CN209286685U - A kind of microwave heating acid purification devices - Google Patents
A kind of microwave heating acid purification devices Download PDFInfo
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- CN209286685U CN209286685U CN201821716897.8U CN201821716897U CN209286685U CN 209286685 U CN209286685 U CN 209286685U CN 201821716897 U CN201821716897 U CN 201821716897U CN 209286685 U CN209286685 U CN 209286685U
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- valve door
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- 239000002253 acid Substances 0.000 title claims abstract description 93
- 238000010438 heat treatment Methods 0.000 title claims abstract description 19
- 238000000746 purification Methods 0.000 title claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 105
- 239000007921 spray Substances 0.000 claims abstract description 30
- 238000001816 cooling Methods 0.000 claims abstract description 27
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000012530 fluid Substances 0.000 claims description 6
- 239000010453 quartz Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000003507 refrigerant Substances 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims 1
- 238000002604 ultrasonography Methods 0.000 claims 1
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 23
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 22
- 238000009835 boiling Methods 0.000 description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 14
- 238000000034 method Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 5
- 238000009833 condensation Methods 0.000 description 5
- 230000005494 condensation Effects 0.000 description 5
- 229910017604 nitric acid Inorganic materials 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- 238000011084 recovery Methods 0.000 description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 239000011737 fluorine Substances 0.000 description 3
- 238000012544 monitoring process Methods 0.000 description 3
- 235000021110 pickles Nutrition 0.000 description 3
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
Abstract
The utility model discloses a kind of microwave heating acid purification devices, including tetrafluoro tank, microwave generator, escape pipe, cooling cylinder, liquid-collecting barrel, vent gas treatment bucket, liquid valve door, liquid feeding pump, spent acid slot, liquid inlet electromagnetic valve door, spray head, shell, liquid collecting tank, microwave waveguide, circulating pump, circulating electromagnetic valve door;The utility model realizes the purity that ensure that acid purifying to sour purification process, realizes the purpose of continuous-stable work, and safe operation is simple, and selectivity is good, low energy consumption.
Description
Technical field
The utility model relates to a kind of microwave heating acid purification devices, are specifically related to the purifying of intelligentized control method waste acidity recovery
Management control in the process.
Background technique
Experimental analysis will often use high purity acid, and generate a large amount of spent acid, it is therefore desirable to will be in mixing acid pickle
Acid slow evaporation under sub- boiling state comes out, and condenses, is collected into the higher acid of purity, meets economical environment-protective.
Sour purifier is that heating keeps fluid temperature to evaporate lower than boiling temperature, then its acid vapor is condensed to prepare height
Pure water and high purity reagent are widely used in sample treatment and analysis.Ultrapure acid currently on the market is difficult since price is more expensive
Meet routine analysis demand, therefore purify the quality of optimization acid, is approach the most economically viable.It is that super clean laboratory is extracted
The competent assistant of high purity acid.
Usually there is the shortcomings that the following aspects during acid solution purification and recovery on the market at present;
(1) strong acid is highly corrosive, and people's multiple-contact strong acid, easily causes to endanger to human body usually in removal process
Evil.
(2) traditional monitor mode is all that staff passes through instrument monitoring in real time, without warning note.Once work
Personnel's carelessness, be easy to cause the generation of defect ware, and the serious equipment excess load that will lead to causes equipment burnout and laboratory fire
The great risk of calamity.
(3) for the liquid level of original acid solution, traditional solution judges liquid using the mode of range estimation liquid level tube
Position.Once personnel forget to estimate in time, it will the great risk for having dry combustion method even on fire.
(4) for the liquid level of high-purity acid solution, existing solution does not have any to detect and control measure automatically.Once liquid
Position is excessively high, and acid solution will overflow, and corrodes periphery object.
(5) traditional condensation process does not in real time monitor condensate temperature, easily causes and heat in gas condensation process
Liquid for condensation can not condense in time, can generate a large amount of strong acid steam, and recovery efficiency has very big discount.
