CN105709676A - Composite preparation system capable of effectively improving composite interface bonding - Google Patents
Composite preparation system capable of effectively improving composite interface bonding Download PDFInfo
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- CN105709676A CN105709676A CN201610083837.6A CN201610083837A CN105709676A CN 105709676 A CN105709676 A CN 105709676A CN 201610083837 A CN201610083837 A CN 201610083837A CN 105709676 A CN105709676 A CN 105709676A
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Abstract
The invention provides a composite preparation system which comprises a reaction kettle and a device for providing an induced alternating magnetic field.Reactants and base materials for the induced alternating magnetic field are put into the reaction kettle, the base materials generate a current by cutting induction lines of the induced alternating magnetic field, and therefore the purpose of being heated is achieved.
Description
Technical field
The invention belongs to the synthesis technical field of material, relate to a kind of composite preparation system that can be effectively improved composite material interface combination.
Background technology
Along with advancing by leaps and bounds of most advanced branches of science technology, the performance requirement of material is more and more higher, in many aspects, the performance of traditional monophase materials can not meet the needs of reality, this promotes people to study to prepare by the composite of many phase compositions, to improve performance [Zhou Xiya, " composite " of material, Chemical Industry Press, Beijing].
But, composite will be made to produce the cooperative effect of 1+1 > 2, its interface plays vital effect.In order to obtain the interface cohesion of excellence, reinforcement surface treatment (such as chemical attack, roentgenization and add silane coupler etc.), the method such as face coat adding specific element, reinforcement in matrix are widely used [SuF, ZhangZ, WangK, JiangW, LiuW.Tribologicalandmechanicalpropertiesofthecompositesm adeofcarbonfabricsmodifiedwithvariousmethods.CompositesP artA:AppliedScienceandManufacturing.2005；36 (12): 1601-7.].
For the preparation of nano composite material, mainly there are Physical and two kinds of methods of chemical method.Wherein, Physical mainly includes mechanical lapping composite algorithm, dry type ballistic method, high-energy ball milling method, blending method, heterocoagulation method and high temperature evaporation method etc., although nano composite material prepared by these methods has surface cleaning, free from admixture, granule advantages of higher controlled, active, but current productivity is mostly relatively low and cost is high.Chemical method mainly includes sol-gal process, hydro-thermal method, microemulsion method, chemical vapour deposition technique, solvent evaporated method etc., although these method productivity are high, but the composite of preparation contains certain impurity.
Said method is mostly that then third party's material transfers heat to reactant, thus realizing the synthesis of material at a certain temperature by heating third party's material.When using these methods to prepare composite, matrix material and reactant are heated by third party's material simultaneously, being formed of interface do not guide be entirely random, reactant being unevenly distributed on matrix material and interface cohesion poor.Want to realize pinpointing controlled nucleating growth and forming good interface on matrix, its selective active site must be made by advanced processing matrix material (make them charged or there is certain functional group), thus realizing the control of composite construction, obvious this technique is more complicated, and is difficulty with industrialized production.
In addition, when Template synthesis has the material of a fixed structure, template is required, namely template itself is answered active site or can introduce avtive spot by certain process, so could realize reactant growth on matrix material, this makes some have the template of special construction and can not be used [the old evident rising sun, Zheng Ping Yun, Li Xianxue, Fu Minglian, thank to administration's light, Deng Chao, Hu Yanhua, " template synthesis nano materials research progress " [J]. " chemical industry progress ", 2010, (the 1st phase)].
Summary of the invention
In view of the above-mentioned problems in the prior art, the technical problem to be solved is in that a kind of composite preparation system that can be effectively improved composite material interface combination, can utilize sensing heating under the premise of controllable temperature and pressure, utilize the heated feature of reactant itself to prepare and there is the composite that excellent interface combines.
In order to solve above-mentioned technical problem, on the one hand, the invention provides a kind of composite preparation system, including reactor (6) and the device providing sensing alternating magnetic field, reactant it is placed with and for sensing the matrix material of alternating magnetic field in described reactor, described matrix material produces electric current by cutting the line of induction of sensing alternating magnetic field, thus reaching heated purpose.
