CN107271320A - A kind of thermogravimetric analyzer that can be achieved to be rapidly heated - Google Patents
A kind of thermogravimetric analyzer that can be achieved to be rapidly heated Download PDFInfo
- Publication number
- CN107271320A CN107271320A CN201710421248.9A CN201710421248A CN107271320A CN 107271320 A CN107271320 A CN 107271320A CN 201710421248 A CN201710421248 A CN 201710421248A CN 107271320 A CN107271320 A CN 107271320A
- Authority
- CN
- China
- Prior art keywords
- temperature
- heater
- furnace
- thermal insulation
- thermocouple
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The invention belongs to sample analysis instrument field, and a kind of thermogravimetric analyzer that can be achieved to be rapidly heated, including meausring apparatus, heating furnace, sample lowering or hoisting gear, protection lowering or hoisting gear and temperature control device are disclosed, the meausring apparatus includes pedestal platform and electronic balance；The heating furnace includes being provided with resistive heater, setting-out passage, reaction gas air inlet pipe and reactor off-gas escape pipe on stove seat and body of heater, the body of heater；The sample lowering or hoisting gear includes the first actuating unit, the first transmission device, lifting platform and suspension rod；The protection lowering or hoisting gear includes the second actuating unit, the second transmission device and thermal insulation protection set；The temperature control device is connected with the heating furnace, for controlling the temperature of the burner hearth.The thermal insulation protection set of the present invention protects hanging basket, can elimination reaction initial stage data exception fluctuation, improve measurement integrality, reliability and accuracy.
Description
Technical field
The invention belongs to sample analysis instrument field, more particularly, to a kind of thermogravimetric analysis that can be achieved to be rapidly heated
Instrument.
Background technology
Thermogravimetric analyzer refers to that at a temperature of certain procedures control the quality of accurate measurement and recorded matter is varied with temperature
A kind of analytical instrument, the changing rule of material mass in heat treatment process can be reflected in, be widely used in chemical industry, geology,
The fields such as biology, the energy, environment.The conventional application method of thermogravimetric analyzer is programmed temperature method (non isothermal method), that is, refers to sample
Temperature is gradually increasing according to program setting in burner hearth in course of reaction, it is therefore an objective to obtain material mass change and the relation of temperature,
Measure commonly used to carry out material composition analysis, material discriminating, thermal parameter and kinetic parameter etc..Recently, in some science
, it is necessary to simulate real industrial environment (such as coal dust enters boiler combustion, and lime stone enters calcined by rotary kiln) in research, probe into
The response characteristic of material at a constant temperature is, it is necessary to quickly make mass temperature reach assigned temperature, i.e. isothermal method.But, due to
Heating technique is limited, and the rate of heat addition of current routine business thermogravimetric analyzer is relatively low (being no more than 100 DEG C/min), material be intended to through
The longer heating-up time is gone through, in temperature-rise period, material may some or all of reaction, it is impossible to meet scientific research demand.
In the current thermogravimetric analyzer achievement in research on being rapidly heated, including a kind of (1) controllable thermobalance that is rapidly heated
Sample feeding burner hearth is realized and is rapidly heated by reacting furnace (CN2010101045919), the invention using lift, but lift
Caused vibration can produce influence to the accurate measurement of sample quality；(2) constant temperature Thermgravimetric Analysis Apparatus (CN201610364154),
The invention carries out constant temperature thermogravimetric analysis by running gear and temperature control device, wherein the problem of be sample in the wink being quickly put into
Between will start reaction but now balance is because setting-out vibration can not obtain accurately and reliably data, so actual measurement has larger
Error.
It has been investigated that, there is problems with the existing thermogravimetric technology of being rapidly heated：(1) using the existing heat that is rapidly heated
When carrying out isothermal method experiment again, sample, which is put into the vibration at heating furnace initial stage and the change of air-flow, can influence the stable reading of balance,
Produce larger systematic error.Sample needs quickly to be put into burner hearth, and the vibration of system is inevitable, and balance can not accurately be read
Number, data reliability is poor, it is impossible to reflect that incipient stage sample quality changes；(2) thermocouple is arranged at furnace wall, and inside burner hearth
Thermograde is larger, it is impossible to accurately reflect out the temperature at sample, causes temperature control accuracy poor.
The content of the invention
For the disadvantages described above or Improvement requirement of prior art, the invention provides a kind of thermogravimetric that can be achieved to be rapidly heated
Analyzer, its object is to be rapidly heated and overcome sample to be put into the excessive caused data precision of early stage fluctuation very to sample
Poor the problem of, while also causing easy to operate.
To achieve the above object, it is proposed, according to the invention, there is provided a kind of thermogravimetric analyzer that can be achieved to be rapidly heated, its feature
It is, including meausring apparatus, heating furnace, sample lowering or hoisting gear, protection lowering or hoisting gear and temperature control device, wherein,
The meausring apparatus includes being provided with balance room on pedestal platform and electronic balance, the pedestal platform, the electronics day
Prosposition is in the balance room；
The heating furnace is including stove seat and body of heater, body of heater described in the stove seat supports, pedestal platform described in the converter body support,
Resistive heater, setting-out passage, reaction gas air inlet pipe are provided with the formation of body of heater the enclosed space burner hearth, and the body of heater
With reactor off-gas escape pipe；
The sample lowering or hoisting gear includes the first actuating unit, the first transmission device, lifting platform and suspension rod, and described first moves
Force mechanisms are arranged on the pedestal platform and it is moved up and down by lifting platform described in the actuator drives, the lifting
Platform is located in the balance room and the lifting platform accepts the electronic balance, and the upper end of the suspension rod is suspended on the electronics day
Flat upper and its lower end hanging basket, the change of sample quality is obtained for undertaking sample and by electronic balance, described to hang
The burner hearth of the heating furnace is stretched into the lower end of bar；
The protection lowering or hoisting gear includes the second actuating unit, the second transmission device and thermal insulation protection set, and described second moves
Force mechanisms are arranged on stove seat above and it is moved up and down by thermal insulation protection set described in second actuator drives, institute
State thermal insulation protection set top and be provided with opening, the passage to pass in and out the thermal insulation protection set as hanging basket；
The temperature control device is connected with the heating furnace, for controlling the temperature of the burner hearth.
