CN105396521B - Pisces shaped reaction device - Google Patents
Pisces shaped reaction device Download PDFInfo
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- CN105396521B CN105396521B CN201510817976.2A CN201510817976A CN105396521B CN 105396521 B CN105396521 B CN 105396521B CN 201510817976 A CN201510817976 A CN 201510817976A CN 105396521 B CN105396521 B CN 105396521B
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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
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
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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
- B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
- B01J2219/00277—Apparatus
- B01J2219/00279—Features relating to reactor vessels
- B01J2219/00281—Individual reactor vessels
-
- 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
- B01J2219/24—Stationary reactors without moving elements inside
- B01J2219/2401—Reactors comprising multiple separate flow channels
- B01J2219/2402—Monolithic-type reactors
- B01J2219/2403—Geometry of the channels
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The present invention provides a kind of Pisces shaped reaction device, including a reaction runner, two head-on collision runners, side runner, 24 branch flow passages, the import for reacting runner is connected with the shock mouthful of two head-on collision runners, react runner and branch flow passage outlet, the import of branch flow passage is connected with side runner, side runner is located at the both sides of reaction runner, compartment of terrain is located at the both sides for reacting runner to 24 branch flow passages successively, it is characterized in that, side runner is four, wherein first group of two side runners are symmetrically located at the both sides for the leading portion for reacting runner, and 6 branch flow passages that first group of two side runners close on homonymy respectively are connected；Other second group of two side runners symmetrically located at reaction runner back segment both sides, and 6 branch flow passages that second group of two side runners close on homonymy respectively connect.The present invention makes the regulation of branch flow passage flow distribution become to be more prone to, and branch flow distribution is more stable, and each operating parameter has the function of certain flexible modulation.
Description
This case is to be in August, 2014 applying date 4, Application No. 201410380345.4, entitled " Pisces shaped reaction
The divisional application of device ".
Technical field
The present invention relates to the technical field for the nano-complex particle for preparing core shell structure, specifically, the present invention is especially related to
And a kind of Pisces shaped reaction device.
Background technology
Core-shell type nano compound particle be using a size micron to nano grade particle as core, in its Surface coating number
A kind of compound heterogeneous structure of layer even film formation.It is be combined with each other between core and shell by physically or chemically acting on one
Forming composite structure is played, by controlling nucleocapsid thickness to realize the regulation and control of composite performance.By cutting out nucleocapsid structure, size,
The properties such as controllable their magnetics, optics, mechanics, calorifics, electricity, catalysis, absorption, thus with being different from monocomponent nanocomposite
The property of particle, in materialogy (such as：Solid electrolyte, semiconductor, ceramics, light-sensitive material), Chemical assembly, drug delivery, life
The numerous areas such as thing chemical diagnosis, photonic crystal, catalytic adsorption material are all widely used.
In recent years, design, synthesize single dispersing, controllable core-shell type nano compound particle as numerous hybrid materials, nanometer
The focus of the area researches such as material.The design of core shell structure is all to have very strong specific aim, such as：It is relatively stable using property
Physics, chemical change do not occur for nuclear particle in shell protection, or by shell particle and interior nuclear particle each distinctive electromagnetic property,
Optical characteristics, catalysis characteristics, characterization of adsorption assign integral etc..
Realizing industrialization low cost, producing on a large scale is with high-quality, high performance core-shell nano-composite material
The focus of Chemical Reaction Engineering technical field research.With going deep into for research, the preparation method of hud typed composite is increasingly
It is many, mainly there are surface deposition, ion-exchange, sonochemical method, self-assembly method (electrostatic assembly, vapour deposition, chemical plating)
Deng, but there are three obvious technological deficiencies in existing method：1) during coating, nano inner core particle is easily reunited；2)
Cladding precursor is intended to itself nucleation, rather than is coated to the surface of interior nuclear particle；3) film of cladding is uneven, imperfect.
The Chinese invention patent application of Application No. 201210394616.2 discloses a kind of Road narrows formula impact flow reactor, its
Road narrows are laid out in shaped heat dissipating fins, and Road narrows include sprue, side runner and branch flow passage, and outside feed liquid induction system is conveyed not to Road narrows
Same feed liquid, each feed liquid collides in Road narrows, ultimately produces the particle with core shell structure, but the Road narrows formula shaped heat dissipating fins are anti-
Answer device can not ensure that reaction and deposition process are carried out only in sprue first, the super of high frequency direction transformation can not be also produced in addition
Effect that weight position and high frequency liquid-liquid film hit, therefore, it is impossible to realize effect of multiple dimensioned mixing, is an impediment to prepare nucleocapsid
Type nano composite material.
