CN104062201B - Measure the experimental provision of vacuum drying and vacuum lyophilization process parameter - Google Patents
Measure the experimental provision of vacuum drying and vacuum lyophilization process parameter Download PDFInfo
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- CN104062201B CN104062201B CN201410300777.XA CN201410300777A CN104062201B CN 104062201 B CN104062201 B CN 104062201B CN 201410300777 A CN201410300777 A CN 201410300777A CN 104062201 B CN104062201 B CN 104062201B
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Abstract
A kind of experimental provision measuring vacuum drying and vacuum lyophilization process parameter, belongs to experimental observation Instrument technology field, relates to a kind of experimental provision measuring vacuum drying and vacuum lyophilization process parameter.This invention removes and affect quality of material and thermometric factor, it is achieved measure during the high-precision real of various process of vacuum drying technological parameters.The present invention includes vacuum drying oven, mass measurement mechanism, refrigeration heating arrangements, temperature survey mechanism, material sampler structure, bleed desiccant body, refrigeration machine and computer control and record system, mass measurement mechanism is made up of link and electronic scale, refrigeration heating arrangements is by pillar, fixed tray and on, in, lower floor's temperature control plate composition, temperature survey mechanism is by suspending pallet in midair, temperature probe, signal adapter and temperature data emitter composition, material sampler structure is by shift fork, transfer tray, driven rod, gate valve and sampling cabinet composition, desiccant body of bleeding is made up of vacuum pump and cold-trap.
Description
Technical field
The invention belongs to experimental observation Instrument technology field, relate to a kind of measurement and be vacuum dried and vacuum lyophilization process
The experimental provision of parameter.
Background technology
It is dried to refer to from wet stock, removes moisture or the various operations of other hygroscopic waters, be to be widely used in society's all trades and professions
One of unit operation process.For optimizing technique, improving efficiency, time-consuming, the demand of reduction energy consumption, research
Personnel have had been extricated from simple dependence practical experience and have worked out drying technology process and the traditional habit of technological parameter, start to close more
Note is dried inherent heat and mass transfer process and the mechanism of material.Along with the further investigation to dry technology, to dry run mechanism
Analyze and the monitoring of dry run technological parameter seem more and more important, wherein in dry run the quality of material of real-time change,
Temperature of charge and material sample image are the dry run process datas that research worker is paid close attention to the most, these data measure skill in real time
Art, method and apparatus, further investigation and development for dry technology have important supporting role.
But, existing drying experiment test device and experimental test procedures, still can not high-acruracy survey the studies above personnel simultaneously
The dry run process data paid close attention to the most.As a example by the measurement of quality of material, current existing most experimental provisions are all
Material and bearing tray thereof being directly placed on electronic scale and complete drying experiment, the most not only electronic scale disturbs drying experiment
Normal heat and mass transfer process, and the vibration of plant equipment and dry diabatic process can make electronic scale mass measurement error occur.
Most commonly seen inevitable mass measurement error again comes from temperature of charge and measures process, and the temperature element assigned on material draws
Outlet can bring uncertain active force because of internal stress to electronic scale, thus the high accuracy limiting quality of material change is surveyed
Amount.And for needing the vacuum drying that completes under vacuum and vacuum lyophilization experiment, again material extracting directly and
Bring difficulty between persistently the carrying out of dry run, it is common practice to vacuum drying oven is also exitted by interrupt experiments, by material from
Vacuum drying oven takes out, and weighs or the intermediate detection such as sample image observation, the most again material is put back to vacuum drying oven, again
Evacuation proceeds drying experiment.It is obvious that this way destroys vacuum drying seriality, the data deficiency obtained
Enough precision reliabilities, and complex operation, it is impossible to adapt to the current demand to dry run Precision measurement.In a word, the most still
Do not have a kind of experimental provision can carry out the high precision online measuring of multinomial Drying Technology Parameter simultaneously.Therefore, it is developed to more
For the experimental provision of on-line measurement dry run technological parameter that is accurate, reliable and that be suitable under different condition, for dry technology
Further investigation has the highest practical value.
Summary of the invention
The problem existed for prior art, the present invention provides a kind of and measures vacuum drying and vacuum lyophilization process parameter
Experimental provision, compared with existing drying experiment equipment, the present invention will eliminate from root mechanical vibration, temperature element lead-in wire
Etc. factor on quality of material and thermometric impact, it is achieved measure during the high-precision real of various process of vacuum drying technological parameters,
Thus the further investigation for dry technology provides strong experimental tool and means.