Preferably, the protection gas air inlet pipe connected with the balance room and the first middle gas transmission are provided with the pedestal platform
Be provided with the second middle gas distribution channel connected with the burner hearth on passage, the body of heater, the first middle gas distribution channel and
Second middle gas distribution channel connection.
Preferably, the thermal insulation protection set includes shell body and the thermal insulation layer being arranged on the shell body inwall.
Preferably, the temperature control device includes temperature sense adjusting means, and the temperature sense adjusting means includes furnace wall
Thermocouple and and Furnace Temperature Controller, the furnace wall the installation of TC on the inboard wall of furnace body, the Furnace Temperature Controller with it is described
Furnace wall thermocouple and resistive heater connection, for obtaining the temperature of burner hearth, and are based on obtaining from the furnace wall thermocouple
Fire box temperature control the size of current on the resistive heater, so as to control fire box temperature.
Preferably, the temperature control device also includes data analysis set-up, and the data analysis set-up includes host computer sum
According to transmission line, the host computer is connected with the electronic balance and temperature sense adjusting means respectively by data line.
Preferably, be also equipped with suspending thermocouple in midair on the suspension rod, the suspention thermocouple stretched into the hanging basket, with
Temperature in measurement hanging basket, the Furnace Temperature Controller is also connected with the suspention thermocouple, for obtaining the temperature of burner hearth,
And based on the size of current on the resistive heater is controlled from the fire box temperature that obtains of suspention thermocouple, so as to control
Fire box temperature.
Preferably, the stove seat includes base and the supporting table being arranged on base, and the supporting table supports the body of heater,
The top of the supporting table is provided with cooling bath, using the parking space covered as the thermal insulation protection.
Preferably, the body of heater includes furnace wall and is arranged on the cooling block on furnace wall top, and the bottom of the cooling block is set
There is cooling bath, using the parking space as the hanging basket.
In general, by the contemplated above technical scheme of the present invention compared with prior art, it can obtain down and show
Beneficial effect：
1) thermal insulation protection set of the invention protects hanging basket, when sample moves to burner hearth medium position from top to bottom,
Just start sample hanging basket to cover interior into thermal insulation protection and enter burner hearth medium position under thermal insulation protection set parcel, because thermal insulation protection
The heat-blocking action of set, sample heating is slower, will not immediately begin to reaction, after sample is being put into burner hearth complete stability, and second moves
Force mechanisms drive thermal insulation protection set to move down, and hanging basket is left thermal insulation protection set, and sample starts reaction and start recording data,
Can elimination reaction initial stage data exception fluctuation, improve measurement integrality, reliability and accuracy；
2) present invention is by setting furnace wall thermocouple and suspention thermocouple thermometric in varied situations, and utilizes the heat of switching two
It is connected to reach accurately feedback temperature control effect with Furnace Temperature Controller under galvanic couple different situations；
3) present invention reduces the requirement to operation, only temperature adjustment sample need to be indicated according to thermocouple after setting assigned temperature
Product lowering or hoisting gear and protection lowering or hoisting gear can complete setting-out, and experiment etc. is operated.
Brief description of the drawings
Fig. 1 is the structural representation of the present invention；
Fig. 2 a, Fig. 2 b are the top view and profile of supporting table in the present invention respectively；
Fig. 3 is that setting-out passage is arranged on the schematic diagram on body of heater in the present invention；
Structural representation when Fig. 4 is thermal insulation protection set work in the present invention；
Fig. 5 a~Fig. 5 c are that the protection lowering or hoisting gear and sample lowering or hoisting gear of the present invention are engaged three main shapes of work
The process schematic of state.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in each embodiment of invention described below
Not constituting conflict each other can just be mutually combined.
With reference to each accompanying drawing, a kind of thermogravimetric analyzer that can be achieved to be rapidly heated, including meausring apparatus 1, heating furnace 2, sample
Lowering or hoisting gear 4, protection lowering or hoisting gear 3 and temperature control device, wherein,
The meausring apparatus 1 includes being provided with balance room on pedestal platform 1-1 and electronic balance 1-2A, the pedestal platform 1-1
1-2, the electronic balance 1-2A are located in the balance room 1-2；
The heating furnace 2 includes stove seat 2-1 and body of heater 2-3, the stove seat 2-1 support the body of heater 2-3, the body of heater 2-
Heating electricity is provided with the 3 support pedestal platform 1-1, the formation of body of heater 2-3 the enclosed spaces burner hearth, and the body of heater 2-3
Hinder silk, setting-out passage 2-6, reaction gas air inlet pipe 2-5 and reactor off-gas escape pipe；
The sample lowering or hoisting gear 4 includes the first actuating unit 4-1, the first transmission device 4-2, lifting platform 4-3A and suspension rod
4-4, the first actuating unit 4-1 are arranged on the pedestal platform 1-1 and it described in the actuator drives by rising
Drop platform 4-3A is moved up and down, and the lifting platform 4-3A is located in the balance room 1-2 and lifting platform 4-3A accepts the electricity
Sub- balance 1-2A, the suspension rod 4-4 upper end are suspended on the electronic balance 1-2A and its lower end hanging basket 4-4A, with
For accepting sample and the change of sample quality being obtained by electronic balance 1-2A, the lower end of the suspension rod 4-4 stretch into it is described plus
The burner hearth of hot stove 2；
The protection lowering or hoisting gear 3 includes the second actuating unit 3-1, the second transmission device 3-2 and thermal insulation protection set 3-3,
The second actuating unit 3-1 be arranged on stove seat 2-1 it is upper and its by the second transmission device 3-2 drive described in every
Thermal protection set 3-3 is moved up and down, and opening is provided with above thermal insulation protection set 3-3, using as described in hanging basket 4-4A turnover every
Thermal protection covers 3-3 passage；
The temperature control device is connected with the heating furnace 2, for controlling the temperature of the burner hearth.
