CN206688701U - Hit target formula supersonic flow and accelerate low fever solid phase reaction device - Google Patents
Hit target formula supersonic flow and accelerate low fever solid phase reaction device Download PDFInfo
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- CN206688701U CN206688701U CN201720186251.2U CN201720186251U CN206688701U CN 206688701 U CN206688701 U CN 206688701U CN 201720186251 U CN201720186251 U CN 201720186251U CN 206688701 U CN206688701 U CN 206688701U
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Abstract
Target formula supersonic flow, which is hit, the utility model discloses one kind accelerates low fever solid phase reaction device, the device includes air-flow supply unit, solid material particle supply unit, reactor, reactor includes supersonic nozzle, mixing accelerating chamber, target head, coaxial direction is through setting axial admission pipe inside supersonic nozzle, the arrival end connection hopper and powder feeder, the port of export of axial admission pipe of axial admission pipe extend to mixing accelerating chamber.The utility model is by controlling rare earth chemical reaction process in supersonic flow, and quantitative measurment relevant parameter, solve seizure about transient state interphase during synthesis in solid state and determination, the evolutionary step of transient state interphase, each step speed determination the problems such as, there is important application value.
Description
Technical field
The system that the utility model is related to low fever solid phase reaction synthesis condensed state matter, and in particular to based on supersonic flow
Accelerate the low fever solid phase reaction complexes and its application process with impacting technology.
Background technology
Low fever solid phase reaction synthetic technology is material new preparation technology fast-developing in recent years, it is characterised in that room temperature or
Energy transmission under low temperature, i.e., by introducing mechanical energy into powdered reaction agent system, and it is allowed to be changed into the change of reaction system
Energy is learned, so as to realize the synthesis in solid state under room temperature or low temperature.Low fever solid phase reaction synthetic technology both do not needed high temperature and also without using
Solvent, and synthesis cycle is short, yield is high, technological process is simple and practical.The material that low fever solid phase reaction synthetic technology can synthesize
System enumerates amorphous, nanocrystalline, quasi-crystalline substance, supersaturated solid solution, high-ratio surface catalyst, high-activity compound, fine mineral
A large amount of condensed state matters such as powder.Exemplified by synthesizing NiO nanometer powders, solid state chemical reaction synthetic technology such as is used, it is prepared
Cycle can decline two orders of magnitude than traditional high-temperature heating synthesis technique.Therefore, low fever solid phase reaction synthetic technology is near
The forward position of research and development and focus in an important branch over year in fast-developing green syt field, and international coverage, should
Technology is for reducing energy consumption, the meaning of green production has been become a consensus of the international community, and its popularization and application will produce huge economy and society
Can benefit.
At present, low fever solid phase reaction synthesis equipment is based on ball milling, grinding, including impact grinding (impact grinder, hammer
Mill), cutting mill (such as roll mill), impact pressurization cutting mill (including bulb mill, vibromill, planetary mills).Though ball milling and grinding
The low fever solid phase reaction synthesis of lot of materials system can be so carried out, but its is inefficient, and effective feed in energy analysis is less than total energy consumption
5%, energy utilization rate is extremely low.In addition, ball milling and griding reaction mechanism are complicated, Quantitative study is more difficult, right for a long time
Relevant mechanism is rested in subjective supposition or summary of experience.
In the recent period, substantial amounts of experimental study passes through in present utility model application people research team, and in terms of hydrodynamics
Rich Research foundation, it is creative hypersonic flow body technique to be combined with solid state reaction synthetic technology, form one
Kind supersonic flow accelerates low fever solid phase reaction new technology, and this technology is in traditional low fever solid phase reaction, supersonic flow
Tremendous change on impacting technology, open a kind of brand-new solid-solid reaction, the reaction of gas-solid low-heat efficiently synthesizes technology.Grind
Study carefully team's early stage equipment build and improvement in terms of done numerous studies work, have developed first generation supersonic flow accelerate low-heat
Solid state reaction kinetics device, and applied for utility model patent CN102198388B, disclosed in the patent using Supersonic Gas
The method and apparatus that stream carries out solid state reaction kinetics, wherein, disclosed device includes solid phase reactor, carrier gas stream supply dress
Put and microwave device, solid phase reactor are target formula reactors, be made up of target head and target frame, target head is located at target inframe, solid phase reaction
Device is arranged in radome, applies microwave field by solid reactor of the microwave device into radome.On the whole, the first generation
Solid state reaction kinetics device is vertical reaction device, and reactor is shaped as straight tube structure, and supersonic flow primary air inlet is located at
The axial direction of vertical reactor, reaction-ure inlet and outlet are arranged on the radial direction of vertical reactor, this from the point of view of the situation of experiment
Aspect to be modified be present in design method：First, designed on nozzle structure unreasonable, it is difficult to ultrasound is kept in whole flow field
Fast air-flow.Two be due to jet pipe side wall static pressure it is directly proportional to incoming stagnation pressure, can cause charging aperture when upstream stagnation pressure increase
Pressure, which exceedes atmospheric pressure, causes solid material particle addition air-flow to become difficult.Three be due to that charging aperture is opened in side wall, is destroyed
The uniformity in flow field, air turbulence so that the flow field in downstream is difficult to reach or is maintained supersonic speed state, causes solids
Material particle is difficult to obtain enough kinetic energy.Fourth, solid material particle is added by side wall, solid material particle is with disorderly gas
Stream is randomly dispersed in whole pipeline, does not converge to air-flow center so that is hit target probability reduction, be have impact on the efficiency of reaction.