To achieve these goals, the present invention adopts the following technical scheme that a kind of measurement is vacuum dried and vacuum lyophilization process
The experimental provision of technological parameter, including vacuum drying oven, mass measurement mechanism, refrigeration heating arrangements, temperature survey mechanism, thing
Material sampling mechanism, desiccant body of bleeding, refrigeration machine and computer control and record system, and described mass measurement mechanism is by link
Forming with electronic scale, electronic scale is arranged in vacuum drying oven by link；Described refrigeration heating arrangements is by pillar, fixing torr
Dish and upper, middle and lower layer temperature control plate composition, upper, middle and lower layer temperature control plate is arranged in vacuum drying oven by pillar, fixing torr
Dish is fixed between middle level temperature control plate and lower floor's temperature control plate, and fixed tray is loaded with the first material；Described temperature survey mechanism is by hanging
Hanging pallet, temperature probe, signal adapter and temperature data emitter composition, suspention pallet is positioned at upper strata temperature control plate and middle level temperature
Between control plate, suspention pallet is connected with the hook of weighing of electronic scale, and suspention pallet is loaded with the second material, and temperature probe is arranged
At the second material；Described material sampler structure is made up of shift fork, transfer tray, driven rod, gate valve and sampling cabinet, and shift fork sets
Putting on vacuum drying oven, sampling cabinet is connected with vacuum drying oven, is provided with gate valve between sampling cabinet and vacuum drying oven,
Transfer tray is arranged in sampling cabinet, and transfer tray is connected with driven rod；Described desiccant body of bleeding is by vacuum pump and cold-trap group
Becoming, the air inlet of cold-trap is connected with vacuum drying oven, and the gas outlet of cold-trap is connected with vacuum pump, vacuum pump and sampling cabinet phase
Connection, described refrigeration machine is connected with the condenser coil in cold-trap；Described computer controls and record system is by computer, control
Device and temperature data receptor composition, temperature probe is connected with temperature data emitter by signal adapter, and temperature data is launched
Device matches with temperature data receptor, and temperature data receptor, electronic scale are connected with computer by controller respectively.
Described vacuum drying oven is provided with drying baker vacuometer and drying baker vent valve；Described sampling cabinet is provided with sampling
Case vacuometer and sampling cabinet vent valve.
Described sampling cabinet connects pipeline by sampling and is connected with vacuum drying oven, and described gate valve is arranged on sampling and connects on pipeline,
The through hole that described transfer tray connects pipeline with sampling is corresponding.
Described link is arranged on the top board of vacuum drying oven, is connected by damping spring between the base of electronic scale and link
Connect.
Described suspention pallet is connected with the hook of weighing of electronic scale by suspention plate, by suspention between suspention pallet and suspention plate
Silk is connected, and signal adapter and temperature data emitter are fixed on suspention plate.
Dry chamber door and sampling chamber door it is respectively arranged with in the front portion of described vacuum drying oven and sampling cabinet.
The spacing between spacing and middle level temperature control plate and lower floor's temperature control plate between described upper strata temperature control plate and middle level temperature control plate is identical.
The bottom of described pillar is arranged on the base plate of vacuum drying oven by fixed plate；Fixed plate is fixed with several pallets
Location bar, the top of several pallets location bar is fixing with the bottom of fixed tray to be connected.
It is provided with refrigerant coil and armouring electrical heating in the inside of described upper strata temperature control plate, middle level temperature control plate and lower floor's temperature control plate
Silk, refrigeration machine refrigerant coil with upper strata temperature control plate, middle level temperature control plate and lower floor's temperature control plate respectively is connected.
Beneficial effects of the present invention:
1, the temperature data emitter of the present invention, temperature data receptor use wireless technology, have been inherently eliminated due to temperature
The probe mass measurement error that brought of lead-out wire internal stress, thus improve the Surveying Actual Precision of electronic scale, makes measurement the
The minor variations of two quality of material is it is achieved that each item data obtained by Tong Shi has certain seriality；
2, owing to present invention employs pendulum spring, thus fully completely cut off the produced vibration of vacuum drying oven external equipment, protected
Protect electronic scale not affected by mechanical vibration, improve certainty of measurement, reduce measurement error；Accurately embody the quality of the second material
Change；
3, owing to present invention employs material sampler structure, it is possible to obtain the first material in the case of not interrupt experiments, it is achieved right
Comprehensive observation of experimentation；
4, owing to present invention employs temperature probe, it is achieved that measure the temperature of the internal certain point of the first material, for research material
Internal heat transfer situation is favourable；
5, drying condition can be changed with requirement of experiment due to the present invention, be not limited in single experiment model, many to obtain
Plant the data under drying condition, significant especially for vacuum drying and vacuum lyophilization experiment.
