CN104614272A - High-temperature pressuring thermobalance and application method thereof - Google Patents
High-temperature pressuring thermobalance and application method thereof Download PDFInfo
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Abstract
The invention relates to a high-temperature pressuring thermobalance. The high-temperature pressuring thermobalance comprises a tube type resistance furnace (4), a balance (12) and a sample taking and placing system, wherein the tube type resistance furnace (4) is arranged inside a pressure tank (3), the middle part of a reaction tube (5) is located inside the tube type resistance furnace (4), a gas inlet (2) and a thermocouple interface (22) are formed at the lower part of the reaction tube (5), a pressure regulating hole is formed at the upper part of the reaction tube (5), the bottom end of the reaction tube (5) is connected with a lifting rod (1), a motor (23) rotates to enable the lifting rod (1) and the pressure tank (3) as well as the reaction tube (5) to move up and down, and the top end of the reaction tube (5) is connected with the sample taking and placing system by a ball valve (6). The high-temperature pressuring thermobalance has the advantages of simple structure and convenience in operation, and is suitable for operation in corrosive atmosphere and various atmospheres.
Description
Technical field
The invention belongs to a kind of high-temperature pressurizing thermobalance and application process.
Background technology
Thermobalance is a kind of instrument micro-example being carried out to thermogravimetric analysis and thermogravimetric differential measurement.General thermogravimetric analyzer major part is tested at ambient pressure, market sold high-temperature pressurizing thermobalance less.Commercially available pressurized thermogravimetry comprises the compositions such as pressure-bearing balance, crystal reaction tube, electric furnace, bearing shell, control desk, source of the gas, but its price comparison is expensive, complex operation, amount of samples is few, cannot realize fast pyrogenation experiment and constant temperature gasification experiment, when testing under steam atmosphere, water vapor has entered balance cavity internal corrosion balance, and weigh inaccurate, cannot apply in the aggressive atmosphere such as sulfur-bearing, nitrogen, chlorine again.
Summary of the invention
The object of this invention is to provide a kind of structure simple, easy and simple to handle, the high-temperature pressurizing thermobalance operated under being applicable to aggressive atmosphere and various atmosphere and application process.
A kind of high-temperature pressurizing thermobalance, it comprises tube type resistance furnace, it is gentle picks and places sample system, it is characterized in that head tank there is pressurising mouth, exhausr port and power interface, there is tube type resistance furnace head tank inside, tubular electric resistance furnace interior is positioned in the middle part of reaction tube, air intake opening and thermopair interface are arranged at reaction tube bottom, pressure modulating opening is arranged at reaction tube top, pressure modulating opening is connected with cooling device, cooling device there is gas vent, the bottom of reaction tube is connected with elevating lever, by the rotation of motor, elevating lever is moved up and down together with reaction tube with head tank, motor is connected with firm banking, reaction tube top is connected with connecting pipe by ball valve, pick and place sample system and comprise sample basket, platinum wire, Balance Air exports, seal flange, telescoping inner and outer telescopic tube, outer telescopic tube is connected with hold-down support and positions, telescoping inner is free to slide and keeps pressure seal in outer telescopic tube, protection gas entrance is arranged at outer telescopic tube top, balance cage is arranged at outer telescopic tube top, balance is positioned at balance cage, platinum wire top is connected with balance, platinum wire lower end is connected with sample basket, sample basket is arranged in telescoping inner, on the connecting pipe of Balance Air outlet between ball valve and seal flange, connecting pipe is connected with seal flange.