(6) traditional heating method often just uses resistance heating, and not only power consumption is big, low to temperature adjusting sensitivity, cannot
Temperature in reacting furnace is adjusted in time, leads to the purity for influencing recycling acid solution.
(7) temperature controller of traditional solution is multi gear bit-type, rather than continuously adjustable type, can only probably be set
A fixed temperature value, can not accurately set.
(8) traditional solution is that temperature sensor is avoided to be corroded easily by high-temperature strong acid, temperature sensor peace
Mounted in container exterior, avoid contacting with strong acid, but such mounting means measurement be container outer wall temperature, can not reflect
The true temperature of acid solution, usual solution temperature will differ 5-20 DEG C with the temperature of container outer wall, and the measurement error of temperature is very big.
Summary of the invention
In view of the problems of the existing technology and insufficient, the utility model provides a kind of microwave heating acid purification devices, benefit
With microwave heating, continuous automatic production is realized, low energy consumption, and sour purifying rate is high, can satisfy the requirement of waste acidity recovery purification, tool
There is good application prospect.
A kind of microwave heating acid purification devices, including tetrafluoro tank 1, microwave generator 4, escape pipe 5, cooling cylinder 7, liquid-collecting barrel
9, vent gas treatment bucket 10, liquid valve door 11, liquid feeding pump 12, spent acid slot 13, liquid inlet electromagnetic valve door 14, spray head 15, shell 16, liquid collecting
Tank 17, microwave waveguide 18, circulating pump 19, circulating electromagnetic valve door 20;
Tetrafluoro tank 1, microwave generator 4, microwave waveguide 18 are arranged inside shell 16, and microwave waveguide 18 is arranged in tetrafluoro tank
Outside 1, microwave waveguide 18 is connected in microwave generator 4;Multiple spray heads 15, spray head 15 and two branches are set inside tetrafluoro tank 1
Connection, a branch is to be sequentially connected liquid feeding pump 12, spent acid slot 13, and liquid inlet electromagnetic valve door is arranged between spray head 15 and liquid feeding pump 12
14, another branch is to be sequentially connected circulating pump 19,1 bottom of tetrafluoro tank, setting circulation electromagnetism between spray head 15 and circulating pump 19
Valve 20,1 bottom of tetrafluoro tank are also connected with liquid collecting tank 17, and fluid valve 11, tetrafluoro is provided in 1 bottom of tetrafluoro tank between liquid collecting tank 17
Exhanst gas outlet is equipped at the top of tank 1, exhanst gas outlet is connect with escape pipe 5, and escape pipe 5 is connect after passing through cooling cylinder 7 with liquid-collecting barrel 9,
Liquid-collecting barrel 9 is connect with vent gas treatment bucket 10.
Described device further includes thermocouple temperature sensor 2, PLC control system 3, ultrasonic level gage 6, electric thermo-couple temperature
Sensor 2, ultrasonic level gage 6 are separately positioned on 1 top of tetrafluoro tank, for measuring temperature and liquid level inside tetrafluoro tank 1,
PLC control system 3 is electric with thermocouple temperature sensor 2, microwave generator 4, ultrasonic level gage 6, liquid feeding pump 12, feed liquor respectively
Magnet valve door 14, circulating pump 19, circulating electromagnetic valve door 20 connect, and PLC control system 3 includes PLC controller, circuit, display,
PLC controller is regular market purchase controller, and circuit is the route for connecting PLC controller and each sensor, component, power supply etc.,
Display is used to show that the temperature of the feedback of thermocouple temperature sensor 2, the power of microwave generator 4, ultrasonic level gage 6 to be fed back
Liquid level.
The vent gas treatment bucket 10 is equipped with lye, and lye is sodium hydroxide solution, sodium bicarbonate solution etc..
The part that cooling cylinder 7 is arranged in the escape pipe 5 is spiral cooling tube 8, is more advantageous to condensation, sets on cooling cylinder 7
There are refrigerant outlet and condensing agent entrance, condensing agent is water etc..