Accompanying drawing explanation
Fig. 1 is the structural representation of the experimental provision measuring vacuum drying and vacuum lyophilization process parameter of the present invention；
Fig. 2 is the circuit theory frame of the experimental provision measuring vacuum drying and vacuum lyophilization process parameter of the present invention
Figure；
In figure, 1 vacuum drying draw box mechanism, 11 vacuum drying ovens, 12 drying baker vacuometers, 13 drying baker vent valves,
14 are dried chamber door, 2 mass measurement mechanisms, 21 electronic scales, 22 electronic scale supporting plates, 23 damping springs, and 24 claim
Heavily link up with, 25 links, 3 refrigeration heating arrangements, 30 grooves, 31 upper strata temperature control plates, 32 middle level temperature control plates, 33
Lower floor's temperature control plate, 34 pillars, 35 fixed trays, 36 pallet location bars, 37 fixed plates, 38 flexible conduit,
39 first materials, 4 temperature survey mechanisms, 41 suspention plates, 42 suspention silks, 43 suspention pallets, 44 temperature probes,
45 signal adapters, 46 temperature data emitters, 47 second materials, 5 bleed desiccant body, 51 vacuum pumps, and 52
First pump-line, 53 first vacuum valves, 54 cold-traps, 55 the 3rd vacuum valves, 56 condenser coils, 57 second
Vacuum valve, 58 second pump-lines, 59 the 3rd pump-lines, 6 refrigeration mechanisms, 61 first refrigeration pipes, 62
One refrigeration valve, 63 second refrigeration valve, 64 second refrigeration pipes, 65 refrigeration machines, 7 material sampler structures, 71 shift forks,
72 transfer trays, 73 driven rods, 74 sampling cabinets, 75 gate valves, 76 samplings connect pipeline, 77 sampling cabinet vacuum
Meter, 78 sampling cabinet vent valves, 79 sampling chamber doors, 8 computers control and record system, 81 computers, 82 controls
Device processed (PLC), 83 temperature data receptors.
Detailed description of the invention
The present invention is described in further detail with specific embodiment below in conjunction with the accompanying drawings.
As shown in Figure 1 and Figure 2, a kind of experimental provision measuring vacuum drying and vacuum lyophilization process parameter, including
Vacuum drying mechanism 1, mass measurement mechanism 2, refrigeration heating arrangements 3, temperature survey mechanism 4, desiccant body 5 of bleeding, system
Cold structure 6, material sampler structure 7 and computer control and record system 8；Described vacuum drying draw box mechanism 1 is by cube shaped
Vacuum drying oven 11 and be arranged on the drying baker vacuometer 12 at top of vacuum drying oven 11 and drying baker vent valve 13 forms,
Described mass measurement mechanism 2 is arranged in vacuum drying oven 11, by link 25, damping spring 23, electronic scale supporting plate 22 and
The electronic scale 21 being arranged on electronic scale supporting plate 22 forms, and electronic scale supporting plate 22 is fixed on vacuum drying oven by link 25
On the top board of 11, link 25 is connected by bolt and damping spring 23 with electronic scale supporting plate 22, and damping spring 23 is set with
On the bolt at link 25 top, at the through hole that is provided centrally with of electronic scale supporting plate 22, the hook of weighing bottom electronic scale 21
The lower section of electronic scale supporting plate 22 it is arranged on through through hole；Described refrigeration heating arrangements 3 is by upper strata temperature control plate 31, middle level temperature control plate
32,33, four pillars 34 of lower floor's temperature control plate and fixed tray 35 form；Upper strata temperature control plate 31, middle level temperature control plate 32 and under
Layer temperature control plate 33 is rectangular flat, is all provided with in the inside of upper strata temperature control plate 31, middle level temperature control plate 32 and lower floor's temperature control plate 33
Being equipped with refrigerant coil and armouring electrical heating wire, four pillars 34 are arranged on the base plate of vacuum drying oven 11, upper strata temperature control plate
31, middle level temperature control plate 32 and lower floor's temperature control plate 33 are vertically sequentially fixed on pillar 34, and have spacing between three；
Fixed tray 35 is fixed between middle level temperature control plate 32 and lower floor's temperature control plate 33, is placed with the first material on fixed tray 35
