CN208414586U - Novel microwave hydrothermal electrodeposition system - Google Patents

Novel microwave hydrothermal electrodeposition system Download PDF

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Publication number
CN208414586U
CN208414586U CN201820815864.2U CN201820815864U CN208414586U CN 208414586 U CN208414586 U CN 208414586U CN 201820815864 U CN201820815864 U CN 201820815864U CN 208414586 U CN208414586 U CN 208414586U
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CN
China
Prior art keywords
microwave
kettle
power supply
reaction kettle
electrodeposition system
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Expired - Fee Related
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CN201820815864.2U
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Chinese (zh)
Inventor
熊信柏
雷灵均
于朔
刘玲
马俊
曾燮榕
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Shenzhen University
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Shenzhen University
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Abstract

The utility model discloses a kind of novel microwave hydrothermal electrodeposition system.The system includes reaction kettle device, bogey, microwave power supply, switch controlling device, DC power supply and cooling back installation;Equal grafting is installed on the temperature control element on kettle cover and extending respectively to reaction kettle, the positive and negative electrode for carrying out electro-deposition;Reaction kettle device include autoclave body open at one end, kettle cover, be installed on the intracorporal microwave penetration separation layer of kettle, be installed on autoclave body bottom microwave generator and circumferentially around and be embedded in inner wall of kettle cooling tube;Reaction kettle device is fixed on bogey;Microwave power supply is electrically connected with microwave generator;Switch controlling device is electrically connected with microwave power supply, while receiving the signal of temperature control element;DC power supply is electrically connected with positive and negative electrode;Cooling back installation is electrically connected with switch controlling device and is connected to cooling tube.The utility model structure is simple, reaction efficiency is high, control is accurate, runnability is stable and easy to operate, is suitble to preparation quality coating.

Description

Novel microwave hydrothermal electrodeposition system
Technical field
The utility model relates to composite material Preparation equipment technical field more particularly to a kind of novel microwave hydrothermal electrodepositions System.
Background technique
Hydrothermal electrodeposition method is placed in the conductive material with certain resistivity containing coating to be deposited or film composition Solion in, then by electric heating, under the action of microwave field, by control electrolyte temperature, current density or Voltage, to reduce the Gibbs free energy that coating or film are formed the technique of realizing the preparation of coating or film.The technique is not The advantages of only inheriting electrochemical process, and due to the introducing of microwave, new structure and functional material are necessarily formed, because This is a kind of technique having a extensive future.However, can not catchment about this at present actually since device is related to microwave The report for the device that thermoelectricity deposition and microwave are integrated.
Application No. is the microwaves that 200520079453.4 Chinese utility model patent discloses a kind of prepares coating or film Hydrothermal electrodeposition device, but the device has the following deficiencies: the microwave oven body working method that (1) is controlled by relay, it is difficult to it is real Existing stability contorting hydrothermal temperature, in middle low temperature range, temperature fluctuation range is larger, influences the effect of deposition;(2) temperature fluctuation When larger, it is cooling to cannot achieve Rapid Circulation, it is difficult to guarantee the relatively stable of hydrothermal deposition temperature;(3) two electrodes of power supply and Conducting wire and thermocouple and its conducting wire are placed directly in microwave, it may appear that sparking causes microwave generator to damage, or even causes whole A device is on fire, explodes;(4) reaction kettle of whole device is entirely located in micro-wave oven, it is desirable that micro-wave oven is sufficiently large, for microwave Furnace structure and material requirements are relatively high, and safety is poor.In short, there are a series of safe hidden danger for the utility model equipment, need It improves.
Utility model content
It can not obtain stable temperature for existing microwave hydrothermal electrodeposition device is existing in use and have peace The problems such as full hidden danger, the utility model provide a kind of novel microwave hydrothermal electrodeposition system.