The escape pipe 5 is branched off into more than one pipeline after passing through cooling cylinder 7, and valve and company are respectively provided on each pipeline
A liquid-collecting barrel is connect, liquid-collecting barrel is connect with vent gas treatment bucket 10.
The inner wall of the shell 16 is quartz wall, further prevents microwave leakage.
In use, forming according to the spent acid in the spent acid slot 13 of detection early period, the boiling point of each acid in spent acid, PLC are determined
Control system 3 opens microwave generator 4, opens liquid inlet electromagnetic valve door 14, starts liquid feeding pump 12, and the spent acid in spent acid slot 13 is pumped
Enter in tetrafluoro tank 1, spent acid is sprayed from spray head 15, and during spent acid is pumped into, thermocouple temperature sensor 2 is supervised in real time
The temperature for surveying spent acid in tetrafluoro tank 1 adjusts microwave when 5-8 DEG C of boiling point of the temperature acid minimum lower than spent acid mid-boiling point
The power of device 4 allows microwave generator 4 to 1 inside heated at constant temperature of tetrafluoro tank, the acid of the boiling point is evaporated, and pushes up from tetrafluoro tank 1
The escape pipe 5 in portion is discharged, and escape pipe 5 flows into liquid-collecting barrel 9 after cooling cylinder 7 is cooling, and the tail gas not being condensed is from liquid-collecting barrel
After 9 come out, into vent gas treatment bucket 10, the tail gas after being cleaned is emptied, and ultrasonic level gage 6 monitors the liquid inside tetrafluoro tank 1
Face height, and spent acid liquid level is fed back into PLC control system 3, when spent acid liquid level reaches its highest order, highest order need to be lower than spray
First 15, PLC control system 3 closes liquid feeding pump 12 and liquid inlet electromagnetic valve door 14, stops feed liquor, and microwave generator 4 continues constant temperature and adds
Spent acid in hot tetrafluoro tank 1 no longer changes and liquid in liquid-collecting barrel 9 until ultrasonic level gage 6 feeds back the liquid level in tetrafluoro tank 1
Body is not further added by, and closes the valve on the liquid-collecting barrel at this time, opens the valve on another liquid-collecting barrel, and PLC control system 3 is opened
Circulating pump 19 and circulating electromagnetic valve door 20, the spent acid in tetrafluoro tank 1 are evacuated to spray head 15 again and are sprayed, and microwave is adjusted
Temperature is promoted to 5-8 DEG C of boiling point of acid next to the lowest lower than spent acid mid-boiling point, adjusts microwave after reaching temperature by the power of device 4
The power of generator 4 no longer changes and collects until ultrasonic level gage 6 feeds back the liquid level in tetrafluoro tank 1 to spent acid heated at constant temperature
Liquid in liquid bucket 9 is not further added by, and closes the valve on this liquid-collecting barrel at this time, and so on, until all spent acid detected
After being evaporated out, microwave generator 4, circulating pump 19, circulating electromagnetic valve door 20 are closed, opens liquid valve door 11, it will be remaining
Waste liquid be discharged into liquid collecting tank 17.
The beneficial effects of the utility model are:
(1) present apparatus uses microwave heating, and low energy consumption, can quickly adjust temperature in tetrafluoro tank, and sour purifying rate is high.
(2) ultrasonic level gage is arranged in the present apparatus, can not only observe liquid level variation, but also can control liquid feeding, and can also control
Removal waste fluid processed;Avoiding funnel before and after traditional funnel, liquid level tube and removal waste fluid valve scheme disconnected from each other add acid solution needs to pacify
The trouble unloaded is assembled and disassembled, pollution on the environment in liquid feeding discharge opeing process is avoided.
(3) present apparatus uses ultrasonic level gage and thermocouple temperature sensor, and is fully sealed with device, can be realized
Reaction process is monitored, solves the difficult status precisely detected.
(4) present apparatus is controlled using PLC system, realizes full-automatic continuous production, is detected and is operated convenient for operative employee.
