CN105233897B - The built-in sour purifier of temperature sensor - Google Patents
The built-in sour purifier of temperature sensor Download PDFInfo
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- CN105233897B CN105233897B CN201510760564.XA CN201510760564A CN105233897B CN 105233897 B CN105233897 B CN 105233897B CN 201510760564 A CN201510760564 A CN 201510760564A CN 105233897 B CN105233897 B CN 105233897B
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Abstract
A kind of sour purifier, including：Sour container to be purified, for accommodating acid to be purified；Heater, for heating sour container to be purified, to obtain hot acid steam；Condenser, is configured to be condensed for hot acid steam；The purifying acid solution receiving flask being connected with condenser, for collecting condensed purifying acid；Controller, for controlling all parts to run to carry out sour purifying process；Acid liquor temperature sensor, is placed in the inside of acid to be purified, the temperature for measuring acid solution body to be purified；Wherein controller sets temperature threshold, receives the temperature of acid liquor temperature sensor measurement, the temperature is compared with temperature threshold, and correspondingly control heater.Sour purifier according to embodiments of the present invention, temperature sensor is placed in inside acid solution, and measured temperature is equal or substantially equal to the temperature of acid solution, it is ensured that the accuracy of temperature survey.
Description
Technical field
The present invention relates generally to acid solution purifying, more particularly to sour purifier apparatus.
Background technology
Trace, the ultra trace analysis in laboratory will often use ultrapure acid, it is therefore desirable to the acid of ordinary purity is boiled in Asia
Slow evaporation out, and is condensed, is collected into purity acid higher under state.
Sour purifier typically has heating function, temperature control function, liquid level monitoring function and condensation function, so as to acid
Liquid is heated, temperature control, liquid level monitoring and condensed and collected.
Generally there are following several respects in obtainable sour purifier design on the market at present；
1st, temperature control：
(1) traditional solution to avoid temperature sensor from being corroded easily by high-temperature strong acid, pacify by its temperature sensor
Mounted in container exterior, it is to avoid contacted with strong acid, but such mounting means measurement be container outer wall temperature, it is impossible to 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.
(2) temperature controller of traditional solution is multi gear bit-type, rather than continuously adjustabe type, can only probably be set
A fixed temperature value, it is impossible to accurate setting.
2nd, Liquid level：
(1) for the liquid level of original acid solution, the mode that traditional solution uses range estimation liquid level tube judges liquid
Position.Once personnel forget range estimation in time, it will have dry combustion method great risk even on fire.
(2) for the liquid level of high-purity acid solution, existing solution does not have any automatic detection and control measure.Once liquid
Position overfill, acid solution will overflow bottle, corrode periphery object.
3rd, control condensation and computer heating control：
(1) existing solution uses air cooling or originally water cooling mode.Both modes are without temperature
Indicate cooling effect.
(2) both modes are easily influenceed by air themperature and tap water temperature condition, once temperature or water temperature rise, and it is cold
But effect will be impacted.
(3) the originally mode of water cooling, also because cut off the water and caused by the risk that cannot cool down.
(4) existing solution is used as thermal source using infrared lamp or resistance wire, is naked light, surrounding of easily igniting it is inflammable
Gas；
(5) once temperature controller fails, infrared lamp or resistance wire will continue to heat, and cause instrument to burn even laboratory
The great risk of fire.
The content of the invention
For the present situation of prior art, the present invention is made that.
According to an aspect of the invention, there is provided a kind of sour purifier, including：Sour container to be purified, treats for accommodating
Purifying acid；Heater, for heating sour container to be purified, to obtain hot acid steam；Condenser, is configured to enter for hot acid steam
Row condensation；The purifying acid solution receiving flask being connected with condenser, for collecting condensed purifying acid；Controller, it is each for controlling
Individual part runs to carry out sour purifying process；Acid liquor temperature sensor, is placed in the inside of acid to be purified, to be purified for measuring
The temperature of acid solution body；Wherein controller sets temperature threshold, receives the temperature of acid liquor temperature sensor measurement, by the temperature and temperature
Degree threshold value compares, and correspondingly controls heater.
In one example, the acid liquor temperature sensor is thermocouple type temperature sensor, two thermocouple wire quilts
It is placed in polytetrafluoroethylene PTFE capillary, PTFE capillary is placed in support tube, support tube is placed in sour container to be purified
Interior, the connecting hole on wall that PTFE capillary passes through sour container to be purified is extended to outside sour container to be purified.
In one example, the support tube lower end is connected with tube wrapping device, and the PTFE capillary in the support tube is passed through
Support pipe orifice out, and after being wound with one circuit on tube wrapping device and enters support tube through the hole of support tube, then along support tube
Upwardly extend, finally from the hole of support tube and pass through sour container to be purified wall on connecting hole extend to sour container to be purified
Outward, wherein thermocouple head is partially in one week that the PTFE capillary is wound, and thermocouple head part and PTFE capillarys
Pipe is contacted.
