Background technology
Microwave can improve the speed of some chemical reaction significantly.At present, the chemical reaction that the overwhelming majority of reported in literature utilizes microwave technology to carry out is all finished in business-like household microwave oven, and this micro-wave oven cost is low, and volume is little, is suitable for various breadboard application.Yet there is obvious defects in the microwave chemical reactor of reported in literature aspect three: 1. power output is micro-wave oven manufactory design typification (to call acquiescence power in the following text), changes average output power by regulating the logical and disconnected time of microwave output.That is to say in the time period of microwave output " leading to " with the output of acquiescence power; And in the time period of " breaking " with zero energy output, different average output powers is acquiescence power and the zero energy mean value by the time weight on actually; 2. the distribution of the power in the microwave cavity is uneven, concentrates near the bottom tray; 3. the reactant in the reactor also is uneven to the absorption of microwave energy, and is more than paracentral near the bottle wall.
Microwave chemical reactor should have following performance: 1. power is adjustable continuously, 2. exports the firm power (not being mean power) of varying level; 3. control constant temperature, its precision<± 1 ℃; 4. have adjustable speed and show the mechanical agitator of mixing speed; 5. show microwave power; 6. the micro-wave oven furnace chamber internal power is evenly distributed; 7. by the parameters in computer sampling, the record course of reaction; 8. microwave leakage meets national standard.But commercially available microwave chemical reactor is difficult to satisfy all sidedly above-mentioned requirements at present, emphasis is set about from the defective of improving above-mentioned three aspects for this reason, designed the scheme that household microwave oven is transformed, improved microwave chemical reactor, obviously eliminated the defective of this three aspect, its function can satisfy above eight requirements.
Summary of the invention
Technical problem emphasis to be solved by this invention is to improve the open defect that above-mentioned microwave chemical reactor exists aspect three, and function can satisfy the microwave chemical reactor of above eight requirements.
The technical solution adopted in the present invention is: 1. regulate and control part: the mode of operation that can continuously change constant output (not being mean power), not taking must be through the way of professional micro-wave oven manufactory specialized designs manufacturing modulation anode of magnetron high pressure, but with the method for the input voltage that continuously changes the microwave power supply transformer, and adopt polymeter such as intelligent power/electric energy to show and the delivering power data; In the mode of operation work of constant temperature, be different from switching of reported in literature, but between by two kinds of output voltages of height that adjustable transformer is set in advance, switch, thereby reduced the fluctuation range of power at acquiescence power and not having between the zero energy; Former rotating disk is replaced with the irregularly shaped sets of fan blades of aluminum becomes the fan motor combination, improve the uniformity that microwave power distributes in furnace chamber; The mechanical agitator that employing has adjustable speed and shows mixing speed improves the reappearance of experiment condition to improve reactant in the reactor to the uniformity of the absorption of microwave energy; At last by the parameters (power, temperature, rotating speed etc.) in computer sampling, the record course of reaction; 2. reactor part: the furnace chamber upper wall perforate at micro-wave oven is used to install there-necked flask; Stirring vane and stirring vane sub-assembly are installed in the mouth in the middle of the there-necked flask; Tachogenerator is housed on the agitator; Glass straight cold finger and survey, temperature-control senser combination are installed in two side mouths of there-necked flask respectively; The diameter that there-necked flask is fixed on the furnace chamber bottom is on the polytetrafluoroethylene (PTFE) spiral lifting platform of 4.5cm; Agitator is installed on the agitator support.
The firm power output of microwave of the present invention is not mean power output, but constant microwave power.Under this duty, by adjustable transformer the input voltage of microwave power supply transformer is implemented modulation, make magnetron output microwave power varying level, constant within the specific limits.This firm power state can be kept uniform temperature for system self under the constant microwave power effect of research, for example during the boiling temperature of weak solution the firm power of varying level to the boiling point state under the influence that changes of system.It is that adjustment and control system reacts under steady temperature that present technique provides another kind of pattern.Under this pattern, the output voltage of the signal controlling adjustable transformer that intelligent temperature controller transmits according to platinum resistance thermometer switches between two kinds of voltages of the height that sets in advance that (high voltage of setting can make system be raised to the temperature of a little higher than setting, and low-voltage can make system temperature drop to the temperature that is lower than setting slightly), can reduce the amplitude that power fluctuation changes like this.