Detailed description of the invention
The structural schematic diagram of 1 device of Fig. 1 embodiment;
In figure, 1- tetrafluoro tank, 2- thermocouple temperature sensor, 3-PLC control system, 4- microwave generator, 5- escape pipe,
6- ultrasonic level gage, 7- cooling cylinder, 8- spiral cooling tube, 9- liquid-collecting barrel, 10- vent gas treatment bucket, 11- liquid valve door, 12- into
Liquid pump, 13- spent acid slot, 14- liquid inlet electromagnetic valve door, 15- spray head, 16- shell, 17- liquid collecting tank, 18- microwave waveguide, 19- circulation
Pump, 20- circulating electromagnetic valve door.
Specific embodiment
The utility model is described in detail with reference to the accompanying drawings and examples, but the utility model is not by following implementations
The limitation of example.
Embodiment 1
A kind of microwave heating acid purification devices, as shown in Figure 1, including tetrafluoro tank 1, thermocouple temperature sensor 2, PLC control
System 3 processed, microwave generator 4, escape pipe 5, ultrasonic level gage 6, cooling cylinder 7, spiral cooling tube 8, liquid-collecting barrel 9, at tail gas
Manage bucket 10, liquid valve door 11, liquid feeding pump 12, spent acid slot 13, liquid inlet electromagnetic valve door 14, spray head 15, shell 16, liquid collecting tank 17, micro-
Sonic wave guide 18, circulating pump 19, circulating electromagnetic valve door 20;
Tetrafluoro tank 1, microwave generator 4, microwave waveguide 18 are arranged inside shell 16, and the inner wall of shell 16 is in quartz
Wall further prevents microwave leakage, and microwave waveguide 18 is arranged outside tetrafluoro tank 1, and microwave waveguide 18 and microwave generator 4 connect
It connects;Four spray heads 15 are set inside tetrafluoro tank 1, spray head 15 connect with two branches, a branch be sequentially connected liquid feeding pump 12,
Spent acid slot 13, between spray head 15 and liquid feeding pump 12 be arranged liquid inlet electromagnetic valve door 14, another branch be sequentially connected circulating pump 19,
Circulating electromagnetic valve door 20 is arranged in 1 bottom of tetrafluoro tank between spray head 15 and circulating pump 19,1 bottom of tetrafluoro tank is also connected with liquid collecting tank 17,
Fluid valve 11 is provided between 1 bottom of tetrafluoro tank and liquid collecting tank 17, exhanst gas outlet is equipped at the top of tetrafluoro tank 1, electric thermo-couple temperature passes
Sensor 2, ultrasonic level gage 6, exhanst gas outlet are connect with escape pipe 5, and escape pipe 5 connects after passing through cooling cylinder 7 with a liquid-collecting barrel 9
It connects, the part that cooling cylinder 7 is arranged in escape pipe 5 is spiral cooling tube 8, is more advantageous to condensation, cooling cylinder 7 goes out equipped with condensing agent
Mouth and condensing agent entrance, condensing agent is water, and liquid-collecting barrel 9 is connect with vent gas treatment bucket 10, and vent gas treatment bucket 10 is equipped with lye, lye
The sodium hydroxide solution for being 1mol/L for concentration, thermocouple temperature sensor 2, ultrasonic level gage 6 are for measuring in tetrafluoro tank 1
The temperature and liquid level in portion, the sensor conductive line surfaces that electric thermo-couple temperature passes 2 wrap up PTFE wrapping layer, prevent from being influenced to make by acid corrosion
With the service life, PLC control system 3 respectively with thermocouple temperature sensor 2, microwave generator 4, ultrasonic level gage 6, liquid feeding pump
12, liquid inlet electromagnetic valve door 14, circulating pump 19, circulating electromagnetic valve door 20 connect, PLC control system 3 include PLC controller, circuit,
Display, PLC controller are regular market purchase controller, and circuit is connection PLC controller and each sensor, component, power supply etc.
Route, display be used for show thermocouple temperature sensor 2 feed back temperature, microwave generator 4 power, supersonic liquid level
The liquid level of 6 feedback of meter.