Further, the protection gas air inlet pipe 1-3 connected with the balance room 1-2 and is provided with the pedestal platform 1-1
It is provided with one middle gas distribution channel, the body of heater 2-3 in the second middle gas distribution channel connected with the burner hearth, described first
Between gas distribution channel and the connection of the second middle gas distribution channel.
Further, the temperature control device includes temperature sense adjusting means 5, and the temperature sense adjusting means 5 includes stove
Wall thermocouple 5-1 and with Furnace Temperature Controller 5-3, the furnace wall thermocouple 5-1 be arranged on the body of heater 2-3 inwalls on, the stove
Temperature controller 5-3 is connected with the furnace wall thermocouple 5-1 and the resistive heater, for obtaining the temperature of burner hearth, and base
The size of current on the resistive heater is controlled in the fire box temperature obtained from the furnace wall thermocouple 5-1, so as to control
Fire box temperature.
Further, the temperature control device also includes data analysis set-up 6, and the data analysis set-up 6 includes host computer 6-2
With data line 6-1, the host computer 6-2 by data line 6-1 respectively with the electronic balance 1-2A and temperature sense
Adjusting means 5 is answered to connect.
Further, suspention thermocouple 5-2, the suspention thermocouple 5-2 are also equipped with the suspension rod 4-4 and stretches into described hang
In basket 4-4A, for the temperature in measurement hanging basket 4-4A, the Furnace Temperature Controller 5-3 also connects with the suspention thermocouple 5-2
Connect, for obtaining the temperature of burner hearth, and the heating is controlled based on the fire box temperature obtained from the suspention thermocouple 5-2
Size of current on resistance wire, so as to control fire box temperature.
As shown in figure 1, the real-time measurement that electronic balance is used to complete sample quality is set in meausring apparatus 1, while weighing dress
Put 1 inner passage numerous, sample lowering or hoisting gear can be accommodated and the multi-tasks such as air inlet are completed；Heating furnace 2 is used to be put into sample
Product and test specimen is heated according to program setting, wherein protection lowering or hoisting gear 3 is by controlling the lifting that thermal insulation protection covers
To be thermally shielded protection to hanging basket, wherein sample lowering or hoisting gear 4 controls the liter of electronic balance, suspension rod and hanging basket by lift
Drop to be engaged guarantee effect of heat insulation with thermal insulation protection set, wherein temperature sense adjusting means 5 is used to measure and control warm in stove
Degree, it has a pair of thermocouples according to circumstances to switch using being used to monitor in real time, and wherein data analysis set-up 6 is used for collection analysis
Weight and temperature signal.It is the stabilization for the experiment that can be achieved to be rapidly heated, continuous, high-precision by the mutual cooperation of above-mentioned all parts
The measurement of degree, it is adaptable to the various reactions for needing isothermal method to measure, it is small etc. with the high error of simple in construction, easy to operate, precision
Advantage.
As shown in figure 1, the meausring apparatus 1 of the present invention has pedestal platform 1-1, balance room 1-2 and protection gas air inlet pipe 1-3,
Pedestal platform 1-1 is installed in the horizontal plane, and its middle part offers the space 1-1A for accommodating sample lowering or hoisting gear 4, and its top is opened up
There are the suspension rod passage 1-1C that is connected with balance room 1-2 and the first gas distribution channel 1-1B to heating furnace gas transmission, suspension rod 4-4 is through hanging
Electronic balance 1-2A is provided with bar passage 1-1C, balance room 1-2 rooms.Protect gas admission line 1-3 out of balance room 1-2 to pedestal
Platform 1-1 is overhang, for being passed through protective gas to balance room 1-2 and then into heating furnace 2.Specifically, the pedestal platform 1-1 is excellent
Inverted L-shaped is selected, bottom is integrally fixed, opened up in the top of stretching and put balance room 1-2, balance room 1-2 is used to accommodate electronic balance 1-
2A and lifting platform 4-3A etc., electronic balance 1-2A and suspension rod 4-4, which are connected, collects the weight signal of sample.Balance room 1-2 is just right
Heating furnace portion is provided separately suspension rod passage 1-1C, and channel internal diameter is 3~5mm.Protect the protruding pedestal platforms of gas air inlet pipe 1-3
30mm, inwardly straight-through balance room 1-2, (for example N of protective gas during work2Or inert gas) from the outside through protection gas air inlet pipe 1-
Body of heater 2-3 is blowed to by gas distribution channel 1-1B after 3 entrance balance room 1-2.Sealant 1-4 is mounted in heating furnace 2 and the pedestal
Between platform 1-1, sealant 1-4 is compressed by adjusting the height of heating furnace 2 and play sealing effectiveness.
