CN103267777A - Heat type differential scanning calorimeter - Google Patents

Heat type differential scanning calorimeter Download PDF

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Publication number
CN103267777A
CN103267777A CN2013102276312A CN201310227631A CN103267777A CN 103267777 A CN103267777 A CN 103267777A CN 2013102276312 A CN2013102276312 A CN 2013102276312A CN 201310227631 A CN201310227631 A CN 201310227631A CN 103267777 A CN103267777 A CN 103267777A
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Prior art keywords
heating furnace
interlayer chamber
differential scanning
scanning calorimeter
type differential
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CN2013102276312A
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CN103267777B (en
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虞雄华
包慧敏
何树春
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SHANGHAI TECHCOMP INSTRUMENT Ltd
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SHANGHAI TECHCOMP INSTRUMENT Ltd
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Abstract

The invention discloses a heat type differential scanning calorimeter which comprises a shell, a bracket arranged in the shell, a flange plate fixed on the bracket, a heating furnace fixed on the flange plate, and an evaporator which is annularly sleeved on the heating furnace, wherein a sample testing area is formed on the top of the heating furnace; the evaporator has a cavity for placing the heating furnace and a cooling liquid interlayer cavity around the periphery of the cavity; the cooling liquid interlayer cavity is divided into an upper interlayer cavity and a lower interlayer cavity through a middle clapboard; a liquid outlet pipe is connected to the upper interlayer cavity; a liquid inlet pipe is arranged on the part, which is positioned under the liquid outlet pipe, of the lower interlayer cavity; and a small hole is formed in the position, which is in the farthest distance away from the liquid inlet pipe, of the clapboard. The heat type differential scanning calorimeter has the advantages of being accurate in temperature control, high in cooling efficiency, uniform in temperature exchange and wide in application range.