Composite preparation system according to the present invention, first makes recirculated water flow into induction coil through the internal pipeline of induction heating equipment before the reaction, and after flowing out from induction coil, the internal pipeline then through induction heating equipment flows out, and is finally discharged.Then reactant and matrix material are joined in reactor, and reactor is sealed, and by the temperature and pressure in temperature detecting unit and pressure sensing cell detection reactor.Finally being fixed in induction coil by reactor, running temperature detects unit and pressure sensing cell, opens induction heating equipment, by controlling induction frequencies and the output electric current of induction heating equipment, reactor carries out hydro-thermal sensing and heats.Reaction closes induction heating equipment, temperature detecting unit and pressure sensing cell after terminating, and is cooled to closedown recirculated water after room temperature until still, takes out reactor, takes out product.
Composite preparation system according to the present invention, first makes recirculated water discharge after flowing into induction coil and induction heating equipment before the reaction.Then the mixed liquor as reactant is proceeded in reactor, addition can sense the matrix material of alternating magnetic field, seal in the heating unit being placed on the present invention and carry out hydro-thermal reaction, then room temperature is naturally cooled to, product is isolated from reacted suspension, again by this product respectively with deionized water and soaked in absolute ethyl alcohol washing, can obtain being loaded with the combination product of product after drying.Thereby, it is possible to utilize hydro-thermal induction technology synthetic composite material or there is special construction material, it is effectively improved composite material interface and combines.
Again, in the present invention, it is also possible to be, the temperature value detected according to described temperature detecting unit control electric current in described induction heating equipment be switched on or switched off the temperature in described reactor is controlled.
According to the present invention, the temperature value of induction heating equipment collecting temperature detection unit detection can be passed through, be fed back to induction heating equipment, thus being switched on or switched off of electric current in induction heating equipment can be passed through realize being automatically adjusted and controlling of temperature.
The invention is not restricted to this, it is also possible to be, the temperature value of described temperature detecting unit detection can be observed by people, and mode manually controls being switched on or switched off of electric current in induction heating equipment, thus the temperature in described reactor is carried out Non-follow control.
Again, in the present invention, it is also possible to be, described temperature detecting unit includes the fibre optic temperature sensor or the infrared radiation thermometer that are connected with described reactor.
According to the present invention, adopt fibre optic temperature sensor or infrared radiation thermometer as temperature detecting unit, they have essential safety, by electromagnetic interference, can remotely monitor, precision and highly sensitive, high pressure resistant, anticorrosive, can work in the presence of a harsh environment and low cost and other advantages.Thus the electromagnetism interference of temp measuring system can be significantly improved, improve the precision of thermometric and reduce cost.
Again, in the present invention, it is also possible to be, described pressure sensing cell includes the pressure transducer and the pressure digital readout system that are connected with described reactor.
According to the present invention, pressure sensing cell is mainly by sensing in reactor the pressure transducer of gas pressure to realize the mensuration of pressure, and can convert electrical signals to digital signal by such as high-pressure mini reactor stored program controlled, then shows.Further, air bleeding valve also can be set and terminate the effect of rear pressure release to play reaction.
According to the present invention, induction heating equipment can be passed through and gather the force value of pressure sensing cell detection, be fed back to induction heating equipment, thus being switched on or switched off of electric current in induction heating equipment can be passed through realize being automatically adjusted and controlling of pressure.
The invention is not restricted to this, it is also possible to be, the force value of described pressure sensing cell detection can be observed by people, and mode manually controls being switched on or switched off of electric current in induction heating equipment, thus the pressure in described reactor is carried out Non-follow control.
According to the present invention, controlled can be switched on or switched off switch by arranging in the position of air bleeding valve, then pass through the pressure feedback value that pressure detecting system detects and control being switched on or switched off of switch, and then realize the accurate control of pressure.
Again, in the present invention, it is also possible to be, the gas pressure sensor sensor as pressure sensing cell of nonmetal, non-carbon (mainly macromolecule) material probe is selected.
Again, in the present invention, it is also possible to be, also including the agitating device for the material in described reactor is stirred, described agitating device includes: be arranged at the drive link in the kettle of described reactor；It is installed on the stirring paddle on described drive link；It is located at the outside of described kettle and the driving device for driving described drive link to rotate.
According to the present invention, by adopting above-mentioned agitating device, it is ensured that reactant has good uniformity and dispersibility.
Again, in the present invention, it is also possible to be, described stirring paddle includes one or more in axial impellers, radial flow stirring paddle or mixed flow stirring paddle, it is preferable that the gap between the inwall of described stirring paddle and described kettle is 0.5～1cm.