To reach above-mentioned purpose of utility model, the utility model embodiment is adopted the following technical scheme that:
A kind of novel microwave hydrothermal electrodeposition system, including reaction kettle device, the reaction kettle device include open at one end Autoclave body, be covered on the opening kettle cover, be installed on the intracorporal microwave penetration separation layer of the kettle, be installed on the autoclave body The microwave generator of bottom and circumferentially around and the insertion inner wall of kettle cooling tube;
It further include for installing and fixing the bogey of the reaction kettle device, microwave power supply, switch controlling device, straight Galvanic electricity source and cooling back installation;
It and further include that equal grafting is installed on the kettle cover and extends respectively to the temperature control element of the reaction kettle, uses In the positive electrode and negative electrode that carry out electro-deposition;
Wherein, the reaction kettle device is detachably secured on the bogey;The microwave power supply and the microwave Generator electrical connection;The switch controlling device is electrically connected with the microwave power supply, and is electrically connected with alternating current, at the same also with it is described Temperature control element has signal transmission;The DC power supply is electrically connected with the positive electrode, negative electrode respectively;The cooling back installation It is electrically connected with the switch controlling device and passes through pipeline and be connected to the cooling tube.
Preferably, the positive electrode, negative electrode are carbon/carbon composite electrode using heat-resistant insulating macromolecular as clad.
Preferably, the density of the carbon/carbon composite electrode is 1.7~2.0g/cm3
Preferably, also there is the Microwave emission to microwave penetration separation layer transmitting microwave on the microwave generator End.
Preferably, seal groove is offered on the autoclave body end face where the opening, is placed with sealing ring on the seal groove.
Preferably, the spiral slide bar that the kettle cover lifting is adjusted, the spiral slide bar are installed on the bogey It is connect by briquetting with the kettle cover.
Preferably, the bogey is a body structure, and the bottom close to the body structure is equipped with for radiating Fan.
Preferably, the microwave penetration separation layer is quartz layer or sapphire glass layer.
Preferably, the switch controlling device has circulating cooling control module and microwave occurrence frequency adjustment module.
The utility model novel microwave hydrothermal electrodeposition system has the beneficial effect that
Compared with the existing technology, the novel microwave hydrothermal electrodeposition system of the utility model, is equipped in reactor bottom Microwave generator, and cooling tube is wound in reaction kettle wall body, the microwave that microwave generator generates directly is radiated to reaction kettle In interior liquid phase conducting medium solution, so that liquid phase conducting medium solution generates heat, and measures and monitor by temperature control element and react Temperature and kettle wall temperature in kettle, feed back to microwave power supply and cooling back installation, by microwave power supply and cooling back installation from The dynamic adjusting for carrying out microwave power and circulation rate, with the relatively stable of maintaining reaction temperature.The system has structure simple, anti- Answer high-efficient, control precisely, the features such as runnability is stable, easy to operate, highly-safe, suitable quality coating, film or Prepared by the hydrothermal electrodeposition of composite material, the coating being prepared, binding force can achieve 50MPa or more.
Detailed description of the invention
In order to illustrate more clearly of the technical scheme in the embodiment of the utility model, will make below to required in embodiment Attached drawing is briefly described, it should be apparent that, the drawings in the following description are merely some embodiments of the present invention, For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings Other attached drawings.
Fig. 1 is the utility model novel microwave hydrothermal electrodeposition system structure diagram;
Fig. 2 is reaction kettle device schematic top plan view in the utility model novel microwave hydrothermal electrodeposition system;
Fig. 3 is the elevational schematic view of reaction kettle device kettle cover in the utility model novel microwave hydrothermal electrodeposition system;
Fig. 4 is that reaction kettle device section view of line A-A along Fig. 2 is shown in the utility model novel microwave hydrothermal electrodeposition system It is intended to;
Wherein, 1- reaction kettle device, 11- autoclave body, 12- microwave penetration separation layer, 13- microwave generator, 131- microwave hair Penetrate end, 14- cooling tube, 15- kettle cover, 151- pressure gauge, 16- seal groove, 17- temperature control element, 18- bolt;
2- bogey, 21- spiral slide bar, 22- briquetting, 23- fan;
3- microwave power supply;
4- switch controlling device;
5- DC power supply;
6- cooling back installation, 61- coolant liquid inlet tube, 62- coolant liquid outlet tube.
Specific embodiment
In order to make the purpose of the utility model, technical solutions and advantages more clearly understood, below in conjunction with attached drawing and implementation Example, the present invention will be further described in detail.It should be appreciated that specific embodiment described herein is only used to explain The utility model is not used to limit the utility model.