39；Described temperature survey mechanism 4 by suspention plate 41, suspention pallet 43,46, four temperature probes 44 of temperature data emitter,
Four suspention silks 42 and self-powered signal adapter 45 form；At the hook that is provided centrally with of suspention plate 41, suspention plate
41 are connected with the hook 24 of weighing of electronic scale 21 by hook, and suspention silk 42 top is connected, on upper strata with suspention plate 41
Being provided with groove 30 on temperature control plate 31, suspention silk 42 bottom is connected with suspention pallet 43 through groove 30, suspends plate 41 in midair
Being connected by suspention silk 42 with suspention pallet 43, suspention pallet 43 is between upper strata temperature control plate 31 and middle level temperature control plate 32；
Suspention pallet 43 is placed with the second material 47, signal adapter 45 and temperature data emitter 46 be each attached to suspend plate in midair
On 41, temperature probe 44 is arranged at the second material 47；
Described material sampler structure 7 is by shift fork 71, transfer tray 72, sampling cabinet vent valve 78, sampling cabinet vacuometer 77, magnetic
Power driven rod 73, gate valve 75, sampling connection pipeline 76 and sampling cabinet 74 form；Shift fork 71 is arranged on vacuum by supporting seat
On drying baker 11, shift fork 71 can swing around supporting seat, and shift fork 71 is connected by the way of vacuum dynamic seal with supporting seat,
The inner of shift fork 71 is arranged on the top of fixed tray 35, is used for stirring the first material 39 on fixed tray 35, shift fork 71
Outer end be arranged on the outside of vacuum drying oven 11 through the sidewall of vacuum drying oven 11；Sampling cabinet 74 is taken by horizontally disposed
It is logical with the bottom connection of vacuum drying oven 11 that sample connects pipeline 76, and through hole and first material 39 of sampling connection pipeline 76 are relative
Should, connect in sampling and be provided with gate valve 75 on pipeline 76, sampling cabinet 74 is respectively arranged with sampling cabinet vent valve 78 and takes
Sample case vacuometer 77, is provided with through hole on the sidewall away from vacuum drying oven 11 of sampling cabinet 74, magnetic force driven rod 73
The inner through hole that passes is arranged in sampling cabinet 74, and the outer end of magnetic force driven rod 73 is arranged on outside sampling cabinet 74, magnetic force driven rod
The centrage of 73 is connected the centrage of pipeline 76 and arranges on the same line with sampling, and magnetic force driven rod 73 can along sampling even
The axis direction in adapter road 76 moves, and the lateral wall of magnetic force driven rod 73 and the inner side of sampling cabinet 74 through hole in moving process
Seal between wall and arrange, be fixed with transfer tray 72 in the inner of magnetic force driven rod 73；Transfer tray 72 is connected pipeline with sampling
The through hole of 76 is corresponding, and can enter into vacuum drying oven by sampling connection pipeline 76 under the drive of magnetic force driven rod 73
In 11；
Described desiccant body 5 of bleeding is true by vacuum pump the 51, first pump-line the 52, first vacuum valve 53, cold-trap 54, second
Empty valve the 57, second pump-line the 58, the 3rd pump-line 59 and the 3rd vacuum valve 55 form, and the air inlet of cold-trap 54 is with true
Empty drying baker 11 is connected by the 3rd pump-line 59, is provided with the 3rd vacuum valve 55 on the 3rd pump-line 59, cold
The gas outlet of trap 54 is connected by the first pump-line 52 with vacuum pump 51, is provided with first on the first pump-line 52
Vacuum valve 53, vacuum pump 51 is connected with the inside of sampling cabinet 74 by the second pump-line 58, at the second pump-line 58
On be provided with the second vacuum valve 57；Described refrigeration mechanism 6 by refrigeration machine the 65, first refrigeration pipe the 61, first refrigeration valve 62,
Second refrigeration valve the 63, second refrigeration pipe 64 forms, and the delivery outlet of refrigeration machine 65 is by the first refrigeration pipe 61 and cold-trap 54
Interior condenser coil 56 is connected, and is provided with the first refrigeration valve 62 on the first refrigeration pipe 61；The delivery outlet of refrigeration machine 65 leads to