As shown in figure 1, the heating furnace 2 of the present invention is preferably vertical tubular furnace, it has base 2-1, supporting table 2-2, stove
Transmission device is provided with the middle part of body 2-3, cooling block 2-4, reaction gas air inlet pipe 2-5 and setting-out passage 2-6, base 2-1 and is accommodated and is led to
The road 2-1A and cavity motor room 2-1B for placing motor, supporting table 2-2 are arranged on base 2-1, are provided with the middle part of supporting table 2-2
3-3 cooling bath 2-2C is covered for accommodating thermal insulation protection, using the parking space covered as the thermal insulation protection；Body of heater 2-3 is installed
On supporting table 2-2, for heating, roof of the furnace, which is provided with the middle part of cooling block 2-4, cooling block 2-4, to be offered and bottom cooling
The corresponding cooling chamber 2-4A of groove 2-2C, using the parking space as the hanging basket 4-4A.Reaction gas admission line 2-5 passes through body of heater
Is overhang to heating furnace in 2-3 and cooling chamber 2-4A, for being passed through reacting gas (for example O into heating furnace 22、N2Or CO2Deng).
Setting-out passage 2-6 is stretched into cooling block 2-4 after passing through body of heater 2-3, for the hanging basket 4-4A for being placed with sample to be suspended into suspension rod 4-4
Take down above or from suspension rod 4-4.Specifically, base is in integrally rectangular shape, the transmission device receiving channel 2-1A at middle part is
Cylindrical cavity, transmission device receiving channel 2-1A with motor room 2-1B while communicate and another side and supporting table 2-2 cylinder
Passage is communicated, and motor room 2-1B is that the square cavity of stove seat bottom is used to place the second actuating unit.Specifically, such as Fig. 2 a, figure
Shown in 2b, supporting table 2-2 is two-stage round boss formula structure, and subordinate's boss 2-2A diameters are more than higher level's boss 2-2B diameters, in
Portion is provided with cylindrical cooling bath 2-2C, and cooling bath 2-2C diameters are slightly larger than the diameter that thermal insulation protection covers, bottom portion of groove and supporting table
Transmission device receiving channel 2-1A communicate, supporting table side provided with reactor off-gas escape pipe 2-2D be used for furnace gas is led
Go out.Body of heater 2-3 is cylinder, and lower openings are closed by supporting table, and top is passed through by gas distribution channel 1-1B.Cooling block 2-4 is resistance to
The cylinder of hot material, is close at the top of body of heater 2-3, and its middle part offers hanging basket 4-4A before cylindrical cooling chamber 2-4A, setting-out
As suspension rod 4-4 is risen in cooling chamber 2-4A, thermal insulation protection set 3-3 rises to cold under the second actuating unit 3-1 driving
But room 2-4A close beneaths, the opening that then hanging basket 4-4A covers from thermal insulation protection on 3-3 again enters in thermal insulation protection set 3-3, this
Sample ensures that sample is put into smoothly and reaction will not be immediately begun to due to high temperature during setting-out.Reaction gas air inlet pipe 2-5 is protruding to be added
Hot stove 30mm, passes inwardly through oven wall and reaches cooling block 2-4, the bending guarantee downwards in cooling block of reaction gas air inlet pipe is passed through
Gas does not affect suspension rod so that balance measurement is more accurate.Setting-out passage 2-6 is opened in the side of heating furnace 2, works as work
When making state for lift, suspension rod rising, hanging basket is put into stove by it.Specifically, being illustrated in figure 3 setting-out passage 2-6
Mounting structure figure, setting-out passage 2-6 passes through body of heater 2-3 and cooling block 2-4 outside stove, leads directly to cooling chamber 2-4A, window channel
2-6B is in square, and section is less than cylinder cooling chamber lateral section, and window channel is longer closed good, scuttle 2-6A and hinge 2-
6C hypomeres are welded, and hinge 2-6C upper ends are connected on furnace wall by screw 2-6D.
As shown in figure 1, the sample lowering or hoisting gear 4 of the present invention has the first actuating unit 4-1, the first transmission device 4-2, rise
Ladder 4-3 and suspension rod 4-4 drops, and lift 4-3 of the invention movement is similar to the movement of elevator, the first actuating unit 4-1 with
First transmission device 4-2 is placed in the lowering or hoisting gear space 1-1A of the pedestal platform 1-1, and lift 4-3 is arranged on balance room
In 1-2.First transmission device 4-2 is reached in balance room 1-2 to be connected with lift 4-3, suspension rod 4-4 and electronic balance 1-2A phases
Connection, and stretched into by the suspension rod passage 1-1C in burner hearth, suspension rod 4-4 bottoms hang with hanging basket 4-4A.Specifically, the first power
Mechanism 4-1 is arranged on pedestal platform 1-1, and the first transmission device 4-2 is arranged between the first actuating unit 4-1 and balance room 1-2.
Lift 4-3 is arranged among balance room, including lifting platform 4-3A and ladder 4-3B, lifting platform 4-3A are used to fix electronic balance
1-2A, so as to control electronic balance 1-2A and suspension rod 4-4 to lift.Suspension rod 4-4 can reach highest point and just locate for hanging basket 4-4A
In the cooling bath 2-4A of the cooling block, it is hanging basket 4-4A just in the middle part of burner hearth that suspension rod 4-4, which can reach lowest part,.