It should be noted that it can be directly another when element is referred to as " being fixed on " or " being set to " another element On one element or indirectly on another element.When an element is known as " being connected to " another element, it can To be directly to another element or be indirectly connected on another element.
It is to be appreciated that term " length ", " width ", "upper", "lower", "front", "rear", "left", "right", "vertical", The orientation or positional relationship of the instructions such as "horizontal", "top", "bottom" "inner", "outside" is that orientation based on the figure or position are closed System, is merely for convenience of describing the present invention and simplifying the description, rather than the device or element of indication or suggestion meaning are necessary It with specific orientation, is constructed and operated in a specific orientation, therefore should not be understood as limiting the present invention.
In addition, term " first ", " second " are used for descriptive purposes only and cannot be understood as indicating or suggesting relative importance Or implicitly indicate the quantity of indicated technical characteristic.Define " first " as a result, the feature of " second " can be expressed or Implicitly include one or more of the features.The meaning of " plurality " is two or two in the description of the present invention, More than, unless otherwise specifically defined.
Also referring to Fig. 1, Fig. 2, Fig. 3, Fig. 4, now the utility model novel microwave hydrothermal electrodeposition system is said It is bright.
Referring to Fig. 1, the utility model embodiment provides a kind of novel microwave hydrothermal electrodeposition system.
The novel microwave hydrothermal electrodeposition system includes reaction kettle device 1, bogey 2, microwave power supply 3, switch control Device 4, DC power supply 5 and cooling-cycle device 6.
Wherein, Fig. 2, Fig. 3, Fig. 4 are please referred to, reaction kettle device 1 includes following component:
(a) autoclave body 11 and microwave generator 13, autoclave body 11 are that the entire novel microwave hydro-thermal electricity that can be used as open at one end sinks Product system carries out the reaction accommodating chamber of hydrothermal electrodeposition reaction, the autoclave body effect having the same with common reaction kettle;It is another End is equipped with microwave generator 13.
Preferably, the material of autoclave body 11 is stainless steel.
(b) microwave penetration separation layer 12, microwave penetration separation layer 12 is clamped and is installed in autoclave body 11, that is, is mounted on In the reaction accommodating chamber that autoclave body 11 is formed.
Preferably, microwave penetration separation layer 12 is by quartz glass or sapphire glass material by being process.
(c) microwave generator 13, as previously mentioned, microwave generator 13 is removably installed in the bottom of autoclave body 11, and It is additionally provided with Microwave emission end 131 towards the direction of microwave penetration separation layer 12, so that the microwave that microwave generator 13 generates, It can all directly emit into reaction accommodating chamber, improve the function and effect to liquid phase conducting medium solution.
(c) cooling tube 14, cooling tube 14 is circumferential to be embedded in and is surrounded in 11 wall of autoclave body, for microwave hydrothermal electro-deposition Liquid phase conducting medium solution carries out cooling or constant temperature;
(d) kettle cover 15, kettle cover 15 and autoclave body 11 are two components being separated from each other, and lid is located at the opening of autoclave body 11, Kettle cover 15 is the kettle cover for reacting accommodating chamber, and three pre-manufactured holes are at least offered on kettle cover 15, for grafting temperature control element 17, just Electrode, negative electrode.When kettle cover 15 is installed on the open end of autoclave body 11, temperature control element 17 extends to the formation of autoclave body 11 from kettle cover 15 Reaction accommodating chamber in, play and real time temperature induction monitoring and transmission carried out to the solution and 11 wall of autoclave body of microwave hydrothermal electro-deposition Effect;In addition, kettle cover 15 is also plugged with positive electrode and negative electrode for carrying out electro-deposition respectively, and the positive electrode and Negative electrode extends respectively in the reaction accommodating chamber of the formation of autoclave body 11;It is also equipped on kettle cover 15 for monitoring autoclave body 11 simultaneously React the pressure gauge 151 of accommodating chamber air pressure inside.
Preferably, temperature control element 17 is temperature sensor, and such as thermocouple can have multiple probes, and one of probe is set In liquid phase conducting medium solution, another probe is contacted with 11 wall of autoclave body.