Cross the second refrigeration pipe 64 to be connected with the inside of vacuum drying oven 11, the second refrigeration pipe 64 is provided with the second refrigeration valve
63, one end that the second refrigeration pipe 64 is connected with vacuum drying oven 11 respectively with upper strata temperature control plate 31, middle level temperature control plate 32
It is connected by flexible conduit 38 with the refrigerant coil of lower floor temperature control plate 33；Refrigeration mechanism 6 is respectively bled desiccant body 5
In cold-trap 54 and upper, middle and lower layer temperature control plate in refrigeration heating arrangements 3 low-temperature refrigerant is provided；Described computer control and
Record system 8 is made up of computer 81, controller (PLC) 82 and temperature data receptor 83；Temperature data receptor 83
Be arranged on the outside of vacuum drying oven 11, controller (PLC) 82 respectively with temperature data receptor 83, electronic scale 21, dry
Dry case vacuometer 12, sampling cabinet vacuometer 77 are connected by wire, and read measurement data；
The outfan of temperature probe 44 is connected by wire with the input of signal adapter 45, the outfan of signal adapter 45
Being connected by wire with temperature data emitter 46, the transmitting terminal of temperature data emitter 46 connects with temperature data receptor 83
Receiving end matches；Temperature data receptor 83, electronic scale 21, drying baker vacuometer 12 and the outfan of sampling cabinet vacuometer 77
Be connected by wire with the input of controller (PLC) 82, the outfan of controller (PLC) 82 respectively with vacuum pump 51,
First vacuum valve the 53, second vacuum valve the 57, the 3rd vacuum valve the 55, first refrigeration valve 62 and the second refrigeration valve 63 pass through wire
Being connected, controller (PLC) 82 is connected by wire with computer 81；The temperature of the second material 47 that temperature probe 44 will record
Degrees of data passes to signal adapter 45, and signal adapter 45 is sent out by temperature data after the temperature data received is done analog digital conversion
Emitter 46 sends, and passes to computer 81 through controller (PLC) 82 and keep a record, protect after being received by temperature data receptor 83
Deposit；Electronic scale 21 the qualitative data via controller (PLC) 82 of the second material 47 recorded is passed to computer 81 keep a record,
Preserve；Controller (PLC) 82 receives instruction from computer 81 and controls vacuum pump the 51, first vacuum valve the 53, second vacuum valve
57, the 3rd vacuum valve the 55, first refrigeration valve 62 and the second refrigeration valve 63 operation.
Dry chamber door 14 and sampling chamber door 79 it is respectively arranged with in the front portion of described vacuum drying oven 11 and sampling cabinet 74.
Between spacing and middle level temperature control plate 32 and lower floor's temperature control plate 33 between described upper strata temperature control plate 31 and middle level temperature control plate 32
Spacing identical, and spacing can be adjusted as required.
The bottom of described pillar 34 is arranged on the base plate of vacuum drying oven 11 by fixed plate 37；Fixed plate 37 is fixed
Having four pallet location bars 36, be provided with four through holes on lower floor's temperature control plate 33, the top of four pallet location bars 36 is respectively
It is connected through four through holes are fixing with the bottom of fixed tray 35.
Described drying baker vacuometer 12 and sampling cabinet vacuometer 77 all use model to be the resistance vacuum gauge of ZDZ-52T；Described temperature
Degrees of data emitter 46 uses the low-voltage wireless module that model is RF24L01；Described temperature data receptor 83 uses
There is the wireless receiver that model is PIC16F877A chip, there is voltage and feature low in energy consumption；Described computer 51 uses
Control and the notebook personal computer of logging software are installed；
The model of described controller (PLC) 52 is LR7055；It is IS-K15100 that described temperature probe 22 uses model
A pin multipoint mode thermoprobe simultaneously and rapidly；Described first, second, third vacuum valve all uses model to be the electronic of GID-40
Vacuum butterfly valve, the model of described cold-trap 7 is TLR6XI150QF, and the model of described refrigeration machine 8 is CS-208L, described vacuum
The rotary-vane vaccum pump 31 that pump 31 uses model to be 2X-4.