The invention has the beneficial effects as follows, operations such as improved micro-wave oven not only is convenient to feed in raw material, condensation, backflow, stirring, thermometric, and also loading and unloading are also very convenient.In order to reduce microwave leakage, the furnace chamber upper wall tapping of micro-wave oven protects with aluminium foil.Leak and can measure by tester through MHJ-2 type microwave, the microwave leakage amount of tapping is less than 0.3mW/cm
2, be lower than national safety standard 1mW/cm
2
The specific embodiment
The chemical reactor of microwave chemical reactor is partly seen Fig. 1.Reactor is made up of following each several part: open three holes at the furnace chamber upper wall of micro-wave oven, be used to stretch out three standard grounds of there-necked flask (1); 24 of centre
#Ground (10) is used to install the stirring vane sub-assembly (4) that comprises stirring vane (3) on the agitator (2); Stirring vane sub-assembly (4) also comprises overlapping joins 24
#The polytetrafluoroethylene (PTFE) stirring-head of mouth has through hole that can pass through stirring rod and the freight space that seals the O type tetrafluoroethene sealing ring of usefulness on the stirring-head, can be at the sub-assembly of maintenance system sealing under the stirring; Agitator is installed on the agitator support (5); Tachogenerator (6) is housed on the agitator; 19 of there-necked flask (1)
#Ground A (9) and 19
#Ground B (11) is respectively applied for installation glass straight cold finger (7) and survey, temperature-control senser make up (8); One end of glass straight cold finger (7) is and 19
#Ground (9) is supporting; Survey, temperature-control senser combination (8) is by with 19
#Ground B (11) supporting 19
#Ground and the glass bushing that has an end closure are formed, and can stretch into platinum resistance thermometer in the pipe, see Fig. 2 (0) sealing end that goes directly; Glass straight tube condenser (7) or survey, the conventional feeder that uses of the replaceable one-tenth chemical experiment of temperature-control senser combination (8) are so that add the reaction system to system; The diameter that there-necked flask (1) is fixed on furnace chamber (21) bottom of micro-wave oven is on the polytetrafluoroethylene (PTFE) spiral lifting platform (12) of 4.5cm.
The each several part of the measurement of microwave chemical reactor, control and power supply instrument is connected as shown in Figure 2: the output of adjustable transformer (16) connects microwave power supply transformer (14) through the protection switch (15) on the door for microwave oven and becomes the loop.The output of microwave power supply transformer (14), one tunnel low-voltage connects the filament of magnetron, and another road high voltage connects the anode of magnetron.The electrical quantity of adjustable transformer (16) modulation back output shows power data by polymeters such as intelligent power/electric energy (17), and flows to computer (22) by communication interface.Platinum resistance thermometer (0) is connected to intelligent temperature controller (19) and shows material temperature and be transferred to computer (22) by communication interface.The mixing speed signal of tachogenerator (6) shows rotating speed and is transferred to computer (22) by communication interface through intelligent revolution meter (18).Remove the rotating disk of former micro-wave oven furnace chamber bottom, be replaced with the irregularly shaped sets of fan blades of aluminum and become fan and motor (20), when machine operation, the aluminum fan blade can make to the irregular reflection of microwave that microwave energy distributes more even in the stove; Power switch and fuse are drawn and be connected in series to the 220V power line (23) of each several part.Each several parts such as the measurement of above microwave chemical reactor, control and power supply are connected measurement, demonstration, control and the power supply assembled unit that a relatively independent microwave chemical reactor is formed in the back, no longer dismantle when removing maintenance.
The parts of microwave chemical reactor (power is 1000W) are unaccounted to belong to general, conventional specification.
Intelligent revolution meter (18): its matching used tachogenerator: self-control, 1 pulse signal/commentaries on classics; The intelligence velocity metre should have communication function.LU-70 intelligence rotating speed/frequency meter of producing with An Dong Electronics Co., Ltd. among the utility model embodiment.
