral flow deflector (5) formed along hand of helix.
3. double-sided cooled concentric locking collar tubular sulfonator according to claim 2, is characterized in that, described turbulence columns (6) diameter gets 1/6 ~ 1/3 of runner axial width; Turbulence columns (6) highly gets 0.5 ~ 1 times of spiral flow deflector (5) width.
CN201420489866.9U 2014-08-28 2014-08-28 Double-sided cooled concentric locking collar tubular sulfonator Expired - Fee Related CN204107483U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105328978A (en) * 2015-11-27 2016-02-17 佛山市南海区三简包装有限公司 Strengthening heat transfer type die pressing printing roller

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105328978A (en) * 2015-11-27 2016-02-17 佛山市南海区三简包装有限公司 Strengthening heat transfer type die pressing printing roller

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

Granted publication date: 20150121

Termination date: 20170828

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