CN104258796B - A kind of novel high flux multi-layer helical is around pipe micro passage reaction - Google Patents
A kind of novel high flux multi-layer helical is around pipe micro passage reaction Download PDFInfo
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- CN104258796B CN104258796B CN201410539205.7A CN201410539205A CN104258796B CN 104258796 B CN104258796 B CN 104258796B CN 201410539205 A CN201410539205 A CN 201410539205A CN 104258796 B CN104258796 B CN 104258796B
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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
- B01J19/0053—Details of the reactor
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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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00002—Chemical plants
- B01J2219/00027—Process aspects
- B01J2219/00033—Continuous processes
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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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00761—Details of the reactor
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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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00788—Three-dimensional assemblies, i.e. the reactor comprising a form other than a stack of plates
- B01J2219/00792—One or more tube-shaped elements
- B01J2219/00795—Spiral-shaped
Abstract
The present invention relates to chemical reactor design field, disclose a kind of novel high flux multi-layer helical around pipe micro passage reaction, mainly comprise reactant and import and export section, import and export end socket, flange, inlet-outlet tube plate, stainless steel capillary, fixing filler strip, cylindrical shell, around cylinder, thermostatic medium imports and exports section, baffle plate, left and right bearing, central support tube, support member.Central support tube two ends connect inlet-outlet tube plate, around cylinder and central support tube on the same axis and be welded to connect by support member; Stainless steel capillary along around cylinder twist multi-lay winding arrange, the adjacent winding layer hand of spiral is contrary, formed multiple be the center of circle around cylinder, the bundle of reaction tubes in different circle footpath, stainless steel capillary two ends are connected on inlet-outlet tube plate; Import and export end socket passes through Flange joint with inlet-outlet tube plate respectively.The present invention has high flux, move that heat energy power is high, synthetic ratio is high, safe and efficient, processing cost is low, can be continuously produced, the easy advantage such as parallel amplification.
Description
Technical field
The present invention relates to chemical reactor design field, especially for carrying out chemical intermediate synthesis, the micro passage reaction that prepared by biomedical material etc., particularly relate to a kind of novel high flux multi-layer helical around pipe micro passage reaction, react for some Fast exothermic.
Background technology
Reactor is the equipment of realization response process, is widely used in the industries such as chemical industry, oil refining, metallurgy, light industry.Conventional consersion unit has mixing kettle, extraction tower, static mixer etc., and their treating capacities are large, can meet the needs of large-scale production.But on the whole, these mixing apparatus are the mixing that fluid provides macro-scale, there is the shortcomings such as mixing is uneven, power consumption is large, equipment volume is large, continuous prodution is difficult.
Along with the progress of science, the lifting of people to reaction requirement and the development of micro-processing technology, micro-reacting tcchnology and equipment thereof become the focus that people pay close attention to and study.Micro passage reaction refers to that characteristic dimension is below hundreds of micron, can constrain in wherein by sample, carry out the micromodule equipment of technical process, and it has, and mass-and heat-transfer efficiency is high, back-mixing probability is little and can control the advantage such as reaction temperature and the time of staying better.Micro passage reaction uses the pattern of continued operation, the relatively laminar flow of the fluid flow state in micro passage reaction, so just greatly weakens the axial diffusion in reactor, thus very accurately can control the reaction time.In addition, because micro passage reaction has very large specific area, make it in heat and mass transport, have great advantage, effectively can control the temperature of reacting, thus improve the selective of chemical reaction, improve the quality of product.Therefore, micro passage reaction presents many advantages being better than conventional reactor, comprises and greatly improves reaction speed, reaction yield, security, reliability and scalability etc.
