CN106475025A - A kind of Impinging coaxial flow reactor and the continuous method preparing nano material - Google Patents
A kind of Impinging coaxial flow reactor and the continuous method preparing nano material Download PDFInfo
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 33
- 238000011437 continuous method Methods 0.000 title claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- 238000013461 design Methods 0.000 claims abstract description 10
- 239000000376 reactant Substances 0.000 claims description 44
- 230000002572 peristaltic effect Effects 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 11
- 230000000694 effects Effects 0.000 claims description 4
- 239000007921 spray Substances 0.000 claims description 4
- 230000005611 electricity Effects 0.000 claims description 2
- 239000000047 product Substances 0.000 claims 2
- 239000007795 chemical reaction product Substances 0.000 claims 1
- 239000007791 liquid phase Substances 0.000 abstract description 8
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 230000001737 promoting effect Effects 0.000 abstract description 3
- 238000005728 strengthening Methods 0.000 abstract description 2
- 238000002834 transmittance Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 9
- 238000010079 rubber tapping Methods 0.000 description 5
- 230000035939 shock Effects 0.000 description 5
- 239000012530 fluid Substances 0.000 description 4
- 238000009527 percussion Methods 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- 238000001311 chemical methods and process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000003116 impacting effect Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
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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
- B01J14/00—Chemical processes in general for reacting liquids with liquids; Apparatus specially adapted therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/20—Jet mixers, i.e. mixers using high-speed fluid streams
- B01F25/27—Mixing by jetting components into a conduit for agitating its contents
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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
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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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
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2405—Stationary reactors without moving elements inside provoking a turbulent flow of the reactants, such as in cyclones, or having a high Reynolds-number
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F2025/91—Direction of flow or arrangement of feed and discharge openings
- B01F2025/918—Counter current flow, i.e. flows moving in opposite direction and colliding
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Abstract
The invention discloses a kind of Impinging coaxial flow reactor and the continuous method preparing nano material, can be used for liquid phase method preparation nano material.Its primary structure includes reactor inner tube, reactor outer tube, feed pipe, hot water circulation type couveuse etc..Described reactor inner and outer pipes adopt vertical design mode, keep coaxial, to form annular microchannel reaction zone；Reaction zone inner tube uniformly opens up 6 row's micropores vertically, often row micropore spacing be 12mm, radially uniform open up 5 micropores, aperture be 0.5mm, inner tube bottom lock, opening between inner and outer pipes, can make product flow out.Product formation process and reclaiming process can be carried out simultaneously, it is achieved thereby that the continuous preparation of nano material.The present invention can not only provide good reaction condition for the alternate heat of strengthening, matter transmittance process, has more great application potential in terms of promoting liquid phase method continuously to prepare nano material.
Description
Technical field
The present invention relates to continuously preparation nano material equipment and preparation method field are and in particular to a kind of connect for liquid phase method
Continue the method that the Impinging coaxial flow reactor producing nano material and liquid phase method continuously prepare nano material.
Technical background
At present, the research of nano material has become one of focus of current scientific research, and it is in magnetic material, electronics material
The aspects such as material, optical material, sensing, catalysis, high compactedness material sintering, ceramic toughening have broad application prospects, nanometer
Material market gradually expands, and creates huge economic benefit.The method of existing preparation nano material has vapor phase method, liquid phase method
And solid phase method, wherein impact-flow equipment be used for liquid phase method preparation nano material be widely used, its principle is two strands from difference
The streaming flow that direction is ejected, the place of meeting formed strong clash into, and respectively impingement region transverse and longitudinal two to forming one
Strong turbulence state, after two fluids is mutually clashed into, under the influence of frictional force, penetrates into the lateral velocity of rightabout granule
Gradually reduce, when lateral velocity reaches minima, in the presence of reverse acceleration, flow of fluid is to rightabout shock
Area, longitudinal velocity transient rise simultaneously, and reach maximum at short notice, heat transfer, mass-transfer efficiency can greatly be promoted simultaneously
Accelerate the reaction of two kinds of reactant liquors.It is successfully applied at present absorb, the chemical process such as mix, conduct heat.In recent years, people make
Also achieve impressive progress with impact flow reactor preparation field of nanometer material technology, such as T-shaped reactor, Y type microchannel road reactor.