The using method of high-temperature pressurizing thermobalance of the present invention is as follows:
(1), by 0.1mg-100g sample put into sample basket, close seal flange;
(2), pyrolytic gasification reaction
A slow pyrolysis: open protection gas entrance and pressurising mouth, pass into inert gas, close pressurising mouth after reaching experimental pressure, open coupling cock and ball valve, pass into inert gas from air intake opening, utilize pressure regulator valve regulating system pressure, open the data acquisition software of balance and computing machine, starter motor utilizes elevating lever reaction tube and head tank to be raised, and makes sample basket be in reaction tube constant temperature zone, switch on power, start program heats up and starts pyrolysis;
B fast pyrogenation: switch on power, start program heats up, after reaching temperature of reaction, open protection gas entrance and pressurising mouth, pass into inert gas, after reaching experimental pressure, close pressurising mouth, open coupling cock and ball valve successively, inert gas is passed into from air intake opening, utilize pressure regulator valve regulating system pressure, open the data acquisition software of balance and computing machine, starter motor utilizes elevating lever reaction tube and head tank to be raised, make sample basket be in reaction tube constant temperature zone, start pyrolytic reaction;
C program intensification gasification reaction: open protection gas entrance and pressurising mouth, pass into inert gas, close pressurising mouth after reaching experimental pressure, open coupling cock and ball valve successively, pass into reacting gas from air intake opening, utilize pressure regulator valve regulating system pressure, open the data acquisition software of balance and computing machine, starter motor utilizes elevating lever reaction tube and head tank to be raised, and makes sample basket be in reaction tube constant temperature zone, switch on power, start program heats up and starts gasification reaction;
D constant temperature gasification reaction: switch on power, start program heats up, after reaching temperature of reaction, open protection gas entrance and pressurising mouth, pass into inert gas, after reaching experimental pressure, close pressurising mouth, open coupling cock and ball valve successively, reacting gas is passed into from air intake opening, utilize pressure regulator valve regulating system pressure, open the data acquisition software of balance and computing machine, starter motor utilizes elevating lever reaction tube and head tank to be raised, make sample basket be in reaction tube constant temperature zone, start gasification reaction;
(3), after pyrolysis or reaction complete, starter motor utilizes elevating lever reaction tube and head tank to be reduced, and sample basket is speeded away reaction zone;
(4), open pressure regulator valve regulating system pressure and reduce to normal pressure, close ball valve, coupling cock successively, stop protection gas, open seal flange, take out sample basket.
Temperature of reaction as above can reach 1600 DEG C.
Reaction pressure scope as above is: normal pressure-4.0MPa.
Balance as above is electronic balance, can be connected directly read data with computing machine.
Reaction atmosphere as above can be nitrogen, water vapor, carbon monoxide, carbon dioxide, methane and oxygen etc.
Coal as above, the carbonaceous materials such as living beings.
The present invention's advantage compared with the prior art:
(1) cost performance is high, easy and simple to handle, and structure is simple
(2) dirigibility is high, can observe the change of example weight intuitively
(3) sample size wide ranges, can the reaction of 0.1mg-100g weight
(4) various atmosphere gasification can be carried out.
Accompanying drawing explanation
Fig. 1 is the structural representation of high-temperature pressurizing thermobalance of the present invention.
Fig. 2 is the process chart of high-temperature pressurizing thermobalance of the present invention.
Fig. 3 is the Pingshuo Coal temperature-programmed pyrolysis weight-loss curve figure of embodiment 1.
Fig. 4 is the Huolinhe lignite isothermal pyrolysis weight-loss curve figure of embodiment 2.
Fig. 5 is the corncob isothermal pyrolysis weight-loss curve figure of embodiment 3.
Fig. 6 is Shenmu County's bituminous coal temperature programme steam gasification weight-loss curve figure of embodiment 4.
Fig. 7 is the Bin County coal constant temperature CO of embodiment 5
2gasification weight-loss curve figure.
As shown in the figure, 1 elevating lever, 2 air intake openings, 3 head tanks, 4 tube type resistance furnaces, 5 reaction tubes, 6 ball valves, 7 sample baskets, 8 seal flanges, 9 telescoping inner, 10 outer telescopic tubes, 11 hold-down supports, 12 balances, 13 balance protective covers, 14 protection gas entrances, 15 platinum wires, 16 Balance Air outlets, 17 cooling devices, 18 gas vents, 19 exhausr ports, 20 pressurising mouths, 21 power interfaces, 22 thermopair interfaces, 23 motors, 24 firm bankings, 25 coupling cocks, 26 pressure regulator valves, 27 temperature controllers, 28 steam evaporators, 29 nitrogen, 30 carbon dioxide, 31 oxygen.