The Chinese invention patent application of Application No. 20130087052.2 discloses a kind of fish shaped reaction device, and the reactor is first
First ensure that reaction and deposition process are only carried out in reaction runner, disclose in addition inside reactor structural parameters and operating parameter it
Between inner link, and can realize high frequency direction transformation super gravity field, high frequency liquid-liquid film hit, etc. frequency hit and
The effects such as isoconcentration is coated.But the fish shaped reaction device still suffers from apparent technological deficiency：
First, in fish shaped reaction device, every side runner is connected with 12 Zhi Liuliang, the tributary connected due to side runner
Road number is too many, causes flow design and regulation to become extremely difficult, and the flow distribution of branch flow passage is very unstable.
Second, each main operating parameters are restricted clearly by branch flow passage flow distribution, whole reactor is lacked spirit
The function of modulation living, causes fish shaped reaction device to lack necessary modulation function.
3rd, in fish shaped reaction device, because the projected angle of impact of high frequency liquid-liquid film knockout process is higher than 60 degree, formed
Elastic Impact, Elastic Impact is unfavorable for reacting covering liquid in the slurries and branch flow passage in runner between the two quick mixed
Close.
Therefore, it is necessary to carry out structure improvement and optimization to the fish shaped reaction device.
The content of the invention
It is an object of the invention to provide a kind of Pisces shaped reaction device, to solve the operational and real of existing fish shaped reaction device
With property it is not good the problem of.
In order to solve the above problems, the technical scheme that the present invention is provided is：
A kind of Pisces shaped reaction device, including reaction runner, two head-on collision runners, side runner, 24 branch flow passages, it is described
The import for reacting runner is connected with the shock mouthful of two head-on collision runners, and the reaction runner is exported with the branch flow passage to be connected
Logical, the import of the branch flow passage is connected with the side runner, and the side runner is located at the both sides of the reaction runner, described in 24
Compartment of terrain is located at the both sides for reacting runner to branch flow passage successively, wherein, the side runner is four, wherein two of first group
The side runner symmetrically located at it is described reaction runner leading portion both sides, and first group two side runners respectively with together
6 branch flow passage connections that side is closed on；Other second group of two side runners are symmetrically located at the reaction runner
The both sides of back segment, and 6 branch flow passages that second group of two side runners close on homonymy respectively connect.
According to a kind of preferred embodiment of above-mentioned Pisces shaped reaction device, along the length direction of the reaction runner, institute
Stating reaction runner includes multiple semicircular segmental arcs set gradually, and causes the overall undulate of reaction runner.
According to a kind of preferred embodiment of above-mentioned Pisces shaped reaction device, the number of the segmental arc is more than or equal to described
The number of branch flow passage.
According to a kind of preferred embodiment of above-mentioned Pisces shaped reaction device, the connectivity points of the reaction runner and branch flow passage exist
Residing angle is referred to as confluent angle in the segmental arc, and the confluent angle is equal between the reaction runner and the branch flow passage
Converge angle.
According to a kind of preferred embodiment of above-mentioned Pisces shaped reaction device, the confluent angle, converge angle between 0 to 60 degree
Between.
According to a kind of preferred embodiment of above-mentioned Pisces shaped reaction device, the confluent angle, converge angle between 30 degree to 60
Between degree.
According to a kind of preferred embodiment of above-mentioned Pisces shaped reaction device, the confluent angle, converge angle for 45 degree.
According to a kind of preferred embodiment of above-mentioned Pisces shaped reaction device, in the import and outlet of the reaction runner
Between, along the length direction of the reaction runner, the diameter of the segmental arc gradually increases.
Analysis understands that the present invention carries out structure improvement and optimization by the fish shaped reaction device to prior art, makes branch flow passage
The regulation of flow distribution becomes to be more prone to, and branch flow distribution is more stable, and each operating parameter has the work(of certain flexible modulation
Can, it can be widely used for preparing the nano-complex particle of various core shell structures.Further, the present invention can also make slurries and cladding
Shock between liquid reaches non-resilient shock, quick mixing of both promotions on molecular scale
Brief description of the drawings
Structure drawing of device when Fig. 1 applies for the embodiment of the present invention；
Fig. 2 is the internal structure Parameter Map of the embodiment of the present invention；
The signal that changes and branch flow passage of the Fig. 3 for super gravity field direction in the reaction runner of the reaction embodiment of the present invention are connected
Figure；
Fig. 4 is the TEM electromicroscopic photographs of the nano-complex particle with core shell structure prepared by the embodiment of the present invention；
Fig. 5 is super gravity field direction change frequency in the embodiment of the present invention with the variation diagram for hitting number of times.
Fig. 6 is sample manufactured in the present embodiment and pure nanometer Fe3O4The XRD spectra of particle.