Such as Chinese patent CN 103611487 A discloses a kind of T-shaped impact flow reactor, and reactor is single using controlling
Unit, by controlling the predetermined waveform fluctuation of two proportioning valves of inlet, reaches the effect controlling feed rate, causes striking face
Rectilinear oscillation, thus improve the facilitation for fluid mixing and chemical reaction for the impact flow reactor.Patent CN
104353405 A disclose a kind of horizontal three-dimensional percussion flow mixing reactor, and this reactor arranges three fluid streams via feed pipe
Nozzle eject, in impingement region hard hit, being sufficiently mixed and react of achievable percussion flow.For another example patent
201410843409.X discloses a kind of intensified by ultrasonic wave impact flow reactor, using percussion flow and the reinforcer simultaneously of ultrasonic wave energy
The principle of material mixing it is adaptable to fast reaction process, particularly reaction precipitation process, in order to prepare nano material.
In the impact flow reactor of the above patent, microchannel is all one-dimensional, two-dimentional, and typically two strands to three plumes
Scapus carries out clashing into, mixes so that impingement region only produces one clashes into bundle, and mixing efficiency is low, product is few it is impossible to meet actual need
Will.It is an object of the invention to overcoming traditional percussion flow list to clash into bundle, the shortcoming of low production efficiency, led to by designing new reaction
Road structure realizes multiple multiple mixing clashing into bundle it is achieved that the continuous preparation of nano material, thus improve production efficiency, solves
The limitation that preparation nano material yields poorly at present, promotes the Industrialization Progress of nano material preparation.
Content of the invention
The present invention is to improve composite rate and the production efficiency of two liquid, there is provided a kind of Impinging coaxial flow reactor, it is only
Special structure design, overcomes the single shortcoming of material impacting stream reaction channel, its inner tube opens up multiple micropores, so that reactant liquor is existed
Multiple shock bundles are produced in impingement mix and course of reaction.Can not only be good for the alternate heat of strengthening, the offer of matter transmittance process
Reaction condition, has pole promoting liquid phase method continuously to prepare the aspects such as the various chemical process of nano material and microcell mixing
Big application potential.
In order to realize this purpose, the present invention adopts the following technical scheme that：Reactor inner tubal wall opens up multiple micropores, and each is micro-
Hole and annular micro- reaction zone intersection form one and clash into bundle, based on CFD orthogonal test, optimize position of opening and micropore chi
Very little, determine the radially uniform micropore opening up 5 a diameter of 0.5mm of every row, axially 6 row's micropores are uniformly opened up with the pitch-row of 12mm
For best design, using this kind of perforate mode so that each clashes into bundle produces relatively uniform pressure environment, promote two
Planting the abundant impingement mix of reactant liquor, thus reaching the purpose of abundant reaction, obtaining the nano material of uniform particle sizes.
The Impinging coaxial flow reactor generally vertical structure of the present invention, inner and outer pipes adopt vertical design mode, in addition micro-
Hole adopts top-down multiple rows of design, can make reactant liquor in the presence of gravity and pressure, in flow process from top to bottom
In carry out multiple impacts and reaction, thus promoting being sufficiently mixed and chemical reaction of two kinds of reactant liquors.
The attemperator of the present invention adopts hot water circulation type couveuse, and the hot water of steady temperature constantly flows from bottom to top,
To keep reaction zone constant temperature, thus being applied to the preparation of nano material under different temperatures.