Embodiment
Embodiment 1
A kind of high-temperature pressurizing thermobalance, it comprises tube type resistance furnace 4, balance 12 and pick and place sample system, it is characterized in that head tank 3 has pressurising mouth 20, exhausr port 19 and power interface 21, there is tube type resistance furnace 4 head tank 3 inside, head tank 3 is located at inner in the middle part of reaction tube 5, air intake opening 2 and thermopair interface 22 are arranged at reaction tube 5 bottom, pressure modulating opening is arranged at reaction tube 5 top, pressure modulating opening is connected with cooling device 17, cooling device 17 there is gas vent 18, the bottom of reaction tube 5 is connected with elevating lever 1, by the rotation of motor 23, elevating lever 1 is moved up and down together with reaction tube 5 with head tank 3, motor 23 is connected with firm banking 24, reaction tube 5 top is connected with connecting pipe by ball valve 6, pick and place sample system and comprise sample basket 7, platinum wire 15, Balance Air outlet 16, seal flange 8, telescoping inner 9 and outer telescopic tube 10, outer telescopic tube 10 is connected with hold-down support 11 and positions, telescoping inner 9 is free to slide and keeps pressure seal in outer telescopic tube 10, protection gas entrance 14 is arranged at outer telescopic tube 10 top, balance cage 13 is arranged at outer telescopic tube 10 top, balance 12 is positioned at balance cage 13, platinum wire 15 top is connected with balance 12, platinum wire 15 lower end is connected with sample basket 7, sample basket 7 is arranged in telescoping inner 9, on the connecting pipe of Balance Air outlet 16 between ball valve 6 and seal flange 8, connecting pipe is connected with seal flange 8.
50g Pingshuo Coal is put into sample basket 7, closes seal flange 8; Open and protect gas entrance 14 and pressurising mouth 20 to pass into nitrogen 29, after reaching experimental pressure 1.0MPa, close pressurising mouth 20; Open coupling cock 25 and ball valve 6 successively, inert gas 29 is passed into from air intake opening 2, utilize pressure regulator valve 26 regulating system pressure, open the data acquisition software of balance 12 and computing machine, starter motor 23 utilizes elevating lever 1 reaction tube 5 and head tank 3 to be raised, and makes sample basket 7 be in reaction tube 5 constant temperature zone, switch on power, start program heats up and starts pyrolysis, and heating rate is 10 DEG C/min, and pyrolysis final temperature is 1000 DEG C; After pyrolysis completes, start electricity, 23 utilize elevating lever 1 reaction tube 5 and head tank 3 to be reduced, and sample basket 7 is speeded away reaction zone; Open pressure regulator valve 26 regulating system pressure and reduce to normal pressure, close ball valve 6, coupling cock 25 successively, open seal flange 8, take out sample basket 7.Experimental data is shown in Fig. 3.
Embodiment 2
50g Huolinhe lignite is put into sample basket 7, closes seal flange 8; Switch on power, start program heats up, and temperature of reaction is 900 DEG C; After reaching temperature of reaction, open protection gas entrance 14 and pressurising mouth 20, pass into inert nitrogen gas 29, after reaching experimental pressure 1.0MPa, close pressurising mouth 20; Open coupling cock 25 and ball valve 6 successively, pass into inert nitrogen gas 29 from reaction gas inlet 2, utilize pressure regulator valve 26 regulating system pressure; Open the data acquisition software of balance 12 and computing machine; Starter motor 23 utilizes elevating lever 1 reaction tube 5 and head tank 3 to be raised, and makes sample basket 7 be in reaction tube 5 constant temperature zone, starts pyrolytic reaction; After pyrolysis completes, starter motor 23 utilizes elevating lever 1 reaction tube 5 and head tank 3 to be reduced, and sample basket 7 is speeded away reaction zone; Open pressure regulator valve 26 regulating system pressure and reduce to normal pressure, close ball valve 6, coupling cock 25 successively, open seal flange 8, take out sample basket 7.Experimental data is shown in Fig. 4.All the other are with embodiment 1.
Embodiment 3
30g corncob is put into sample basket 7, closes seal flange 8; Switch on power, start program heats up, and temperature of reaction is 800 DEG C; After reaching temperature of reaction, open protection gas entrance 14 and pressurising mouth 20, pass into inert nitrogen gas 29, after reaching experimental pressure 1.0MPa, close pressurising mouth 20; Open coupling cock 25 and ball valve 6 successively, pass into inert nitrogen gas 29 from reaction gas inlet 2, utilize pressure regulator valve 26 regulating system pressure; Open the data acquisition software of balance 12 and computing machine; Starter motor 23 utilizes elevating lever 1 reaction tube 5 and head tank 3 to be raised, and makes sample basket 7 be in reaction tube 5 constant temperature zone, starts pyrolytic reaction; After pyrolysis completes, starter motor 23 utilizes elevating lever 1 reaction tube 5 and head tank 3 to be reduced, and sample basket 7 is speeded away reaction zone; Open pressure regulator valve 26 regulating system pressure and reduce to normal pressure, close ball valve 6, coupling cock 25 successively, open seal flange 8, take out sample basket 7.Experimental data is shown in Fig. 5.All the other are with embodiment 1.