Embodiment
The present invention is described in further details with reference to the accompanying drawings and detailed description.
Fig. 1 shows structure when one embodiment of the invention is applied, Pisces shaped reaction device provided in an embodiment of the present invention with
Feed liquid is supplied and storage system connection, and the supply of this feed liquid and storage system include six storage tanks, can produce stable and continuous
The high-pressure air source of nitrogen N 2 is (such as：Air compressor or cyclinder gas) and a plurality of connecting line, pipe fitting, multiple flowmeters 17
(including fluid flowmeter and gas flowmeter), pressure gauge (not shown), triple valve 18 etc..Six storage tanks be respectively storage tank 11,
Storage tank 12, storage tank 13, storage tank 14, storage tank 15, storage tank 16, because of institute's material stock liquid quantity, property difference, the size of each storage tank,
Material etc. is also different, in this regard, it should be understood by those skilled in the art that.
As shown in Figure 1, Figure 2, Figure 3 shows, Pisces shaped reaction device provided in an embodiment of the present invention is included：1 reaction runner 5,2
Clash runner 2,4 side runners and 24 branch flow passages 6, wherein, side runner includes being located at two sides of reaction runner 5 leading portion both sides
Runner 4, two side runners 3 positioned at reaction runner 5 back segment both sides.React the import and the shock of two head-on collision runners 2 of runner 5
Mouthful connection, reaction runner 5 and the outlet of branch flow passage 6, the import of branch flow passage 6 is connected with side runner 3,4,24 branch flow passages 6 according to
Respectively there are 12 branch flow passages located at the both sides of reaction runner 5, namely in the both sides of reaction runner 5 minor tick.Two 4 pairs of side runners
Ground is claimed to be connected located at the leading portion both sides of reaction runner 5, and 6 branch flow passages 6 that each side runner 4 closes on homonymy respectively.Two
Side runner 3 is symmetrically located at the back segment both sides of reaction runner 5, and 6 branch flow passages 6 that each side runner 3 closes on homonymy respectively
Connection.
24 branch flow passages 6 are divided into four groups, every group of 6 branch flow passages 6 are connected with a side runner 3 or side runner 4, are easy to control
Make the flow of 24 branch flow passages 6.Overall View it, the present embodiment exactly likes two travelling fishes from the appearance, therefore is referred to as double
Fish shaped reaction device.
As shown in Fig. 2 on reaction runner 5, reacting the length length between the import of runner 5 and adjacent branch flow passage 6
Parameter a0Length between expression, the import of each adjacent branch flow passage 6 is respectively with 23 length parameter a1~a23Represent；24 tributaries
The length in road 6 is respectively with other 24 length parameter l1~l24Represent；On side runner 3,4, between the import of adjacent branch flow passage 6
Length respectively with other 22 length parameter L1~L16Represent.
Preferably, the width of all runners is 1.1mm, and depth is 5.0mm.React the connection of runner 5 and branch flow passage 6
Part is by multiple more than or equal to the number of branch flow passage 6, such as 24, and the segmental arc 31 (half round runner) that radius changes from small to big
Docking is formed so that reaction runner 5 is in the waveform that overall width gradually increases.24 branch flow passages 6 are symmetrically arranged in reaction
The both sides of runner 5.Such as Fig. 3, angle of the joint residing in segmental arc 31 between reaction runner 5 and branch flow passage 6 is referred to as handing over
Converge angle, confluent angle is equal between reaction runner 5 and branch flow passage 6 and converges angle, confluent angle, converge angle be preferably between 0 to 60 ° it
Between, it is highly preferred that between 30 to 60 °, such as in Fig. 3, confluent angle, to converge angle size be 30 °, still, confluent angle, remittance
Close angle and be preferably equal to 45 °.Again as shown in figure 3, making outlet in the stainless steel lag screws 8 that each exit of branch flow passage 6 inserts a 1mm
Flow area reduced width is to below 0.1mm.
Below in conjunction with the application of the present embodiment, the parameter to each runner in the present embodiment is described in detail, in order to
Skilled artisan understands that of the invention.
Before nano-complex particle is prepared, it is necessary first to test to adjust the flow of each runner by repetition several times
Reach design requirement.The device of experiment is repeated every time all as shown in figure 1, using a gas flowmeter to two head-on collision runners 2
The total flow of middle feed liquid is controlled, the flow of uncomfortable solar term flowmeter body during material is walked, only using two fluid floies
The total flow of each 12 branch flow passages 6 in both sides before and after the accurate control of meter, and determine the volume of feed liquid in outlet feed liquid unit interval
(volume for the feed liquid that storage tank 16 is received), then calculates the total flow of two head-on collision runners 2, gas is adjusted according to result of calculation
Flowmeter carries out next experiment again, until the flow reaches sets requirement.