But, mainly there is following problem in existing micro passage reaction: 1, existing micro passage reaction generally adopts the method manufacture such as photoetching, the three-dimensional write of laser chemistry, these micro passage reaction complex structures, and processing cost is high, be unfavorable for industrial amplification, shortcoming is obvious; 2, the disposal ability of some micro passage reactions can be realized by the method for parallel amplification, namely increase the quantity of micro passage reaction and expand the outside dimension of micro passage reaction, these methods Systematical control point in industry park plan is many, required precision is high, production cost is high, fluid property is unequal, the overall mixing of impact and reaction effect.
Summary of the invention
The present invention is intended to overcome the shortcomings such as traditional reactor mixing is uneven, power consumption is large, equipment volume is large, continuous prodution is difficult, overcome general micro passage reaction complex structure, processing cost is high, be unfavorable for shortcoming such as industry amplification etc., a kind of high flux is provided, move that heat energy power is high, synthetic ratio is high, safe and efficient, processing cost is low, the novel high flux multi-layer helical of serialization is around pipe micro passage reaction.
To achieve these goals, a kind of novel high flux multi-layer helical provided by the invention, around pipe micro passage reaction, mainly comprises reactant import and export section, import and export place end socket, flange, import and export tube sheet, stainless steel capillary, fixing filler strip, cylindrical shell, around cylinder, thermostatic medium import and export section, baffle plate, left and right bearing, central support tube, support member.Wherein:
Described central support tube two ends connect described import and export tube sheet by welding manner, be provided with outside described central support tube around cylinder, described around cylinder and described central support tube on the same axis, describedly to be welded to connect by support member around between cylinder and described central support tube, described import and export tube sheet, central support tube, to form the supporting frame of spirally-wound tube micro passage reaction around cylinder and support member;
Stainless steel capillary edge is around cylinder multi-lay winding layout twist, the adjacent winding layer hand of spiral is contrary, formed multiple be the center of circle around cylinder, the bundle of reaction tubes in different circle footpath, stainless steel capillary two ends are connected on import and export tube sheet, reaction tube is not only by described stainless steel capillary pipe, is also heat-transfer pipe.
Novel high flux multi-layer helical as above is around pipe micro passage reaction, preferably, each interlayer of described stainless steel capillary is equipped with fixing filler strip, to ensure longitudinal direction, horizontal spacing, the longitudinal pitch of stainless steel capillary is not less than 1mm, and horizontal spacing is not less than 1mm.
Novel high flux multi-layer helical as above is around pipe micro passage reaction, and preferably, described stainless steel capillary specification is 1mm/0.15mm (external diameter/wall thickness), and material is 304 stainless steels; Described stainless steel capillary total quantity is 50 ~ 200, and single tube length is 100 ~ 300 meters.
Novel high flux multi-layer helical as above is around pipe micro passage reaction, and preferably, the spiral angle of described stainless steel capillary can change, and angle excursion is 3 ° ~ 10 °.
Novel high flux multi-layer helical as above is around pipe micro passage reaction, and preferably, described inlet-outlet tube plate is connected with adopting brazing mode between stainless steel capillary, to ensure welding quality, guarantees not leak.
Novel high flux multi-layer helical as above is around pipe micro passage reaction, and preferably, the cross section of described central support tube can be circular or regular polygon.
Novel high flux multi-layer helical as above is around pipe micro passage reaction, preferably, on import and export tube sheet, the circumference place of different-diameter is provided with the aperture identical with stainless steel capillary diameter equably to ensure the brazing of described stainless steel capillary and import and export tube sheet; Described import and export tube sheet outer ring is evenly equipped with 16 bolts hole, to ensure the connection of import and export end socket and flange.
Novel high flux multi-layer helical as above is around pipe micro passage reaction, preferably, thermostatic medium import and export section lays respectively at lower-left end and the upper right side of described cylindrical shell, the internal connection of thermostatic medium import and export section and described cylindrical shell is provided with baffle plate, to prevent the short circuit of thermostatic medium, affect the appropriate reaction temperature of reactant.