In one example, two thermocouple wires are to seeming a wire to making contact to, to contact portion into
It is thermocouple head.
In one example, the acid liquor temperature sensor is thermocouple type temperature sensor, the surface of thermocouple wire
Parcel PTFE integuments, the position of thermocouple probe causes that thermocouple probe is closely tied with PTFE integuments using hot-press method
Close.
In one example, there are one or more seal points on thermocouple wire, hot pressing side is used at seal point
Method causes thermocouple wire and PTFE integument brought closes.
In one example, the controller being capable of continuity ground setting temperature threshold.
In one example, the condenser includes Peltier peltier coolers, condenser bodies and refrigerant temperature
Sensor, in Peltier peltier coolers cooled " cold water ", by the pressure of water pump enter condenser bodies pair with it is cold
The acid vapor of condenser main body cover contact is cooled down, and " hot water " enters cold in Peltier peltier coolers by water pump again
But, go round and begin again, circulate work, the temperature of refrigerant in refrigerant temperature sensors measurement Peltier peltier coolers.
In one example, the condenser bodies bottom is barrier film of the thickness less than predetermined threshold, and barrier film steams with hot acid
Vapour is contacted, and hot acid steam is cooled down, and condensed purifying acid enters purifying acid solution receiving flask by drainage tube.
In one example, the middle part of condenser bodies is divided into two parts by a baffle plate, to guide water (flow) direction, makes interior
Portion's more uniform temperature.
In one example, the refrigerant temperature sensors use capillary type thermocouple；In peltier cooler and
On pipeline between condenser bodies, capillary type thermocouple injects pipeline, and insert port has been carried out encapsulation process.
In one example, sour purifier is placed in fume hood, but the peltier cooler and controller are placed
Outside fume hood.
In one example, sour purifier also includes：Non-contact type ultrasonic liquid level sensor, installed in the appearance of container
Face, and not with container surfaces contact, in automatic measurement sour container to be purified it is to be purified acid liquid level, and by measure
The signal of liquid level is indicated to be sent to controller, controller receives the signal of the instruction liquid level, when the signal of the instruction liquid level
During less than predetermined threshold, control signal is sent, to control to stop sour purifying process.
In one example, sour purifier also includes：Pressure sensor, the weight of acid solution receiving flask is purified for automatic sensing
Amount, and the signal of weight will be indicated to send controller to；And controller receives the signal of the instruction weight, when the instruction weight
Signal exceed predetermined threshold when, send control signal, to control to stop sour purifying process.
In one example, purifying acid solution receiving flask is positioned on pallet, and pallet is designed using flange, prevents acid solution from dripping to
Pressure sensor inside；And the pressure sensor design has leakage outlet, so as to there is acid solution to enter in sensor internal
In the case of, the leakage can be discharged.
In one example, pressure sensor has carried out PTFE surface sprayings.
In one example, heater is ptc heater.
In one example, controller includes the computer as host computer and the single-chip microcomputer as slave computer, all sensings
Data transfer between device and computer is carried out by communication.
Sour purifier according to embodiments of the present invention, temperature sensor is placed in inside acid solution, measured temperature be equal to or
The substantially equal to temperature of acid solution, it is ensured that the accuracy of temperature survey.
Brief description of the drawings
From detailed description below in conjunction with the accompanying drawings to the embodiment of the present invention, these and/or other side of the invention and
Advantage will become clearer and be easier to understand, wherein：
Fig. 1 shows the schematic perspective view of sour purifier according to embodiments of the present invention.
Fig. 2 shows the structural representation of sour purifier according to embodiments of the present invention.
Fig. 3 (a) and (b) respectively illustrate integrated form according to embodiments of the present invention acid solution position control unit 300 to be purified
Three-dimensional view and profile.
Fig. 4 (a) and (b) respectively illustrate thermocouple type temp sensor device 400 according to an embodiment of the invention
Stereogram and profile.
Fig. 5 shows the schematic perspective view of thermocouple type temperature sensor 500 according to embodiments of the present invention.
Fig. 6 shows the topology example of condenser bodies 600 according to embodiments of the present invention.
Fig. 7 (a) and (b) show the interim collection device 700 of pure acid according to embodiments of the present invention structural representation and
Profile.
Fig. 8 (a) and (b) show the stereogram of the structure of heater according to an embodiment of the invention 800 and face
Figure.
Fig. 9 (a) and (b) show the acid purifying for being configured with ultrasonic liquid level sensor 900 according to embodiments of the present invention
The stereogram and profile of device.
Figure 10 (a) shows pure acid solution receiving flask 4 and pressure sensor and relevant portion according to embodiments of the present invention
The schematic perspective view of relative position relation between 1000, Figure 10 (b) shows pressure sensor according to embodiments of the present invention and phase
Close the profile of part 1000.