The adjusting method of assignment of traffic is to insert stainless steel lag screws into the big head-on collision runner 2 of flow in two head-on collision runners 2,
The distribution of flow is controlled by adjusting the flow area of stainless steel lag screws, until the feed liquid in two head-on collision runners 2 has flowed simultaneously
Untill.
The indicator that the flow of 4 side runners 3,4 and the flow of 24 branch flow passages 6 are exported by storage tank 12 observes flow
Size.In experimentation, triple valve 18 is opened, indicator is flowed to the side runner 3,4 and branch flow passage 6 of front and rear sides respectively
In, if the import of two side runners 3 changes colour simultaneously, illustrate that the flow of 2 side runners 3 is equal, if corresponding 12 branch flow passages 6
Outlet changes colour simultaneously, illustrates that the flow of 12 branch flow passages 6 has reached design requirement.If above-mentioned flow is not reaching to requirement,
Insert a diameter of 1mm stainless steel lag screws 8 to adjust the stream of these runners by the specified location into branch flow passage 6 and side runner 3
Amount.In a word, the regulation to the present embodiment flow needs certain regulation number of times and tested repeatedly.
When indicator is flowed into side runner 3,4 and branch flow passage 6, if the same time-varying of import of two side runners 3 or side runner 4
Color, and corresponding 12 branch flow passages 6 outlet also simultaneously change colour when, the internal structure parameter (as shown in Figure 2) of the present embodiment and
Just the contact of inherence is there occurs between flow, collision frequency, exit precursor concentration distribution parameter, it is as follows：
Coat in the total flow of the output of liquid storage tank 13,15 and the flow and 24 branch flow passages 6 in two pairs of side runners 3,4
There is following relational expression in flow：
F1-24=F1-12+F13-24 (1)
F1-12=F1-11+F2-12 (2)
F13-24=F13-23+F14-24 (3)
F1-11=F1+F3+F5+F7+F9+F11 (4)
F2-12=F2+F4+F6+F8+F10+F12 (5)
(1) F in formula1-12And F13-24(Fig. 1, Fig. 2 are marked to this two parameters, and each F represents flow) is two
Individual cladding liquid storage tank 13,15 respective total flows, F1-24Then represent cladding flow quantity sum；(2) F in formula and (3) formula1-11、
F2-12、F13-23And F14-24(Fig. 1, Fig. 2 are marked to this four parameters) is four side runners 3,4 respective total flows；
(4), (5) formula gives the relation between six flows of branch flow passage 6 that the total flow of side runner 3 is connected with it.For effluent
Discharge relation between road 4 and corresponding branch flow passage, can be analogized according to (4), (5) formula.In (4), (5) formula, 6 tributaries
Flow distribution principle between road 6 is equal to the Distribution Principle of 12 branch flow passages in the fish shaped reaction device of prior art, i.e. branch flow passage 6
Flow distribution is associated with the drawingdimension of side runner 3 and branch flow passage 6, and correlation is as follows：
, can be according to (6), (7) for the relation between side runner 4 and the flow distribution and runner design size of branch flow passage 6
Formula is analogized.
Due to inserting some nails in branch flow passage 6 and side runner 3,4, the volume of nail does not calculate above formula
It is central, so in the presence of certain systematic error, why it is referred to as systematic error, it is due to when designing the present embodiment and does not know
Several nails can be inserted in each runner in road, result in and there is certain deviation between design discharge and actual flow.In addition, seeing
Examine in each runner color change process that there is also certain accidental error.
Hit and 24 collision time intervals in addition, co-existing in 25 times in reaction runner 5, therefore, also there is 24
Collision frequency is distributed, this 24 collision frequency f distributions and the initial flow F of reaction runner 50, 24 Zhi Liuliang and reaction streams
There is following relation between the size of road 5：
The frequency distribution and collision frequency distribution of overweight force direction transformation are essentially identical, do not elaborate herein.