Novel high flux multi-layer helical as above is around pipe micro passage reaction, and preferably, cylindrical shell is provided with left and right bearing, to support the position of whole reactor and fixed reactor.
Novel high flux multi-layer helical as above is around pipe micro passage reaction, and preferably, the medium that thermostatic medium import and export section flows through is according to the required optimum temperature of reflection and the liquid of constant temperature, to ensure that reaction is carried out safely and efficiently.
Described novel high flux multi-layer helical is reactor around pipe micro passage reaction, is also a kind of heat exchanger, and tube side medium is reactant, and shell side medium is thermostatic medium.
Technological means disclosed in the present invention program is not limited only to the technological means disclosed in above-mentioned technological means, also comprises the technical scheme be made up of above technical characteristic.
The present invention has great advantage compared to traditional consersion unit: the charge ratio that accurately can control reactant, and strict control reaction time and reaction temperature, remove reaction heat in time, prevent " temperature runaway ", realize the safety in production of high efficiency continuously.In addition, increase yield can also be carried out by using parallel mode of amplifying, being highly suitable for the optimization from laboratory to actual production process, can greatly saving R&D costs and reaction time.
Accompanying drawing explanation
Fig. 1 is that the novel high flux multi-layer helical of the embodiment of the present invention is around pipe micro passage reaction schematic diagram.
Fig. 2 is the supporting frame schematic three dimensional views of novel high flux multi-layer helical around pipe micro passage reaction of the embodiment of the present invention.
Fig. 3 is inlet-outlet tube plate front view, the side view of novel high flux multi-layer helical around pipe micro passage reaction of the embodiment of the present invention.
Fig. 4 is the left and right bearing sectional view of novel high flux multi-layer helical around pipe micro passage reaction of the embodiment of the present invention.
Fig. 5 is that the novel high flux multi-layer helical that utilizes of the embodiment of the present invention synthesizes the esterification technique flow chart of two second methyl esters around pipe micro passage reaction.
In figure, Reference numeral is expressed as: 1a, 1b-reactant import and export section; 2a, 2b-import and export place end socket; 3a, 3b-flange; 4a, 4b-import and export tube sheet; 5-stainless steel capillary; 6-fixes filler strip; 7-cylindrical shell; 8-is around cylinder; 9a, 9b-thermostatic medium import and export section; 10a, 10b-baffle plate; The left and right bearing of 11a, 11b-; 12-central support tube; 13-support member.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, illustrate the present invention further.The example of described embodiment is shown in the drawings, and wherein same or similar label represents same or similar element or has element that is identical or similar functions from start to finish.Be exemplary below by the embodiment be described with reference to the drawings, be intended to for explaining the present invention, and can not limitation of the present invention be interpreted as.It should be noted that, the word "front", "rear" of use is described below, "left", "right", "up" and "down" refer to direction in width figure, word " interior " and " outward " refer to the direction towards or away from particular elements geometric center respectively.
Embodiment 1
The novel high flux multi-layer helical that the embodiment of the present invention proposes, around pipe micro passage reaction, see Fig. 1, mainly comprises reactant import and export section 1a, 1b, import and export place end socket 2a, 2b, flange 3a, 3b, import and export tube sheet 4a, 4b, stainless steel capillary 5, fixing filler strip 6, cylindrical shell 7, around cylinder 8, thermostatic medium import and export section 9a, 9b, baffle plate 10a, 10b, left and right bearing 11a, 11b, central support tube 12, support member 13.
Particularly, see Fig. 2, central support tube 12 two ends connect inlet-outlet tube plate 4a, 4b to ensure the rigidity of whole reactor by welding manner, around cylinder 8 and central support tube 12 on the same axis, be welded to connect by support member 13 around between cylinder 8 and central support tube 12, inlet-outlet tube plate 4a, 4b, central support tube 12, form the supporting frame of spirally-wound tube micro passage reaction around cylinder 8 and support member 13.