It can be seen that the reactant of solid phase reactor imports efficiency in first generation solid state reaction kinetics device and capacity usage ratio needs further
Improve, in order to realize reaction synthesis, separately added microwave radiation field, so as to improve the total energy density of reaction particles.Therefore,
The key of problem be how by the Curve guide impeller of device come further improve reaction solid material particle energy feed-in it is close
Degree.
Utility model content
The utility model further optimizes existing apparatus on the basis of existing technology, by structure design and experimental verification
Performance.The utility model provides one kind and hits target formula supersonic flow acceleration low fever solid phase reaction device, and the device can be realized
Solid reaction solid material particle high efficiency feed-in supersonic flow, and rare earth chemistry in energy quantitative measurment supersonic flow
Relevant parameter is reacted, accurately controls course of reaction, realizes the low-temperature solid phase reaction synthesis of different materials system.
Hitting target formula supersonic flow accelerates low fever solid phase reaction device to include solid material particle supply unit, air-flow conveying
Unit and reactor, described solid material particle supply unit include axial admission pipe, hopper, powder feeder, circular response dress
Put, described circular response device one end is connected with powder feeder, and the powder feeder is connected by automatic on-line thief sampler and hopper
Connect, hopper is connected with axial admission pipe；Described reactor includes supersonic nozzle, mixing accelerating chamber, target head, reactor case
Body；Through axial admission pipe is set, the arrival end of axial admission pipe connects hopper and sent coaxial direction inside supersonic nozzle
Powder device, the port of export of axial admission pipe extend to mixing accelerating chamber.
Further, described air-flow supply unit includes compressed air source unit, filtering and drier, air accumulator, pressure regulator valve, numeral
Valve, flowmeter, these parts are contacted successively, formed a gas passage, described compressed air source unit 1 can be air compressor or
Specific gas steel cylinder, described digital valve by equalization chamber, 12 Venturi tubes and 12 solenoid valve blocks into.
Described reactor includes supersonic nozzle, mixing accelerating chamber, target head, reactor casing.The supersonic nozzle
It is connected with air-flow supply unit, and is designed by flowmeter control air-flow conveying, supersonic nozzle for Laval nozzle multi-segment structure,
Including contraction section and accelerating sections, the air-flow come from air-flow supply unit is formed after the contraction section and accelerating sections of supersonic nozzle
Supersonic flow.Pressure in the axially arranged feed pipe of supersonic nozzle inlet end, feed pipe is higher than in mixing accelerating chamber
Pressure, solid material particle enters air-flow by injection, and accelerates to supersonic flow, and low fever solid phase reaction occurs at target head, hits
Solid phase reaction material is connected along pipeline flow-direction circular response device, circular response device with powder feeder after target, realizes reaction solid
Particle hits target response along whole airflow circulating, treats that the sample detection result display reaction that automatic on-line thief sampler is collected is abundant
Afterwards, in the collection of products unit collecting reaction product of circular response device one end.
Mixing accelerating chamber set Dual-Phrase Distribution of Gas olid diagnostic system, including dual pulse welding, laser output modulating unit,
Trace particle produces and seeding device, image record and processing unit, wherein, dual pulse welding connects with laser output modulating unit
Connect, realize generation-output-modulation of laser, and laser is imported to the conversion zone of reactor, trace particle produces and seeding device
It is connected with axial admission pipe, realizes trace particle feed-in reactant, the treatment fluid that image record and processing unit 20 are collected
Image information.Before reaction unit is opened, Dual-Phrase Distribution of Gas olid diagnostic system parameter is set, collects flux map during the course of the reaction
Picture simultaneously carries out computer disposal.