In reaction runner 5 there is following relational expression in flow velocity u distribution：
The distribution of the horizontal g' of super gravity field in reaction runner 5 can be calculated according to the distribution of flow velocity, relational expression is as follows：
According to the distribution of flow and the concentration of covering in storage tank in each flow distribution of branch flow passage 6, reaction runner 5, when
The concentration c distribution of cladding precursor can be calculated under conditions of microcosmic mixing is highly uniform, relational expression is as follows：
It is can be seen that from relation above formula for the present embodiment, Zhi Liuliang distribution is basis, it is necessary to be designed, see
Examine, adjust and check, its distribution to other important response parameters plays important influence.And suspension initial flow F0
It is an independent variable for branch flow distribution
Followed by the preparation process of the nano-complex particle of core shell structure：High pressure gas valve is first turned on, is made certain
The N2 gases (5atm) of pressure enter in other storage tanks outside storage tank 16, under the pressure effect of gases at high pressure, oppress each storage
Feed liquid in tank is flowed into the Pisces shaped reaction device of the present embodiment, the feed liquid from storage tank 11 first with the feed liquid from storage tank 14
Clash the strong slurries for hitting generation nano inner core particle of the exit of runner 2 generation, reaction of the slurries along bending at two
Formd during the flow at high speed of runner 5 high-frequency direction transformation super gravity field (such as Fig. 5, wherein, ordinate represents hypergravity
, abscissa represent hit number of times), and this super gravity field effect under with the feed liquid from storage tank 13 and storage tank 15 at 24
Strong shock occurs for the exit of branch flow passage 6, and this strong shock greatly enhances the feed liquid of branch flow passage 6 and reaction runner 5
In slurries between Jie see and micro mixing, exceed dispersion rate of the cladding precursor in slurries that reaction is generated
Homogeneous nucleation rate, the Determining Micromixing Characteristic Time of cladding precursor is shorter than nucleation induction period, and then realizes cladding precursor
Out-phase uniformly coats nucleation process.Hit end rear slurry to be expelled in storage tank 16 from reaction runner 5 exit, produce hud typed
The slurries of nano-complex particle, then obtain final products by a series of last handling process.Before splicing or after splicing, if needing
Branch flow passage flow distribution situation is observed, triple valve 18 can be opened, separately flows into the indicator in storage tank 12 front and rear each 12
Observed in branch flow passage 6, during splicing, triple valve 18 is closed all the time.
Fe is prepared with the present embodiment3O4Exemplified by/MnOOH nano-complex particles, storage tank 11 is ferric sulfate, ferrous sulfate and very
A small amount of manganese sulfate mixed solution, storage tank 14 is sodium hydroxide solution, and storage tank 13,15 is that the mixing of manganese sulfate and hydrogen peroxide is molten
Liquid, storage tank 12 is red indicator storage tank.In experimentation, the feed liquid of storage tank 11 and storage tank 14 is exported in head-on collision runner 2 first
The strong nanometer Fe for hitting generation black occurs for position3O4Kernel gel particles and minimal amount of Mn (OH)2Milky colloidal sol,
This colloidal sol easily generates MnOOH by hydrogen peroxide oxidation, therefore can protect nanometer Fe3O4Fe in kernel2+, prevent it double
Oxygen water oxygen.The black slurries (slurries show strong basicity, wherein containing sodium hydroxide) of generation in quick flow process forward,
Occurs strong shock with the mixed solution of the manganese sulfate from storage tank 13,15 and hydrogen peroxide, sodium hydroxide reacts first with manganese sulfate
Generate Mn (OH)2, then with hydrogen peroxide react generation black MnOOH be coated to Fe3O4Core surface, obtains Fe3O4/ MnOOH receives
Rice compound particle.Confluent angle between branch flow passage 6 and reaction runner 5 is 30 degree, as shown in Figure 3.
By testing the nano-complex particle that clad ratio to be prepared is 0.125.The Mn/Fe that clad ratio refers in product rubs
You compare.When preparing the product, branch flow passage flow distribution is：F1-12=6.67ml/s, F13-24=8.33ml/s, as shown in Figure 4；
It is F to react the initial flow of runner 50=10.0ml/s.Different claddings can be realized by adjusting the concentration of storage tank 14,13,15
Rate.
TEM/EDS (high-resolution projects Electronic Speculum/energy spectrum analysis), XRD (X-ray crystal diffractions point have been carried out to gained sample
Analysis), VSM (specific saturation magnetization) and BET (specific surface area) analyze.Fig. 4 show the TEM electromicroscopic photographs of the sample of acquisition,
The particle that Nano composite granules are almost sphericals, the very clean light of particle surface are can be seen that from the TEM electromicroscopic photographs of low power number
Sliding, particle shows good dispersiveness.The small lattice of the class quasi-lattice of surface coating layer are can see from high power TEM electromicroscopic photographs
These sub-boxes and nanometer Fe on son, surface3O4The lattice of kernel is entirely different.It follows that why the latter
Particle surface is very clean smooth, is because surface coating layer has occurred in that partially-crystallized phenomenon.Fig. 6 is that the sample is (empty
Stem is represented) and pure nanometer Fe3O4The XRD spectra of particle (solid post is represented).From XRD spectra as can be seen that the sample with
Pure nanometer Fe3O4Spectrogram is basically identical, and other crystalline phases are not found, illustrates that MnOOH only has heterogeneous nucleation not have homogeneous nucleation, does not also have
There is generation amorphous phase precipitation, because if some clouds and mists can be observed from TEM electromicroscopic photographs by amorphous phase precipitation occur
Reunion is very serious between shape or detritus, and particle.The BET specific surface area measured value of the sample is 90.53m2/
G and VSM specific saturation magnetization results are 61.1emu/g.In a word, the nano-complex particle has good magnetic intensity and paramagnetic
Property and very high specific surface area.