Description

Heat type differential scanning calorimeter
Technical field
The invention belongs to the lab analysis equipment technical field, relate to a kind of heat type differential scanning calorimeter.
Background technology
Differential scanning calorimeter, be used for measuring characteristic temperature, absorption or the liberated heat of material when thermal response, comprise material phase transformation, decomposition, chemical combination, solidify, physics or chemical reaction such as dehydration, evaporation, being widely used in fields such as organic and inorganic, silicate, pottery, mineral metal, space flight temperature-resistant material, is that various relevant industries institutes carries out thermoanalytical important instrument.
Material often is accompanied by the variation of micromechanism and character such as macroscopical physics, chemistry in temperature changing process.Physics on the macroscopic view, the variation of chemical property are associated with composition and the micromechanism of material usually.By measure and amalyzing substances heat or cooling procedure in physics, the variation of chemical property, can carry out qualitative, quantitative test to material, carry out the evaluation of material to help us, for the research and development of new material provides thermal behavior data and structural information.
Heat flow flux type differential scanning calorimeter, make sample be in certain temperature program(me) (lifting/lowering/constant temperature) control down, can observe differential heat flow between sample and the reference substance with the change procedure of temperature or time, its principle of work is: in program temperature (linear temperature increase, cooling, constant temperature and combination thereof) process, when sample generation thermal effect, between sample segments and reference substance end, produce differential heat flow, used thermopair that this differential heat flow is measured, thereby obtained to measure collection of illustrative plates.
Typical heat flow flux type differential scanning calorimeter comprises heating furnace, evaporator.Have the sample test zone at the heating furnace top, evaporator is around arranging around the heating furnace, thus the temperature variation of control heating furnace.Existing evaporator is to adopt coil pipe to be wrapped in around the heating furnace.There is following shortcoming in the heat flow flux type differential scanning calorimeter of this spline structure: the flowing time of liquid coolant in coil pipe is long, and the tube wall of coil pipe is that line contacts with heating furnace, so just cause the cooling effectiveness of evaporator lower, and non-uniform temperature around the heating furnace, and the fast cooling required time is long.
Summary of the invention
For this reason, technical matters to be solved by this invention provides the heat type differential scanning calorimeter that a kind of temperature control is accurate, cooling effectiveness is high, temperature exchange is even, applied widely, to overcome the deficiency that prior art exists.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of heat type differential scanning calorimeter, comprise shell, be located at the support in the shell, be fixed on the ring flange on the support, be fixed on the heating furnace on the ring flange, around the evaporator that is enclosed within on the heating furnace, described heating furnace top has the prototype test zone, it is characterized in that: described evaporator comprises internal ring wall plate, outer shroud wallboard, base plate, dividing plate, cover plate; Described internal ring wall plate is positioned at the inside of described outer shroud wallboard, and the inside of internal ring wall plate forms the cavity of ccontaining heating furnace, and described internal ring wall pastes on the outer wall of heating furnace; Interval between described internal ring wall plate and the described outer shroud wallboard forms around the liquid coolant interlayer chamber around the cavity; Described base plate is positioned at the bottom in liquid coolant interlayer chamber, and the middle part that described dividing plate is fixed on liquid coolant interlayer chamber is divided into interlayer chamber and following interlayer chamber with described liquid coolant interlayer chamber; The cover plate shutoff is arranged at the top in described liquid coolant interlayer chamber; Described going up on the interlayer chamber is connected with drain pipe, be positioned on the described interlayer chamber down drain pipe under be provided with feed tube, have aperture from feed tube maximum distance position on the set dividing plate.
In the specific embodiment of the present invention, the bore of described feed tube is littler than the bore of described drain pipe.
In the specific embodiment of the present invention, described aperture has a plurality of.
In the specific embodiment of the present invention, described evaporator comprises internal ring wall plate, outer shroud wallboard, base plate, dividing plate, cover plate; Described internal ring wall plate is positioned at the inside of described outer shroud wallboard, the inside of internal ring wall plate forms described cavity, interval between described internal ring wall plate and the described outer shroud wallboard forms described liquid coolant interlayer chamber, described base plate is positioned at the bottom in liquid coolant interlayer chamber, described dividing plate is fixed on the middle part in liquid coolant interlayer chamber, and the cover plate shutoff is arranged at the top in described liquid coolant interlayer chamber.
The lower ends downward of described outer shroud wallboard is extended the ring-like bilge ways that carries out assembling and positioning with ring flange.
Be provided with heat insulating washer between described base plate and the ring flange.
Adopt technique scheme, evaporator of the present invention specifically has following advantage for reheat furnace system provides the temperature environment of a stable and controllable:
1) liquid coolant is filled in the interlayer entirely, no dead volume, and temperature exchange is more even, makes the effective temperature zone temperature accuracy height centered by specimen, good stability; Realized high-precision temperature control.
2) because evaporator is to adopt liquid coolant to be full of sandwich construction entirely, not that coil pipe is wrapped in heating furnace line contact structures all around, temperature exchange is just more even, makes that temperature programme control is more accurate.
3) because evaporator is to adopt the liquid coolant of invention at present to be full of sandwich construction entirely, no dead volume, temperature exchange is more even, and exchange velocity is faster, makes instrument can realize the requirement of fast cooling, being wrapped in around the heating furnace line contact structures with present coil pipe compares, under identical heating furnace volume, the liquid coolant of invention is full of sandwich construction entirely at present, and cooling velocity is faster, chilling temperature is lower, has enlarged the use field of instrument.
Description of drawings
The present invention is described in detail with concrete enforcement below in conjunction with accompanying drawing:
Fig. 1 is structural representation of the present invention;
Fig. 2 is the structural representation of evaporator;
Fig. 3 is that the A-A of Fig. 2 is to cut-open view;
Fig. 4 is that the B-B of Fig. 2 is to cut-open view.
Embodiment
As shown in Figure 1, heat type differential scanning calorimeter of the present invention comprises shell 100, is located at support 200, heating furnace 300, evaporator 400 in the shell 100.
Wherein, have ring flange 201 at support 200, heating furnace 300 is fixed on the ring flange 201, evaporator 400 around be enclosed within the heating 300 around.Has sample test zone 301 at the top of heating furnace 300.
As Fig. 2, Fig. 3 and shown in Figure 4, evaporator 400 comprises internal ring wall plate 401, outer shroud wallboard 402, base plate 403, dividing plate 404, cover plate 405, feed tube 406 and drain pipe 407.
Wherein, internal ring wall plate 401, outer shroud wallboard 402, base plate 403 are integral mechanism, and internal ring wall plate 401 is positioned at outer shroud wallboard 402, the internal ring wall plate 401 inner cavitys 410 that form ccontaining heating furnace 300, and internal ring wall plate 401 pastes on the outer wall of heating furnace 300.And internal ring wall plate 401 and outer shroud wallboard 402 between clearance space form liquid coolant interlayer chamber 420, the bottom in liquid coolant interlayer chamber 420 is sealed by base plate 403.Dividing plate 404 is fixed on the middle part in liquid coolant interlayer chamber 420, and liquid coolant interlayer chamber 420 is divided into interlayer chamber 421 and following interlayer chamber 422, and the top accent that cover plate 405 then will be gone up interlayer chamber 421 seals.
Be connected with drain pipe 407 on the last interlayer chamber 421, be connected with feed tube 406 on the following interlayer chamber 422, and, feed tube 406 be positioned at drain pipe 407 under.The bore of feed tube 406 is littler than the bore of drain pipe 407, has formed the feed liquor throttling effect, increases the feed liquor flow velocity, makes liquid coolant be full of liquid coolant interlayer chamber 420 fast.Feed tube 406 is connected down interlayer chamber 422, drain pipe 421 is connected interlayer chamber 421, namely from the bottom feed liquor, the top fluid, it is easy like this that air is all discharged with air discharge in the chamber, and refrigerating fluid just is full of entirely, is conducive to improve refrigeration.
(being the right opposite position of feed tube 406) has the aperture 408 of a plurality of circumferential symmetrical distributions from feed tube 406 maximum distance positions on dividing plate 404.
In addition, the lower ends downward of outer shroud wallboard 402 is extended ring-like bilge ways 409, and this ring-like side plate 409 makes that evaporator 400 can be well in ring flange 201 location assemblings.And between the base plate 403 of evaporator 400 and ring flange 201, also be provided with heat insulating washer 500, guarantee that chilling temperature does not spread to the base direction.
More than be exactly heat type differential scanning calorimeter of the present invention, working method of the present invention is as follows:
Liquid coolant at first enters down interlayer chamber 422 from feed tube 406, flowing from both sides to aperture 408 in the interlayer chamber 422 down, flow into through aperture 408 then and go up interlayer chamber 421, in last interlayer chamber 421, flow from both sides to drain pipe 407 again, flow out from drain pipe 407 at last.The regulating and controlling to furnace temp that liquid coolant by turnover liquid coolant interlayer chamber 420 realizes.

