CN206173234U - Controllable maximization combustion synthesis equipment of temperature pressure - Google Patents

Controllable maximization combustion synthesis equipment of temperature pressure Download PDF

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Publication number
CN206173234U
CN206173234U CN201621255598.XU CN201621255598U CN206173234U CN 206173234 U CN206173234 U CN 206173234U CN 201621255598 U CN201621255598 U CN 201621255598U CN 206173234 U CN206173234 U CN 206173234U
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temperature
reaction chamber
phase
pressure
maximization
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刘光华
杨增朝
贺刚
李江涛
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Technical Institute of Physics and Chemistry of CAS
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Technical Institute of Physics and Chemistry of CAS
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Abstract

The utility model discloses a controllable maximization combustion synthesis equipment of temperature pressure, including reaction chamber main part, reactor, hydraulic control system, temperature measuring system, phase change energy storage module control system, reaction chamber cooling system and pressure measuring system. The reactor is located in the reaction chamber main part, even there are hydraulic control system, temperature measuring system, phase change energy storage module control system, reaction chamber cooling system and pressure measuring system in the reaction chamber main part. The utility model discloses a maximization combustion synthesis equipment passes through reaction chamber cooling system and the accurate control to total heat in the combustion synthesis reaction chamber has been realized to the phase change energy storage component, has solved the not matching problem because exothermal reaction that the increase of reaction chamber volume brought and cooling power do all can, maintains within range between reasonable temperature and pressure zone with the inside temperature of reaction chamber to the production safety of equipment after guaranteeing to maximize.