Embodiment 4
5g Shenmu County bituminous coal is put into sample basket 7, closes seal flange 8; Open protection gas entrance 14 and pressurising mouth 20, pass into inert nitrogen gas 29, after reaching experimental pressure 2.0MPa, close pressurising mouth 20; Open coupling cock 25 and ball valve 6 successively, pass into reacting gas from reaction gas inlet 2, gas composition is 60%H
2o+40%N
2, utilize pressure regulator valve 26 regulating system pressure; Open the data acquisition software of balance 12 and computing machine; Starter motor 23 utilizes elevating lever 1 reaction tube 5 and head tank 3 to be raised, and makes sample basket 7 be in reaction tube 5 constant temperature zone; Switch on power, start program heats up and starts pyrolysis, and heating rate is 30 DEG C/min, and reaction final temperature is 1000 DEG C; After pyrolysis completes, starter motor 23 utilizes elevating lever 1 reaction tube 5 and head tank 3 to be reduced, and sample basket 7 is speeded away reaction zone; Open pressure regulator valve 26 regulating system pressure and reduce to normal pressure, close ball valve 6, coupling cock 25 successively, open seal flange 8, take out sample basket 7.Experimental data is shown in Fig. 6.All the other are with embodiment 1.
Embodiment 5
5g Bin County coal is put into sample basket 7, closes seal flange 8; Switch on power, start program heats up, and temperature of reaction is 1500 DEG C; After reaching temperature of reaction, open protection gas entrance 14 and pressurising mouth 20, pass into inert nitrogen gas 29, after reaching experimental pressure 3.0MPa, close pressurising mouth 20; Open coupling cock 25 and ball valve 6 successively, pass into reacting gas from reaction gas inlet 2, gas composition is 60%CO
2+ 40%N
2, utilize pressure regulator valve 26 regulating system pressure; Open the data acquisition software of balance 12 and computing machine; Starter motor 23 utilizes elevating lever 1 reaction tube 5 and head tank 3 to be raised, and makes sample basket 7 be in reaction tube 5 constant temperature zone, starts pyrolytic reaction; After pyrolysis completes, starter motor 23 utilizes elevating lever 1 reaction tube 5 and head tank 3 to be reduced, and sample basket 7 is speeded away reaction zone; Open pressure regulator valve 26 regulating system pressure and reduce to normal pressure, close ball valve 6, coupling cock 25 successively, open seal flange 8, take out sample basket 7.Experimental data is shown in Fig. 7.All the other are with embodiment 1.
Claims (7)
1. a high-temperature pressurizing thermobalance, it comprises tube type resistance furnace (4), balance (12) and pick and place sample system, it is characterized in that head tank (3) has pressurising mouth (20), exhausr port (19) and power interface (21), there is tube type resistance furnace (4) head tank (3) inside, it is inner that reaction tube (5) middle part is positioned at tube type resistance furnace (4), air intake opening (2) and thermopair interface (22) are arranged at reaction tube (5) bottom, pressure modulating opening is arranged at reaction tube (5) top, pressure modulating opening is connected with cooling device (17), cooling device (17) there is gas vent (18), the bottom of reaction tube (5) is connected with elevating lever (1), by the rotation of motor (23), elevating lever (1) is moved up and down together with head tank (3) and reaction tube (5), motor (23) is connected with firm banking (24), reaction tube (5) top is connected with connecting pipe by ball valve (6), pick and place sample system and comprise sample basket (7), platinum wire (15), Balance Air outlet (16), seal flange (8), telescoping inner (9) and outer telescopic tube (10), outer telescopic tube (10) is connected with hold-down support (11) and positions, telescoping inner (9) is free to slide and keeps pressure seal in outer telescopic tube (10), protection gas entrance (14) is arranged at outer telescopic tube (10) top, balance cage (13) is arranged at outer telescopic tube (10) top, balance (12) is positioned at balance cage (13), platinum wire (15) top is connected with balance (12), platinum wire (15) lower end is connected with sample basket (7), sample basket (7) is arranged in telescoping inner (9), Balance Air outlet (16) is positioned on the connecting pipe between ball valve (6) and seal flange (8), connecting pipe is connected with seal flange (8).