Preferably, the positive electrode, negative electrode are carbon/carbon composite electrode using heat-resistant insulating macromolecular as clad. Further select density for 1.5~2.0g/cm3Carbon/carbon composite electrode.Using heat-resistant insulating macromolecular as carbon/carbon of clad Sparking can be effectively prevented in positive and negative electrode of the combination electrode as hydrothermal electrodeposition, guarantees the deposition that is powered, and excludes security risk.
Preferably, heat-resistant insulating macromolecular is polytetrafluoroethylene (PTFE).
As a result, as shown in Figure 1 and Figure 4, reaction kettle device 1 is removably clamped and is installed on bogey 2;Microwave power supply 3 are electrically connected with reaction kettle device 1, are specifically electrically connected with the microwave generator 13 of reaction kettle device 1;Switch controlling device 4 divides It is not electrically connected with microwave power supply 3, temperature control element 17 and cooling-cycle device 6, and is electrically connected by switch controlling device 4 with alternating current, To form the overall structure of the utility model novel microwave hydrothermal electrodeposition system.
When in use, it first using object to be deposited as cathode, and is attached with the negative electrode for carrying out electro-deposition, And it regard other electric conductors such as graphite plate (block) etc. as anode, and be attached with the positive electrode for carrying out electro-deposition, cathode It is hung on simultaneously with anode in the reaction accommodating chamber of the formation of autoclave body 11, contains liquid phase conducting medium solution in reaction accommodating chamber, So that liquid phase conducting medium solution did not had the cathode, anode, and it is ensured that temperature control element 17 is immersed in liquid phase conducting medium It in solution, covers kettle cover 15 and seals, be fixed on bogey 2, cooling tube 14 is connected to cooling-cycle device 6, Subsequent start-up switch controlling device 4 connects alternating current, starts switch control device 4 and microwave power supply 3, monitors microwave hydrothermal in real time Temperature, pH of electro-deposition etc. adjust input voltage, electric current, microwave in real time according to monitored results and power occur, to temperature it is suitable it Afterwards, start DC power supply 5, while adjusting sedimentation time, can obtain in object surface to be deposited has good pattern, high quality Depositing coating.
The novel microwave hydrothermal electrodeposition system of the utility model, there is the characteristics of following several respects:
(1) microwave generator is installed in reactor bottom, the microwave of generation only to the solution of electro-deposition work without Other components of system can be heated;
(2) cooling tube is wound in reaction kettle wall body, the microwave that microwave generator generates directly is radiated in reaction kettle Liquid phase conducting medium solution in so that liquid phase conducting medium solution generate heat, and by temperature control element measurement and monitoring reaction kettle Interior temperature and kettle wall temperature, feeds back to microwave power supply and cooling back installation, adjusts the frequency that microwave occurs by microwave power supply And in cooling-cycle device circulating cooling liquid flowing velocity and flow, so that automatic control is realized, with maintaining reaction temperature It is relatively stable;
It (3) is carbon/carbon composite electrode of clad as the positive and negative electrode of hydrothermal electrodeposition using heat-resistant insulating macromolecular, it can To effectively prevent striking sparks, guarantee the deposition that is powered, excludes security risk.
In summary the effect of several respects, the system is with structure is simple, at low cost, reaction efficiency is high, control is easy to be fast The features such as prompt accurate, runnability is stable, highly-safe, the hydro-thermal suitable for quality coating, film or composite material Electro-deposition preparation.
Even more important is that three kinds of microwave method, hydro-thermal method and electrodeposition process methods are successfully carried out good combination by this system, It can effectively solve the problems, such as that electrodeposition technology coating or film binding force are poor, the coating being prepared, binding force can reach To 50MPa or more, while solving the problems, such as that the coating of induction electro-deposition or film composition, object phase and pattern are not easy to control.
Further, referring to Fig. 4, a kind of tool as novel microwave hydrothermal electrodeposition system provided by the utility model Body embodiment offers seal groove 16 on 11 end face of autoclave body just opposite with kettle cover 15, places fastening on the seal groove 16 On the one hand sealing ring avoids the rigid of autoclave body 11 and kettle cover 15 by placing fit sealing circle on the end face of 11 open end of autoclave body Property contact, on the other hand play the role of seal autoclave body 11, avoid the spilling of reaction solution in microwave hydrothermal electrodeposition process.