The use process of the present embodiment is described below in conjunction with the accompanying drawings:
As shown in Figure 1 and Figure 2, in the Preparatory work of experiment stage: open dry chamber door 14, temperature survey mechanism 4 is taken out, by second
Material 47 loads in suspention pallet 43, is inserted by temperature probe 44 at second material 47；Then temperature survey mechanism 4 is put
Enter in vacuum drying oven 11, make four suspention silks 42 be moved rearwards by along the groove 30 on upper strata temperature control plate 31, finally make to hang
What the link of boatswain chair 41 was enclosed within electronic scale weighs on hook 24, so that suspention pallet 43 and the second material 47 are positioned at upper strata
Between temperature control plate 31 and middle level temperature control plate 32；The first material 47 of equivalent is placed, in case sampling is observed in fixed tray 35
Use, connect temperature data receptor 83, electronic scale 21, temperature data emitter 46 and the power supply of signal adapter 45, make
They are in normal operating conditions, the rear dry chamber door 14 closing vacuum drying oven 11 of pallet 43 to be suspended；
Confirming that cold-trap 54 is internal to have cleaned totally, gate valve 75, the discharging valve of cold-trap 54 are closed, unlatching computer 81,
Controller (PLC) 82, drying baker vacuometer 12 and sampling cabinet vacuometer 77, make at control and the logging software of computer 51
In normal operating conditions；
Process of vacuum drying: computer 81 starts vacuum pump 51 by controller (PLC) 82, opens the first vacuum valve 53,
To cold-trap 54 evacuation, then open the 3rd vacuum valve 55, by cold-trap 54 to vacuum drying oven 11 evacuation, start refrigeration
Machine 65, opens the first refrigeration valve 62, provides cold-producing medium to the condenser coil 56 in cold-trap 54, makes the surface of condenser coil 56
Temperature reduces, thus collects the water vapour evaporating or distilling out from the first material 39 and the second material 47, makes the first material
39 and second material 47 be dehydrated.Made the temperature in cold-trap 54 reduce before to vacuum drying oven 11 evacuation, with avoid from
First material 39 and the second material 47 evaporate or the steam out that distils enters vacuum pump 51；
Then power for the armouring electrical heating wire in the layer temperature control plate of upper, middle and lower, when armouring electrical heating wire heating power, upper,
In, the temperature of lower floor's temperature control plate raise, first, second material is heated, heating process is always radiant heating pattern,
By regulation output power and time, first, second material is realized the heating operation that heating rate is controlled；
In experimentation, temperature probe 44 records the temperature signal data of the second material 47, then temperature signal data is passed
Passing signal adapter 45, the temperature signal data received is done after analog digital conversion by temperature data emitter by signal adapter 45
46 send, and pass to controller (PLC) 82 after being received by temperature data receptor 83；Read by drying baker vacuometer 12 simultaneously
Take the vacuum in vacuum drying oven 11, and vacuum signal data is passed to controller (PLC) 82；By electronic scale 21
Read the quality of the second material 47, and quality signal data are passed to controller (PLC) 82, last controller (PLC)
The temperature of acquisition, vacuum and quality signal data are all passed to computer 81 by 82 carries out real time record, storage.
Vacuum lyophilization process, i.e. carries out frozen cooling operation to first, second material during vacuum drying experiment,
Start refrigeration machine 65, computer 81 by controller (PLC) 82 open the second refrigeration valve 63 upwards, in, lower floor's temperature control plate
Low-temperature refrigerant is provided；During frozen cooling, upper, middle and lower layer temperature control plate and the first material 39 and the second material 47 it
Between be always radiation heat transfer mode.By cryogenic temperature and the flow of cold-producing medium of regulation refrigeration machine 65, to first, second thing
Material realizes the cooling operation of controllable-rate.
When needing to be sampled observing during vacuum drying and vacuum lyophilization, close sampling chamber door 79 and sampling cabinet is put
Air valve 78, computer 81 cuts out the first vacuum valve 53 by controller (PLC) 82, opens the second vacuum valve 38, by very
The empty pump 51 inside evacuation to sampling cabinet 74, opens sampling cabinet vacuometer 77, when the sampling cabinet vacuum of computer 81 display
When the vacuum that meter 77 records reaches predetermined value (identical with the predetermined value of drying baker vacuometer 12), open gate valve 75, promote
Magnetic force driven rod 73, connects pipeline 76 by transfer tray 72 through sampling and moves the side to fixed tray 35, stir shift fork
The first material 39 that need to take out is allocated on transfer tray 72 by 71, then pulls magnetic force driven rod 73 to be moved to by transfer tray 72
In sampling cabinet 74, closing gate valve the 75, second vacuum valve 38, open sampling cabinet vent valve 78, broken sky venting, open sampling cabinet
Room door 79, carries out microscopic section observation by the first feeding 39 sample taken out, and above operation can be according to repeating behaviour needed for experiment
Make.