Description

A kind of controllable maximization conbustion synthesis equipment of temperature, pressure
Technical field
The present invention relates to materials synthesis engineering device technique field.More particularly, to a kind of controllable maximization of temperature, pressure Conbustion synthesis equipment.
Background technology
Combustion synthesis method (being also called self-propagating high-temperature synthesis) is come synthetic material using exothermic heat of reaction between reactant A kind of method, reactant is once ignited, the regional spread that will be not yet reacted from trend, until reaction is complete, whole mistake Journey with little need for the external world provide energy, and be swift in response, generated time it is short.Combustion synthesis method has process is simple, cycle Short, energy consumption is low, it is with low cost the features such as, be one of important process method of synthesized high-performance ceramic powder material.
In terms of special cermacis powder is prepared using burning synthesis method, existing substantial amounts of patent and research paper are reported, For example, " a kind of method for preparing alpha-phase silicon nitride " (the patent US5032370) and " oneself of former Soviet Union Merzhanov et al. inventions Spread and prepare silicon nitride " (patent RU2257338), successfully prepared using burning synthesis method earlier except α phase silicon nitride powder Body, but the nitrogen pressure for using is (up to 30MPa) higher, it is very high to equipment requirement, it is unfavorable for amplifying production, while using A large amount of ammonium halide salts, can produce substantial amounts of hydrogen halide after reaction, both cause heavy corrosion to equipment, and also operating personnel are made Into harm, if directly discharged without treatment, also pollute the environment.Lin Zhiming of Physical Chemistry Technology Inst., Chinese Academy of Sciences et al. " method that temperature control activates Self- propagating Sintering Synthetic α phase silicon nitride powders " (the Chinese patent CN1673070A) of invention, by right Raw material is activated, and has prepared alpha-phase silicon nitride powder under relatively low nitrogen pressure, but because also need to use ammonium salt, therefore The problems such as there is also etching apparatus.New et al. the inventions of Tsing-Hua University Chen Ke " a kind of low-pressure combustion synthesizes alpha-phase silicon nitride powder Method " (Chinese patent CN1362358A), using silica flour suspension Nitriding Technology, can further reduce nitrogen pressure, realize It is continuously synthesizing to, but operation is more, the production cycle is more long, and energy consumption is also relatively large.
The conbustion synthesis equipment of current main flow includes two kinds:One kind is horizontal high-pressure reactor, and another kind is vertical high pressure Reactor, Central South University's Wang De will et al. have carried out structure improvement (Chinese patent to existing vertical autoclave CN2703594Y), prefabricating plate is provided with inside reaction chamber, controls prefabricating plate to transport up and down by the helical clamping device for being arranged on upper end It is dynamic, the precompressed to reaction chamber materials inside is realized, the patent does not carry out substantial improvement to reactor.
At present, in the existing equipment of special cermacis powder is prepared using burning synthesis method, volume of equipment not less than 100L, the volume and synthesis scale of equipment is all smaller, and single synthetic quantity is no more than 10kg, and overall production efficiency is relatively low, influence The performance of conbustion synthesis low-cost advantages.Therefore, the maximization of conbustion synthesis equipment is excellent with matching technological parameter Change is the key issue place of combustion synthesis technology industrialization, wherein the improvement to equipment is particularly difficult, combustion synthesis reaction one As carried out under the conditions of high temperature high pressure enclosed, the reaction chamber of equipment needs high temperature resistant, high pressure resistant, corrosion-resistant, and pressure and temperature Acutely, thermal shock resistance, compressive resistance mutability for reaction chamber etc. have requirement higher for the change of degree, in this case, Do not change on the basis of original structure is designed and blindly amplify conbustion synthesis equipment, be easily caused device temperature and pressure after amplifying Operating mode changes, such as when the reaction total heat that the volume increase that the lifting of reaction chamber cooling capacity is significantly smaller than reaction chamber brings During the increase of amount, can cause to maintain temperature higher inside reaction chamber, metal material used by reaction chamber is long-term in this case In high temperature and high pressure environment, tolerance declines, and easily triggers security incident.
Therefore, the present invention proposes a kind of controllable maximization conbustion synthesis equipment of temperature, pressure, improved to it is critical only that Exothermic reaction and the cooling capacity mismatch problem brought due to the increase of reaction chamber volume are solved, reaction chamber internal temperature is maintained In rational temperature and pressure interval range, so as to ensure the production safety of equipment after maximization.
The content of the invention
It is an object of the present invention to provide a kind of controllable maximization conbustion synthesis equipment of temperature, pressure.
To reach above-mentioned purpose, the present invention uses following technical proposals:
A kind of controllable maximization conbustion synthesis equipment of temperature, pressure, including reaction cavity main body, reactor, hydraulic control system System, temperature measurement system, phase-change accumulation energy module control system, reaction chamber cooling system and pressure-measuring system;The reactor In reaction cavity main body;Hydraulic control system, temperature measurement system, phase-change accumulation energy module control are connected with the reaction cavity main body System processed, reaction chamber cooling system and pressure-measuring system;
The reaction cavity main body includes reaction chamber lid, reaction chamber, cooling chamber, relief valve, pressure measuring element, temperature survey Element, phase-change accumulation energy element and phase-change accumulation energy detection means;
The reaction chamber side is provided with reaction chamber lid, and opposite side is provided with relief valve;The reaction chamber lid is connected by wire Hydraulic control system;
Reactor is provided with inside the reaction chamber;
The inwall of the reaction chamber is provided with phase-change accumulation energy element;
The upper end of the reaction chamber is provided with pressure measuring element, and lower end is provided with temperature-measuring element and phase-change accumulation energy detection dress Put;The pressure measuring element connects pressure-measuring system by wire, realizes the in good time collection and control of reaction cavity pressure; The temperature-measuring element connects temperature measurement system by wire, realizes the collection and detection of temperature;The phase-change accumulation energy inspection The upper end connection phase-change accumulation energy element of device is surveyed, lower end connects phase-change accumulation energy module control system by wire, by phase-change accumulation energy Control system is monitored and controlled the working condition of phase-change accumulation energy element;
Cooling chamber is arranged with outside the reaction chamber;The cooling chamber is hollow structure, and cooling water can be flowed to from one end The other end realizes circulation, takes away the partial heat of reaction chamber;The cooling chamber is passed through by wire coupled reaction chamber cooling system Cooling system can realize the precise control of cooling velocity.