Preferably, also kettle cover 15 and autoclave body 11 are fastened using bolt 18, it is ensured that entire Microwave Water thermoelectricity is heavy Product process safety is without danger.
Further, heavy as novel microwave hydro-thermal electricity provided by the utility model also referring to Fig. 1, Fig. 2 and Fig. 3 A kind of specific embodiment of product system, bogey 2 are a body structure, on the end face of clamping installation reaction kettle device 1 Spiral slide bar 21 is installed, spiral slide bar 21 is realized by briquetting 22 and kettle cover 15 and connected, and in the rotation of spiral slide bar 21 Under, realization is gone up and down to kettle cover 15 and is pressed control.
Preferably, there is the slot of installation briquetting 22 on kettle cover 15, kettle cover 15 is run through in 22 one end of briquetting, and extends to spiral shell Slide bar 21 is revolved, integrated with spiral slide bar 21, briquetting 22 is also fixed by bolt with kettle cover 15, and briquetting 22 is opened in autoclave body 11 The shape at the position of mouth face matches with 11 mouthfuls of autoclave body.
Bogey 2 is body structure, and the reaction kettle device 1 for the ease of being mounted in body structure can quickly dissipate Heat, it is preferable that be equipped in the bottom of body structure for cooling fan 23.Accelerate reaction kettle body device 1 by fan 23 External gas circulation, to play heat dissipation effect.
In addition, Fig. 1 and Fig. 4 are please referred to, one kind as novel microwave hydrothermal electrodeposition system provided by the utility model Specific embodiment, cooling tube 14 are connected to cooling back installation 6 by pipeline.Specifically the lower end of cooling tube 14 connects cooling Liquid input duct 61, upper end connect coolant liquid liquid outlet pipe 62, and the coolant line inversely transmitted improves cooling effect, due to Cooling back installation 6 is electrically connected with switch controlling device 4, and in entire reaction process, temperature control element 17 is monitored and fed back Temperature conditions can automatically adjust the flow velocity size of cooling circulation liquid after the analysis feedback of switch controlling device 4, thus Acceleration cooling can be played to the liquid phase conducting medium solution in autoclave body 11 or slows down cooling effect, to fast implement temperature It is constant, while adjusting the microwave occurrence frequency of microwave generator 13.
Preferably, coolant liquid can be water and be also possible to oil, and water or oil can fast implement the adjusting of temperature and steady It is fixed.
In order to preferably carry out monitoring temperature and adjusting to hydrothermal electrodeposition, need to the information of temperature control element feedback into The module that row accordingly regulates and controls, that is, there is the control module controlled cooling back installation 6 in switch controlling device 4 And the adjustment module that microwave occurrence frequency is adjusted is carried out to microwave generator 13.
The utility model is used to prepare calcium phosphorus biological coating or film in the above-mentioned novel microwave hydrothermal electrodeposition system of offer Or the method for composite materials may comprise steps of:
(1) the liquid phase conducting medium solution of deposition is contained in reaction kettle;
(2) by depositing base (for carrying the medium of coating or film or composite material) and anode material respectively with negative electricity Pole, positive electrode connection, guarantee that contact is good, are then immersed in liquid phase conducting medium solution;
(3) pre-manufactured hole that thermocouple is passed through to kettle cover 15 and briquetting 22, protrudes into the liquid phase conducting medium solution in reaction kettle In, compression is fixed to briquetting 22, kettle cover 15 and bogey 2 in blending bolt 17;
(4) start cooling back installation 6, the pipeline of guarantee feed liquor and out liquid is unimpeded, checks the registration of pressure gauge 151;
(5) microwave power supply 3, switch controlling device 4 are connected, setting microwave power, pre-heating temperature and time, starting is automatic Adjust shelves;
(6) after reaching preset temperature, start DC power supply 5, start the deposition for carrying out coating or film or composite material;
(7) after required sedimentation time to be achieved, it is first shut off DC power supply 5, stops deposition process;Microwave electricity is closed afterwards Source 3;
(8) valve is closed after continuing logical a period of time circulating cooling liquid, after reaction kettle is cooled to room temperature, turns off the switch control The master switch of device 4 processed takes out the matrix (i.e. product) that surface is deposited with coating or film, and it is clear to carry out deionized water to product It washes, dry, obtain the product for being prepared for coating, film or composite material.