After completing vacuum drying or vacuum lyophilization experiment and recording on computer 81, preserve complete experimental data, calculate
Machine 81 cuts out all vacuum valves and refrigeration valve, vacuum pump 51 by controller (PLC) 82, is then shut off refrigeration machine 65, meter
Calculation machine 81, controller (PLC) 82, drying baker vacuometer 12 and sampling cabinet vacuometer 77, open drying baker vent valve 15,
Broken sky venting；Open dry chamber door 14, break-off signal data sink 83, electronic scale 21, temperature data emitter 46 and
The power supply of signal adapter 45, removes temperature probe 44, takes out remaining first, second material, finally opens cold-trap 54
Discharging valve, defrosts to cold-trap 54, discharge water, dries operation.
Finally, according to user's needs, by computer 81 records, stores observation data (include time dependent temperature,
The clean mass figures of the second material 47 after vacuum and conversion) it is organized into file with the form of data form or curve chart, and preserve.
Claims (8)
1. the experimental provision measuring vacuum drying and vacuum lyophilization process parameter, it is characterised in that include that vacuum is done
Dry case, mass measurement mechanism, refrigeration heating arrangements, temperature survey mechanism, material sampler structure, desiccant body of bleeding, refrigeration
Machine and computer control and record system, and described mass measurement mechanism is made up of link and electronic scale, and electronic scale passes through link
Being arranged in vacuum drying oven, described link is arranged on the top board of vacuum drying oven, between base and the link of electronic scale
It is connected by damping spring；Described refrigeration heating arrangements is made up of pillar, fixed tray and upper, middle and lower layer temperature control plate, upper,
In, lower floor's temperature control plate be arranged in vacuum drying oven by pillar, fixed tray be fixed on middle level temperature control plate and lower floor's temperature control plate it
Between, fixed tray is loaded with the first material；Described temperature survey mechanism is by suspending pallet, temperature probe, signal adapter and temperature in midair
Degrees of data emitter forms, and suspention pallet is between upper strata temperature control plate and middle level temperature control plate, and suspention pallet is weighed with electronic scale
Hook is connected, and suspention pallet is loaded with the second material, and temperature probe is arranged at the second material, by upper, middle and lower layer temperature
First and second material is heated in control plate radiation or heat exchange realizes the heating to first and second material or refrigeration；Described material
Sampling mechanism is made up of shift fork, transfer tray, driven rod, gate valve and sampling cabinet, and shift fork is arranged on vacuum drying oven, sampling
Case is connected with vacuum drying oven, is provided with gate valve between sampling cabinet and vacuum drying oven, and transfer tray is arranged in sampling cabinet,
Transfer tray is connected with driven rod；Described desiccant body of bleeding is made up of vacuum pump and cold-trap, and the air inlet of cold-trap is done with vacuum
Dry case is connected, and the gas outlet of cold-trap is connected with vacuum pump, and vacuum pump is connected with sampling cabinet, in described refrigeration machine and cold-trap
Condenser coil be connected；Described computer controls and record system is made up of computer, controller and temperature data receptor,
Temperature probe is connected with temperature data emitter by signal adapter, and temperature data emitter matches with temperature data receptor,
Temperature data receptor, electronic scale are connected with computer by controller respectively.
The experimental provision measuring vacuum drying and vacuum lyophilization process parameter the most according to claim 1, it is special
Levy and be on described vacuum drying oven, be provided with drying baker vacuometer and drying baker vent valve；Described sampling cabinet is provided with and takes
Sample case vacuometer and sampling cabinet vent valve.
The experimental provision measuring vacuum drying and vacuum lyophilization process parameter the most according to claim 1, it is special
Levying and be that described sampling cabinet connects pipeline by sampling and is connected with vacuum drying oven, described gate valve is arranged on sampling and connects on pipeline,
The through hole that described transfer tray connects pipeline with sampling is corresponding.
The experimental provision measuring vacuum drying and vacuum lyophilization process parameter the most according to claim 1, it is special
Levy and be that described suspention pallet is connected with the hook of weighing of electronic scale by suspention plate, by outstanding between suspention pallet and suspention plate
Hang spring is connected, and signal adapter and temperature data emitter are fixed on suspention plate.
The experimental provision measuring vacuum drying and vacuum lyophilization process parameter the most according to claim 1, it is special
Levy and be to be respectively arranged with dry chamber door and sampling chamber door in the front portion of described vacuum drying oven and sampling cabinet.