Specifically, the Pisces shaped reaction device that either the fish shaped reaction device of prior art or the present invention are provided all is included
24 branch flow passages, the two reactors should all have the function of significantly strengthening multiple dimensioned mixing to make from engineering philosophy
For the nano-complex particle with core shell structure is gone out, so-called multiple dimensioned mixing refers to contain micromixing, is situated between and sees mixing and micro-
See the mixing of three kinds of different scales in being blended in.In the two reactors, the object of multiple dimensioned mixing is nano suspending liquid
Multiple dimensioned between covering liquid mixes.Reinforcing micromixing is the macroscopic view distribution by 24 branch flow passages to suspension formation 24
What secondary high-frequency shock was realized.The knockout process between covering liquid and suspension includes four steps every time：(1) covering liquid is hit
Enter in suspension；(2) react generation cladding presoma with suspension；(3) presoma Quick uniform in suspension is coated
Ground is dispersed into very low concentration；(4) the cladding presoma of low concentration all deposits to a nanometer nuclear particle by heterogeneous nucleation process
Surface completes once to coat process.
If being less than the adjacent time interval hit twice the total time of aforementioned four step, (inverse of time interval is to hit
Hit frequency), it is possible to ensure that concentration distribution of the covering liquid in suspension reaches floor level, otherwise, covering liquid is in suspension
In concentration distribution will raise and cause the appearance of homogeneous nucleation.
In addition, Zhi Liuliang macroscopic view distribution is not only the basis for strengthening micromixing, due to point of other important parameters
Cloth includes：In collision frequency, knockout process precursor concentration distribution, impact strength, super gravity field level etc. all with this 24 branch
The macroscopic view distribution of flow has a close association, and these above-mentioned parameters some see mixing to being situated between and play a decisive role, some are right
Microcosmic mixing plays a decisive role, therefore, and Zhi Liuliang macroscopic view distribution is also that reinforcing Jie sees mixing and the microcosmic basis mixed.By
This draws a conclusion, and played for reactor is basic effect for Zhi Liuliang macroscopic view distribution.
The flow of each 12 branch flow passages in every side is mutual tight association in fish shaped reaction device, and Pisces shaped reaction device will
Each 6 branch flow passages each side 12 branch flow passages are divided into again before and after, this branch flow passage number that just makes to be mutually related is subtracted by 12
As little as 6.From formula (4), (5) it can be seen that the structure limitation parameter of Pisces shaped reaction device branch flow distribution reduces half
It is many, the adjustability of branch flow distribution is enhanced in turn.The adjustability enhancing of branch flow distribution, makes other important parameter distributions
Adjustability also strengthens therewith.Furthermore, because the flow distribution of branch flow passage is what is realized by adjusting the pressure distribution of branch flow passage, stream
Mutual restriction between amount distribution, necessarily causes the mutual restriction between pressure distribution.Therefore, mutually restriction is got between Zhi Liuliang
By force, the mutual restriction between pressure is also stronger, can be more difficult and more unstable for regulation flow distribution.So, Pisces
Shaped reaction device not only increases the adjustability of flow distribution, also enhances the adjustability of pressure distribution.Experiment discovery, fish shaped reaction
The branch Flow-rate adjustment of device is extremely difficult, is almost difficult to realize, comparatively, and the branch Flow-rate adjustment of Pisces shaped reaction device is then held very much
Easily realize, the branch flow distribution regulated is changed by other independent parameters (refers mainly to suspension initial flow F0Change) it is anti-
Interference performance is remarkably reinforced.From macroscopically analyzing, due to 24 branch flow passages need the continuous both sides for hitting suspension thread and
Zhi Liuliang is consecutive variations, is divided into each 12 of left and right two halves, although solve symmetrical sex chromosome mosaicism, but the chi of consecutive variations
Degree is too big, is further divided into all around each 6, then solves the scale problem of consecutive variations substantially, and this also complies with " all one's life
The metaphysics of two, two lifes four, four life everythings ".
