CN208043722U - Heat analysis bevel cylinder crucible - Google Patents

Heat analysis bevel cylinder crucible Download PDF

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Publication number
CN208043722U
CN208043722U CN201820321241.XU CN201820321241U CN208043722U CN 208043722 U CN208043722 U CN 208043722U CN 201820321241 U CN201820321241 U CN 201820321241U CN 208043722 U CN208043722 U CN 208043722U
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China
Prior art keywords
crucible
sidewall
sample
inner face
reaction gas
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CN201820321241.XU
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Chinese (zh)
Inventor
赵岩
邵春岩
陈刚
裴江涛
范群
臧雪莉
侯海盟
曾乐
张广鑫
蒋帅
李述贤
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Shenyang Academy Environmental Sciences
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Shenyang Academy Environmental Sciences
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Abstract

The utility model is related to a kind of heat analysis bevel cylinder crucibles, solve during the heat analysis of burning/gasification reaction of solid powdery sample, the mass transfer condition between sample and reaction gas is bad.The main points of the utility model are:It is made of sidewall of crucible and crucible bottom, it is characterised in that:Sidewall of crucible is cylindrical in hollow bevel, and it is in pipe angular cut to make mouth of pot, and crucible bottom inner face is in slope shape, and the minimum point of crucible bottom inner face is with the minimum point of the sidewall of crucible to just.Sample is uniformly tiltedly laid on the inner face of the crucible bottom, the minimum point and peak of crucible bottom inner face face the reaction gas from horizontal direction, reaction gas directly reaches sample layer by forcing to transport, and the gas-phase product that simultaneous reactions generate quickly escapes up by the pressure of reaction gas transports.

Description

Heat analysis bevel cylinder crucible
Technical field
The utility model is related to heat analysis crucibles, and such crucible of application to carry out burning/gas of solid powdery sample Change the method for response characteristic test.
Background technology
Heat analysis is measured between the physical property of sample and temperature or time under the conditions of specified atmosphere and temperature programmed control A kind of analysis of modernization measuring technology of relationship includes mainly hot weight method (TG), derivative thermogravimetric amount method (DTG), differential scanning Calorimetry (DSC), poor (showing) heat analysis (DTA), thermo-mechanical analysis (TMA) and dynamic thermomechanical analysis (DMA) etc..Currently, hot Analytical technology has obtained in fields such as the energy, environment, physics, chemistry, chemical industry, metallurgy, geology, building materials, light textile, food, biologies To being widely applied, especially in energy and environment field, TG, DTG, DTA and DSC have become test and analysis sample Burning/gasification reaction characteristic and instruct reactor in actual industrial system to characterize and evaluation fuel fundamental property The important tool of design and operation.These four thermoanalysis technologies are both needed to sample (most of is solid powdery) being placed in certain knot In structure and the crucible of material, then the crucible for containing sample is put into heating furnace chamber, be passed through later specific reaction gas and Start to test under the temperature condition of program control, finally obtains quality, weight loss rate, temperature or the input thermal power and ginseng of sample Than object difference with test temperature or the change curve of time, to analyze burning/gasification reaction characteristic of sample.Currently, above-mentioned The structure of heating furnace chamber is divided into horizontal and two kinds rectilinear, wherein horizontal can not only ensure the measurement of sample quality not by The influence of its position, and heat buoyancy and the disturbance of the next quality signal of reaction gas turbulent zone can be made to minimize, thus obtain It is widely applied.For example, global famous precision instrument and Mettler Toledo Inc. of weighing apparatus manufacturer surmounts series TG/DSC thermal analyzers, with regard to all using horizontal heating furnace chamber.
In horizontal heating furnace chamber, reaction gas is imported by capillary near sample crucible, and with horizontal direction Initial velocity enters reaction compartment, when reaction gas is contacted with sample, that is, the change for chemically reacting and causing sample physical property occurs Change.However, the widely used crucible of institute has been all made of the hollow cylindrical structure with bottom surface, and the inside and outside table of bottom surface at present Face is level.Sample tiles on the inner surface of bottom surface forms a horizontal sample layer, and crucible wall will be higher by sample layer top Portion is many, thus make it is horizontal come to reaction gas cannot rely on pressure and transport and directly reach sample layer, and need by nature Diffusion crosses the obstruction of crucible wall, enters in crucible from the upper space of sample layer and contacts and react with sample.Together When, the effusion for reacting the gas-phase product of generation also needs to realize by natural diffuseness.The above process causes diffusion and makees The increase of contribution degree in overall reaction process control mechanism, the test data to make are anti-to the intrinsic chemistry of sample Active symbolical meanings are answered to weaken, especially in the constant-temperature combustion of higher temperature/gasification reaction characteristic test, this influence is more Significantly.
Invention content:
In order to effectively reduce the influence of diffusion in solid powdery sample combustion/gasification reaction characteristic test, to Enhance symbolical meanings of the obtained data to the intrinsic chemical reaction characteristic of sample, the utility model provides a kind of heat analysis With bevel cylinder crucible.
Heat analysis provided by the utility model is integrally formed with bevel cylinder crucible by sidewall of crucible and crucible bottom group, special Sign is:Sidewall of crucible is cylindrical in hollow bevel, and it is in pipe angular cut to make mouth of pot, and crucible bottom inner face is in slope shape, the earthenware To just, the sidewall of crucible height of the minimum point is the minimum point of the minimum point of crucible bottom inner face and the sidewall of crucible, that is, pipe angular cut 0.6 ~ 1 mm, the peak and sidewall of crucible peak of crucible bottom inner face are to just, the height of the sidewall of crucible of the peak is 1.5 ~ 2.5 mm;The tangent value of angle is 1 between slope shape crucible bottom inner face and horizontal plane:5~1:2.
The material of the utility model is high purity aluminium oxide or platinum.
The combustion gasification response characteristic that solid powdery sample is carried out with bevel cylinder crucible using above-mentioned heat analysis is surveyed The method of examination, specifically, sample are uniformly tiltedly laid on the inner face of the crucible bottom, the minimum point and peak face of crucible bottom inner face The reaction gas from horizontal direction, reaction gas directly reaches sample layer by forcing to transport, the gas phase production that simultaneous reactions generate Object can also quickly escape up by the pressure of reaction gas transports.
Compared with prior art, the utility model has the advantages that:
1, due to the inclined distribution of sample layer in crucible, and mouth of pot is in pipe angular cut, where almost all sample Position is higher than the minimum point of sidewall of crucible, that is, pipe angular cut, i.e. almost all sample is exposed to the reaction gas from horizontal direction In, effectively reduce contribution degree of the external diffusion in overall reaction process control mechanism before reaction.
2, the gas-phase product that reaction generates again may be by the pressure of reaction gas and transport and quickly escape, to reduce Contribution degree of the external diffusion in overall reaction process control mechanism after reaction.
3, compared with the horizontal inner bottom surface of conventional crucibles, the area for tilting inner bottom surface increases, therefore makes in identical sample Under dosage, the sample layer that the utility model is contained is thinner, to the resistance for making reaction gas and gas-phase product be spread in sample layer Power reduces, and reduces the contribution degree being diffused in sample layer in overall reaction process control mechanism.
The advantageous effect of above-mentioned three aspect means that influence of the diffusion to overall reaction process obtains in different links Weakening has been arrived, symbolical meanings of the obtained test data to the intrinsic chemical reactivity of sample are finally enhanced.
Description of the drawings
The utility model is described in further detail in the following with reference to the drawings and specific embodiments.
Fig. 1 is the sectional axonometric drawing of heat analysis bevel cylinder crucible.
Fig. 2 is the elevation cross-sectional view of heat analysis bevel cylinder crucible.
Specific implementation mode
Referring to Fig. 1, heat analysis is integrally formed with bevel cylinder crucible by 3 groups of sidewall of crucible 2 and crucible bottom, and sidewall of crucible is in sky Heart bevel is cylindrical, and it is in pipe angular cut to make mouth of pot, and referring to Fig. 2, crucible bottom inner face 31 is in slope shape, crucible bottom inner face Minimum point and the sidewall of crucible, that is, pipe angular cut minimum point to just, the sidewall of crucible height h1 of the minimum point is 0.6 ~ 1 Mm, the peak and sidewall of crucible peak of crucible bottom inner face are to just, the height h2 of the sidewall of crucible of the peak is 1.5 ~ 2.5 mm; The tangent value of angle is 1 between slope shape crucible bottom inner face and horizontal plane:5~1:2.Crucible wall thickness is 0.5 mm, outside crucible bottom A diameter of 10 ~ 17 mm on surface 32.
The material of the utility model is high purity aluminium oxide or platinum.
The utility model additionally provides a kind of above-mentioned heat analysis of use and carries out solid powdery sample with bevel cylinder crucible The method of the combustion gasification response characteristic test of product, specifically, the sample of 5 ~ 9 mg is uniformly tiltedly laid on the inner face of the crucible bottom, And the particle diameter distribution of solid powdery sample is assessed, and investigation can make maximum crucible of the sample remains stationary without downslide Inner bottom surface gradient selects the foundation of crucible as test.The minimum point and peak of crucible bottom inner face are faced from level The reaction gas in direction starts to test according to preset heating and gas changeover program, and wherein the flow control of reaction gas is 30 ~ 80 mL·min-1Range.Reaction gas directly reaches sample layer by forcing to transport, and the gas-phase product that simultaneous reactions generate can also It is quickly escaped up by the pressure of reaction gas transports.