Preferably, the reaction chamber is in cylinder type, and volume is 0.2-20m3
Preferably, the movable connection of the phase-change accumulation energy element or fixed it is connected on the inwall of reaction chamber;The phase It is one group to become energy-storage travelling wave tube;
Preferably, the temperature-measuring element is at least two groups;
Preferably, the pressure measuring element is at least two groups;
Preferably, the reactor includes more than one layer of material boat, and one end of the material boat is provided with ignition location, the material More than two temperature of charge measurement points are equidistantly positioned on boat, the temperature of charge measurement point connects temperature survey by wire Element, it is possible to achieve the temperature survey of reaction mass.
Preferably, the phase-changing energy storage material of the phase-change accumulation energy element is selected from Sodium acetate trihydrate, NH4Al(SO4)2·6H2O、 Mg(NO3)2·6H2O、KCl-ZnCl2、NaCl-MgCl2、NaF-KF-LiF-MgF2、Al-Si、Al-Cu-Si、Mg-Zn、Al-Mg- One or more in Zn;
Preferably, the structure of the phase-change accumulation energy element is bent-tube boiler, coiled or array tubular type, pipe interior sealing phase transformation storage Can material;
Preferably, the structure of the phase-change accumulation energy element is circular or cylindric, and annulus or the phase transformation of cylinder interior sealing are stored up Can material.
Preferably, the phase transition temperature interval of the phase-changing energy storage material is 50-600 DEG C, and latent heat of phase change is 150-500kJ/ kg。
Technical scheme is realized to the accurate of combustion synthesis reaction cavity total heat by two technological means Control.One is the precise control of reaction chamber cooling system, and the stream of cooling water in cooling chamber is controlled by described cooling system Speed and flow;Two is that phase-change accumulation energy element is set inside reaction chamber, leading portion and stage casing in combustion synthesis reaction, reaction chamber During temperature and pressure rapid growth, phase-change accumulation energy element can absorb heat, until phase transition temperature, slows down in reaction chamber The elevated speed of temperature, when entering posterior segment with combustion synthesis reaction, the temperature of reaction chamber starts progressively to decline, when less than phase When becoming the phase transition temperature of energy-storage travelling wave tube, phase-change accumulation energy element starts to discharge heat energy to reaction chamber, so as to slow down reaction cavity temperature The speed of reduction, it can be seen that, phase-change accumulation energy element reduces the gradient of temperature in whole course of reaction, it is ensured that conbustion synthesis Reaction is completed under a metastable environment temperature and pressure.
Beneficial effects of the present invention are as follows:
Maximization conbustion synthesis equipment of the invention is realized to combustion by reaction chamber cooling system and phase-change accumulation energy element Burnt together is solved due to the exothermic reaction that the increase of reaction chamber volume brings and cooling energy into the precise control of total amount of heat in reaction chamber Power mismatch problem, reaction chamber internal temperature is maintained in rational temperature and pressure interval range, so as to ensure maximization The production safety of equipment afterwards.
Brief description of the drawings
Specific embodiment of the invention is described in further detail below in conjunction with the accompanying drawings.
Fig. 1 shows the schematic diagram of the medium-and-large-sizedization conbustion synthesis equipment of embodiment 1.
Specific embodiment
In order to illustrate more clearly of the present invention, the present invention is done further with reference to preferred embodiments and drawings It is bright.Similar part is indicated with identical reference in accompanying drawing.It will be appreciated by those skilled in the art that institute is specific below The content of description is illustrative and be not restrictive, and should not be limited the scope of the invention with this.
Embodiment 1
One kind maximization conbustion synthesis equipment, including reaction cavity main body, reactor 2, hydraulic control system, temperature survey system System, phase-change accumulation energy module control system, reaction chamber cooling system and pressure-measuring system;
Reaction cavity main body includes that reaction chamber lid 1, reaction chamber 4, cooling chamber 5, relief valve 7, pressure measuring element 3, temperature are surveyed Amount element 8, phase-change accumulation energy element 6 and phase-change accumulation energy detection means 9;Reaction chamber 4 is in cylinder type, and volume is 0.2-20m3
The side of reaction chamber 4 is provided with reaction chamber lid 1, and opposite side is provided with relief valve 7;Reaction chamber lid 1 connects hydraulic pressure by wire Control system;Reactor 2 is provided with inside reaction chamber 4;Reactor 2 includes more than one layer of material boat, and two are equidistantly positioned on material boat Temperature of charge measurement point more than individual, temperature of charge measurement point connects temperature-measuring element by wire, it is possible to achieve reactant The temperature survey of material;
The inwall upper and lower ends of reaction chamber 4 are respectively equipped with one group of phase-change accumulation energy element 6;
The upper end of reaction chamber 4 is provided with two groups of pressure measuring elements 3, and lower end is provided with two groups of temperature-measuring elements 8 and phase transformation storage Can detection means 9;The pressure measuring element 3 connects pressure-measuring system by wire, realizes the in good time of reaction cavity pressure Collection and control;The temperature-measuring element 8 connects temperature measurement system by wire, realizes the collection and detection of temperature;Institute The upper end for stating phase-change accumulation energy detection means 9 connects phase-change accumulation energy element 6, and lower end connects phase-change accumulation energy module and controls system by wire System, the working condition of phase-change accumulation energy element is monitored and controlled by phase-change accumulation energy control system;
Cooling chamber 5 is arranged with outside reaction chamber 4;Cooling chamber 5 is hollow structure, and cooling water can flow to the other end from one end Circulation is realized, the partial heat of reaction chamber is taken away;Cooling chamber 5 passes through wire coupled reaction chamber cooling system, by cooling system It is capable of achieving the precise control of cooling velocity.
The movable connection of phase-change accumulation energy element 6 fixed is connected on the inwall of reaction chamber;Phase-change accumulation energy element 6 is by normal With phase-changing energy storage material be made, the form of bend pipe, coil pipe or array tube, pipe interior sealing phase-changing energy storage material are taken in structure; Circular or cylinder-like structure, annulus or cylinder interior sealing phase-changing energy storage material can also be taken.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not right The restriction of embodiments of the present invention, for those of ordinary skill in the field, may be used also on the basis of the above description To make other changes in different forms, all of implementation method cannot be exhaustive here, it is every to belong to this hair Obvious change that bright technical scheme is extended out changes row still in protection scope of the present invention.