In addition, in Pisces shaped reaction device, can be in main flow direction when suspension flows in half round runner high speed
Vertical plane on form the flowing of a secondary superposition, be referred to as Secondary Flow or dien vertex in engineering.Half round runner relative to
Dien vertex is more readily formed in waveform runner.Further, since the outlet stream section of 24 branch threads is less than 0.1 millimeter, therefore,
Collision between branch thread and suspension belongs to the shock of high speed thin liquid film, for the shock between high speed thin liquid film from 20th century 50
Just there has been numerous studies report in age, and when the projected angle of impact of thin liquid film is more than 60 degree, this shock belongs to elastic collision, touches
Breakhead degree belongs to inelastic collision between being spent 0 to 60.Inelastic collision can greatly be strengthened between two stock material liquid in molecule
Mixing on yardstick.Therefore, the collision in Pisces shaped reaction device between branch thread and suspension thread belongs to non-resilient shock, and
Shock in fish shaped reaction device therebetween belongs to Elastic Impact.
Because the width of fish shaped reaction device, Pisces shaped reaction device internal-response runner is all 1.1 millimeters, suspension and cladding
The mixing that liquid is carried out in the reaction runner of 1.1 mm wides belongs to Jie and sees mixing.Be situated between the step of seeing mixing in two reactors
Including first three step in four steps described above.In order to prevent covering liquid reacts with suspension in the moment of contact from generating
(precipitation from homogeneous solution includes two ways to precipitation from homogeneous solution：Generation nucleus or amorphous sediment) also need to meet two preconditions：The
One, the concentration of covering liquid can be diluted to needed for homogeneous nucleation in extremely short moment below critical concentration, prevent from forming nucleus
Shape is precipitated；Second, continuing rapid dilution on this basis prevents generation amorphous phase precipitation.In order to meet first premise bar
Part, the mode that 24 high speed thin liquid films hit suspension must be non-Elastic Impact, i.e. branch thread and reaction runner converges angle
It is necessarily less than 60 degree；In order to meet second precondition, the suspension flowed in reaction runner, which necessarily be formed, to be rotated at a high speed
Dien vertex Forced Dispersion, that is, need to form continual super gravity field.Therefore, Pisces shaped reaction device can pass through 24 non-ballistic
Property thin liquid film hit and the dien vertex of continuous semicircle reaction flow passage formation high intensity sees mixing to strengthen to be situated between, still
Fish shaped reaction device hit due to stiff thin liquid film can not be formed and dien vertex intensity also than relatively low, therefore, fish shape is anti-
Answer the effect for the sight mixing that is situated between in device substantially poor.
The influence that the micro mixing for coating presoma coats process for heterogeneous nucleation is mainly reflected in two aspects：
First, microcosmic mixability is higher, and coating is finer and close；Second, when microcosmic mixability reaches equally distributed state, nucleation
Process only by the assertive evidence dynamics Controlling of heterogeneous nucleation, is not disturbed by microcosmic mixing.
The main distinction of the Pisces shaped reaction device with fish shaped reaction device on reaction runner design is：Fish shaped reaction device it is anti-
It is that linear pattern or wave are linear to answer runner, and linear pattern can not produce super gravity field (i.e. centrifugal force field), the structure of wave line style
Not specific enough and clear and definite, the super gravity field of generation is often consecutive variations.The reaction runner of Pisces shaped reaction device is continuous
Semi-circular runner docking is formed, and the structure of this runner is specific and clear and definite, and super gravity field exists and positive and anti-all the time
It it is non-consecutive variations (as shown by the arrows in Figure 3) to super gravity field.In Pisces shaped reaction device, due to the nanometer in suspension
The super gravity field that nucleus is overturned by high frequency direction is acted on, and occurs high-frequency intense oscillations, this high-frequency to shake strongly
Flowing of the feed liquid in micro-scale can significantly be strengthened with mixing by swinging, and then realize quick micro mixing, more anti-than fish shape
Device is answered to be more beneficial for forming out-phase homogeneous nucleation cladding process.
In summary, the achievable advantages below of the present invention and effect：
1st, branch flow distribution is more easily adjusted, and the branch flow distribution regulated has very high stability, therefore, more
It is easy to operate and prepares the nano-complex particle of core shell structure.
2nd, can with the other important parameters of time modulation distribution, the modulation of fish shaped reaction device in this respect is very poor, lacks
Necessary flexibility.
3rd, it can be used for the nano-complex particle for preparing core-shell structure copolymer-shell structure, and fish shaped reaction device can only prepare core-shell structure copolymer
The nano-complex particle of type structure.
4th, the super gravity field of the reverse discontinuous change of both forward and reverse directions can be produced.
5th, the collision between interior branch thread and suspension thread belongs to inelastic collision, and this collision can make two stock material liquid
Mixed on molecular scale.