Microwave generator 4 is made of components such as magnetrons, is fixed in the quartz wall of crust of the device, microwave generator
4 rated power is 500 ~ 2000W, and power adjustable, microwave generator 4 fixes with 18 nut of microwave waveguide, and microwave is by magnetron
It generates, converts electrical energy into microwave energy and be transferred to inside device.
Steps are as follows for the present apparatus specifically used:
(1) it mixes and detects hydrofluoric acid in acid pickle, the boiling point of hydrofluoric acid is 19.54 DEG C, opens the valve on liquid-collecting barrel 9
Door closes liquid valve door 11, liquid feeding pump 12, liquid inlet electromagnetic valve door 14, circulating pump 19, circulating electromagnetic valve door 20;
(2) PLC control system 3 opens microwave generator 4, opens liquid inlet electromagnetic valve door 14, starts liquid feeding pump 12, by spent acid
Spent acid in slot 13 is pumped into tetrafluoro tank 1, and spent acid is sprayed from spray head 15, during spent acid is pumped into, thermocouple temperature
It spends the temperature of spent acid in 2 real-time monitoring tetrafluoro tank 1 of sensor and feeds back to PLC control system 3, when temperature is lower than hydrogen fluorine in spent acid
Acid 5-8 DEG C of boiling point when, take at this time temperature be 19 DEG C, adjust microwave generator 4 power, allow microwave generator 4 to tetrafluoro tank 1
Internal heated at constant temperature, hydrofluoric acid is evaporated, and hydrofluoric acid vapor is discharged from the escape pipe 5 at 1 top of tetrafluoro tank, and escape pipe 5 passes through
Cross cooling cylinder 7 it is cooling after, flow into liquid-collecting barrel 9, after the tail gas not being condensed comes out from liquid-collecting barrel 9, into vent gas treatment bucket 10,
Tail gas emptying after being cleaned, ultrasonic level gage 6 monitor the liquid level inside tetrafluoro tank 1, and by the spent acid in tetrafluoro tank 1
Liquid level feedback is to PLC control system 3, and when spent acid liquid level reaches its highest order, highest order is lower than spray head 15, the present embodiment setting
Highest order closes liquid feeding pump 12 and liquid inlet electromagnetic valve door 14 apart from spray head 20cm, PLC control system 3, stops feed liquor, and microwave occurs
Device 4 continues the spent acid in heated at constant temperature tetrafluoro tank 1, keeps temperature-resistant in tetrafluoro tank 1, until ultrasonic level gage 6 is fed back
Liquid level in tetrafluoro tank 1 no longer changes and the liquid in liquid-collecting barrel 9 is not further added by, and hydrofluoric acid extraction finishes;
(3) PLC control system 3 closes microwave generator 4, circulating pump 19, circulating electromagnetic valve door 20, opens liquid valve door
11, remaining liquid is discharged into liquid collecting tank 17.
Found through detection, the purity for the hydrofluoric acid being collected into liquid-collecting barrel 9 is very high, metals content impurity down to
0.01ppb。
Embodiment 2
A kind of microwave heating acid purification devices, the quantity of spray head 15 are 6, and escape pipe 5 is branched off into three after passing through cooling cylinder 7
A branch, each road are equipped with one liquid-collecting barrel of valve and connection, and the quantity of liquid-collecting barrel is 3, and liquid-collecting barrel is and tail gas
It handles bucket 10 to connect, other component and connection type are same as Example 1.
Steps are as follows for the present apparatus specifically used:
(1) it mixes and detects hydrofluoric acid and nitric acid in acid pickle, the boiling point of hydrofluoric acid is 19.54 DEG C, and the boiling point of nitric acid is
122 DEG C, the valve on one of liquid-collecting barrel is opened, the valve on another two liquid-collecting barrel is closed, liquid valve door 11, liquid feeding pump
12, liquid inlet electromagnetic valve door 14, circulating pump 19, circulating electromagnetic valve door 20 are closed;
(2) PLC control system 3 opens microwave generator 4, opens liquid inlet electromagnetic valve door 14, starts liquid feeding pump 12, by spent acid
Spent acid in slot 13 is pumped into tetrafluoro tank 1, and spent acid is sprayed from spray head 15, during spent acid is pumped into, thermocouple temperature
It spends the temperature of spent acid in 2 real-time monitoring tetrafluoro tank 1 of sensor and feeds back to PLC control system 3, when temperature is lower than hydrogen fluorine in spent acid
Acid 5-8 DEG C of boiling point when, take at this time temperature be 19 DEG C, adjust microwave generator 4 power, allow microwave generator 4 to tetrafluoro tank 1
The hydrofluoric acid is evaporated by internal heated at constant temperature, and hydrofluoric acid vapor is discharged from the escape pipe 5 at 1 top of tetrafluoro tank, escape pipe 5
After cooling cylinder 7 is cooling, liquid-collecting barrel 9 is flowed into, after the tail gas not being condensed comes out from liquid-collecting barrel 9, into vent gas treatment bucket
10, the tail gas emptying after being cleaned, ultrasonic level gage 6 monitors the liquid level inside tetrafluoro tank 1, and will be in tetrafluoro tank 1
Spent acid liquid level feeds back to PLC control system 3, and when spent acid liquid level reaches its highest order, highest order is lower than spray head 15, the present embodiment
Highest order is set apart from spray head 20cm, PLC control system 3 closes liquid feeding pump 12 and liquid inlet electromagnetic valve door 14, stops feed liquor, microwave
Generator 4 continues the spent acid in heated at constant temperature tetrafluoro tank 1, keeps temperature-resistant in tetrafluoro tank 1, until ultrasonic level gage 6
Liquid level in feedback tetrafluoro tank 1 no longer changes and the liquid in liquid-collecting barrel 9 is not further added by, and closes the valve on the liquid-collecting barrel at this time
Door, opens the valve on another liquid-collecting barrel;
(3) PLC control system 3 opens circulating pump 19 and circulating electromagnetic valve door 20, and the spent acid in tetrafluoro tank 1 is evacuated to again
Spray head 15 sprays, and the power of adjustment microwave generator 4 heats spent acid, and the boiling point of the high nitric acid of boiling point second is
122 DEG C, and the boiling point of water is 100 DEG C, water can first evaporate, it is possible to first water evaporation be come out, adjusted after temperature reaches 95 DEG C
The power of whole microwave generator 4 keeps temperature-resistant in tetrafluoro tank 1, until ultrasonic level gage 6 to spent acid heated at constant temperature
Liquid level in feedback tetrafluoro tank 1 no longer changes and the liquid in liquid-collecting barrel 9 is not further added by, and closes the valve on this liquid-collecting barrel at this time
Door, opens the valve on another liquid-collecting barrel;
(4) circulating pump 19 and circulating electromagnetic valve door 20 are continued starting, the spent acid in tetrafluoro tank 1 is evacuated to spray head 15 again and sprayed
It spills, adjusts the power of microwave generator 4, after temperature reaches 117 DEG C, which is lower than 5 DEG C of nitric acid boiling point, adjusts microwave
The power of generator 4 keeps temperature-resistant in tetrafluoro tank 1 to spent acid heated at constant temperature, until ultrasonic level gage 6 feeds back four
Liquid level in fluorine tank 1 no longer changes and the liquid in liquid-collecting barrel 9 is not further added by, and spent acid evaporation purifying finishes;
(5) PLC control system 3 closes microwave generator 4, circulating pump 19, circulating electromagnetic valve door 20, passes to electric thermo-couple temperature
After the temperature of extraction raffinate in 2 feedback tetrafluoro tanks 1 reaches room temperature, liquid valve door 11 is opened, remaining liquid is discharged into liquid collecting tank 17.
It is found through detection, the purity of the hydrofluoric acid and nitric acid that are collected into two liquid-collecting barrels 9 is very high, metals content impurity
Down to 0.01ppb.
Claims (6)
1. a kind of microwave heating acid purification devices, which is characterized in that including tetrafluoro tank (1), microwave generator (4), escape pipe
(5), cooling cylinder (7), liquid-collecting barrel (9), vent gas treatment bucket (10), liquid valve door (11), liquid feeding pump (12), spent acid slot (13), into
Liquid electromagnetic valve (14), spray head (15), shell (16), liquid collecting tank (17), microwave waveguide (18), circulating pump (19), circulation electromagnetism
Valve (20);Tetrafluoro tank (1), microwave generator (4), microwave waveguide (18) setting are internal in shell (16), microwave waveguide (18)
Setting is external in tetrafluoro tank (1), and microwave waveguide (18) is connect with microwave generator (4);Multiple spray heads are set inside tetrafluoro tank (1)
(15), spray head (15) is connect with two branches, and a branch is to be sequentially connected liquid feeding pump (12), spent acid slot (13), spray head (15)
Liquid inlet electromagnetic valve door (14) are set between liquid feeding pump (12), another branch is to be sequentially connected circulating pump (19), tetrafluoro tank (1)
Circulating electromagnetic valve door (20) are arranged between spray head (15) and circulating pump (19) in bottom, and tetrafluoro tank (1) bottom is also connected with liquid collecting tank
(17), it is provided between tetrafluoro tank (1) bottom and liquid collecting tank (17) fluid valve (11), exhanst gas outlet is equipped at the top of tetrafluoro tank (1),
Exhanst gas outlet is connect with escape pipe (5), and escape pipe (5) passes through cooling cylinder (7) and connect afterwards with liquid-collecting barrel (9), liquid-collecting barrel (9) and tail
Gas disposal bucket (10) connection.
2. microwave heating acid purification devices according to claim 1, which is characterized in that further include thermocouple temperature sensor
(2), PLC control system (3), ultrasonic level gage (6), thermocouple temperature sensor (2), ultrasonic level gage (6) are set respectively
Set at the top of the tetrafluoro tank (1), PLC control system (3) respectively with thermocouple temperature sensor (2), microwave generator (4), ultrasound
Wave liquidometer (6), liquid feeding pump (12), liquid inlet electromagnetic valve door (14), circulating pump (19), circulating electromagnetic valve door (20) connection.
3. microwave heating acid purification devices according to claim 1, which is characterized in that the vent gas treatment bucket (10) is equipped with alkali
Liquid.
4. microwave heating acid purification devices according to claim 1, which is characterized in that escape pipe (5) setting is condensing
The part of case (7) is spiral cooling tube (8), and cooling cylinder (7) is equipped with refrigerant outlet and condensing agent entrance.
5. microwave heating acid purification devices according to claim 1, which is characterized in that the escape pipe (5) passes through cooling cylinder
(7) it is branched off into more than one pipeline after, valve is respectively provided on each pipeline and connects a liquid-collecting barrel, liquid-collecting barrel is and tail gas
Handle bucket (10) connection.
6. microwave heating acid purification devices according to claim 1, which is characterized in that the inner wall of the shell (16) is quartz
Inner wall.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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CN201821716897.8U CN209286685U (en) | 2018-10-23 | 2018-10-23 | A kind of microwave heating acid purification devices |
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CN201821716897.8U CN209286685U (en) | 2018-10-23 | 2018-10-23 | A kind of microwave heating acid purification devices |
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CN201821716897.8U Expired - Fee Related CN209286685U (en) | 2018-10-23 | 2018-10-23 | A kind of microwave heating acid purification devices |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115108814A (en) * | 2022-07-27 | 2022-09-27 | 广东长信精密设备有限公司 | Oxide ceramic powder purification system and method |
-
2018
- 2018-10-23 CN CN201821716897.8U patent/CN209286685U/en not_active Expired - Fee Related
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115108814A (en) * | 2022-07-27 | 2022-09-27 | 广东长信精密设备有限公司 | Oxide ceramic powder purification system and method |
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