To sum up, the utility model microwave hydrothermal electrodeposition device is due to improving precipitation equipment, microwave heating equipment Structure is more simple, at low cost, and operation control is more convenient, and the design of sealed shell of tank and circulating cooling system realizes more stable Temperature, the closed depositional environment of pressure condition, consider experiment Security and feasibility structure design, ensure that depositing electrode and The stabilization and sensitivity of thermocouple work, obtained product appearance structure characteristic is more controllable, and surface is more uniform, stablizes Property is stronger, and binding force is higher, and the scope of application is wider.
The above is only the preferred embodiment of the utility model only, is not intended to limit the utility model, all at this Made any modification, equivalent replacement or improvement etc., should be included in the utility model within the spirit and principle of utility model Protection scope within.

Claims (9)

1. a kind of novel microwave hydrothermal electrodeposition system, which is characterized in that including reaction kettle device, the reaction kettle device includes Autoclave body open at one end, is installed on the intracorporal microwave penetration separation layer of the kettle, is installed on the kettle cover for being covered on the opening The microwave generator of the autoclave body bottom and circumferentially around and the insertion inner wall of kettle cooling tube;
It further include for installing and fixing the bogey of the reaction kettle device, microwave power supply, switch controlling device, direct current Source and cooling back installation;
And further include equal grafting be installed on the kettle cover and extend respectively to the reaction kettle temperature control element, for into The positive electrode and negative electrode of row electro-deposition;
Wherein, the reaction kettle device is detachably secured on the bogey;The microwave power supply and the microwave occur Device electrical connection;The switch controlling device is electrically connected with the microwave power supply, and is electrically connected with alternating current, at the same also with the temperature control Element has signal transmission;The DC power supply is electrically connected with the positive electrode, negative electrode respectively;The cooling back installation and institute It states switch controlling device and is electrically connected and passes through pipeline and be connected to the cooling tube.
2. novel microwave hydrothermal electrodeposition system as described in claim 1, which is characterized in that the positive electrode, negative electrode are equal For using heat-resistant insulating macromolecular as carbon/carbon composite electrode of clad.
3. novel microwave hydrothermal electrodeposition system as claimed in claim 2, which is characterized in that the carbon/carbon composite electrode Density is 1.7~2.0g/cm3
4. novel microwave hydrothermal electrodeposition system as described in claim 1, which is characterized in that also have on the microwave generator The Microwave emission end of the oriented microwave penetration separation layer transmitting microwave.
5. novel microwave hydrothermal electrodeposition system as described in claim 1, which is characterized in that the autoclave body end where the opening Seal groove is offered on face, is placed with sealing ring on the seal groove.
6. novel microwave hydrothermal electrodeposition system as described in claim 1, which is characterized in that be equipped on the bogey The spiral slide bar of the kettle cover lifting is adjusted, the spiral slide bar is connect by briquetting with the kettle cover.
7. novel microwave hydrothermal electrodeposition system as described in claim 1, which is characterized in that the bogey is a cabinet Structure, the bottom close to the body structure are equipped with for cooling fan.
8. novel microwave hydrothermal electrodeposition system as described in claim 1, which is characterized in that the microwave penetration separation layer is Quartz layer or sapphire glass layer.
9. novel microwave hydrothermal electrodeposition system as described in claim 1, which is characterized in that the switch controlling device has Circulating cooling control module and microwave occurrence frequency adjustment module.
CN201820815864.2U 2018-05-29 2018-05-29 Novel microwave hydrothermal electrodeposition system Expired - Fee Related CN208414586U (en)

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Application Number Priority Date Filing Date Title
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110280196A (en) * 2019-07-01 2019-09-27 东莞理工学院 A kind of domestic waste microwave-driven hydrothermal carbonization reaction kettle device and method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110280196A (en) * 2019-07-01 2019-09-27 东莞理工学院 A kind of domestic waste microwave-driven hydrothermal carbonization reaction kettle device and method

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