The experimental provision measuring vacuum drying and vacuum lyophilization process parameter the most according to claim 1, it is special
Levy the spacing phase between the spacing and middle level temperature control plate and lower floor's temperature control plate being between described upper strata temperature control plate and middle level temperature control plate
With.
The experimental provision measuring vacuum drying and vacuum lyophilization process parameter the most according to claim 1, it is special
Levy and be that the bottom of described pillar is arranged on the base plate of vacuum drying oven by fixed plate；Fixed plate is fixed with several torr
Dish location bar, the top of several pallets location bar is fixing with the bottom of fixed tray to be connected.
The experimental provision measuring vacuum drying and vacuum lyophilization process parameter the most according to claim 1, it is special
Levy and be to be provided with refrigerant coil in the inside of described upper strata temperature control plate, middle level temperature control plate and lower floor's temperature control plate and armouring electricity adds
Heated filament, refrigeration machine refrigerant coil with upper strata temperature control plate, middle level temperature control plate and lower floor's temperature control plate respectively is connected.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410300777.XA CN104062201B (en) | 2014-06-27 | 2014-06-27 | Measure the experimental provision of vacuum drying and vacuum lyophilization process parameter |
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| CN201410300777.XA CN104062201B (en) | 2014-06-27 | 2014-06-27 | Measure the experimental provision of vacuum drying and vacuum lyophilization process parameter |
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| Publication Number | Publication Date |
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| CN104062201A CN104062201A (en) | 2014-09-24 |
| CN104062201B true CN104062201B (en) | 2016-08-24 |
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| CN104502130A (en) * | 2014-12-08 | 2015-04-08 | 浙江工业大学 | Energy efficiency measuring method for helical ribbon vacuum drier |
| WO2016191799A1 (en) * | 2015-06-04 | 2016-12-08 | Freeze Dry Industries Pty Ltd | Freeze drying improvements |
| CN105987856A (en) * | 2016-02-16 | 2016-10-05 | 安徽出入境检验检疫局检验检疫技术中心 | Vacuum drying moisture measurement device for down feather |
| CN106500762B (en) * | 2016-10-14 | 2018-10-19 | 合肥工业大学 | A kind of combined type intelligent vacuum drying dynamic experiment platform |
| CN107687990B (en) * | 2017-08-16 | 2020-08-11 | 武汉锐致科技有限公司 | Moisture transfer law survey device |
| CN115900831B (en) * | 2022-12-22 | 2024-01-19 | 滨州市宏诺新材料有限公司 | Environment-friendly detection equipment with freeze dryer |
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| DE3041820A1 (en) * | 1980-11-06 | 1982-07-22 | Willi 6453 Seligenstadt Fischer | METHOD AND DEVICE FOR DETERMINING THE WATER CONTENT IN FRESH CONCRETE |
| JPS5988643A (en) * | 1982-11-12 | 1984-05-22 | Sumio Ando | Apparatus for measuring water content of substance to be dried in vacuum dryer |
| SU1265537A1 (en) * | 1984-08-22 | 1986-10-23 | Казанский Химико-Технологический Институт Им.С.М.Кирова | Method for determining moisture content of specimen made,mainly,from foam rubber |
| SU1499185A1 (en) * | 1986-02-19 | 1989-08-07 | Казанский Научно-Исследовательский Технологический И Проектный Институт Химико-Фотографической Промышленности | Apparatus for measuring moisture content in film and sheet materials |
| JPH026727A (en) * | 1988-06-27 | 1990-01-10 | Japan Tobacco Inc | Drying balance estimation type moisture meter |
| JPH02151728A (en) * | 1988-12-05 | 1990-06-11 | Daido Kogyosho:Kk | Vacuum drying and weighing apparatus |
| SU1728720A1 (en) * | 1989-11-23 | 1992-04-23 | Казанский Химико-Технологический Институт Им.С.М.Кирова | Device for determining moisture content of sponge and fibrous materials |
| CN101201268A (en) * | 2007-09-28 | 2008-06-18 | 浙江大学 | Device for continuously measuring variation of freeze drying example weight |
| CN201233354Y (en) * | 2008-08-06 | 2009-05-06 | 上海中药制药技术有限公司 | Vacuum drying dynamics research experimental apparatus |
| CN101846439B (en) * | 2010-06-08 | 2011-11-09 | 农业部南京农业机械化研究所 | Microwave vacuum freeze-drying device |
| CN203424259U (en) * | 2013-07-18 | 2014-02-12 | 上海海洋大学 | Ice temperature vacuum drying experiment machine with additional cooler |
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