2. a kind of high-temperature pressurizing thermobalance as claimed in claim 1, is characterized in that described balance (12) is electronic balance.
3. a kind of high-temperature pressurizing thermobalance as claimed in claim 1 or 2 and application process, is characterized in that comprising the steps:
(1), by 0.1mg-100g sample put into sample basket 7, close seal flange (8);
(2), pyrolytic gasification reaction
A slow pyrolysis: open protection gas entrance (14) and pressurising mouth (20), pass into inert gas, pressurising mouth (20) is closed after reaching experimental pressure, open coupling cock (25) and ball valve (6), inert gas (29) is passed into from air intake opening (2), utilize pressure regulator valve (26) regulating system pressure, open the data acquisition software of balance (12) and computing machine, starter motor (23) utilizes elevating lever (1) reaction tube (5) and head tank (3) to be raised, sample basket (7) is made to be in reaction tube (5) constant temperature zone, switch on power, start program heats up and starts pyrolysis,
B fast pyrogenation: switch on power, start program heats up, after reaching temperature of reaction, open protection gas entrance (14) and pressurising mouth (20), pass into inert gas (29), pressurising mouth (20) is closed after reaching experimental pressure, open coupling cock (25) and ball valve (6) successively, inert gas (29) is passed into from air intake opening (2), utilize pressure regulator valve (26) regulating system pressure, open the data acquisition software of balance (12) and computing machine, starter motor (23) utilizes elevating lever (1) reaction tube (5) and head tank (3) to be raised, sample basket (7) is made to be in reaction tube (5) constant temperature zone, start pyrolytic reaction,
C program intensification gasification reaction: open protection gas entrance (14) and pressurising mouth (20), pass into inert gas (29), pressurising mouth (20) is closed after reaching experimental pressure, open coupling cock (25) and ball valve (6) successively, reacting gas is passed into from air intake opening (2), utilize pressure regulator valve (26) regulating system pressure, open the data acquisition software of balance (12) and computing machine, starter motor (23) utilizes elevating lever (1) reaction tube (5) and head tank (3) to be raised, sample basket (7) is made to be in reaction tube (5) constant temperature zone, switch on power, start program heats up and starts gasification reaction,
D constant temperature gasification reaction: switch on power, start program heats up, after reaching temperature of reaction, open protection gas entrance (14) and pressurising mouth (20), pass into inert gas (29), pressurising mouth (20) is closed after reaching experimental pressure, open coupling cock (25) and ball valve (6) successively, reacting gas is passed into from air intake opening (2), utilize pressure regulator valve (26) regulating system pressure, open the data acquisition software of balance (12) and computing machine, starter motor (23) utilizes elevating lever (1) reaction tube (5) and head tank (3) to be raised, sample basket (7) is made to be in reaction tube (5) constant temperature zone, start gasification reaction,
(3), after pyrolysis or reaction complete, starter motor (23) utilizes elevating lever (1) reaction tube (5) and head tank (3) to be reduced, and sample basket (7) is speeded away reaction zone;
(4), open pressure regulator valve (26) regulating system pressure and reduce to normal pressure, close ball valve (6), coupling cock (25) successively, stop protection gas (29), open seal flange (8), take out sample basket (7).
4. a kind of high-temperature pressurizing thermobalance as claimed in claim 3 and application process, is characterized in that described temperature of reaction is up to 1600 DEG C.
5. a kind of high-temperature pressurizing thermobalance as claimed in claim 3 and application process, is characterized in that described reaction pressure scope is: normal pressure-4.0MPa.
6. a kind of high-temperature pressurizing thermobalance as claimed in claim 3 and application process, is characterized in that described reacting gas is nitrogen, water vapor, carbon monoxide, carbon dioxide, methane or oxygen.
7. a kind of high-temperature pressurizing thermobalance as claimed in claim 3 and application process, is characterized in that described sample is coal or living beings.
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| CN113092302A (en) * | 2021-04-29 | 2021-07-09 | 桂林电子科技大学 | Sliding rail thermobalance system with double temperature zones and use method thereof |
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| CN113092302A (en) * | 2021-04-29 | 2021-07-09 | 桂林电子科技大学 | Sliding rail thermobalance system with double temperature zones and use method thereof |
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