Described stainless steel capillary 5 along around cylinder 7 twist multi-lay winding arrange, the adjacent winding layer hand of spiral is contrary, formed multiple be the center of circle around cylinder 7, the bundle of reaction tubes in different circle footpath, described stainless steel capillary 5 two ends are connected on import and export tube sheet 4a, 4b.
End socket 2a, 2b are connected by flange 3a, 3b with import and export tube sheet 4a, 4b respectively for described import and export place.
Stainless steel capillary 5 along around cylinder 8 twist multi-lay winding arrange, the adjacent winding layer hand of spiral is contrary, formed multiple be the center of circle around cylinder 8, the bundle of reaction tubes in different circle footpath, stainless steel capillary 5 two ends are connected on inlet-outlet tube plate 4a, 4b.
In the present embodiment, each interlayer of stainless steel capillary 5 is equipped with fixing filler strip 6, and to ensure longitudinal direction, horizontal spacing, the longitudinal pitch of stainless steel capillary is 1mm, and horizontal spacing is 1mm.
In the present embodiment, stainless steel capillary 5 material is 304 stainless steels, and specification is 1mm/0.15mm (external diameter/wall thickness); Described stainless steel capillary 5 total quantity is 100, and single tube length is 180 meters.
In the present embodiment, the spiral angle of each layer of stainless steel capillary 2 successively increases progressively from inside to outside, and angle excursion is 3 ° ~ 10 °.
In the present embodiment, brazing mode is adopted to be connected between inlet-outlet tube plate 4a, 4b with stainless steel capillary 5.
In the present embodiment, the stainless steel solid round steel pipe of central support tube 12 to be external diameters be 50mm.
In the present embodiment, see Fig. 3, it is that the aperture of 1mm is to ensure the brazing of described stainless steel capillary 5 and tube sheet 4a, 4b that the circumference place of the upper different-diameter of inlet-outlet tube plate 4a, 4b is provided with diameter equably, wherein, at diameter 100mm place, pore number is 10, diameter 150mm place pore number is 15, diameter 200mm place pore number is 20, diameter 250mm place pore number is 25, diameter 300mm place pore number is 30, and therefore tube sheet having five layers of same diameter is the aperture of 1mm; Tube sheet 1 outer ring is provided with 16 bolts hole, to ensure the connection of import and export end socket and flange.
In the present embodiment, the medium that thermostatic medium import and export section (9a, 9b) flows through is according to the required optimum temperature of reflection and the liquid of constant temperature, to ensure that reaction is carried out safely and efficiently.
In the present embodiment, novel high flux multi-layer helical is reactor around pipe micro passage reaction, is also a kind of heat exchanger, and the tube side medium of reactor is reactant, and shell side medium is thermostatic medium.
Embodiment 2
Present invention also offers a kind of esterification technique flow process of the two second methyl esters of spirally-wound tube micro passage reaction synthesis utilized in embodiment 1, see Fig. 4, relate to the high-order liquid bath that two are equipped with methyl alcohol+catalyst mixed liquid and ketene dimer respectively, two explosion-proof measuring pumps, static mixer, spirally-wound tube micro passage reaction, extension tube, thermostatted water bathing pool, frozen water bathing pool, thermometric pressure instrumentation and comprise anti-explosion electric ball valve, check-valves, rupture pressure disc, explosion-proof flowmeter is at interior coupling assembling, the method comprises: by two explosion-proof measuring pumps respectively by the liquid in two high-order liquid baths successively by anti-explosion electric ball valve with return and only pump in static mixer after valve, reaction solution is fully mixed, spirally-wound tube micro passage reaction is passed into rapidly after mixing, react in the stainless steel capillary of spirally-wound tube micro passage reaction and fully carried out, liquid after having reacted in spirally-wound tube micro passage reaction is by passing in extension tube after explosion-proof flowmeter, finally deliver to rectification working process again, the method comprises: whole static mixer and spiral micro passage reaction all infiltrate in thermostatted water bathing pool to remove rapidly reaction heat or to ensure reaction temperature, guarantee that reaction is normally carried out, water bath with thermostatic control temperature is preferably 70 DEG C ~ 90 DEG C, extension tube is placed in frozen water bathing pool makes liquid in pipe cool cessation reaction.
Said method embodiment also comprises: the flow controlling described explosion-proof measuring pump, makes the flow velocity of reactant liquor in stainless steel capillary in laminar flow domain, controls the time that reactant liquor stops in stainless steel capillary simultaneously, is preferably 10 ~ 20min.
What said method embodiment was set forth utilizes the esterification technique of the two second methyl esters of spirally-wound tube micro passage reaction synthesis also as required multiple spirally-wound tube micro passage reaction can be carried out parallel connection use with increase yield, improves reaction treatment amount.
As can be seen from the above embodiments, spirally-wound tube micro passage reaction provided by the present invention and utilize the esterification technique method of the two second methyl esters of its synthesis, achieve the continuous prodution of esterification, accurately can control the charge ratio of reactant, strict control reaction time and reaction temperature, remove reaction heat in time, prevents " temperature runaway ", make product yield reach maximization, reduce the production cost of product.In addition, increase yield can also be carried out by using parallel mode of amplifying, being highly suitable for the optimization from laboratory to actual production process, can greatly saving R&D costs and reaction time.
The above is the specific embodiment of the present invention; should be understood that; for those skilled in the art; under the prerequisite not departing from the principle of the invention and aim; can also make some replacements, modification, improvements and modifications, these replacements, modification, improvements and modifications are also considered as protection scope of the present invention.
Claims (10)
1. a high flux multi-layer helical is around pipe micro passage reaction, it is characterized in that: comprise reaction-ure inlet section (1a), outlet section (1b), import department's end socket (2a), exit end socket (2b), flange (3a, 3b), import tube sheet (4a), outlet tube sheet (4b), stainless steel capillary (5), fixing filler strip (6), cylindrical shell (7), around cylinder (8), thermostatic medium inducer (9a), outlet section (9b), central support tube (12), support member (13);
Described central support tube (12) two ends connect described import tube sheet (4a) by welding manner, outlet tube sheet (4b), described central support tube (12) peripheral hardware has described around cylinder (8), described around cylinder (8) and described central support tube (12) on the same axis, describedly to be welded to connect by described support member (13) around between cylinder (8) and described central support tube (12), described import tube sheet (4a), outlet tube sheet (4b), central support tube (12), the supporting frame of spirally-wound tube micro passage reaction is formed around cylinder (8) and support member (13),
Described stainless steel capillary (5) along described around cylinder (8) twist multi-lay winding arrange, the adjacent winding layer hand of spiral is contrary, formed multiple with described around cylinder (8) be the center of circle, the bundle of reaction tubes in different circle footpath, described stainless steel capillary (5) two ends are connected in import tube sheet (4a), outlet tube sheet (4b);
Described import department end socket (2a), exit end socket (2b) respectively with import tube sheet (4a), export tube sheet (4b) and be connected by flange (3a, 3b);
The spiral angle of described stainless steel capillary (5) changes, and angle excursion is 3 ° ~ 10 °;
Described import tube sheet (4a), outlet tube sheet (4b) adopt brazing mode to be connected with between stainless steel capillary (5); The circumference place of described import tube sheet (4a), the upper different-diameter of outlet tube sheet (4b) is provided with the aperture identical with stainless steel capillary (5) diameter equably to ensure described stainless steel capillary (5) and import tube sheet (4a), the brazing exporting tube sheet (4b).
2. high flux multi-layer helical according to claim 1 is around pipe micro passage reaction, it is characterized in that, described stainless steel capillary (5) each interlayer is equipped with fixing filler strip (6), to ensure longitudinal direction, horizontal spacing; The longitudinal pitch of described stainless steel capillary (5) is not less than 1mm, and horizontal spacing is not less than 1mm.
3. high flux multi-layer helical according to claim 1 is around pipe micro passage reaction, it is characterized in that, described stainless steel capillary (5) material is 304 stainless steels; Described stainless steel capillary (5) total quantity is 50 ~ 200, and single tube length is 100 ~ 300 meters.
4. high flux multi-layer helical according to claim 1 is around pipe micro passage reaction, it is characterized in that, described import tube sheet (4a), outlet tube sheet (4b) outer ring are evenly equipped with 16 bolts hole, to ensure import end socket (2a), to export the connection of end socket (2b) and flange (3a, 3b).
5. high flux multi-layer helical according to claim 1 is around pipe micro passage reaction, it is characterized in that, described thermostatic medium inducer (9a), outlet section (9b) lay respectively at lower-left end and the upper right side of described cylindrical shell (7), described thermostatic medium inducer (9a), outlet section (9b) are provided with baffle plate (10a, 10b), to prevent the short circuit of thermostatic medium with the internal connection of described cylindrical shell (7).
6. high flux multi-layer helical according to claim 1 is around pipe micro passage reaction, it is characterized in that, described cylindrical shell (7) is provided with left support abutment (11a), right support abutment (11b), to support the position of whole reactor and fixed reactor.
7. high flux multi-layer helical according to claim 1 is around pipe micro passage reaction, it is characterized in that, the cross section of described central support tube (12) is circular or regular polygon; The medium that described thermostatic medium inducer (9a), outlet section (9b) flow through is according to the required optimum temperature of reaction and the liquid of constant temperature.
8. one kind utilizes high flux multi-layer helical described in claim 1 around the esterification process of the two second methyl esters of pipe micro passage reaction synthesis, relate to the high-order liquid bath that two are equipped with methyl alcohol+catalyst mixed liquid and ketene dimer respectively, two explosion-proof measuring pumps, static mixer, spirally-wound tube micro passage reaction, extension tube, thermostatted water bathing pool, frozen water bathing pool, thermometric pressure instrumentation and comprise anti-explosion electric ball valve, check-valves, rupture pressure disc, explosion-proof flowmeter is at interior coupling assembling, it is characterized in that: by two explosion-proof measuring pumps respectively by the liquid in two high-order liquid baths successively by anti-explosion electric ball valve with return and only pump in static mixer after valve, reaction solution is fully mixed, spirally-wound tube micro passage reaction is passed into rapidly after mixing, react in the stainless steel capillary of spirally-wound tube micro passage reaction and fully carried out, liquid after having reacted in spirally-wound tube micro passage reaction is by passing in extension tube after explosion-proof flowmeter, finally deliver to rectification working process again.
9. esterification process according to claim 8, it is characterized in that: whole static mixer and spiral micro passage reaction all infiltrate in thermostatted water bathing pool to remove rapidly reaction heat or to ensure reaction temperature, guarantee that reaction is normally carried out, water bath with thermostatic control temperature is 70 DEG C ~ 90 DEG C; Extension tube is placed in frozen water bathing pool makes liquid in pipe cool cessation reaction.
10. esterification process according to claim 8, it is characterized in that: the flow controlling described explosion-proof measuring pump, make the flow velocity of reactant liquor in stainless steel capillary in laminar flow domain, control the time that reactant liquor stops in stainless steel capillary, be 10 ~ 20min simultaneously.
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| CN102605065A (en) * | 2012-03-14 | 2012-07-25 | 华南师范大学 | Continuously mobile nest type PCR (polymerase chain reaction) microfluidic method |
| CN202898426U (en) * | 2012-07-12 | 2013-04-24 | 北京工业大学 | Space-oriented spiral micro-fluidic PCR (Polymerase Chain Reaction) real-time fluorescence detection system |
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