Claims (5)

1. heat type differential scanning calorimeter, comprise shell, be located at the support in the shell, be fixed on the ring flange on the support, be fixed on the heating furnace on the ring flange, around the evaporator that is enclosed within on the heating furnace, described heating furnace top has the prototype test zone, it is characterized in that: described evaporator comprises internal ring wall plate, outer shroud wallboard, base plate, dividing plate, cover plate; Described internal ring wall plate is positioned at the inside of described outer shroud wallboard, and the inside of internal ring wall plate forms the cavity of ccontaining heating furnace, and described internal ring wall pastes on the outer wall of heating furnace; Interval between described internal ring wall plate and the described outer shroud wallboard forms around the liquid coolant interlayer chamber around the cavity; Described base plate is positioned at the bottom in liquid coolant interlayer chamber, and the middle part that described dividing plate is fixed on liquid coolant interlayer chamber is divided into interlayer chamber and following interlayer chamber with described liquid coolant interlayer chamber; The cover plate shutoff is arranged at the top in described liquid coolant interlayer chamber; Described going up on the interlayer chamber is connected with drain pipe, be positioned on the described interlayer chamber down drain pipe under be provided with feed tube, have aperture from feed tube maximum distance position on the set dividing plate.
2. heat type differential scanning calorimeter according to claim 1, it is characterized in that: the bore of described feed tube is littler than the bore of described drain pipe.
3. heat type differential scanning calorimeter according to claim 1, it is characterized in that: described aperture has a plurality of.
4. heat type differential scanning calorimeter according to claim 3, it is characterized in that: the lower ends downward of described outer shroud wallboard is extended the ring-like bilge ways that carries out assembling and positioning with ring flange.
5. heat type differential scanning calorimeter according to claim 1 is characterized in that: be provided with heat insulating washer between described base plate and the ring flange.
CN201310227631.2A 2013-06-07 2013-06-07 Heat type differential scanning calorimeter Active CN103267777B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104316558A (en) * 2014-10-15 2015-01-28 中国海洋石油总公司 Device and method for measuring heat conductivity of sediments of gas hydrates
CN108507900A (en) * 2018-06-14 2018-09-07 南通大学 A kind of thermal analyzer and its control method
CN112912721A (en) * 2018-10-22 2021-06-04 沃特世科技公司 High sample flux differential scanning calorimeter

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2566266Y (en) * 2002-09-11 2003-08-13 长沙三德实业有限公司 Improved constant temp. calorimeter
JP3141861U (en) * 2008-03-07 2008-05-22 株式会社島津製作所 Differential scanning calorimeter

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2566266Y (en) * 2002-09-11 2003-08-13 长沙三德实业有限公司 Improved constant temp. calorimeter
JP3141861U (en) * 2008-03-07 2008-05-22 株式会社島津製作所 Differential scanning calorimeter

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
MUSTAFA VERSAN KOK: ""Thermal behavior and kinetics of crude oils at low heating rates by differential scanning calorimeter"", 《FUEL PROCESSING TECHNOLOGY》, vol. 96, 20 January 2012 (2012-01-20), pages 123 - 127 *
郭健: ""浅析差示扫描量热法测定材料的比热容"", 《高分子材料研究》, no. 10, 31 December 2007 (2007-12-31), pages 19 - 20 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104316558A (en) * 2014-10-15 2015-01-28 中国海洋石油总公司 Device and method for measuring heat conductivity of sediments of gas hydrates
CN108507900A (en) * 2018-06-14 2018-09-07 南通大学 A kind of thermal analyzer and its control method
CN112912721A (en) * 2018-10-22 2021-06-04 沃特世科技公司 High sample flux differential scanning calorimeter

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