Described supersonic nozzle is Laval nozzle, is gathered from polytetrafluoroethylene (PTFE) or stainless steel, or using liner
The stainless steel of tetrafluoroethene.Described target head material can be with titanium, 20Cr, tungsten carbide, Al2O3。
Hit the operation logic that target formula supersonic flow accelerates low fever solid phase reaction device：High pressure gas is produced by compressed air source unit
Body, multistage filtering, purification, drying are carried out to gas by filtering and drier, into air accumulator, air-flow passes through pressure regulation successively
Valve, digital valve, flowmeter enter supersonic nozzle, and supersonic nozzle designs for multi-segment structure, including contraction section and accelerating sections, from
The air-flow that air-flow supply unit comes forms supersonic flow after the contraction section and accelerating sections of supersonic nozzle.Sprayed in supersonic speed
The axially arranged feed pipe of pipe inlet end, the pressure in feed pipe is higher than the pressure in mixing accelerating chamber, and solid material particle is in ring
Enter under shape ejector action and accelerate air-flow, and supersonic speed is accelerated to air-flow, low fever solid phase reaction occurs at target head, after hitting target
Solid phase reaction material enters material bin by powder feeder by circular response device, passes through axle along pipeline flow-direction circular response device
Mixed supersonic acceleration conversion zone is again introduced into feed pipe, and target response is hit at target head, it is solid to be achieved in reaction
Target response is hit in the circulation of body material particles, after circular response certain time, the collection of products in circular response device one end
The isolated reaction product of unit.During device continued operation, Dual-Phrase Distribution of Gas olid diagnostic system is opened as needed, will be shown
In track particle feed-in solid phase air-flow, and tracer is carried out to reaction gas flow with modulating unit by dual pulse welding and laser output
Detection, the analog feature of reaction gas flow is obtained by image record and processing unit.Automatic on-line thief sampler 9 is collected in good time
Reactive material sample, phase composition and Micro-Structure Analysis result to different time sections sample come obtain plant running it is optimal when
Between scope.
Low fever solid phase reaction device is accelerated to carry out low fever solid phase reaction using the target formula supersonic flow of the present utility model that hits
Technological process specifically include following steps：Air-flow supply unit parameter is adjusted, the stream pressure into supersonic nozzle 13 is steady
1.2-1.5MPa is scheduled on, 100-200g solid phase particles are weighed by balance, solid phase particles are added and carry closed loop Weighing control system
The storage bin hopper of the powder feeder 10 of system, opens the powder feeder setting charging rate with closed loop weighing control system, and solid phase particles are equal
The hopper and axial admission pipe of reactor are transported to evenly, and supersonic nozzle produces supersonic flow, in supersonic speed annular jet flow
Under ejector action, solid material particle ejects in axial admission pipe along supersonic flow is central axial.Solid phase particles enter
Enter reactor, accelerated in the presence of supersonic flow, obtain very high mechanical energy, particle is rubbing, touched between each other
Hit and the knock-on process of reactant system in, realize conversion of the mechanical energy to chemical energy, with big contact area and high connect
Tactile probability expedites the emergence of rare earth synthesis, and the solid phase particles not reacted completely are again introduced into reaction after the separation of circular response device
Device.In the process of running, the real time sample by automatic on-line thief sampler 9 to low fever solid phase reaction intermediate product, sampling
Interval time is set as 3-5 minutes, and sampling quantity is set as 1-3g, and the reactant interphase sample of taking-up is surveyed for microstructure
Examination, to obtain the evolutionary process for reacting interphase.Meanwhile Dual-Phrase Distribution of Gas olid diagnostic system is realized by pulsed laser system
High-energy, short pulse, high-repetition-rate, the output of high performance 532nm laser, by high-precision synchronous controller, realize that 0.25 receives
Second high-precise synchronization control, by 64 core parallel processing control softwares, is realized at high speed synchronous sample and flow field data
Reason, by multiple dedicated modules, fatware analysis platform is built, realizes that transient flow field accurately measures, passes through image software
The particle image of different-grain diameter is identified, the particle concentration, speed before clash target or head-on collision measure.Examined by Dual-Phrase Distribution of Gas olid
The data that disconnected system obtains calculate the procedure parameters such as the kinematics of Dual-Phrase Distribution of Gas olid, thermodynamics, and total score is synthesized by reacting
Software is analysed, realizes the modeling analysis to course of reaction.