Claims (10)

1. the controllable maximization conbustion synthesis equipment of a kind of temperature, pressure, it is characterised in that including reaction cavity main body, reactor, Hydraulic control system, temperature measurement system, phase-change accumulation energy module control system, reaction chamber cooling system and pressure-measuring system; The reactor is in reaction cavity main body;Hydraulic control system, temperature measurement system, phase transformation are connected with the reaction cavity main body Energy-storage module control system, reaction chamber cooling system and pressure-measuring system.
2. the controllable maximization conbustion synthesis equipment of a kind of temperature, pressure according to claim 1, it is characterised in that described Reaction cavity main body includes reaction chamber lid, reaction chamber, cooling chamber, relief valve, pressure measuring element, temperature-measuring element, phase transformation storage Can element and phase-change accumulation energy detection means;
The reaction chamber side is provided with reaction chamber lid, and opposite side is provided with relief valve;The reaction chamber lid connects hydraulic pressure by wire Control system;
Reactor is provided with inside the reaction chamber;
The inwall of the reaction chamber is provided with phase-change accumulation energy element;
The upper end of the reaction chamber is provided with pressure measuring element, and lower end is provided with temperature-measuring element and phase-change accumulation energy detection means; The pressure measuring element connects pressure-measuring system by wire;The temperature-measuring element connects temperature survey by wire System;The upper end connection phase-change accumulation energy element of the phase-change accumulation energy detection means, lower end connects phase-change accumulation energy module by wire Control system;
Cooling chamber is arranged with outside the reaction chamber;The cooling chamber is hollow structure;The cooling chamber connects anti-by wire Answer chamber cooling system.
3. the controllable maximization conbustion synthesis equipment of a kind of temperature, pressure according to claim 2, it is characterised in that described Reaction chamber is in cylinder type, and volume is 0.2-20m3
4. the controllable maximization conbustion synthesis equipment of a kind of temperature, pressure according to claim 2, it is characterised in that described Reactor includes more than one layer of material boat.
5. the controllable maximization conbustion synthesis equipment of a kind of temperature, pressure according to claim 4, it is characterised in that described Expect that one end of boat is provided with ignition location.
6. the controllable maximization conbustion synthesis equipment of a kind of temperature, pressure according to claim 4, it is characterised in that described More than two temperature of charge measurement points are equidistantly positioned on material boat, the temperature of charge measurement point connects temperature and surveys by wire Amount element.
7. the controllable maximization conbustion synthesis equipment of a kind of temperature, pressure according to claim 2, it is characterised in that described The movable connection of phase-change accumulation energy element fixed is connected on the inwall of reaction chamber.
8. the controllable maximization conbustion synthesis equipment of a kind of temperature, pressure according to claim 2, it is characterised in that described Phase-change accumulation energy element is one group;The temperature-measuring element is at least two groups;The pressure measuring element is at least two groups.
9. the controllable maximization conbustion synthesis equipment of a kind of temperature, pressure according to claim 2, it is characterised in that described The structure of phase-change accumulation energy element is bent-tube boiler, coiled or array tubular type, pipe interior sealing phase-changing energy storage material.
10. a kind of controllable maximization conbustion synthesis equipment of temperature, pressure according to claim 2, it is characterised in that institute It is circular or cylindrical shape, annulus or cylinder interior sealing phase-changing energy storage material to state the structure of phase-change accumulation energy element.
CN201621255598.XU 2016-11-16 2016-11-16 Controllable maximization combustion synthesis equipment of temperature pressure Active CN206173234U (en)

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Application Number Priority Date Filing Date Title
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Application Number Priority Date Filing Date Title
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