According to the present invention, the selection of above-mentioned gap parameter is more beneficial for producing uniform mixing effect, thus reaching to make reactant in reactor not reunite, do not settle and mixed uniformly purpose.
Again, in the present invention, it is also possible to be, described reactor is located in ultrasound unit and is stirred.
According to the present invention it is also possible to be placed in by reactor in such as Ultrasound Instrument, realize the dispersion of reactant by controlling ultrasonic power, such that it is able to make product homoepitaxial and distribution on matrix material.
Again, in the present invention, it is also possible to be, the material side of the being copper pipe of described induction coil, coil shape is circular, and outer layer is wound around insulating barrier, and coil turn is 2～10, and loop length is 0.5～2m, and internal coil diameter is 20～200mm.
According to the present invention, as induction coil, selection side's copper pipe has that resistance is little, power consumption is low, convenient welding and intensity advantages of higher.The selection of circular induction coil is more beneficial for generation and the inductor cutting magnetic induction line of alternating magnetic field, and this contributes to the heating of faradic generation and inductor.When frequency is too low, equipment will be protected automatically, can not shake or autostop, and when frequency is higher, equipment can reduce heating power automatically, when frequency too Gao Shihui power device in moment scaling loss equipment.The difference of coil turn, length and internal diameter can cause that the difference of induction frequencies and output, very few coil turn and too small internal coil diameter are likely to cause frequency too high and cause equipment fault, and long coil is unfavorable for the fixing of reactor.Therefore for an induction heating equipment determined, its induction frequencies and what power bracket determined that, this requires that the number of turn of coil, length and internal diameter have being well matched with property, and can not arbitrarily arrange.To sum up, these parameters that the present invention protects, are premised on induction heating equipment trouble free service, are more beneficial for producing alternating magnetic field, are more conducive to reach good cooling effect, are more conducive to produce good heats.
Again, in the present invention, it is also possible to be, the material of described reactor includes high molecular polymer.
According to the present invention, reactor can adopt the high molecular polymer such as polyparaphenylene phenol (PPL) or politef (PTFE), it is possible to improve the performances such as the electromagnetism interference of reactor, heat-resisting quantity, heat stability, corrosion resistance, radiation resistance, resistance to chemical attack and solvent resistance.
According to the present invention, whole sealing system adopts nonmetal, non-carbon (mainly macromolecule) material, so can avoid the alternating magnetic field impact on metal sealing system.Additionally, whole reactor includes kettle cover, kettle and sealing system adopts macromolecule material, thus whole system is very light, it is easy to fixes and carries.Reactor fixing on induction coil, can realize by arranging the mode of draw-in groove bottom reactor, can also by reactor being arranged to stepped cylindrical shape, reactor Upper cylindrical diameter is utilized to realize more than induction coil internal diameter, it is also possible to realize by building the support bracket fastened mode of reactor.
According to the present invention, it is contemplated that security problems, the material of air bleeding valve adopts metal material, and in order to avoid air bleeding valve is subject to the impact of alternating magnetic field, the air bleeding valve distance from induction coil may be configured as more than 50cm.
Again, in the present invention, can also be, described reactor is sealed by sealing mechanism, and described sealing mechanism includes being located at the flanged plate of the open end of the kettle of described reactor, the blind flange being located on the kettle cover of described reactor and for being closely attached the fastening component of described flanged plate and described blind flange.
According to the present invention, the sealing of reactor can be effectively realized by above-mentioned sealing mechanism, and be prone to open reactor taking-up product after the completion of reaction.
On the other hand, present invention also offers a kind of method adopting above-mentioned composite preparation system to prepare composite, including: make the induction coil of recirculated water circulation heating unit and the inside of induction heating equipment；By reactant and material matrix held in the reactor sealed；Described reactor is placed in described induction coil；Temperature in described reactor is detected；Pressure in described reactor is detected；Based on the temperature value detected and the force value detected, control described induction heating equipment and described reactor is carried out hydro-thermal sensing；Described reactor is made to cool down to obtain product after reaction.
In accordance with the invention it is possible to utilize hydro-thermal induction technology synthetic composite material or there is special construction material, it is effectively improved composite material interface and combines.
Again, in the present invention, it is also possible to be, the induction frequencies of described induction heating equipment output is 10～500KHz, and faradic current is 0～1200A.