As shown in figure 1, the present invention protection lowering or hoisting gear 3 have the second actuating unit 3-1, the second transmission device 3-2 and
Thermal insulation protection covers 3-3, and second actuating unit 3-1 is arranged in the motor room 2-1B of the base 2-1, is thermal insulation protection set 3-
3 lifting provides power.Specifically, the second actuating unit 3-1 is arranged on base 2-1, it is integrally placed in motor room 2-1B,
Motor model can according to the actual requirements and size selection.Second transmission device 3-2 is arranged on 3-1 on actuating unit, and it passes through stove
Seat and supporting table passage 2-1A are extend into burner hearth through cooling bath 2-2C.Specifically, being illustrated in figure 4 thermal insulation protection set work
When structural representation, thermal insulation protection set 3-3 be arranged on the second transmission device 3-2 top, its mainly include shell body 3-3A
With thermal insulation layer 3-3B, shell body 3-3A is heat proof material, and it is made up of two cylindrical sleeves patch bottoms of different sizes, larger circle
Cylinder diameter about 30mm, less cylinder sides are provided with four screw 3-3C, the size of smaller cylinder and the second transmission device 3-2 phases
Fit through mode connects for screw and fix thermal insulation protection set.Thermal insulation layer 3-3B is close to shell body filling, and thickness is determined by heat-barrier material property
It is fixed, while reserved in center is used to place hanging basket 4-4A slightly larger than the big sulculus of hanging basket.
Fig. 5 a~Fig. 5 c show the mistake of three principal states of protection lowering or hoisting gear and sample lowering or hoisting gear cooperating
Journey schematic diagram.Fig. 5 a are the working conditions (being placed with sample in hanging basket 4-4A) when being just put into hanging basket 4-4A, now electronic balance 1-
2A is in balance room 1-2 top, and hanging basket 4-4A is in cooling chamber 2-4A, and thermal insulation protection covers 3-3 just at cooling chamber 2-
4A underface；Fig. 5 b are that hanging basket 4-4A declines wait electronic balance 1-2A stable readings after a segment distance, and wait thermoelectricity
Even temperature reaches working condition during assigned temperature, now electronic balance 1-2A be in balance room 1-2 bottoms, hanging basket 4-4A and every
Thermal protection set 3-3 is in the middle part of burner hearth；Fig. 5 c are the working conditions that sample starts reaction after system is stablized, now at electronic balance
In balance room bottom, hanging basket is in the middle part of burner hearth, and thermal insulation protection set is withdrawn into cooling bath 2-2C coolings.
As shown in figure 1, the present invention temperature sense adjusting means 5 include furnace wall thermocouple 5-1, suspention thermocouple 5-2 and
Furnace Temperature Controller 5-3, the furnace wall thermocouple is arranged on the inside of the furnace wall in the middle part of body of heater 2-3, and its signal wire is out of furnace wall by adding
Hot stove outer covering export, and be connected by signal wire with Furnace Temperature Controller 5-3.Suspention thermocouple 5-2 is arranged on above hanging basket 4-4A,
Suspended in midair by signal wire, its progress lifting moving synchronous with hanging basket and lowering or hoisting gear.In experimentation, two thermocouples are real-time
Measurement shows the temperature of position.Furnace Temperature Controller 5-3 is according to the signal of two thermocouples and the difference of setting heating schedule temperature
Value, forms feedback signal, to adjust body of heater 2-3 heating powers, thermocouple signal is met setting heating schedule temperature.Specifically
The switching of two galvanic couples is used when using, and another one signal is realized not via Furnace Temperature Controller when using one feeds back.Put and hang
During basket 4-4A, the signal wire of suspension rod 4-4 and suspention is up, and hanging basket now suspends thermocouple 5-2 in midair just in cooling bath 2-4A
In upper furnace and furnace wall thermocouple 5-1 in the centre of body of heater 2-3 inwalls, therefore it is switched to furnace wall thermocouple and Furnace Temperature Controller 5-
3 communicate, and make furnace wall thermocouple signal consistent with program setting temperature.Setting-out is completed, and furnace wall thermocouple 5-2 temperature and program are set
After constant temperature degree is consistent, suspension rod 4-4, which is fallen, makes hanging basket 4-4A and thermal insulation protection cover 3-3 just in the middle part of burner hearth, now suspends in midair
Thermocouple 5-2 and furnace wall thermocouple 5-1 is highly roughly the same and suspends thermocouple 5-2 in midair in stove center.Keep the power of heating furnace 2 not
Become, after balance reading is stable, falls thermal insulation protection and cover 3-3, suspension rod 4-4 is motionless, treat that descending thermal insulation protection set 3-3 falls back on cooling
In groove 2-2C, sample can react.When thermocouple 5-2 temperature to be suspended rises to consistent with furnace wall thermocouple 5-1 temperature, cut
Change to suspention thermocouple 5-2 with Furnace Temperature Controller 5-3 to be connected, sample temperature is adjusted using thermocouple 5-2 signals are suspended in midair
Control.
As shown in figure 1, the data analysis set-up 6 of the present invention includes data transfer described in data line 6-1 and computer 6-2
Electronic balance 1-2A, Furnace Temperature Controller 5-3 are connected by line with computer, by the weight signal of electronic balance, the stove of Furnace Temperature Controller
Warm signal is transferred to computer, and computer is acquired analysis to weight and temperature data, and controls the calibration of electronic balance to return to zero
Program realizes the regulation of electronic balance, moreover it is possible to control the temperature of heating furnace 2, and the specific mode that controls to adjust can be using conventional regulation
Mode is carried out, and will not be repeated here.