Claims (2)

1. a kind of heat analysis bevel cylinder crucible, is integrally formed by sidewall of crucible and crucible bottom group, it is characterised in that:Sidewall of crucible In hollow bevel cylinder, make mouth of pot be in pipe angular cut, crucible bottom inner face be in slope shape, crucible bottom inner face it is minimum It puts with the minimum point of the sidewall of crucible, that is, pipe angular cut to just, the sidewall of crucible height of the minimum point is 0.6 ~ 1 mm, crucible bottom The peak of inner face is with sidewall of crucible peak to just, the height of the sidewall of crucible of the peak is 1.5 ~ 2.5 mm;Slope shape crucible The tangent value of angle is 1 between bottom inner face and horizontal plane:5~1:2.
2. heat analysis according to claim 1 bevel cylinder crucible, which is characterized in that crucible wall thickness is 0.5 Mm, a diameter of 10 ~ 17 mm of crucible bottom outer surface.
CN201820321241.XU 2018-03-09 2018-03-09 Heat analysis bevel cylinder crucible Active CN208043722U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201820321241.XU CN208043722U (en) 2018-03-09 2018-03-09 Heat analysis bevel cylinder crucible

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Application Number Priority Date Filing Date Title
CN201820321241.XU CN208043722U (en) 2018-03-09 2018-03-09 Heat analysis bevel cylinder crucible

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CN208043722U true CN208043722U (en) 2018-11-02

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108226214A (en) * 2018-03-09 2018-06-29 沈阳环境科学研究院 Heat analysis bevel cylinder crucible and its application method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108226214A (en) * 2018-03-09 2018-06-29 沈阳环境科学研究院 Heat analysis bevel cylinder crucible and its application method

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