Material except that puddler in the stirring vane sub-assembly (4) is the glass, and miscellaneous part all adopts polytetrafluoroethylmaterial material.
Survey, temperature-control senser combination (8): except that platinum resistance thermometer (0), the miscellaneous part material is a glass.
Intelligent temperature controller (19): and the supporting use of platinum resistance thermometer (0).Intelligent temperature controller (19) has 0.1 ℃ resolution ratio, has communication function.The LU-906 intelligent PID adjusting apparatus of producing with An Dong Electronics Co., Ltd. among the utility model embodiment.
Polymeters such as intelligent power/electric energy (17): voltage: 0~600V, electric current: 0~5A has communication function.Polymeters such as the DW series single-phase intelligent power/energy of producing with three friendly instrument and meter for automation Co., Ltds in the embodiment of the invention.
The operation of reactor: by the conventional feeder that uses of chemical experiment will react system pass through there-necked flask (1) both sides 19
#Ground A (9) and 19
#Ground B (11) adds in the there-necked flask (1).Take out feeder, glass straight tube condenser (7) and survey, temperature-control senser combination (8) are installed respectively, platinum resistance thermometer (0) is inserted the nearly bottom of survey, temperature-control senser combination (8).Connect agitator (2) and install stirring vane sub-assembly (4).The cooling water import and export rubber tube that connects glass straight cold finger (7).After checking that stirring is worked well, close door of microwave oven.
Embodiment 1:
Microwave chemical reactor is worked under constant power-mode.According to specific embodiment operation, measuring with system is 350ml distilled water.After the instrument energising, the rotating speed of regulating mechanical agitator (2) is 350rpm, and it is as follows to measure adjustable transformer (16) constant power level of microwave chemical reactor under the output voltage of varying level:
Output voltage/the V of adjustable transformer (16) |
Constant power level/the Js of microwave chemical reactor
-1 |
Output voltage/the V of adjustable transformer (16) |
Constant power level/the Js of microwave chemical reactor
-1 |
220±1 |
1008±2 |
192±1 |
784±4 |
218±1 |
999±2 |
188±1 |
768±4 |
215±1 |
989±4 |
184±1 |
744±6 |
208±1 |
922±4 |
180±1 |
722±10 |
205±1 |
908±6 |
177±1 |
692±23 |
200±1 |
829±4 |
175±1 |
675±27 |
195±1 |
790±4 |
|
|
Embodiment 2:
Microwave chemical reactor is worked under constant power-mode.According to specific embodiment operation, measuring with system is the sucrose solution of 350ml20%.After the instrument energising, the rotating speed of regulating mechanical agitator (2) is 350rpm, treat the system boiling after, contain the 70mg/5ml aqueous citric acid solution with the 5ml pipette, extract and from glass straight cold finger (7) straight tube suitable for reading, be inserted into 19
#Behind ground A (9) horizontal level, above-mentioned aqueous citric acid solution is added in the system, takes out pipette.Make system under permanent power, fluidized state, react.The adjustable transformer that records (16) constant power level and reaction rate constant of microwave chemical reactor under the output voltage of varying level is as follows:
Output voltage/the V of adjustable transformer (16) |
Constant power level/Js
-1 |
Reaction rate constant/min
-1 |
179±1 |
712±14 |
2.53E-02 |
208±1 |
922±4 |
2.51E-02 |
216±1 |
992±3 |
3.02E-02 |
Embodiment 3:
Microwave chemical reactor is being regulated and control the maintenance system in the steady temperature pattern.Measuring with system is 350ml distilled water.According to specific embodiment operation, but do not add reactant, the temperature fluctuation range when only the temperature of check (difference is a maximum), hierarchy of control when the present technique high voltage appearance is set to 185V and low-voltage and is set to 0V is 60 ℃.Mixing speed: 788 ± 5rpm.Through three duplicate measurements, measure constant temperature more than 1 hour, power excursion: 750 ± 5~0Js at every turn
-1, maximum temperature fluctuation range is ± 0.7 ℃.