6th, with multiple dimensioned mixed function is strengthened, uniform heterogeneous nucleation process is realized.
As known by the technical knowledge, the present invention can be by the embodiment party of other essence or essential feature without departing from its spirit
Case is realized.Therefore, embodiment disclosed above, for each side, is all merely illustrative, and is not only.Institute
Have within the scope of the present invention or be included in the invention in the change being equal in the scope of the present invention.
Claims (8)
1. a kind of Pisces shaped reaction device, including reaction runner, two head-on collision runners, side runner, 24 branch flow passages, described anti-
The import of runner is answered to be connected with the shock mouthful of two head-on collision runners, the reaction runner and the branch flow passage outlet,
The import of the branch flow passage is connected with the side runner, and the side runner is located at the both sides of the reaction runner, 24 branch
Compartment of terrain is located at the both sides for reacting runner to runner successively, it is characterised in that the side runner is four, wherein first group
Two side runners are symmetrically located at the both sides of the leading portion of the reaction runner, and first group of two side runners difference
Connected with 6 branch flow passages that homonymy closes on；
Other second group of two side runners are symmetrically located at the both sides of the back segment of the reaction runner, and the two of second group
6 branch flow passages that side runner described in bar closes on homonymy respectively are connected.
2. Pisces shaped reaction device according to claim 1, it is characterised in that along the length direction of the reaction runner,
The reaction runner includes multiple semicircular segmental arcs set gradually, and causes the overall undulate of reaction runner.
3. Pisces shaped reaction device according to claim 2, it is characterised in that the number of the segmental arc is more than or equal to institute
State the number of branch flow passage.
4. Pisces shaped reaction device according to claim 3, it is characterised in that the connectivity points of the reaction runner and branch flow passage
Residing angle is referred to as confluent angle in the segmental arc, and the confluent angle is equal between the reaction runner and the branch flow passage
Converge angle.
5. Pisces shaped reaction device according to claim 4, it is characterised in that the confluent angle, converge angle between 0 to 60 degree
Between.
6. Pisces shaped reaction device according to claim 5, it is characterised in that the confluent angle, converge angle between 30 degree extremely
Between 60 degree.
7. Pisces shaped reaction device according to claim 6, it is characterised in that the confluent angle, converge angle for 45 degree.
8. Pisces shaped reaction device according to claim 2, it is characterised in that in the import and outlet of the reaction runner
Between, along the length direction of the reaction runner, the diameter of the segmental arc gradually increases.
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Citations (5)
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|---|---|---|---|---|
| DE102005048201A1 (en) * | 2004-10-11 | 2006-04-20 | Penth, Bernd, Dr. | Method and device, for continuous precipitation of nanoscalic product, comprises preparing primary particles by chemical reaction precipitating and optionally modifying the particle surface by chemical precipitating or co-precipitating |
| CN102151533A (en) * | 2011-01-26 | 2011-08-17 | 深圳航天科技创新研究院 | Preparation method of micro-nanometer powder, reinforced micro-reaction device and micro-reaction system |
| CN102872791A (en) * | 2012-10-17 | 2013-01-16 | 浙江海洋学院 | Magnetic nanometer lithium ion sieve adsorbent and preparation method thereof |
| CN103127888A (en) * | 2013-03-18 | 2013-06-05 | 浙江海洋学院 | Fish-shaped reactor |
| CN204034676U (en) * | 2014-08-04 | 2014-12-24 | 浙江海洋学院 | Pisces shaped reaction device |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5076742B2 (en) * | 2006-09-01 | 2012-11-21 | 東ソー株式会社 | Microchannel structure and microparticle manufacturing method using the same |
| US8524173B2 (en) * | 2006-09-01 | 2013-09-03 | Tosoh Corporation | Microchannel structure and fine-particle production method using the same |
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2014
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| DE102005048201A1 (en) * | 2004-10-11 | 2006-04-20 | Penth, Bernd, Dr. | Method and device, for continuous precipitation of nanoscalic product, comprises preparing primary particles by chemical reaction precipitating and optionally modifying the particle surface by chemical precipitating or co-precipitating |
| CN102151533A (en) * | 2011-01-26 | 2011-08-17 | 深圳航天科技创新研究院 | Preparation method of micro-nanometer powder, reinforced micro-reaction device and micro-reaction system |
| CN102872791A (en) * | 2012-10-17 | 2013-01-16 | 浙江海洋学院 | Magnetic nanometer lithium ion sieve adsorbent and preparation method thereof |
| CN103127888A (en) * | 2013-03-18 | 2013-06-05 | 浙江海洋学院 | Fish-shaped reactor |
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| CN104128137B (en) | 2016-01-13 |
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