The specific steps of sample quality are rapidly heated and are detected using the thermogravimetric analyzer that is rapidly heated of the present invention such as
Under：
1) air-tightness is good in regulation heating furnace 2 and pedestal platform 1-1 height, compression sealant 1-4, holding furnace, from guarantor
Shield gas air inlet pipe 1-3 is passed through protection gas into heating furnace；
2) 3-3 and suspension rod height 4-3 is covered by protecting lowering or hoisting gear 3 and sample lowering or hoisting gear 4 to adjust thermal insulation protection, makes to hang
Bar lower end is in cooling chamber 2-4A, the upper end that thermal insulation protection covers 3-3 is reached 2-4A mouthfuls of cooling chamber just；
3) precise about 10mg testing samples, record sample quality, sample are attached in hanging basket 4-4A, open setting-out and lead to
Road 2-6 scuttle 2-6A, suspension rod 4-4 lower ends are attached to by hanging basket 4-4A, close scuttle 2-6A；
4) reacting gas is passed through into heating furnace 2 from reaction gas air inlet pipe 2-5, ventilation a period of time treats that furnace atmosphere is stable
Afterwards, electronic balance 1-2A is returned to zero by computer 6-2；
5) program temperature needed for being set by computer 6-2, switching furnace wall thermocouple 5-1 is connected with Furnace Temperature Controller 5-3；
6) set by the temperature stabilization to program of furnace wall thermocouple during temperature, by protecting lowering or hoisting gear 3 and sample to lift
The regulation thermal insulation protection set 3-3 and suspension rod 4-4 height of device 4, makes suspension rod 4-4 lower ends hanging basket 4-4A be in burner hearth center, heat-insulated to protect
Sheath 3-3 is rolled in outside hanging basket 4-4A；
7) keep heating furnace power constant, after after electronic balance stable reading, regulation protection lowering or hoisting gear 3 makes thermal insulation protection
Set 3-3 exits burner hearth and dropped in cooling bath 2-2C, and hanging basket 4-4A is started reaction exposed to moment in burner hearth immediately reaches experiment
To the effect that is rapidly heated；
8) Furnace Temperature Controller 5-3 is connected using the temperature signal for suspending thermocouple 5-2 feedbacks in midair, and fire box temperature is adjusted
Control.
9) thermogravimetric curve kept stable is treated, collection is terminated, data are preserved.
In this way, by the present invention the thermogravimetric analyzer that is rapidly heated can realize isothermal method measure when data it is accurate, steady
It is fixed to obtain, have the advantages that the high error of simple in construction, easy to operate, precision is small.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, it is not used to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the invention etc., it all should include
Within protection scope of the present invention.
Claims (8)
1. a kind of thermogravimetric analyzer that can be achieved to be rapidly heated, it is characterised in that including meausring apparatus, heating furnace, sample lifting
Device, protection lowering or hoisting gear and temperature control device, wherein,
The meausring apparatus includes being provided with balance room on pedestal platform and electronic balance, the pedestal platform, the electronic balance position
In in the balance room；
The heating furnace includes stove seat and body of heater, body of heater described in the stove seat supports, and pedestal platform, described described in the converter body support
Resistive heater, setting-out passage, reaction gas air inlet pipe and anti-are provided with body of heater enclosed space formation burner hearth, and the body of heater
Answer waste gas escape pipe；
The sample lowering or hoisting gear includes the first actuating unit, the first transmission device, lifting platform and suspension rod, first engine
Structure is arranged on the pedestal platform and it is moved up and down by lifting platform described in the actuator drives, the lifting platform position
In in the balance room and the lifting platform accepts the electronic balance, the upper end of the suspension rod is suspended on the electronic balance
And its lower end hanging basket, the change of sample quality is obtained for undertaking sample and by electronic balance, the suspension rod
The burner hearth of the heating furnace is stretched into lower end；
The protection lowering or hoisting gear includes the second actuating unit, the second transmission device and thermal insulation protection set, second engine
Structure is arranged on that stove seat is upper and it is moved up and down by thermal insulation protection set described in second actuator drives, it is described every
Thermal protection set top is provided with opening, the passage to pass in and out the thermal insulation protection set as hanging basket；
The temperature control device is connected with the heating furnace, for controlling the temperature of the burner hearth.
2. a kind of thermogravimetric analyzer that can be achieved to be rapidly heated according to claim 1, it is characterised in that the pedestal platform
On be provided with the protection gas air inlet pipe connected with the balance room and the first middle gas distribution channel, the body of heater and be provided with and institute
State the second middle gas distribution channel of burner hearth connection, the first middle gas distribution channel and the second middle gas distribution channel connection.
3. a kind of thermogravimetric analyzer that can be achieved to be rapidly heated according to claim 1, it is characterised in that the heat-insulated guarantor
Sheath includes shell body and the thermal insulation layer being arranged on the shell body inwall.
4. a kind of thermogravimetric analyzer that can be achieved to be rapidly heated according to claim 1, it is characterised in that the temperature control dress
Put including temperature sense adjusting means, the temperature sense adjusting means include furnace wall thermocouple and and Furnace Temperature Controller, it is described
Furnace wall the installation of TC is on the inboard wall of furnace body, the Furnace Temperature Controller and the furnace wall thermocouple and the resistive heater
Connection, for obtaining the temperature of burner hearth, and controls the heating based on the fire box temperature obtained from the furnace wall thermocouple
Size of current on resistance wire, so as to control fire box temperature.