Specific embodiment
In order that those skilled in the art more fully understand the present invention, with reference to the accompanying drawings and detailed description to this hair
It is bright to be described in further detail.
First illustratively, herein, term " original acid ", " acid to be purified ", " acid to be purified " represents same and contains
Justice, refers to the acid solution as the purifying sour purifier of object input, and these terms are used interchangeably.Term " purifying acid " and " pure acid "
Same implication is represented, is used interchangeably, refer to the acid solution through being obtained after sour purifier purification process.
Fig. 1 shows the schematic perspective view of sour purifier according to embodiments of the present invention.
Exemplary acids purifier shown in Fig. 1 includes that original acid (acid i.e. to be purified) relevant portion A is (including to be purified
Sour container, heater and condenser, behind will be explained in), purifying acid collect part B, base portion C and with it is to be purified acid hold
The integrated form control unit E in acid solution position to be purified of device connection.Original acid (acid i.e. to be purified) relevant portion A includes acid to be purified
Container, heater and condenser, behind will be explained in.
Fig. 2 shows the structural representation of sour purifier according to embodiments of the present invention.
Sour purifier includes that sour container to be purified 1, heater 2, condenser 3, purifying acid solution receiving flask 4, integrated form treat pure
Change acid solution position control unit (not shown in Fig. 2, the part that label E is indicated in Fig. 1), controller (not shown).
For accommodating acid to be purified, (sometimes referred to as it is original acid to sour container to be purified 1 herein, and both are interchangeable to make
With).Heater 2 heats sour container to be purified, to obtain hot acid steam.Condenser 3 is carried out for the hot acid steam that heating is obtained
Condensation.Purifying acid solution receiving flask 4 is connected with condenser, for collecting condensed purifying acid.Controller is used to control each portion
Part runs to carry out sour purifying process.
In one example, controller includes host computer and slave computer two parts, and host computer can be general-purpose computer such as platform
Formula machine, notebook computer, mobile terminal etc., wherein being provided with the software for being adapted for carrying out control；Slave computer is, for example, monolithic
Machine or Special Programmable Logic Controller etc., wherein each sensor in sour purifier can send signal to slave computer, it is the next
Coherent signal is sent to by host computer with wired or wireless mode after machine treatment, host computer is accordingly calculated, processed, judged
Command signal is sent to slave computer, slave computer is issued an order to all parts again, such as shutdown, startup, alarm, time set
Fixed, threshold value setting etc..But this mode is merely illustrative, can as needed be adjusted or change.
For ease of description, host computer is called " computer " sometimes below, and slave computer is called " single-chip microcomputer ".
In the illustrated example shown in fig. 2, inside sour container to be purified 1, temperature sensor 5 is placed with, the temperature sensor 5
The inside of acid to be purified is placed on, is contacted with acid solution, the temperature for measuring acid solution body to be purified, controller sets temperature threshold
Value, receives the temperature of acid liquor temperature sensor measurement, and the temperature of the measurement is compared with temperature threshold, and correspondingly control adds
Hot device.The implementation example of built-in temperature sensor will be described in detail below.
The overall workflow of the brief once sour purifier of the embodiment of the present invention below.
A) original acid solution is added from addition funnel, and observes liquid level change, to suitable liquid level.
B) software in host computer, setting heating-up temperature (not higher than boiling point) and time are opened, after clicking on " beginning " key, plus
Hot device begins to warm up.
C) temperature sensor constantly gathers the temperature signal of acid solution, and sends computer to, and software is according to setting value and reality
Whether value, automatic decision continues to heat or stop, so as to keep acid liquor temperature stabilization in setting value.
D) at a temperature of less than boiling point, slow evaporation, acid vapor is condensed original acid solution for condenser, and then is pure acid
Collecting frame is collected.The acid solution that these are collected into can enter receiving flask by drainage tube.
E) when the run time of setting is reached, program is automatically stopped, and whole process terminates.
F) in program operation process, original acid solution level controller constantly gathers the liquid level change of original acid solution, and transmits
To computer, when minimum set in advance is reached, can automatic terminator.
G) in program operation process, pure acid solution level controller constantly gathers the change of receiving flask weight, and sends electricity to
Brain, when peak set in advance is reached, can automatic terminator.
The follow-up structure and operation principle that all parts according to embodiments of the present invention will be described referring to the appended drawings.
First, embodiment 1：Integrated form acid solution position control unit to be purified
According to one embodiment of present invention, sour purifier is configured with integrated form acid solution position control unit to be purified.
Fig. 3 (a) and (b) respectively illustrate integrated form according to embodiments of the present invention acid solution position control unit 300 to be purified
The three-dimensional view and profile of (for example, can be used as the part E shown in Fig. 1).Integrated form acid solution position control unit 300 to be purified
It is configured to addition funnel 310, liquid level tube 320 and the integration of removal waste fluid valve 330, acid to be purified is entered by addition funnel 310
Inside sour container to be purified, the liquid level of liquid level tube 320 reflects the liquid level of sour container to be purified, and removal waste fluid valve 330 can when opening
Discharge waste liquid.
Lid 340 is covered on addition funnel 310, and fixed screw holes 350 and 360 are for use by screw by integrated form acid to be purified
Liquid level part 300 is fixed on sour container to be purified 1 as shown in Figure 2.
370 and 380 indicate respectively interface section and lower interface part, with sour container to be purified inside UNICOM.390 indicate
Removal waste fluid mouthful, when head removal waste fluid valve 330 is opened, the solution in sour container to be purified 1 is via lower interface part 380 from removal waste fluid
Mouth 390 is discharged.
The integrated form acid solution position control unit 300 to be purified of the present embodiment can be concentrated realizes that liquid feeding, discharge opeing and liquid level are supervised
Brake, specifically：
Liquid feeding：Lid 340 is opened, original acid solution is poured into addition funnel 310, liquid can be by the He of upper interface section 370
The two paths up and down of the UNICOM of lower interface part 380 enter sour purifier body interior.
Discharge opeing：90 ° of rotary rowed waist valve, waste liquid will be discharged from removal waste fluid mouthful 390.
Liquid level：By observing liquid level tube 320, current level situation can be estimated.
The integrated form of the present embodiment acid solution position control unit 300 to be purified liquid level tube, addition funnel, removal waste fluid valve are closed and
It is one, can have both observed liquid level change, can carrys out liquid feeding as funnel again, can be with removal waste fluid；Avoid traditional funnel, liquid
Position pipe and removal waste fluid valve scheme disconnected from each other add funnel before and after acid solution and need the trouble of installing/dismounting, are deposited so as to avoid funnel
Pollution during putting.
2nd, embodiment 2：Built-in temperature sensor device
As it was previously stated, in traditional sour purifier, to avoid temperature sensor from being corroded easily by high-temperature strong acid, temperature
Sensor is installed in container exterior, it is to avoid contacted with strong acid, but such mounting means measurement be container outer wall temperature
Degree, it is impossible to reflect the true temperature of acid solution, usual solution temperature will differ 5-20 DEG C, the measurement of temperature with the temperature of container outer wall
Error is very big；And in the prior art, typical temperature controller is multi gear bit-type, rather than continuously adjustabe type, can only be general
One temperature value of setting, it is impossible to carry out accurate temperature setting.
Embodiments in accordance with the present invention, there is provided a kind of built-in temperature sensor device, temperature sensor is directly placed
In acid solution.Controller sets temperature threshold, the temperature of acid liquor temperature sensor measurement is received, by the temperature and temperature threshold phase
Compare, and correspondingly control heater.
In one example, using thermocouple type temperature sensor and matching component.The temperature sensor dress of the embodiment
Needs are put to solve two problems：1st, thermocouple wire and thermocouple head can not be with acid solution directly contacts；2nd, thermocouple head is contacted
Medium temperature to be equal or substantially equal to the temperature of acid solution.
In one example, using capillary thermocouple call wire (for example, external diameter about 0.8mm), the thermocouple is penetrated interior
In the e.g., from about PTFE of 1mm (polytetrafluoroethylene (PTFE)) capillary of footpath, then PTFE capillary passes through support pipe orifice, and in tube wrapping device
On wind with one circuit after and enter support tube, then two PTFE capillaries purify the connecting hole on wall and extend bucket by acid again
Outward.
In one example, two thermocouple wires can be placed in polytetrafluoroethylene PTFE capillary, PTFE capillarys
Pipe is placed in support tube, and support tube is placed in sour container to be purified, the wall that PTFE capillary passes through sour container to be purified
On connecting hole extend to outside sour container to be purified.
In one example, the support tube lower end is connected with tube wrapping device, and the PTFE capillary in the support tube is passed through
Support pipe orifice out, and after being wound with one circuit on tube wrapping device and enters support tube through the hole of support tube, then along support tube
Upwardly extend, finally from the hole of support tube and pass through sour container to be purified wall on connecting hole extend to sour container to be purified
Outward, wherein thermocouple head is partially in one week that the PTFE capillary is wound, and thermocouple head part and PTFE capillarys
Pipe is contacted.
In one example, two thermocouple wires can be to seeming a wire to making contact to, to contact site
It is divided into thermocouple head.
Fig. 4 (a) and (b) respectively illustrate thermocouple type temp sensor device 400 according to an embodiment of the invention
Stereogram and profile.
Label 441 indicates, for example into the thermocouple leads line part of support tube 410, PTFE (polytetrafluoros to be cased with outside it
Ethene) capillary.PTFE material can tolerate 250 degree of high temperature and strong acid and strong base corrosion, and one layer of guarantor has been put on equivalent to thermocouple
Cuticula, serves etch-proof effect.Here PTFE material can be replaced by the material that other high temperature resistants and strong acid and strong base corrode.
Then thermocouple leads line is extended downwardly along support tube 410, close at tube wall 420 from support tube 410
Outlet (not shown) stretch out, after then being wound with one circuit on tube wrapping device 420 again enter through the entrance (not shown) on support tube 410
Enter support tube 410, then upwardly extended along support tube 410, finally stretched out from the upper outlet (not shown) of support tube 420, then
The part 442 stretched out from support tube 420 is stretched out outside sour purifier by the connecting hole on acid purifying wall.Thermocouple induction head
450 be located at the PTFE capillary is wrapped in it is interior around one the week of tube wall 420, be for example shown in around tube wall 420 just under
At side, contacted with acid solution.By the circular revolution mode of tube wrapping device, the PTFE capillary that direct doubling can be avoided to cause holds
Easily rupturable problem.
In order that the temperature for obtaining thermocouple induction head sensing is the temperature of acid solution, thermocouple wire and PTFE capillary are carried out
Diameter design so that thermocouple wire and PTFE capillary are in close contact, for example, between PTFE capillary and thermocouple wire
Diameter difference be less than 2mm, even more preferably less than preferably smaller than 1mm, 0.5mm.
Fig. 5 shows the schematic perspective view of thermocouple type temperature sensor 500 according to another embodiment of the present invention.
As shown in figure 5, PTFE integuments 520 in thermocouple wire (two) 510 outer wrappings.Thermocouple induction head is heat
530 medium temperatures of directly contact of thermocouple probe should be equal to or the substantially equal to temperature of acid solution, therefore, thermoelectricity should be caused
Even inductive head is in close contact PTFE integuments, PTFE integument directly contact acid solutions, it is believed that temperature of PTFE integuments etc.
In the temperature of acid solution.To ensure the close contact of this thermocouple induction head and PTFE integuments, in the example depicted in fig. 5,
The thermocouple induction head i.e. position of probe makes probe and PTFE wall perfect adaptations using hot-press method.Further, it is outer to prevent
Boundary's cold air enters and interferes, and multiple seal points 540 are devised on wire, is also adopted by hot-press method sealing.
Thermocouple leads line is such as capillary thermocouple call wire, and such as external diameter about 0.8mm, thermocouple gauge bread wraps up in wall thickness
The PTFE integuments of about such as 0.5mm.PTFE material can tolerate 250 degree of high temperature and strong acid and strong base corrosion, equivalent to thermocouple
Layer protecting film has been put on, etch-proof effect has been served.And probe positions are fully combined by hot-press method with thin-walled, survey
Temperature is more accurately, more rapidly.
3rd, embodiment 3：Condenser, peltier cooler, the interim collection device of pure acid and heater
As it was previously stated, traditional sour purifier uses air cooling or originally water cooling mode.Both modes do not have
There is temperature to indicate cooling effect；And both modes are easily influenceed by air themperature and tap water temperature condition, once temperature
Or water temperature rises, cooling effect will be impacted；The mode of originally water cooling in addition, also because cut off the water and caused by the wind that cannot cool down
Danger.
Condenser according to embodiments of the present invention includes Peltier peltier coolers, condenser bodies, refrigerant temperature
In sensor, wherein Peltier peltier coolers cooled " cold water ", condenser bodies pair are entered by the pressure of water pump
The acid vapor contacted with condenser bodies shell is cooled down, and " hot water " enters Peltier peltier coolers by water pump again
Middle cooling, goes round and begins again, and circulates work,
The temperature of refrigerant in refrigerant temperature sensors measurement Peltier peltier coolers.
Fig. 6 shows the topology example of condenser bodies 600 according to embodiments of the present invention.
Condenser bodies 600 include cover part 610, intermediate 620, barrier film 630, baffle plate 640.
Sealed with sealing ring 650 between cover part 610 and intermediate 620.Cover part 610 is, for example, PVDF materials,
Sealing ring 650 is, for example, silica gel sealing ring.Label 660 indicates the screw hole for fixing lid, label 670 to indicate cooling water to enter
Mouthful.
Barrier film 630 of the bottom of the condenser bodies 600 for thickness less than predetermined threshold, barrier film and hot acid steam (by
Heater 2 for example shown in Fig. 1 heats acid solution to be purified and obtains) contact, hot acid steam is cooled down, condensed purifying
Acid enters purifying acid solution receiving flask (such as the label 3 shown in Fig. 1 is indicated) by drainage tube.
640 points by baffle plate of condenser bodies middle part is two parts, to guide water (flow) direction, makes internal temperature evenly.
On pipeline between Peltier peltier coolers (not shown in Fig. 6) and condenser bodies 600, refrigerant
Temperature sensor (not shown in Fig. 6) --- such as capillary type thermocouple --- is inserted into pipeline, and insert port is carried out
Encapsulation process, it is ensured that do not have refrigerant and ooze out.What such design can ensure thermocouple detection is the actual temperature of refrigerant
Degree, rather than pipeline outside wall temperature.Capillary type thermoelectricity dual diameter e.g., from about 1.0mm, is easy to bending.
Worked under highly corrosive environments for a long time for sour purifier, Peltier peltier coolers are easy to by acid gas
The problem of corrosion, in one example, peltier cooler is placed on outside fume hood and (is noted, the main body of sour purifier is usual
It is placed in fume hood), thus avoid the contact with acid gas.In one example, condenser bodies (also referred to as exchange heat
Device) use PTFE materials, by the cooled refrigerant of semiconductor cooler and acid vapor condenser bodies bottom diaphragm 630
Both sides carry out heat exchange, and the refrigerant after exchange is pumped into cooler and cools down again, and this process is carried out again and again.
Pure acid solution body after being condensed by the condenser typically is collected and then is drained into receiving flask by of short duration.
Fig. 7 (a) and (b) show the interim collection device 700 of pure acid according to embodiments of the present invention structural representation and
Profile.
Acid vapor rises to condensation by the rising mouthful 710 on the interim collection device (or referred to as receiving flask) 700 of pure acid
It is cooled after the barrier film of device main body, condensed pure acid solution body is from barrier film is along the bucket wall backflow of collector or directly drips
Onto catch tray 720.The upper surface of catch tray 720 is designed to obliquely so that pure acid solution body collects under gravity
In draining hole 730, receiving flask is entered by drainage tube.
Heater for heating acid to be purified according to embodiments of the present invention is described below.
As it was previously stated, the sour purifier of prior art is used as thermal source using infrared lamp or resistance wire, and it is naked light, easily ignite
The inflammable gas of surrounding；Once temperature controller fails, infrared lamp or resistance wire will continue to heat, and cause instrument to burn very
To the great risk of laboratory fire.
Sour purifier according to an embodiment of the invention uses ptc heater, due to PTC (Positive
Temperature Coefficient), i.e. positive temperature coefficient effect, electric current is raised by causing temperature after element, i.e. heater
Temperature rise, when more than certain temperature (Curie temperature), its resistance value is almost in rank with the rising of temperature
Jump formula increases, so as to limit electric current increase, the then decline of electric current causes the component temperature to reduce.And the reduction of temperature can make
The reduction of resistance value, so that circuital current increases, component temperature is raised.Go round and begin again, keep the temperature at particular range.PTC
Heater adstante febre is not rubescent, and the flames of anger is nonflammable.Even if temperature controller fails, ptc heater also will not continue to heating
More than Curie temperature, danger of combustion will not be produced.
According to the preferred embodiment of the present invention, worked under highly corrosive environments for a long time for sour purifier, ptc heater is very
Any one of easily by the problem of acid gas corrosion, special design has been carried out to heater, including following, but these are not limited to,
Other designs can be carried out：
(1) ptc heater itself has done PTFE surface sprayings, is effective against acid solution acid gas corrosion；
(2) main body and base of sour purifier connect design using nested type, and a sky for closing is formed therebetween
Between, whole ptc heater is arranged on the space of this closing so that whole ptc heater is wrapped up by main body and base, is prevented
With the contact of extraneous acid gas；
(3) furthermore, it is contemplated that the uniformity of heating, specially devises area much larger than ptc heater heating surface, thickness
Relatively thin such as thickness is the heat conducting disk of 3mm, and this heat conducting disk is brought into close contact with the bottom of acid purified bulk, carries out heat conduction, can be with
Be effectively improved because ptc heater can not fit completely sour purifier main body whole bottom caused by conduct heat inequality problem.
Heat conducting disk can be the extraordinary fine aluminium material of heat conductivility, and can also carry out PTFE surface sprayings.
Fig. 8 (a) and (b) show the stereogram of the structure of heater according to an embodiment of the invention 800 and face
Figure.
As shown in Fig. 8 (a) and (b), heater 800 includes ptc heater main body 810 and heat conducting disk 820.Heat conducting disk 820
Area of the area much larger than ptc heater main body 810, it is preferable that the former is equal to or more than 1.5 times of the latter, heat conducting disk
820 area can be designed according to the bottom area of sour purifier main body, and for example the two area is suitable；Other heat conducting disk 820
The top surface of bottom surface and ptc heater main body 810 is brought into close contact, and carries out heat conduction, can be effectively improved because ptc heater can not
The problem of inequality of being conducted heat caused by the whole bottom of sour purifier main body of fitting completely.
4th, embodiment 4：Sour contactless liquid level sensor to be purified
As it was previously stated, in the sour purifier of prior art, there is no liquid level sensor, it is contemplated that sour purifier is long-term in high temperature
(in the case of higher than 100 DEG C) work, if liquid level sensor is close to container outer wall installation, can easily cause and be close to container
The liquid level sensor of outer wall overheats and fails or damage.According to one embodiment of present invention, the original acid solution position of sour purifier
Sensor uses non-contact type ultrasonic liquid level sensor, and the change of automatic sensing liquid level once liquid level is less than arranges value, that is, sends
To software, software is automatic shutdown to voltage signal, it is to avoid personnel's carelessness and major fire hazard；And implemented according to the present invention
The special liquid level sensor of example, its measurement surface is not directly contacted with container outer wall, keeps the space of certain, such as 2mm,
The Rapid Accumulation that avoids heat and the problem that easily fails or damage, turn avoid measurement surface and solution away from too far away and lose
Lose due sensitivity problem.
Fig. 9 (a) and (b) show the acid purifying for being configured with ultrasonic liquid level sensor 900 according to embodiments of the present invention
The stereogram and profile of device.
As shown in Fig. 9 (b), ultrasonic liquid level sensor 900 according in the outer surface of sour container to be purified 1, and with treat pure
Exist between the wall of change sour container 1 apart from d, d is more than zero.Label 7 indicates the shell of sour purifier.
Sour purifier according to embodiments of the present invention uses contactless specially designed ultrasonic wave infrared level sensors,
Installed in the outer surface of container, and not with container surfaces contact, both avoided sensor with asking that acid solution directly contact is corroded
Topic, turn avoid sensor and high temperature container directly contact and problem that the circuit that causes is damaged.
Pressure sensor for sensing pure acid solution position indirectly according to embodiments of the present invention is described below in conjunction with the accompanying drawings.
Figure 10 (a) shows pure acid solution receiving flask 4 and pressure sensor and relevant portion according to embodiments of the present invention
The schematic perspective view of relative position relation between 1000, Figure 10 (b) shows pressure sensor according to embodiments of the present invention and phase
Close the profile of part 1000.
According to one embodiment of the invention, pressure sensor uses weight resistance strain type pressure sensor, compression weight
Sensor constantly gathers the change of the pressure that receiving flask weight causes, and sends computer to, when reaching peak set in advance
When, can automatically terminate sour purifying procedure, it is to avoid personnel's carelessness and great chemical attack hidden danger.
In one example, in 4 times placement trays of receiving flask 1020, preferably receiving flask pallet 1020 is set using flange
Meter, can accommodate the acid solution of the water clock of 20mL or so, it is to avoid these acid solution sinuous flows, prevent acid solution from dripping to sensor internal.At one
In example, sensor 1010 devises leakage outlet 1030 at such as its support, so that just in case sensor internal has acid solution
Into can discharge in time.
The pressure sensor 1010 and/or other parts, such as pallet, sensor fixed screw holes 1040, data wire
Hole 1050 can carry out PTFE surface sprayings or itself is made using PTFE materials, being capable of anti-acid liquid corrosion.
According to one embodiment of present invention, the instruction that the data and computer software of all the sensors collection send
Transmitted by bluetooth or wifi modes, controller (host computer and slave computer) can be placed on outside fume hood, saved fume hood empty
Between, user of service is also remote controlled.
It is described above various embodiments of the present invention, described above is exemplary, and non-exclusive, and
It is not limited to disclosed each embodiment.In the case of without departing from the scope and spirit of illustrated each embodiment, for this skill
Many modifications and changes will be apparent from for the those of ordinary skill in art field.Therefore, protection scope of the present invention should
Should be defined by scope of the claims.
Claims (13)
1. a kind of sour purifier, including：
Sour container to be purified, for accommodating acid to be purified；
Heater, for heating sour container to be purified, to obtain hot acid steam；
Condenser, is configured to be condensed for hot acid steam；
The purifying acid solution receiving flask being connected with condenser, for collecting condensed purifying acid；
Controller, for controlling all parts to run to carry out sour purifying process,
Acid liquor temperature sensor, is placed in the inside of acid to be purified, the temperature for measuring acid solution body to be purified；
Wherein controller sets temperature threshold, the temperature of acid liquor temperature sensor measurement is received, by the temperature and temperature threshold phase
Compare, and correspondingly control heater,
The acid liquor temperature sensor is thermocouple type temperature sensor, and two thermocouple wires are placed in polytetrafluoroethylene PTFE
In capillary, PTFE capillary is placed in support tube, and support tube is placed in sour container to be purified, and PTFE capillary is by treating
The connecting hole purified on the wall of sour container is extended to outside sour container to be purified,
The support tube lower end is connected with tube wrapping device, and the PTFE capillary in the support tube passes through support pipe orifice out, and
Enter support tube through the hole of support tube again after being wound with one circuit on tube wrapping device, upwardly extended then along support tube, finally from branch
Connecting hole on the hole of stay tube and the wall for passing through sour container to be purified is extended to outside sour container to be purified,
Wherein thermocouple head is partially in one week that the PTFE capillary is wound, and thermocouple head part and PTFE capillarys
Pipe is contacted,
Two thermocouple wires to seeming a wire to making contact to, to turning into thermocouple head, thermocouple to contact portion
The surface parcel PTFE integuments of wire, the position of thermocouple probe causes that thermocouple probe is wrapped up with PTFE using hot-press method
Layer is combined closely,
On thermocouple wire exist one or more seal points, at seal point using hot-press method cause thermocouple wire with
PTFE integument brought closes.
2. sour purifier according to claim 1,
The controller being capable of continuity ground setting temperature threshold.
3. sour purifier according to claim 1,
The condenser includes Peltier peltier coolers, condenser bodies and refrigerant temperature sensors,
In Peltier peltier coolers cooled " cold water ", condenser bodies pair are entered with condensation by the pressure of water pump
The acid vapor of device main body cover contact is cooled down, and " hot water " enters cooling in Peltier peltier coolers by water pump again,
Go round and begin again, circulate work,
The temperature of refrigerant in refrigerant temperature sensors measurement Peltier peltier coolers.
4. sour purifier according to claim 3,
The condenser bodies bottom is barrier film of the thickness less than predetermined threshold, and barrier film is contacted with hot acid steam, to hot acid steam
Cooled down, condensed purifying acid enters purifying acid solution receiving flask by drainage tube.
5. sour purifier according to claim 3,
The middle part of condenser bodies is divided into two parts by a baffle plate, to guide water (flow) direction, makes internal temperature evenly.
6. sour purifier according to claim 3, the refrigerant temperature sensors use capillary type thermocouple；
On pipeline between peltier cooler and condenser bodies, capillary type thermocouple injects pipeline, and insert port
Encapsulation process is carried out.
7. sour purifier according to claim 3, sour purifier is placed in fume hood, but by the peltier cooler and control
Device processed is placed on outside fume hood.
8. sour purifier according to claim 1, also includes：
Non-contact type ultrasonic liquid level sensor, installed in the outer surface of container, and not with container surfaces contact, for automatic survey
The liquid level of the acid to be purified in sour container to be purified is measured, and the signal of the instruction liquid level for measuring is sent to controller,
Controller receives the signal of the instruction liquid level, when the signal of the instruction liquid level is less than predetermined threshold, sends control signal,
To control to stop sour purifying process.
9. sour purifier according to claim 1, also includes：
Pressure sensor, the weight of acid solution receiving flask is purified for automatic sensing, and the signal of weight will be indicated to send control to
Device；And
Controller receives the signal of the instruction weight, when the signal of the instruction weight exceedes predetermined threshold, sends control signal,
To control to stop sour purifying process.
10. sour purifier according to claim 9,
Purifying acid solution receiving flask is positioned on pallet, and pallet is designed using flange, prevents acid solution from dripping to pressure sensor inside；With
And
The pressure sensor design has leakage outlet, in the case of thering is acid solution to enter in sensor internal, Neng Goupai
Go out the leakage.
11. sour purifiers according to claim 9, the pressure sensor has carried out PTFE surface sprayings.
12. sour purifiers according to claim 1, the heater is ptc heater.
13. according to the sour purifier of any one of claim 1 to 9,
Controller includes the computer as host computer and the single-chip microcomputer as slave computer,
Data transfer between all the sensors and computer is carried out by communication.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510760564.XA CN105233897B (en) | 2015-11-10 | 2015-11-10 | The built-in sour purifier of temperature sensor |
| US15/764,433 US10220329B2 (en) | 2015-11-10 | 2016-01-26 | Acid purifier |
| PCT/CN2016/072207 WO2017080113A1 (en) | 2015-11-10 | 2016-01-26 | Acid purifier |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510760564.XA CN105233897B (en) | 2015-11-10 | 2015-11-10 | The built-in sour purifier of temperature sensor |
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| CN105233897A CN105233897A (en) | 2016-01-13 |
| CN105233897B true CN105233897B (en) | 2017-06-20 |
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| DE20019875U1 (en) * | 2000-11-23 | 2001-03-22 | Fischer Margot | Apparatus for micro and semi-micro distillation |
| CN101428243A (en) * | 2007-11-09 | 2009-05-13 | 上海屹尧仪器科技发展有限公司 | Semiconductor refrigeration acid distillation purifier and purification process thereof |
| CN201625542U (en) * | 2010-01-08 | 2010-11-10 | 湖北省疾病预防控制中心 | Acid purifying distiller |
| CN202263412U (en) * | 2011-09-21 | 2012-06-06 | 中国地质大学（武汉） | Automatic high-purity acid condensation and purification control device |
| CN103979497B (en) * | 2014-05-16 | 2016-04-20 | 西陇科学股份有限公司 | A kind of method preparing high-purity hydrochloric acid |
| CN205084757U (en) * | 2015-11-10 | 2016-03-16 | 郝东辉 | Built -in sour purifier of temperature sensor |
| CN105251548A (en) * | 2015-11-10 | 2016-01-20 | 郝东辉 | Acid purifier |
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