During preparation nano material, two kinds of reactant liquors are placed in being heated to assigned temperature in thermostat water bath (6), compacted in electronics
In the presence of dynamic pump 1 (5), reactant liquor A by feed pipe 1 (11) injecting reactor inner tube (1), under pressure, reactant liquor A by
Micropore (4) level sprays, and reactant liquor B, in the presence of electronic peristaltic pump 2 (9), is entered by feed pipe 2 (2), feed pipe 3 (12)
The micro- reaction zone of annular, reactant liquor A and reactant liquor B all produces shock bundle in each tapping, and the raw reaction of hybrid concurrency, finally the bottom of by
Flow out at portion's opening.The design of this Impinging coaxial flow reactor can make Product formation and reclaiming process carry out it is achieved that receiving simultaneously
The continuous preparation of rice material.
Using technical solutions according to the invention, can achieve following beneficial effect：
Present device small volume, simple to operate, its unique structure design is hitting of two kinds and two or more reactant liquor
Hit mixing and chemical reaction provides the chance of many places multiple impact, and uniform product can be obtained, can be used for liquid phase method
Continuous preparation nano material, also can operate with mass transfer, the heat transfer of chemical process.
Brief description
Fig. 1：The Impinging coaxial flow reactor principle schematic diagram. of the present invention.
Wherein：Reactor inner tube (1), feed pipe 2 (2), reactor outer tube (3), micropore (4), electronic peristaltic pump 1 (5), perseverance
Warm water bath (6), accumulator (7), catcher (8), electronic peristaltic pump 2 (9), hot water circulation type couveuse (10), feed pipe 1
(11), feed pipe 3 (12)
Fig. 2：Reaction zone partial schematic diagram.
Wherein：Micropore (4)
Fig. 3 (a) (b) (c)：CFD numerical simulation cloud atlas.
Wherein：Fig. 3 (a) is tapping radial section VELOCITY DISTRIBUTION cloud atlas
Fig. 3 (b) is VELOCITY DISTRIBUTION cloud atlas at the z=0 of cross section
Fig. 3 (c) is tapping streamline cloud atlas
Specific embodiment
Below in conjunction with the accompanying drawings the specific embodiment of the present invention is described in further detail：This embodiment sets
That counts can be used for continuously producing the Impinging coaxial flow reactor of nano material, and its structural representation is shown in Figure of description 1, main bag
Include reactor inner tube (1), feed pipe 2 (2), reactor outer tube (3), micropore (4), electronic peristaltic pump 1 (5), thermostat water bath
(6), accumulator (7), catcher (8), electronic peristaltic pump 2 (9), hot water circulation type couveuse (10), feed pipe 1 (11), charging
Pipe 3 (12).
In this embodiment, reactor inner tube and reaction zone outer tube all using 316L rustless steel, pipe range in reactor
200mm, internal diameter 2mm, external diameter 3mm, uniformly open up 6 row's micropores vertically, and often row's micropore spacing is 12mm, radially uniform opens up 5
Individual micropore, aperture 0.5mm.Reactor outer length of tube 120mm, internal diameter 4mm, external diameter 5mm.
In this embodiment, two kinds of reactant liquors are placed in being heated to assigned temperature, in electricity in thermostat water bath (6)
In the presence of sub- peristaltic pump 1 (5), reactant liquor A by feed pipe 1 (11) injecting reactor inner tube (1), under pressure by micropore
(4) level sprays, and reactant liquor B, in the presence of electronic peristaltic pump 2 (9), enters annular by feed pipe 2 (2), feed pipe 3 (12)
Micro- reaction zone, reactant liquor A and reactant liquor B all produces one in each tapping and clashes into bundle, and top-down multiple perforates just make
Reactant liquor creates multiple shock in top-down flow process and restraints, and then has reached reactant liquor many places, multiple shock
The raw reaction of hybrid concurrency, final reacting product is flowed out by bottom opening.
Impinging coaxial flow reactor provided by the present invention, its unique micropore perforate design, only reactor does not provide
Multiple clash into bundle, two kinds of reactant liquors also can be made to produce multiple impacts in flow process from top to bottom, further promote
The mixing of two liquid and reaction, induce explosion type forming core, can efficiently produce the little nano material of diameter.
The preparation method of nano material is as follows in this embodiment：First two kinds of reactant liquors A, B are placed in perseverance
Warm water bath is heated to assigned temperature in (6), is passed through the hot water of constant temperature to hot water circulation type couveuse (10) simultaneously, anti-to realize
Answer the constant temperature in area, electronic peristaltic pump 1 (5), electronic peristaltic pump 2 (9) are connected respectively to the feed pipe of reactant liquor A and reactant liquor B；
Open electronic peristaltic pump 1 (5), electronic peristaltic pump 2 (9), reactant liquor A, by feed pipe 1 (11) injecting reactor inner tube (1), is pressing
Power effect under, reactant liquor A by micropore (4) level spray, reactant liquor B in the presence of electronic peristaltic pump 2 (9), by feed pipe 2
(2), feed pipe 3 (12) enters annular micro- reaction zone, and reactant liquor A and reactant liquor B produces in multiple tappings and clashes into bundle, and mixing is simultaneously
React, final reacting product is flowed out by bottom opening.Product formation process and reclaiming process can be carried out simultaneously, thus real
Show the continuous preparation of nano material.
Claims (4)
1. a kind of Impinging coaxial flow reactor and the continuous method preparing nano material, can be used for solution mixing and nano material is closed
Become, its structure includes reactor inner tube (1), feed pipe 2 (2), reactor outer tube (3), micropore (4), electronic peristaltic pump 1 (5), perseverance
Warm water bath (6), accumulator (7), catcher (8), electronic peristaltic pump 2 (9), hot water circulation type couveuse (10), feed pipe 1
(11), feed pipe 3 (12).It is characterized in that, inside and outside described reactor, tube wall keeps coaxially formed annular microchannel reaction zone, interior
Bottom of the tube is closed, opening between inner and outer pipes, and product can be made to flow out.Mainly include in nano material preparation process, compacted in electronics
In the presence of dynamic pump 1 (5), reactant liquor A by feed pipe 1 (11) injecting reactor inner tube (1), in the effect of electronic peristaltic pump 2 (9)
Under, reactant liquor B enters annular micro- reaction zone by feed pipe 2 (2) and feed pipe 3 (12), due to electronic peristaltic pump 1,2 (5,9)
Effect, reactant liquor A is sprayed and clashed into reactant liquor B by micropore (4) level, the raw reaction of hybrid concurrency, and final reacting product is by ring
Flow out at the bottom opening of shape microchannel reaction zone.
2. a kind of Impinging coaxial flow reactor according to claim 1 and the continuous method preparing nano material, its feature
It is, inner and outer pipes adopt vertical design mode, micropore adopts top-down multiple rows of design, reactor inner tube is equal vertically
Even open up 6 row's micropores, often row micropore spacing be 12mm, reactor inner tube is radially uniform to open up 5 micropores, aperture 0.5mm so that
Two kinds of reactant liquors, in top-down flow process, create many places, multiple impacts in the reaction zone of annular microchannel, promote
The mixing of two kinds of reactant liquors and reaction.
3. a kind of Impinging coaxial flow reactor according to claim 1 and the continuous method preparing nano material, its feature
It is, using hot water circulation type couveuse, so that the hot water of steady temperature is entered by couveuse water inlet (a), outlet (b) flows
Go out, to keep reaction zone constant temperature, thus being applied to the preparation of nano material under different temperatures.
4. a kind of Impinging coaxial flow reactor according to claim 1 and the continuous method preparing nano material, its feature
It is, it is as follows that it continuously prepares the method for nano material：
A. two kinds of reactant liquors A, B are placed in thermostat water bath (6), are heated to assigned temperature, protect to hot water circulation type simultaneously
Incubator is passed through constant-temperature hot water in (10), so that reaction zone keeps required steady temperature, respectively by electronic peristaltic pump 1 (5), electricity
Sub- peristaltic pump 2 (9) is connected to the feed pipe of reactant liquor A and reactant liquor B；
B. electronic peristaltic pump 1 (5), electronic peristaltic pump 2 (9) are opened, reactant liquor A is by feed pipe 1 (11) injecting reactor inner tube
(1), under pressure, reactant liquor A by micropore (4) level spray, reactant liquor B in the presence of electronic peristaltic pump 2 (9), by
Feed pipe 2 (2), feed pipe 3 (12) enter annular micro- reaction zone, and reactant liquor A and reactant liquor B produces many in annular micro- reaction zone
Place, multiple impacts, reactant liquor A is sufficiently mixed with reactant liquor B and reacts, and end reaction products therefrom is flowed by bottom opening
Go out.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108325492A (en) * | 2018-03-14 | 2018-07-27 | 荆门市熊兴化工有限公司 | A kind of nitration processes and device preparing H acid |
| CN109331759A (en) * | 2018-11-26 | 2019-02-15 | 常州那央生物科技有限公司 | Tubular microreactors and the micro- reaction system of mixed method, tubular type and its working method |
| CN110605036A (en) * | 2019-08-30 | 2019-12-24 | 扬州大学 | Method for impact mixing of non-equal momentum limited jet flow |
| CN114733456A (en) * | 2022-02-28 | 2022-07-12 | 南开大学 | Liquid-drop impact micro-reactor and method for continuously preparing nano-material |
| CN116200212A (en) * | 2023-05-06 | 2023-06-02 | 中国科学院过程工程研究所 | Device and method for dry carbide slag treatment by using impinging stream |
| CN116372179A (en) * | 2023-02-06 | 2023-07-04 | 西陇科学股份有限公司 | Microreactor capable of continuously producing uniform nano silver and preparation method thereof |
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| CN204352850U (en) * | 2014-11-24 | 2015-05-27 | 沈阳化工大学 | A kind of multicomponent laminar submergence impact flow reactor |
| CN204544165U (en) * | 2014-12-30 | 2015-08-12 | 中南大学 | A kind of intensified by ultrasonic wave impact flow reactor |
| CN105771828A (en) * | 2014-12-20 | 2016-07-20 | 中国石油化工股份有限公司 | Impinging stream reactor used for liquid-liquid reaction |
| CN206838034U (en) * | 2016-11-09 | 2018-01-05 | 青岛科技大学 | A kind of Impinging coaxial flow reactor |
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| US5017728A (en) * | 1990-08-20 | 1991-05-21 | Ethyl Corporation | Tetrabromobisphenol-A process |
| CN204352850U (en) * | 2014-11-24 | 2015-05-27 | 沈阳化工大学 | A kind of multicomponent laminar submergence impact flow reactor |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108325492A (en) * | 2018-03-14 | 2018-07-27 | 荆门市熊兴化工有限公司 | A kind of nitration processes and device preparing H acid |
| CN108325492B (en) * | 2018-03-14 | 2023-12-19 | 湖北丽康源化工有限公司 | Nitration technology and device for preparing H acid |
| CN109331759A (en) * | 2018-11-26 | 2019-02-15 | 常州那央生物科技有限公司 | Tubular microreactors and the micro- reaction system of mixed method, tubular type and its working method |
| CN110605036A (en) * | 2019-08-30 | 2019-12-24 | 扬州大学 | Method for impact mixing of non-equal momentum limited jet flow |
| CN114733456A (en) * | 2022-02-28 | 2022-07-12 | 南开大学 | Liquid-drop impact micro-reactor and method for continuously preparing nano-material |
| CN116372179A (en) * | 2023-02-06 | 2023-07-04 | 西陇科学股份有限公司 | Microreactor capable of continuously producing uniform nano silver and preparation method thereof |
| CN116372179B (en) * | 2023-02-06 | 2024-03-22 | 西陇科学股份有限公司 | Microreactor capable of continuously producing uniform nano silver and preparation method thereof |
| CN116200212A (en) * | 2023-05-06 | 2023-06-02 | 中国科学院过程工程研究所 | Device and method for dry carbide slag treatment by using impinging stream |
| CN116200212B (en) * | 2023-05-06 | 2023-06-30 | 中国科学院过程工程研究所 | Device and method for dry carbide slag treatment by using impinging stream |
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| CN106475025B (en) | 2019-12-03 |
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