The utility model uses the technical scheme that coaxial feeding is combined with supersonic speed annular jet injection, by solid phase particles
Logistics introduces reactor, is accelerated in the presence of high velocity air, obtains very high mechanical energy, and particle is rubbing between each other
Wipe, in the knock-on process of collision and reactant system, realize conversion of the mechanical energy to chemical energy, with big contact area with
High contact probability expedites the emergence of rare earth synthesis, and the material not reacted completely can be again introduced into anti-after the separation of circular response device
Answer device.The technical solution of the utility model is fine must to solve the inefficient of solid solid material particle feed-in high velocity air
Problem, so as to improve the energy feed-in density of solid material particle, improve the efficiency of reaction.Simultaneously as this practicality is new
The innovation of type technical scheme, the reaction condition for meeting a variety of solid phase reactions, gas-solid reaction is fully able to, it is therefore, anti-in the first generation
The microwave outfield employed in device is answered to become no longer necessary, this greatly reduces the manufacturing cost of device, while also extension is anti-
The selection space of equipment material is answered, is advantageous to the batch production of complexes.
From the supersonic nozzle of target Mach 2 ship 3.0, jet pipe pneumatic design considers the two kinds of flowings of the gentle solid phase of gas phase
Condition.Solid material particle conveying is reached using the powder feeder with closed loop weighing control system, mass flow control accuracy
1%, accurate feeding system mainly realizes the accurate input of solid material particle, and its inlet amount can accurately be adjusted by control panel
Section.The real time sample of low fever solid phase reaction intermediate product using automatic on-line thief sampler realize, have it is manual with automatic two kinds
Mode of operation, sampling interval time：(0~5) minute, sampling quantity：(0~10) g, product sampling system can be taken out instead as needed
Answer thing interphase to be used for micro-structural test, obtain the evolutionary process of reaction interphase, finally realize to low fever solid phase reaction
Both macro and micro is studied.
Source of the gas supply unit is mainly used in providing reactor defined driving source of the gas, using modularized design, realizes spirit
It is living to change, meet the demand and supply of pressure-air or specific gas during solid phase reaction.Digital valve is as accurate control flow quality
The core component of flow, by equalization chamber, 12 Venturi tubes and 12 solenoid valve blocks into Venturi tube throat area is according to binary system
Arrangement, a corresponding Venturi tube per way solenoid valve, realized using quick open or close of magnetic valve to the quick accurate of flow
Regulation, magnetic valve opening/closing time are less than 100ms, and the gas flow amplitude of accommodation reaches 0.2g/s, and measurement accuracy is better than 0.2%, its
Effect is regulation and control reaction synthesis primary condition and course of reaction.
Dual-Phrase Distribution of Gas olid diagnostic system uses pulsed laser system, realizes high-energy, short pulse, high-repetition-rate, Gao Xing
The 532nm laser output of energy, using high-precision synchronous controller, the high-precise synchronization control of 0.25 nanosecond is realized, using 64 cores
Heart parallel processing control software, realizes high speed synchronous sample and flow field data processing, using multiple modules, builds fatware
Analysis platform, realize that transient flow field accurately measures, identify the particle image of different-grain diameter, for the particle concentration before the target that clashes,
Speed measures.Using solid phase particles as trace particle, flow field is followed to move, laser beam expands light in blocks by compound lens
Flow field is illuminated, (musec order) exposes particle picture twice in the battle array of CCD faces at a certain time interval.Image procossing
When, the image of measured zone is divided into several zonings (inquiry window) first, then to the grain in adjacent two field pictures
Subgraph carries out cross correlation process, (passes through ground so as to obtain the average displacement amount of multiple trace particles pair in each inquiry window
Face calibration obtains the corresponding relation of pixel and actual range).Because the time interval dt of two frame laser pulses is, it is known that can then count
The velocity in each inquiry window is calculated, and then obtains the velocity field result in whole shooting area.
Brief description of the drawings
Fig. 1 accelerates low fever solid phase reaction device system pie graph to hit target formula supersonic flow；
Fig. 2 accelerates low fever solid phase reaction apparatus structure schematic diagram to hit target formula supersonic flow, wherein, 1, air compressor machine；2、
Filtering and drier；3rd, air accumulator；4th, pressure regulator valve；5th, digital valve；6th, flowmeter；7th, axial admission pipe；8th, hopper；9th, exist automatically
Line thief sampler；10th, powder feeder；11st, circular response device；12nd, high pressure positive blower；13rd, supersonic nozzle；14th, mixing accelerates
Room；15th, target head；16th, reactor casing；17th, trace particle generation and seeding device；18th, dual pulse welding；19th, laser exports
With modulating system；20th, image record and processing system；
Fig. 3 is to hit the XRD spectrum that target formula supersonic flow accelerates product in low fever solid phase reaction device embodiment 1；
Fig. 4 is to hit the collection of illustrative plates that target formula supersonic flow accelerates the FTIR of product in low fever solid phase reaction device embodiment 1；
Fig. 5 is to hit the XRD spectrum that target formula supersonic flow accelerates product in low fever solid phase reaction device embodiment 2；
Fig. 6 is to hit the microscopic appearance that target formula supersonic flow accelerates product in low fever solid phase reaction device embodiment 2；
Fig. 7 is to hit the infared spectrum that target formula supersonic flow accelerates product in low fever solid phase reaction device embodiment 3；
Fig. 8 is to hit the microscopic appearance structure that target formula supersonic flow accelerates product in low fever solid phase reaction device embodiment 3.
Embodiment
Structure and the course of work of the present utility model are further described below in conjunction with the accompanying drawings：Include solids as shown in Figure 1
Material particle supply unit, air-flow supply unit and reactor, described solid material particle supply unit include axial admission pipe
7th, hopper 8, powder feeder 10, circular response device 11, described one end of circular response device 11 are connected with powder feeder 10, the powder feeding
Device 10 is connected by automatic on-line thief sampler 9 with hopper 8, and hopper 8 is connected with axial admission pipe 7；Described reactor bag
Include supersonic nozzle 13, mixing accelerating chamber 14, target head 15, reactor casing 16；Passed through in the inside coaxial direction of supersonic nozzle 13
Wear and put axial admission pipe 7, the arrival end connection hopper 8 and powder feeder 10 of axial admission pipe 7, the port of export of axial admission pipe 7
Extend to mixing accelerating chamber 14.
Further as shown in Fig. 2 described air-flow supply unit includes compressed air source unit 1, filtering and drier 2, air accumulator
3rd, pressure regulator valve 4, digital valve 5, flowmeter 6, these parts are contacted successively, form a gas passage, described compressed air source unit 1 can
Think air compressor or specific gas steel cylinder, described digital valve 9 is by equalization chamber, 12 Venturi tubes and 12 solenoid valve blocks
Into.Described solid material particle supply unit includes axial admission pipe 7, hopper 8, powder feeder 10, circular response device 11, institute
The powder feeder 10 stated carries closed loop weighing control system.Described one end of circular response device 11 is connected with powder feeder 10, described to send
Powder device 10 is connected by automatic on-line thief sampler 9 with hopper 8, and hopper 8 is connected with axial admission pipe 7.Described reactor
Including supersonic nozzle 13, mixing accelerating chamber 14, target head 15, reactor casing 16.The supersonic nozzle 13 conveys with air-flow
Unit connects, and controls air-flow to convey by flowmeter 6, and supersonic nozzle 13 designs for Laval nozzle multi-segment structure, including receives
Contracting section and accelerating sections, the air-flow come from air-flow supply unit form ultrasound after the contraction section and accelerating sections of supersonic nozzle 13
Fast air-flow.Pressure in the axially arranged feed pipe 7 of the inlet end of supersonic nozzle 13, feed pipe 7 is higher than in mixing accelerating chamber 14
Pressure, solid material particle enters air-flow by injection, and accelerates to supersonic flow, at target head 15 occur rare earth it is anti-
Should, along pipeline flow-direction circular response device 11, circular response device 11 is connected solid phase reaction material with powder feeder 10, real after hitting target
Now reaction solid particle hits target response along whole airflow circulating, treats the sample detection result that automatic on-line thief sampler 9 is collected
After display reaction fully, the collection of products unit collecting reaction product in the one end of circular response device 11.
In mixing accelerating chamber 14, Dual-Phrase Distribution of Gas olid diagnostic system, including the output modulation of dual pulse welding 18, laser are set
Unit 19, trace particle produces and seeding device 17, image record and processing unit 20, wherein, dual pulse welding 18 and laser
Modulating unit connection is exported, realizes generation-output-modulation of laser, and laser is imported to the conversion zone of reactor, reactor
Trace particle is produced and seeding device 17 is connected with axial admission pipe 7, realizes trace particle feed-in reactant, image record and processing
The image information for the treatment fluid that unit 20 is collected.Before reaction unit is opened, Dual-Phrase Distribution of Gas olid diagnostic system parameter is set,
Flux map picture is collected during the course of the reaction and carries out computer disposal.Described supersonic nozzle 13 is Laval nozzle, is selected
Polytetrafluoroethylene (PTFE) or stainless steel, or the stainless steel using inner liner polytetrafluoroethylene.
Hit the operation logic that target formula supersonic flow accelerates low fever solid phase reaction device：High pressure gas is produced by compressed air source unit
Body, multistage filtering, purification, drying are carried out to gas by filtering and drier 2, into air accumulator 3, air-flow passes through pressure regulation successively
Valve 4, digital valve 5, flowmeter 6 enter supersonic nozzle 13, and supersonic nozzle 13 design for multi-segment structure, including contraction section with add
Fast section, the air-flow come from air-flow supply unit form supersonic flow after the contraction section and accelerating sections of supersonic nozzle 13.
Pressure in the axially arranged feed pipe 7 of the inlet end of supersonic nozzle 13, feed pipe 7 is higher than the pressure in mixing accelerating chamber 14,
Solid material particle enters under annular ejector action accelerates air-flow, and accelerates to supersonic speed with air-flow, occurs at target head 15
Low fever solid phase reaction, solid phase reaction material passes through along pipeline flow-direction circular response device 11 by circular response device 11 after hitting target
Cross powder feeder 10 and enter material bin 8, mixed supersonic acceleration conversion zone is again introduced into by axial admission pipe 7, and at target head
Target response is hit, target response is hit in the circulation for being achieved in reacting solid material particle, after circular response certain time,
The isolated reaction product of collection of products unit of the one end of circular response device 11.During device continued operation, according to need
Dual-Phrase Distribution of Gas olid diagnostic system is opened, by trace particle feed-in solid phase air-flow, and by dual pulse welding 18 and laser
Output carries out Tracing detection with modulating unit 19 to reaction gas flow, and the mould of reaction gas flow is obtained by image record and processing unit
Intend characteristic.Automatic on-line thief sampler 9 collects reactive material sample in good time, phase composition to different time sections sample and microcosmic
Results of structural analysis obtains the Best Times scope of plant running.
Embodiment 1
Air-flow supply unit parameter is adjusted, the stream pressure into supersonic nozzle 13 is stablized in 1.5MPa, passes through balance
Ammonium persulfate 114.0g and aniline hydrochloride 64.5g solid phase particles are weighed, it is well mixed according to nonstoichiometric molar ratio 1: 1, will be solid
Phase particle adds the storage bin hopper of the powder feeder 10 with closed loop weighing control system, opens sending with closed loop weighing control system
Powder device 10 sets charging rate, and solid phase particles are uniformly delivered to the hopper 8 and axial admission pipe 7 of reactor, supersonic nozzle
13 produce supersonic flow, and under the effect of supersonic speed annular jet injection, solid material particle is in axial admission pipe 7 along ultrasound
Fast air-flow is central axial to be ejected, and solid phase particles enter reactor, and particle is in mutual friction, collision and reactant
In the knock-on process of system, conversion of the mechanical energy to chemical energy is realized.During plant running, taken by automatic on-line powder
Sample device 9 is set as 7 minutes to the real time sample of low fever solid phase reaction intermediate product, sampling interval time, and sampling quantity is set as 3g,
Meanwhile pulse laser realize 532nm laser export, by high-precision synchronous controller realize 0.25 nanosecond Synchronization Control, lead to
Cross 64 core parallel processing control units and realize high speed synchronous sample and flow field data processing.Device circulation 7min or so, takes
3g samples are to be measured, purified with ultra-pure water and absolute ethyl alcohol, remove unreacted raw material, vacuum drying, obtain product.With
XRD characterizes to product, and Fig. 3 is XRD spectrum.Analyze XRD spectrum and understand that the characteristic diffraction peak of polyaniline is different from persulfuric acid
The characteristic peak of ammonium and aniline hydrochloride, wherein 2 θ=9.3 °, 14.9 °, 20.2 °, 25.5 °, 26.7 ° be polyaniline feature diffraction
Peak, 001,011,100,110,111 crystal faces are corresponded respectively to, it is consistent with pertinent literature report, it was demonstrated that with supersonic airstream low temperature
Solid phase apparatus successfully synthesizes polyaniline.Product is characterized with infrared, Fig. 4 is FTIR collection of illustrative plates.Analyzing infared spectrum can
Know, 1591cm-1、1483cm-1、 1296cm-1、1142cm-1、1114cm-1It is the characteristic absorption peak of polyaniline, 1591cm-1With
1483cm-1For the stretching vibration peak of C=C in quinoid ring and phenyl ring, 1296cm-1For C-N stretching vibrations, 1142cm-1For proton
The vibration of the C-N functional groups of change, further demonstrates the generation of polyaniline.
Embodiment 2
Air-flow supply unit parameter is adjusted, the stream pressure into supersonic nozzle 13 is stablized in 1.5MPa, passes through balance
Ammonium persulfate 114.0g and 2,5- dimethoxyaniline 76.5g solid phase particles are weighed, is mixed according to nonstoichiometric molar ratio 1: 1 equal
It is even, solid phase particles are added to the storage bin hopper of the powder feeder 10 with closed loop weighing control system, unlatching carries closed loop Weighing control
The powder feeder 10 of system sets charging rate, and solid phase particles are uniformly delivered to the hopper 8 and axial admission pipe 7 of reactor, surpasses
Velocity of sound jet pipe 13 produces supersonic flow, and under the effect of supersonic speed annular jet injection, solid material particle is in axial admission pipe
Ejected in 7 along supersonic flow is central axial, solid phase particles enter reactor, particle mutual friction, collision, with
And in the knock-on process of reactant system, realize conversion of the mechanical energy to chemical energy.During plant running, by existing automatically
Line thief sampler 9 is set as 7 minutes to the real time sample of low fever solid phase reaction intermediate product, sampling interval time, sampling quantity
It is set as 3g, meanwhile, pulse laser realizes that 532nm laser exports, and realizes that 0.25 nanosecond is same by high-precision synchronous controller
Step control, high speed synchronous sample and flow field data processing are realized by 64 core parallel processing control units.Device circulates
7min or so, take 3g samples to be measured, with ultra-pure water and absolute ethyl alcohol purification process, vacuum drying, obtain poly- 2,5- dimethoxys
Aniline.Product is characterized with XRD, Fig. 5 is XRD spectrum.As shown in Figure 5, the diffraction maximum of poly- 2,5- dimethoxyanilines is bright
The aobvious diffraction maximum for being different from two kinds of raw materials, 2 θ=13.2 °, 17.1 °, 20.0 °, 24.0 °, 26.1 °, 27.0 °, 33.0 ° be poly- 2,
The characteristic diffraction peak peak of 5- dimethoxyanilines, wherein 17.1 °, 20.0 °, 26.1 °, 27.0 ° correspond respectively to 011,100,
110th, 111 crystal face, it is consistent with pertinent literature report, it was demonstrated that high velocity air method Low Temperature Solid-Phase synthesis can be with Fast back-projection algorithm poly- 2,5-
Dimethoxy benzene amines.The appearance structure of product is studied with ESEM, Fig. 6 is the microscopic appearance of product.By
Fig. 6 understands that the pattern of poly- 2,5- dimethoxyanilines is uneven granule-morphology, and sized particles are smaller, and existing with polymerization
As, it may be possible to because poly- 2,5- dimethoxyanilines have stronger polarity, caused by the interaction for promoting molecule interchain.
Embodiment 3
Air-flow supply unit parameter is adjusted, the stream pressure into supersonic nozzle 13 is stablized in 1.5MPa, passes through balance
Trimesic acid 114.0g and copper acetate 76.5g solid phase particles are weighed, it is well mixed according to nonstoichiometric molar ratio 2: 3, will be solid
Phase particle adds the storage bin hopper of the powder feeder 10 with closed loop weighing control system, opens sending with closed loop weighing control system
Powder device 10 sets charging rate, and solid phase particles are uniformly delivered to the hopper 8 and axial admission pipe 7 of reactor, supersonic nozzle
13 produce supersonic flow, and under the effect of supersonic speed annular jet injection, solid material particle is in axial admission pipe 7 along ultrasound
Fast air-flow is central axial to be ejected, and solid phase particles enter reactor, and particle is in mutual friction, collision and reactant
In the knock-on process of system, conversion of the mechanical energy to chemical energy is realized.During plant running, taken by automatic on-line powder
Sample device 9 is set as 10 minutes to the real time sample of low fever solid phase reaction intermediate product, sampling interval time, and sampling quantity is set as
3g, meanwhile, pulse laser realize 532nm laser export, by high-precision synchronous controller realize 0.25 nanosecond Synchronization Control,
High speed synchronous sample and flow field data processing are realized by 64 core parallel processing control units.Device circulates 10min, takes 3g
Sample is to be measured, is purified with water and absolute ethyl alcohol, removes unreacted raw material, obtains product.Table is carried out to product with infrared
Sign, Fig. 7 is the infared spectrum of product.It can be seen from figure 7 that 3432cm-1And 1626cm-1There is two absworption peaks, explanation in place
There is the presence of water of coordination or the crystallization water in synthesized Cu-BTC samples.Carbon-based symmetrical stretching vibration absorbs and not right in carboxyl
The absworption peak of stretching vibration is claimed to appear in 1587cm-1、1443cm-1And 1372cm-1Place.In 1110cm-1Locate the weak absorbing peak occurred
For C-O-Cu stretching vibration absworption peak, and Cu-BTC characteristic absorption peak appears in 734cm-1Place, this absworption peak are due to
Group on phenyl ring is substituted by Cu.With reported for work document compares, it can be seen that corresponding peak position is consistent with document,
Prove the generation of product.The pattern of product is analyzed with ESEM, Fig. 8 is the microscopic appearance structure of product.Can from Fig. 8
To see, product is equally distributed hollow club shaped structure, and mainly between 200-300nm scope, this is tied the size of size
Structure can increase its size than surface.
Claims (5)
1. hitting target formula supersonic flow accelerates low fever solid phase reaction device, it is characterised in that is conveyed including solid material particle single
Member, air-flow supply unit and reactor, described solid material particle supply unit include axial admission pipe (7), hopper (8),
Powder feeder (10), circular response device (11), described circular response device (11) one end are connected with powder feeder (10), the powder feeding
Device (10) is connected by automatic on-line thief sampler (9) with hopper (8), and hopper (8) is connected with axial admission pipe (7)；It is described
Reactor include supersonic nozzle (13), mixing accelerating chamber (14), target head (15), reactor casing (16)；Sprayed in supersonic speed
(13) internal coaxial direction is managed through axial admission pipe (7) is set, the arrival end of axial admission pipe (7) connects hopper (8) and sent
Powder device (10), the port of export of axial admission pipe (7) extend to mixing accelerating chamber (14).
2. device according to claim 1, it is characterised in that described air-flow supply unit is by compressed air source unit (1), filtering
And drier (2), air accumulator (3), pressure regulator valve (4), digital valve (5), flowmeter (6) are contacted form a gas passage successively,
Compressed air source unit (1) is air compressor or specific gas steel cylinder, and digital valve (5) is by equalization chamber, 12 Venturi tubes and 12 electricity
Magnet valve forms.
3. device according to claim 1, it is characterised in that described supersonic nozzle (13) is Laval nozzle, choosing
With polytetrafluoroethylene (PTFE) or stainless steel, or the stainless steel using inner liner polytetrafluoroethylene.
4. device according to claim 3, it is characterised in that described target head (15) material can select titanium, 20Cr, carbon
Change tungsten or Al2O3Any of.
5. device according to claim 1, it is characterised in that set Dual-Phrase Distribution of Gas olid to diagnose system in mixing accelerating chamber (14)
System, including dual pulse welding (18), laser output modulating unit (19), trace particle produce and seeding device (17), image note
Record and processing unit (20), wherein, dual pulse welding (18) is connected with laser output modulating unit (19), and trace particle produces
And seeding device (17) is connected with axial admission pipe (7), image record and the image letter of processing unit (20) collection and treatment fluid
Breath.
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| CN201720186251.2U CN206688701U (en) | 2017-02-28 | 2017-02-28 | Hit target formula supersonic flow and accelerate low fever solid phase reaction device |
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| CN201720186251.2U CN206688701U (en) | 2017-02-28 | 2017-02-28 | Hit target formula supersonic flow and accelerate low fever solid phase reaction device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107051364A (en) * | 2017-02-28 | 2017-08-18 | 中国空气动力研究与发展中心高速空气动力研究所 | Hit target formula supersonic flow and accelerate low fever solid phase reaction device and its application process |
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2017
- 2017-02-28 CN CN201720186251.2U patent/CN206688701U/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107051364A (en) * | 2017-02-28 | 2017-08-18 | 中国空气动力研究与发展中心高速空气动力研究所 | Hit target formula supersonic flow and accelerate low fever solid phase reaction device and its application process |
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