5. a kind of thermogravimetric analyzer that can be achieved to be rapidly heated according to claim 4, it is characterised in that the temperature control dress
Putting also includes data analysis set-up, and the data analysis set-up includes host computer and data line, and the host computer passes through number
It is connected respectively with the electronic balance and temperature sense adjusting means according to transmission line.
6. a kind of thermogravimetric analyzer that can be achieved to be rapidly heated according to claim 4, it is characterised in that on the suspension rod
It is also equipped with suspending thermocouple in midair, the suspention thermocouple is stretched into the hanging basket, for the temperature in measurement hanging basket, the stove
Temperature controller is also connected with the suspention thermocouple, for obtaining the temperature of burner hearth, and is based on obtaining from the suspention thermocouple
Fire box temperature control the size of current on the resistive heater, so as to control fire box temperature.
7. a kind of thermogravimetric analyzer that can be achieved to be rapidly heated according to claim 1, it is characterised in that the stove seat bag
Include base and the supporting table being arranged on base, the supporting table supports the body of heater, the top of the supporting table is provided with cold
But groove, using the parking space covered as the thermal insulation protection.
8. a kind of thermogravimetric analyzer that can be achieved to be rapidly heated according to claim 1, it is characterised in that the body of heater bag
Include furnace wall and be arranged on the cooling block on furnace wall top, the bottom of the cooling block is provided with cooling bath, to be used as the hanging basket
Parking space.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710421248.9A CN107271320B (en) | 2017-06-07 | 2017-06-07 | A kind of thermogravimetric analyzer that can be achieved to be rapidly heated |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710421248.9A CN107271320B (en) | 2017-06-07 | 2017-06-07 | A kind of thermogravimetric analyzer that can be achieved to be rapidly heated |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107271320A true CN107271320A (en) | 2017-10-20 |
| CN107271320B CN107271320B (en) | 2019-08-30 |
Family
ID=60065866
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710421248.9A Active CN107271320B (en) | 2017-06-07 | 2017-06-07 | A kind of thermogravimetric analyzer that can be achieved to be rapidly heated |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107271320B (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108871995A (en) * | 2018-05-08 | 2018-11-23 | 中国工程物理研究院化工材料研究所 | A kind of energetic material mass change automatic monitoring system and monitoring method |
| CN109490131A (en) * | 2018-09-21 | 2019-03-19 | 华中科技大学 | It is a kind of for gaseous state heavy metal generation-adsorption test real-time testing system |
| CN109900736A (en) * | 2017-12-07 | 2019-06-18 | 中国电力科学研究院有限公司 | A kind of 65-100K warm area nonmetallic materials thermal conductivity measurement system |
| CN110954435A (en) * | 2019-12-20 | 2020-04-03 | 武汉科技大学 | Evaporation rate measuring device and method under multi-factor coupling effect |
| CN111077037A (en) * | 2019-12-31 | 2020-04-28 | 中国科学院山西煤炭化学研究所 | Online integrated continuous and rapid determination device and method for moisture and ash content |
| CN111380766A (en) * | 2020-04-10 | 2020-07-07 | 兰州华汇仪器科技有限公司 | Vacuum high-temperature friction and wear tester |
| CN111380765A (en) * | 2020-04-10 | 2020-07-07 | 兰州华汇仪器科技有限公司 | Heating furnace assembly of high-temperature friction and wear tester and application method thereof |
| CN111505198A (en) * | 2020-04-22 | 2020-08-07 | 中国特种设备检测研究院 | Large-particle coke combustion characteristic testing system |
| CN112816361A (en) * | 2021-01-05 | 2021-05-18 | 神华神东煤炭集团有限责任公司 | System and method for evaluating thermal conversion of organic matter-containing solid |
| CN113867445A (en) * | 2021-09-26 | 2021-12-31 | 华中科技大学 | Rapid heating system based on condensing heating and thermogravimetric analysis method |
| CN114674589A (en) * | 2022-05-27 | 2022-06-28 | 中国飞机强度研究所 | System and method for applying instantaneous thermal impact load in aerospace plane thermal test |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006071845A3 (en) * | 2004-12-28 | 2007-05-10 | Waters Investments Ltd | System and method for a thermogravimetric analyzer having improved dynamic weight baseline |
| CN101799242A (en) * | 2010-01-29 | 2010-08-11 | 华中科技大学 | Controllable fast-heating up thermobalance reacting furnace |
| CN103439212A (en) * | 2013-08-07 | 2013-12-11 | 华中科技大学 | Double-furnace body thermobalance capable of changing temperature quickly |
| CN103760054A (en) * | 2014-01-16 | 2014-04-30 | 华中科技大学 | Thermal gravimetrical reactor applied to bulk specimen testing |
| CN104237058A (en) * | 2014-09-23 | 2014-12-24 | 中国科学技术大学 | Thermogravimetric molecular beam mass spectrum combined device |
| CN105954137A (en) * | 2016-06-20 | 2016-09-21 | 华中科技大学 | In-situ rapid sampling thermogravimetric analyzer |
-
2017
- 2017-06-07 CN CN201710421248.9A patent/CN107271320B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006071845A3 (en) * | 2004-12-28 | 2007-05-10 | Waters Investments Ltd | System and method for a thermogravimetric analyzer having improved dynamic weight baseline |
| CN101799242A (en) * | 2010-01-29 | 2010-08-11 | 华中科技大学 | Controllable fast-heating up thermobalance reacting furnace |