According to the present invention, the difference according to heated material size, it is possible to be selected to the induction heating equipment of output 10～500KHz induction frequencies.Faradic big I continuously adjustabe in the scope of 0～1200A in sensing apparatus.Induction heating equipment can be connected with and control the controlling organization that the induction frequencies of described induction heating equipment occurs, for instance can the Active foot plate of generation of distant control induction frequencies, the output of induction frequencies can be efficiently controlled by this controlling organization.
According to following detailed description of the invention and with reference to accompanying drawing, it is better understood with foregoing and the other objects, features and advantages of the present invention.
Accompanying drawing explanation
Fig. 1 illustrates the overall structure schematic diagram that can be effectively improved the composite preparation system that composite material interface combines according to the present invention one embodiment；
Fig. 2 illustrates the structural representation of the reactor in the composite preparation system shown in Fig. 1；
Fig. 3 illustrates the structural representation of the agitating device in the composite preparation system shown in Fig. 1；
Fig. 4 is the MnO of embodiments of the invention 4 preparation2Scanning electron microscope (SEM) photo of/graphite composite material.
Accompanying drawing labelling:
1, optic fiber thermometer；2, fibre optic temperature sensor；3, high-pressure mini reactor stored program controlled；4, pressure transducer；5, air bleeding valve；6, reactor；7, induction coil；8, induction heating equipment；9, pedal；10, blind flange；11, kettle cover；12, flanged plate；13, kettle；14, screw thread；15, bolt；16, driving device (motor)；17, drive link；18, stirring paddle.
Detailed description of the invention
The present invention is further illustrated, it should be appreciated that accompanying drawing and following embodiment are merely to illustrate the present invention below in conjunction with accompanying drawing and following embodiment, and the unrestricted present invention.
Specifically, Fig. 1 illustrates the overall structure schematic diagram that can be effectively improved the composite preparation system that composite material interface combines according to the present invention one embodiment；Fig. 2 illustrates the structural representation of the reactor in the composite preparation system shown in Fig. 1；Fig. 3 illustrates the structural representation of the agitating device in the composite preparation system shown in Fig. 1.
For the many disadvantages preparing composite in prior art, the invention provides a kind of composite preparation system, as shown in Figure 1 to Figure 3, including: for holding the reactor 6 of reactant and the sealing of matrix material；Detect the temperature detecting unit of temperature in described reactor 6；Detect the pressure sensing cell of pressure in described reactor 6；The force value that the temperature value detected based on described temperature detecting unit and described pressure sensing cell detect, carries out the heating unit of hydro-thermal sensing heating to described reactor；Described heating unit includes induction coil 7, induction heating equipment 8 and controls the controlling organization 9 that the induction frequencies of described induction heating equipment 8 occurs, described reactor 6 is arranged in described induction coil 7, the two ends of described induction coil 7 are installed on the outer wall of described induction heating equipment 8, and the inside of described induction coil 7 and described induction heating equipment 8 is connected with recirculated water.
The composite preparation system adopting the present invention is able to carry out being effectively improved the hydro-thermal sensing preparation method that composite material interface combines, the method technique is simple and easy to control, the special construction that multiple traditional method is difficult to synthesize can be synthesized, and the interface cohesion of composite can be effectively improved.
Such as, first by AsMaterial is dissolved in AlSolvent obtains solution A after stirring, by BsMaterial is dissolved in BlSolvent obtains B solution after stirring；Then by solution A and B solution mixing and stirring, after regulating pH value, C solution is obtained；Finally C solution is proceeded in reactor 6 as reactant, addition can sense the matrix material D of alternating magnetic field, being sealed by reactor 6 is placed in induction coil 7, during reactor 6 is heated by the electric current exported by induction heating equipment 8, from produced suspension, isolate product after reaction, clean, (E is for by A namely to obtain being loaded with product E after dryingsAnd BsSynthesis product) combination product F.
Specifically, the composite preparation system of the present invention is adopted can to perform following preparation method:
Step one: by AsMaterial is dissolved in AlIn solvent, after magnetic agitation 30～120min (or ultrasonic 30～120min), obtain the solution A of 0.01～5mol/L；
Step 2: by BsMaterial is dissolved in BlIn solvent, after magnetic agitation 30～120min (or ultrasonic 30～120min), obtain the B solution of 0.01～5mol/L；
Step 3: magnetic agitation 30～300min after solution A and B solution are mixed, and regulate pH value, obtain mixed liquor C；
Step 4: C solution is proceeded in reactor, addition can sense the matrix material D of alternating magnetic field, sealing is placed in hydro-thermal induction heating equipment, reaction 10min～24h under the induction frequencies of 10～500KHz and under the output electric current of 0～1200A, then naturally cools to room temperature；
Step 5: isolate product from reacted suspension, then by product respectively with deionized water and soaked in absolute ethyl alcohol washing, can obtain being loaded with the combination product F of product E after drying.
In the present invention, induction coil 7 is distributed in the outer wall of the kettle of reactor 6, and still internal induction material D is exactly in the middle part of induction coil 7, homogeneous heating and efficiency height, it is to avoid produce hot-spot phenomenon；Induction heating equipment 8 output AC electricity, to induction coil, produces alternating magnetic field by induction coil, and in still, material cutting magnetic induction answers line, produces faradic current, so that the material self that can sense alternating magnetic field in still reaches heated purpose；By controlling the size of output electric current, it is possible to achieve the adjustment of output, thus realizing the control of reaction temperature.Meanwhile, the matrix material D that temperature is higher can make material E be prone in nucleation about, regulates and controls the speed of growth of crystal again through adjustment mixing speed or ultrasonic power, thus reaching the purpose that the particle size to product regulates and controls.
And, as shown in Figure 1, it is internal that the kettle of reactor 6 is positioned at induction coil 7, induction coil 7 is installed on the outer wall of induction heating equipment 8, induction coil 7 is internal with induction heating equipment 8 is connected with the recirculated water from circulation, reactor 8 is connected to stored program controlled built with thermometric, pressure measuring system, and stored program controlled can be shown that temperature in the kettle and pressure.
Again, for hydro-thermal induction heating technique, generally along with the increase of output and the prolongation in response time, temperature in the kettle increases, thus wants to realize the invariable of temperature and must be introduced into control system.In the present invention, can being realized the control of temperature by two ways, a kind of is artificial, namely by observing the change of temperature on temperature detecting unit, adopts foot-operated mode to realize switching on and off of sensing heating；Another kind is automatic regulating system, and namely the temperature value of collecting temperature detection unit, is fed back to induction heating equipment, realizes being automatically adjusted and controlling of temperature thereby through induction heating equipment.
It addition, traditional thermocouple sensor mostly adopts metal probe, and metal probe can generate heat under the effect of alternating magnetic field, thus cannot be used in hydro-thermal sensing apparatus.Considering the problems such as the electromagnetism interference of probe, the precision of thermometric and cost, in this embodiment, temperature detecting unit can adopt the fibre optic temperature sensor 2 or infrared radiation thermometer that are connected with reactor 6.
Again, in order to ensure that reactant has good uniformity and dispersibility, agitating device can be introduced on reactor 6, wherein agitating device includes being located at the drive link 17 within kettle, the stirring paddle 18 being located on drive link and the driving device 16 for driving drive link 17 to rotate, and driving device 16 is located at outside kettle.Stirring paddle 18 adopts one or more in axial impellers, radial flow stirring paddle or mixed flow stirring paddle, and the gap between stirring paddle 18 and inner wall of kettle is 0.5～1cm；Can also reactor be placed in Ultrasound Instrument, realize the dispersion of reactant by controlling ultrasonic power, such that it is able to make product E homoepitaxial and distribution on matrix material D.
Again, in this embodiment, pressure sensing cell realizes mainly by the pressure transducer 4 that can sense gas pressure in reactor, and converts electrical signals to digital signal by high-pressure mini reactor stored program controlled 3, then shows.Additionally, the air bleeding valve 5 being connected with reactor 6 shown in Fig. 1 can play reaction terminates the effect of rear pressure release.
Additionally, due to metal can sense alternating magnetic field mostly, thus the selection of reactor 6 material is a crucial problem.Consider that the performances such as the electromagnetism interference of material, heat-resisting quantity, heat stability, corrosion resistance, radiation resistance, resistance to chemical attack and solvent resistance, reactor 6 can adopt the high molecular polymer such as polyparaphenylene phenol (PPL) or politef (PTFE).
Consider the selection (electromagnetism interference of reactor sealingly secure and sealer material, heat-resisting quantity, heat stability, corrosion resistance, radiation resistance, resistance to chemical attack and solvent resistance etc.), adopt the blind flange 10 being threaded 14, flanged plate 12 seals, flanged plate 12 can be located at the open end of the kettle 13 of reactor 6, blind flange 10 is located on the kettle cover 11 of reactor 6, it is closely attached flanged plate 12 and blind flange 10 by the bolt 15 being inserted in screw thread 14, thus, the top seal of reaction kettle body have employed thread seal, additionally can increase the safety to increase equipment such as buckle.
Preferably, adopt in the aforementioned preparation process performed by preparation system of the present invention, also by the product that obtains in above-mentioned steps five after chemical attack or physics calcination processing, matrix material D can be removed, it is possible to obtain the material E with controlled architecture.This provides a kind of new technology to Template synthesis material.
The structure of prepared composite can be membrane structure, coating structure, nucleocapsid structure, lamellar connection grain structure and loose structure etc..
Additionally, mixed liquor can be colloidal sol shape in above-mentioned steps three, thus realizing the combination with sol-gal process.Can also be that pasty state brush is on matrix material D, it is achieved the materials synthesis under air (or atmosphere) condition, rather than under liquid-phase condition.And, the pH value in above-mentioned steps three is employing 0.1～5mol L-1Hydrochloric acid solution, acetum, sodium hydroxide solution, potassium hydroxide solution or ammonia etc. is adjusted.Preferably, the dry detailed process in described step 3, for be placed in electric vacunm drying case by product, heats 12～36 hours at 50～120 DEG C, and the pH value in step 3 is 0～14.
Relative to prior art, the invention have the benefit that
The invention provides a kind of preparation method adopting the preparation of hydro-thermal induction technology to have the composite that excellent interface combines.Solution A and B solution are mixed its pH value of adjustment and obtains C solution, then C solution proceeded in reactor and add the matrix material D that can sense alternating magnetic field, in induction heating equipment after reaction, take out suspension and through separating, washing and dried, finally prepare the composite F being loaded with product E.
The composite with different performance can be synthesized, by selecting the matrix material D with different structure can obtain the composite with different structure by changing output electric current and response time.The heats of matrix material D in hydro-thermal induction heating technique, provides site for reactant nucleation and accelerates the growth of crystal.
It is directly heated that the mode of third party's heating in traditional handicraft is changed into matrix material itself by the present invention, fundamentally (angle of heating and heat transfer) changes the principle preparing composite, technique is simple and easy to control, the composite chemical composition prepared is homogeneous, purity is higher, crystal morphology rule, particle diameter is less and is evenly distributed, and interface cohesion is excellent.Additionally, the manufacturing cycle of composite is considerably reduced, it is not necessary to subsequent treatment and environmentally friendly, thus it is more easily implemented industrialized production.
It has the beneficial effect that more specifically:
(1) traditional hydro-thermal or microwave attenuation materials technology, it is all utilize third party's solvent to be heated, then heat is passed to matrix material and reactant by heated solvent, to reach to prepare the purpose of composite, between such D and E, not directly contact or reaction, causes that their interface cohesion is more weak.The present invention adopts hydro-thermal induction heating technique to change the mode of heating and heat transfer in reaction completely, matrix material itself is heated to higher temperature in the short period of time at first, the temperature in all the other places is all relatively low, As and Bs so can be made to react synthetic product E under the high temperature of matrix material D, such that it is able to be obviously improved the interface cohesion of D and E.
(2) significantly high owing to adding, in sensing, the temperature hankering matrix material, cause that the speed of synthetic material E is very fast, degree of crystallinity is higher and purity is higher, because of without post processing.
(3) this technology can be applied to Template synthesis and has in the preparation method of material of a fixed structure, it is to avoid conventional template needs in advance through processing the shortcoming to obtain avtive spot, and this has widened the application of template.
(4) this technology can also combine with sol-gal process, it is achieved the preparation of composite under air (or atmosphere) condition.
(5) the method is that the preparation of coating and thin film provides a kind of brand-new realization means.
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Embodiment 1
Step one: the potassium permanganate of 0.012mol is dissolved in 30ml distilled water, obtains the potassium permanganate solution of 0.4mol/L after magnetic agitation 30min；
Step 2: be scattered in 30ml distilled water by the benzenpropanal of 0.012mol, obtains the benzenpropanal solution of 0.4mol/L after magnetic agitation 30min；
Step 3: magnetic agitation 30min after potassium permanganate solution and benzenpropanal solution being mixed, obtains reaction precursor liquid C；
Step 4: proceed in reactor by precursor liquid C, adds the graphite flake that can sense alternating magnetic field, seals and is placed in hydro-thermal induction heating equipment, reaction 24h under the induction frequencies of 50KHz and under the output electric current of 200A, then naturally cools to room temperature；
Step 5:: from reacted suspension, isolate combination product, then by product respectively with deionized water and soaked in absolute ethyl alcohol washing, lamellar MnO can be obtained after drying2/ graphite composite material..
Embodiment 2
Step one: the potassium permanganate of 0.015mol is dissolved in 30ml distilled water, obtains the potassium permanganate solution of 0.5mol/L after magnetic agitation 50min；
Step 2: be scattered in 30ml distilled water by the benzenpropanal of 0.015mol, obtains the benzenpropanal solution of 0.5mol/L after magnetic agitation 50min；
Step 3: magnetic agitation 50min after potassium permanganate solution and benzenpropanal solution being mixed, obtains reaction precursor liquid C；
Step 4: proceed in reactor by precursor liquid C, adds the graphite flake that can sense alternating magnetic field, seals and is placed in hydro-thermal induction heating equipment, reaction 16h under the induction frequencies of 50KHz and under the output electric current of 300A, then naturally cools to room temperature；
Step 5: isolate combination product from reacted suspension, then by product respectively with deionized water and soaked in absolute ethyl alcohol washing, lamellar MnO can be obtained after drying2/ graphite composite material.
Embodiment 3
Step one: the potassium permanganate of 0.02mol is dissolved in 30ml distilled water, obtains the potassium permanganate solution of 0.67mol/L after magnetic agitation 70min；
Step 2: be scattered in 30ml distilled water by the benzenpropanal of 0.02mol, obtains the benzenpropanal solution of 0.67mol/L after magnetic agitation 70min；
Step 3: magnetic agitation 70min after potassium permanganate solution and benzenpropanal solution being mixed, obtains reaction precursor liquid C；
Step 4: proceed in reactor by precursor liquid C, adds the graphite flake that can sense alternating magnetic field, seals and is placed in hydro-thermal induction heating equipment, reaction 10h under the induction frequencies of 50KHz and under the output electric current of 400A, then naturally cools to room temperature；
Step 5: isolate combination product from reacted suspension, then by product respectively with deionized water and soaked in absolute ethyl alcohol washing, lamellar MnO can be obtained after drying2/ graphite composite material.
Embodiment 4
Step one: the potassium permanganate of 0.03mol is dissolved in 30ml distilled water, obtains the potassium permanganate solution of 1mol/L after magnetic agitation 90min；
Step 2: be scattered in 30ml distilled water by the benzenpropanal of 0.03mol, obtains the benzenpropanal solution of 1mol/L after magnetic agitation 90min；
Step 3: magnetic agitation 90min after potassium permanganate solution and benzenpropanal solution being mixed, obtains reaction precursor liquid C；
Step 4: proceed in reactor by precursor liquid C, adds the graphite flake that can sense alternating magnetic field, seals and is placed in hydro-thermal induction heating equipment, reaction 1h under the induction frequencies of 50KHz and under the output electric current of 500A, then naturally cools to room temperature；
Step 5: isolate combination product from reacted suspension, then by product respectively with deionized water and soaked in absolute ethyl alcohol washing, lamellar MnO can be obtained after drying2/ graphite composite material.
Fig. 4 illustrates MnO prepared by above-described embodiment 12Scanning electron microscope (SEM) photo of/graphite composite material.The MnO that particle size is less as seen from Figure 42It is carried on graphite flake to define finer and close one layer, and is interconnected between granule and defines relatively regular pore structure.
The present invention incorporates the advantage of sensing heating and hydro-thermal reaction technology, hydro-thermal induction heating technique is applied to the preparation of composite, the interface cohesion of composite can be improved to a great extent, the shortcoming overcoming third party's heating technique synthetic composite material interface cohesion difference.Meanwhile, by introducing temperature detecting unit and pressure sensing cell, it is achieved that the test of reaction temperature and pressure in course of reaction, it is achieved thereby that the controlled synthesis of composite.Additionally, after being removed by matrix material by the method for chemical attack or physics calcining, it is possible to obtain the E material with special construction, thus this technology has the material of a fixed structure to Template synthesis and provides and a kind of new realize method.
Under the objective without departing from the basic feature of the present invention, the present invention can be presented as various ways, therefore the embodiment in the present invention is an illustration for and unrestricted, owing to the scope of the present invention is defined by the claims but not limited by description, and drop on the scope that claim defines, or all changes in the full scope of equivalents of its scope defined are understood to include in detail in the claims.
Claims (10)
1. one kind is effectively improved the composite preparation system that composite material interface combines, it is characterized in that: include reactor (6) and the device of sensing alternating magnetic field is provided, reactant it is placed with and for sensing the matrix material of alternating magnetic field in described reactor, described matrix material produces electric current by cutting the line of induction of sensing alternating magnetic field, thus reaching heated purpose.
2. a kind of composite preparation system being effectively improved composite material interface combination according to claim 1, it is characterized in that: the described device providing sensing alternating magnetic field includes induction coil (7) and induction heating equipment (8), and described induction coil (7) is arranged on the outer wall of reactor (6) and is connected with induction heating equipment (8).
3. a kind of composite preparation system being effectively improved composite material interface combination according to claim 2, it is characterized in that: the material of described induction coil is side's copper pipe, coil shape is circular, outer layer is wound around insulating barrier, coil turn is 2～10, loop length is 0.5～2m, and internal coil diameter is 20～200mm.
4. a kind of composite preparation system being effectively improved composite material interface combination according to claim 1, it is characterized in that: described reactor has farther included material in reactor is carried out scattered dispersal device, this dispersal device is be arranged on agitating device in reactor or the ultrasonic device for placing response still.
5. a kind of composite preparation system being effectively improved composite material interface combination according to claim 4, it is characterized in that: drive link (17) that the described agitating device in reactor includes being arranged in reactor and be used for driving drive link (17) driving device (16), described drive link is evenly arranged with multiple stirring paddle, this stirring paddle is axial impellers, radial flow stirring paddle or the mixed flow stirring paddle of the two, leaves space between the inwall of described stirring paddle and described reactor.
6. a kind of composite preparation system being effectively improved composite material interface combination according to claim 1, it is characterized in that: described reactor (6) includes kettle cover (11) and axe body (13), described reactor (6) is sealed by sealing mechanism, this sealing mechanism includes the flanged plate (12) being located at kettle (13) open end of described reactor, it is located at the blind flange (10) on the kettle cover (11) of described reactor, and it is used for the fastening component being closely attached described flanged plate (12) with described blind flange (10).
7. a kind of composite preparation system being effectively improved composite material interface combination according to claim 1, it is characterized in that: described composite preparation system farther includes the temperature detecting unit for detecting reactor temperature and pressure and pressure sensing cell, and the reactor stored program controlled for temperature and pressure is controlled, described temperature detecting unit is light temperature sensor or infrared radiation thermometer, and described pressure sensing cell is for sensing the pressure transducer of gas pressure in reaction.
8. a kind of composite preparation system being effectively improved composite material interface combination according to claim 2, it is characterized in that: described reactor is provided with air bleeding valve (5), this air bleeding valve (5) is metal material, and the distance of air bleeding valve (5) and induction coil (7) is more than 50cm.
9. a kind of composite preparation system being effectively improved composite material interface combination according to claim 2, it is characterized in that: the described matrix material for sensing alternating magnetic field is positioned at reactor and is positioned at the position corresponding with induction coil, in order to be heated properly.
10. a kind of composite preparation system being effectively improved composite material interface combination according to claim 1, it is characterised in that: the material of described reactor is polyparaphenylene phenol, politef or other high molecular polymers.
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| CN112023844A (en) * | 2020-08-12 | 2020-12-04 | 陕西科技大学 | Hydrothermal induction heating method for material preparation and preparation system thereof |
| CN115090382A (en) * | 2022-07-05 | 2022-09-23 | 长沙理工大学 | Asphalt production equipment capable of dispersing asphalt molecular groups and use method |
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| CN104701517A (en) * | 2015-03-27 | 2015-06-10 | 陕西科技大学 | Method for preparing NH4V3O8 anode material for lithium ion battery |
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