| CN103439212A (en) * | 2013-08-07 | 2013-12-11 | 华中科技大学 | Double-furnace body thermobalance capable of changing temperature quickly |
| CN103760054A (en) * | 2014-01-16 | 2014-04-30 | 华中科技大学 | Thermal gravimetrical reactor applied to bulk specimen testing |
| CN104237058A (en) * | 2014-09-23 | 2014-12-24 | 中国科学技术大学 | Thermogravimetric molecular beam mass spectrum combined device |
| CN105954137A (en) * | 2016-06-20 | 2016-09-21 | 华中科技大学 | In-situ rapid sampling thermogravimetric analyzer |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109900736A (en) * | 2017-12-07 | 2019-06-18 | 中国电力科学研究院有限公司 | A kind of 65-100K warm area nonmetallic materials thermal conductivity measurement system |
| CN108871995B (en) * | 2018-05-08 | 2020-07-07 | 中国工程物理研究院化工材料研究所 | Automatic monitoring system and monitoring method for quality change of energetic material |
| CN108871995A (en) * | 2018-05-08 | 2018-11-23 | 中国工程物理研究院化工材料研究所 | A kind of energetic material mass change automatic monitoring system and monitoring method |
| CN109490131A (en) * | 2018-09-21 | 2019-03-19 | 华中科技大学 | It is a kind of for gaseous state heavy metal generation-adsorption test real-time testing system |
| CN110954435A (en) * | 2019-12-20 | 2020-04-03 | 武汉科技大学 | Evaporation rate measuring device and method under multi-factor coupling effect |
| CN111077037B (en) * | 2019-12-31 | 2021-06-22 | 中国科学院山西煤炭化学研究所 | Online integrated continuous and rapid determination device and method for moisture and ash content |
| CN111077037A (en) * | 2019-12-31 | 2020-04-28 | 中国科学院山西煤炭化学研究所 | Online integrated continuous and rapid determination device and method for moisture and ash content |
| CN111380766A (en) * | 2020-04-10 | 2020-07-07 | 兰州华汇仪器科技有限公司 | Vacuum high-temperature friction and wear tester |
| CN111380765A (en) * | 2020-04-10 | 2020-07-07 | 兰州华汇仪器科技有限公司 | Heating furnace assembly of high-temperature friction and wear tester and application method thereof |
| CN111505198A (en) * | 2020-04-22 | 2020-08-07 | 中国特种设备检测研究院 | Large-particle coke combustion characteristic testing system |
| CN112816361A (en) * | 2021-01-05 | 2021-05-18 | 神华神东煤炭集团有限责任公司 | System and method for evaluating thermal conversion of organic matter-containing solid |
| CN113867445A (en) * | 2021-09-26 | 2021-12-31 | 华中科技大学 | Rapid heating system based on condensing heating and thermogravimetric analysis method |
| CN113867445B (en) * | 2021-09-26 | 2022-11-15 | 华中科技大学 | Rapid heating system based on light-gathering heating and thermogravimetric analysis method |
| CN114674589A (en) * | 2022-05-27 | 2022-06-28 | 中国飞机强度研究所 | System and method for applying instantaneous thermal impact load in aerospace plane thermal test |
| CN114674589B (en) * | 2022-05-27 | 2022-08-26 | 中国飞机强度研究所 | System and method for applying instantaneous thermal impact load in aerospace plane thermal test |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107271320B (en) | 2019-08-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107271320A (en) | A kind of thermogravimetric analyzer that can be achieved to be rapidly heated | |
| JP4658038B2 (en) | Analytical furnace with predictive temperature control | |
| CN103439212B (en) | A kind of quick changeable temperature double-furnace-body double thermobalance | |
| CN108007809A (en) | One kind is rapidly heated wide-range thermogravimetric analyzer | |
| CN101429677A (en) | Polysilicon ingot furnace | |
| CN101900663A (en) | High-temperature cyclic oxidation corrosion simulating test device | |
| US10852221B2 (en) | Magnetic suspension thermobalance based on quick photothermal heating and measurement method thereof | |
| CN109211438B (en) | Device and method for observing heat flux density of continuous casting covering slag in phase change process in situ | |
| CN108956360B (en) | Magnetic suspension thermobalance based on photo-thermal rapid heating | |
| CN112611671A (en) | Multifunctional visual thermogravimetric analysis device and method for experiment | |
| CN106124361A (en) | The measuring method of vitreous humour density and the measurement apparatus of vitreous humour density | |
| CN106092803A (en) | Constant temperature Thermgravimetric Analysis Apparatus | |
| KR20070010739A (en) | Construction of hydrostatic weighing apparatus for density measurement | |
| CN106442622A (en) | Rotary type slow-baking safety test device | |
| US20180073966A1 (en) | Test System Comprising a Heating Device and Method for Implementing a Test System | |
| CN209894627U (en) | High-efficient thermogravimetric analyzer | |
| CN103148892B (en) | Constant-pressure briquette coal carbonization process quality and volume measuring device | |
| CN102538462B (en) | Experiment electric furnace with accurate temperature control | |
| CN108507900A (en) | A kind of thermal analyzer and its control method | |
| CN102865742A (en) | Van type multifunctional experimental resistance furnace for material thermogravimetric analysis | |
| KR100440865B1 (en) | Thermobalance analyzer equipped with heating tube and porous sample basket | |
| CN113092302A (en) | Sliding rail thermobalance system with double temperature zones and use method thereof | |
| CN103869848B (en) | Sheet coupon torture test heating furnace | |
| CN202630658U (en) | Vertical heating furnace with furnace door | |
| CN113008033A (en) | High-temperature reaction tube furnace capable of accurately controlling temperature and atmosphere and rapidly quenching sample |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |