CN107290239B - Reactor assembly for thermal gravimetric equipment and thermal gravimetric equipment - Google Patents
Reactor assembly for thermal gravimetric equipment and thermal gravimetric equipment Download PDFInfo
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- CN107290239B CN107290239B CN201610205813.3A CN201610205813A CN107290239B CN 107290239 B CN107290239 B CN 107290239B CN 201610205813 A CN201610205813 A CN 201610205813A CN 107290239 B CN107290239 B CN 107290239B
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- 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
Abstract
The invention relates to the field of thermogravimetric analysis and discloses a reactor assembly for a thermogravimetric device and the thermogravimetric device, wherein the reactor assembly comprises a container (11) with at least double walls, and a space (13) between adjacent walls of the container (11) is closable and is used for placing a sample to be measured. The reactor component provided by the invention can be suitable for processing the situation of larger sample amount, in the reaction, the solid sample is in a thin layer state in the container, so that the solid sample is completely contacted with gas, the reaction is sufficient, and in addition, because the invention does not adopt the hanging basket to contain the sample to be measured, the problem of inaccurate measurement caused by buoyancy generated by the rising of the gas to the hanging basket in the prior art does not exist.
Description
Technical Field
The invention relates to the field of thermogravimetric analysis, in particular to a reactor assembly for thermogravimetric equipment and the thermogravimetric equipment.
Background
Thermogravimetric analysis refers to the analysis of the mass of a sample as a function of temperature or time under a defined reaction atmosphere, typically by means of tg (thermal gradient analysis) and/or dtg (differential thermal gradient) curves. This thermogravimetric analysis is generally used to study the composition, thermal stability, oxidation and reduction, adsorption and desorption, reaction kinetics, and the influence of additives and catalysts of materials.
Chinese patent application CN103760054A discloses a thermogravimetric reactor for large sample testing, as shown in fig. 1, which comprises a high temperature reactor 2, an electric heating furnace 1, a hydraulic lifting platform 3, a seal box 4 and an air source, wherein, with reference to fig. 2, the high temperature reactor 2 is composed of an inner tube 2-1 and an outer tube 2-2, the inner tube 2-1 is composed of an integral tube body 2-11 and an expansion head 2-12 from bottom to top, the bottom of the tube body 2-11 is provided with uniformly distributed holes, the tube body 2-11 is located in the outer tube 2-2, and the upper part of the outer tube 2-2 is provided with a reaction atmosphere air inlet 2-2A. The outer pipe 2-2 of the high-temperature reactor 2 is arranged in the electric heating furnace 1, the lower end of a seal box 4 is connected with the upper end of an expansion head of the inner pipe 2-1 through a connecting clamping sleeve 7, a protective atmosphere air inlet 4-1 is arranged on the seal box 4, a weighing sensor 5 is arranged on a partition plate 4-2 in the seal box 4, an upper thermocouple is arranged above the weighing sensor 5 and fixed at the top of the seal box 4, the lower end of the weighing sensor 5 is connected with a suspender 10 through a stainless steel wire penetrating through the inner pipe 2-1 of the high-temperature reactor 2, the lower end of the suspender 10 is connected with a hanging basket. The reaction gas from the gas source firstly passes through the annular pipeline of the outer pipe from top to bottom and then enters the inner pipe upwards through the pore plate at the bottom of the inner pipe to participate in the reaction.
However, the above-described thermogravimetric reactors have the following drawbacks: 1) because the gas rises from the bottom of the inner tube 2-1 after being preheated, upward buoyancy is generated on the hanging basket, and the buoyancy finally influences the quality measurement precision of the sample to be tested; 2) when the thermogravimetric reactor processes large amounts of sample, the contact of the gas with the solid sample is incomplete.
Disclosure of Invention
The invention aims to provide a reactor assembly for a thermogravimetric equipment and the thermogravimetric equipment, which overcome the problems of inaccurate measurement and incomplete contact of gas and a solid sample in the prior art.
In order to achieve the above object, the present invention provides a reactor assembly for a thermal gravimetric system, comprising a container having at least two walls, the space between adjacent walls of the container being closable and intended for placing a sample to be measured.
Preferably, the vessel includes an outer bottom wall, an outer side wall extending upwardly from the outer bottom wall, and an inner side wall located inwardly of the outer side wall, the inner and outer side walls being spaced apart in a direction perpendicular to a longitudinal direction of the reactor assembly to form at least a portion of the space.
Preferably, the vessel further comprises an inner bottom wall located at the bottom of the inner side wall and fixedly connected to the inner side wall, the inner bottom wall and the outer bottom wall being spaced apart longitudinally of the reactor assembly to form at least a part of the space.
Preferably, the reactor assembly further comprises a flange for connecting the inner and outer side walls and closing the space from the top.
Preferably, the bottom of the inner side wall is fixedly connected to the inner surface of the outer bottom wall.
Preferably, the outer and inner side walls of the container are each formed as a cylindrical structure, the annulus between the outer and inner side walls forming at least part of the space.
Preferably, the reactor assembly comprises a pick-and-place member capable of being placed in the space for bringing the sample to be measured in or out of the thermostatic zone in the space.
Preferably, the taking and placing component is a screen component provided with a hole structure.
Preferably, the screen member comprises a first screen member tightly fitted on the outside of the inner side wall and a second screen member capable of being connected with the first screen member and fitted on the outside of the first screen member, and the second screen member is tightly fitted on the outer side wall; the first and second screen members each have a bottom wall and a side wall extending upwardly from the bottom wall, the bottom wall of the first screen member being spaced from the bottom wall of the second screen member longitudinally of the reactor assembly.
Preferably, the taking and placing part comprises an inner peripheral wall, an outer peripheral wall and an annular bottom wall, wherein the inner peripheral wall, the outer peripheral wall and the annular bottom wall are coaxially arranged, and the annular bottom wall is connected with the bottom ends of the inner peripheral wall and the outer peripheral wall.
Preferably, the annular bottom wall and the outer bottom wall are arranged at intervals along the longitudinal direction of the reactor assembly so as to place the sample to be tested in the constant-temperature area in the space.
Preferably, the reactor component comprises an air inlet pipe and a gas distributor which is arranged in the space and positioned below the taking and placing component, one end of the air inlet pipe is used for being communicated with an air source, and the other end of the air inlet pipe extends into the gas distributor.
The invention also provides a thermal gravimetric device which comprises the reactor assembly, a heating device for heating the container and a weighing device connected with the container, wherein the container is suspended below the weighing device.
Preferably, the heating device comprises a first heating device arranged around the outer side wall and a second heating device fixedly connected with the first heating device and arranged on the inner side of the inner side wall.
Preferably, the heating means comprises a third heating means disposed spaced below the outer sole wall.
The reactor component for the thermogravimetric equipment provided by the invention can be suitable for the situation of processing a large amount of samples, in the reaction, the solid samples are in a thin layer state in the container, so that the solid samples are completely contacted with gas, the reaction is sufficient, and in addition, because the hanging basket is not adopted for containing the samples to be measured, the problem of inaccurate measurement caused by buoyancy generated by the rising of the gas to the hanging basket in the prior art is solved.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic diagram of a prior art thermogravimetric reactor for large sample testing.
FIG. 2 is a schematic diagram of a prior art high temperature reactor for a thermogravimetric reactor used for large sample testing.
Fig. 3 is a schematic front view of a thermal gravimetric device provided by an embodiment of the present invention.
Fig. 4 is a schematic front view of a portion of a thermal gravimetric device in accordance with an embodiment of the present invention.
Fig. 5 is a top view (partially in section) of a thermal gravimetric apparatus provided by an embodiment of the present invention.
Fig. 6 is an experimental data curve (TG curve) of an embodiment of the present invention.
Description of the reference numerals
1: an electric heating furnace; 2: a high temperature reactor;
2-1: an inner tube; 2-11: a pipe body;
2-12: an expansion head; 2-2: an outer tube;
2-2A: a reaction atmosphere inlet; 3: a hydraulic lifting platform;
4: a sealing box; 4-1: a protective atmosphere gas inlet;
4-2: a partition plate; 5: a weighing sensor;
7: connecting the clamping sleeve; 10: a boom;
11: a container; 12: an outer sidewall;
13: a space; 14: an air outlet;
15: an air inlet; 16: an outer bottom wall;
17: an inner sidewall; 18: an inner bottom wall;
21: a first heating device;
22: a second heating device; 23: a third heating device;
30: a weighing device; 40: a pick-and-place component;
41: a first screen member; 42: a second screen member;
50: a gas distributor; 61: a first thermocouple;
62: a second thermocouple; 70: a bolt;
80: an air inlet pipe; a: the gas outflow direction;
b: the gas inflow direction.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
In the present invention, the use of directional terms such as "upper, lower, left, right" generally means upper, lower, left, right as viewed with reference to the accompanying drawings, unless otherwise specified; "inner and outer" refer to the inner and outer relative to the profile of the components themselves.
Based on the problems that the measurement is inaccurate due to the buoyancy generated by the rising of the gas to the hanging basket and the contact between the gas and the solid sample is incomplete in the thermogravimetric reactor in the prior art, the invention provides a reactor assembly for the thermogravimetric equipment and the thermogravimetric equipment, and aims to solve the technical problems. The reactor assembly and the thermal graving apparatus will be described in detail below with reference to the accompanying drawings.
Embodiment mode 1
Referring to fig. 3 as appropriate, in the present embodiment, the reactor assembly for a thermal gravimetric system provided by the present invention comprises a vessel 11 having at least two walls, the space 13 between adjacent walls of the vessel 11 being closable and serving to house a sample to be tested.
Compared with the prior art, the place for placing the sample to be measured in the invention is completely different from the prior art, the sample to be measured can be placed in the space 13 in a lamellar mode by adopting the container 11 comprising at least two layers of walls, the problem of incomplete contact of gas and solid samples caused by stacking the samples to be measured like the prior art is avoided, and meanwhile, the problem of inaccurate measurement caused by buoyancy generated by rising of the gas to a hanging basket in the prior art is avoided because the structure of the reactor component in the invention is different from the prior art. Moreover, the reactor assembly of the present invention can be adapted to handle larger sample volumes.
As described above, the walls of the container 11 are at least double-walled, and the space between adjacent walls can be used as a place for placing the sample to be measured. For convenience in describing the present invention, the present invention will be described hereinafter in the case where the wall of the container 11 is a double wall.
Wherein the vessel 11 comprises an outer bottom wall 16, an outer side wall 12 extending upwardly from the outer bottom wall 16 and an inner side wall 17 located inside the outer side wall, the inner side wall 17 and the outer side wall 12 being spaced apart in a direction perpendicular to the longitudinal direction of the reactor assembly to form at least a part of the space 13.
In particular, as a specific realization of this embodiment, the vessel 11 further comprises an inner bottom wall 18, the inner bottom wall 18 is located at the bottom of the inner side wall 17 and is fixedly connected with the inner side wall 17, the inner bottom wall 18 and the outer bottom wall 16 are arranged at a distance along the longitudinal direction of the reactor assembly to form at least a part of the space 13, and it can be understood that the space formed by the vessel 11 is in this case concave in shape along the longitudinal section of the reactor assembly. At this time, the inner side wall 17 and the outer side wall 12 of the container 1 may be connected by a rigid means, for example, the inner side wall 17 and the outer side wall 12 may be connected by a flange (for example, the flange and the inner side wall 17 and the outer side wall 12 may be connected by a bolt 70), and the flange is disposed at the top of the container 11 to close the space 13 from the top, wherein the flange and the container 11 may be sealed by a sealing gasket, for example, a graphite gasket.
Wherein the shape of the outer side wall 12 and the inner side wall 17 of the container 11 can have various forms, such as square, rectangle, etc. In the present embodiment, the outer side wall 12 and the inner side wall 17 of the container 11 are each formed in a cylindrical structure, and an annular space between the outer side wall 12 and the inner side wall 17 is formed as at least a part of the space 13. Wherein, the container 11 can be made of 06Cr17Ni12Mo2 material, the outer sidewall 12 of the container 11 can form a cylindrical structure with a specification of phi 150 × 500mm, and the inner sidewall 17 can form a cylindrical structure with various specifications, typically phi 120 × 470mm, and a volume of 3.1L; phi 130 multiplied by 475mm, volume of 2.13L; phi 140X 480mm, and a volume of 1.1L. Typically, the container 11 has a constant temperature section of 220mm, the filling height during the actual experiment is about 200mm, and the effective filling volumes of the three typical containers 11 are 1.23L, 0.85L and 0.44L respectively. In practical cases, containers 11 of different sizes may be selected according to the different properties of the material (i.e. the sample to be tested).
In order to facilitate taking and placing of the sample to be measured and to facilitate adjusting the position of the sample to be measured, the reactor assembly includes a taking and placing component 40 capable of being placed in the space 13, and the taking and placing component 40 is used for enabling the sample to be measured to be in or leave a constant temperature area in the space 13. Specifically, the sample may be placed in the taking and placing part 40 before the reaction, and then the taking and placing part 40 with the sample placed therein may be placed in the space 13. Of course, it is also possible to place the sample directly in the space 13 of the container 11, for example, in the case of a very fine powder of the sample to be measured, in the space 13, it being understood that no gas distributor (see below) is provided here. Preferably, the taking and placing component 40 is a screen component with a hole structure to allow gas to pass through, and the size of the hole can be selected according to actual conditions.
In order to greatly reduce the heat transfer resistance and thus make the temperature distribution more uniform, as shown in fig. 4 and 5, the screen members include a first screen member 41 closely fitted over the inner side wall 17 and a second screen member 42 capable of being connected to the first screen member 41 and fitted over the first screen member 41, and the second screen member 42 closely fits to the outer side wall 12, because if the screen member does not fit to the container 11, gas exists between the container 11 and the screen member, thereby increasing the heat transfer resistance and making the temperature distribution non-uniform. In addition, the first screen member 41 and the second screen member 42 each have a bottom wall and a side wall extending upward from the bottom wall, wherein the bottom wall of the first screen member 41 and the bottom wall of the second screen member 42 are spaced apart in the longitudinal direction of the reactor assembly, that is, in this case, the pick-and-place member 40 has a concave shape in a section along the longitudinal direction of the reactor assembly. When the outer side wall 12 and the inner side wall 17 of the container 11 are formed in a cylindrical structure, the first screen member 41 and the second screen member 42 may be correspondingly provided in a cylindrical shape, and for example, the screen members may be woven using a screen having a mesh smaller than the particle size of the sample.
Of course, as a modified structure of the present embodiment, the taking and placing part 40 may include an inner peripheral wall, an outer peripheral wall, and an annular bottom wall connecting bottom ends of the inner peripheral wall and the outer peripheral wall, which are coaxially disposed. That is, in this case, the pick-and-place means 40 has a ring shape in a cross section perpendicular to the longitudinal direction of the reactor assembly. Wherein, in this variant, the annular bottom wall and the outer bottom wall 16 are arranged at a distance along the longitudinal direction of the reactor assembly, so as to place the sample to be tested in a constant temperature zone in the space 13.
In order to be able to provide gas in case of reaction requiring carrier gas or some reaction gas, the reactor assembly comprises a gas inlet tube 80 and a gas distributor 50 (it is understood that in the present embodiment, the gas distributor 50 is a cylindrical structure) arranged in the space 13 and below the pick-and-place part 40, one end of the gas inlet tube 80 is used for communicating with a gas source, and the other end of the gas inlet tube 80 extends into the gas distributor 50, wherein the gas inlet tube 80 may extend into the gas distributor 50 at a distance of 5-10mm from the outer bottom wall of the container 11, and the gas distributor 50 may be arranged at a distance of 15mm from the outer bottom wall of the container 11. The reaction gas can enter the gas inlet pipe 80 through the gas inlet 15 of the container 11 along the gas inflow direction B in fig. 4, and rises from the gas distributor 50 to participate in the reaction after being preheated, so that the gas is uniformly distributed, the measurement error caused by the gas flow disturbance is reduced, and after the reaction, the residual gas or the gas generated by the reaction flows out along the gas outflow direction a. Preferably, the gas inlet tube 80 is located outside the pick-and-place part 40, so that the gas inlet tube 80 is not directly contacted with the sample, thereby avoiding the problem of quality measurement error caused by temperature variation of the reaction gas, that is, inaccurate measurement caused by temperature variation of the reaction gas if the gas is directly introduced into the sample without preheating. In addition, the gas source can comprise a gas distribution system such as carbon dioxide, carbon monoxide and nitrogen, so that gasification and activation of the thermo-gravimetric reaction can be performed.
In order to ensure the measurement accuracy, the air inlets 15 and the air outlets 14 of the container 11 are both provided in an even number and are symmetrically arranged on the top of the container 11, and the air inlets 15 are communicated with the air inlet pipe 80. For example, as shown in fig. 5, the top of the container 11 is uniformly and symmetrically provided with two air inlets 15 and two air outlets 14, which ensures that possible fine shaking of the container 11 is reduced in both directions, thereby ensuring the accuracy of the measurement.
According to another aspect of the invention, there is also provided a thermal gravimetric system comprising the reactor assembly, heating means for heating the vessel 11 and weighing means 30 connected to the vessel 11, the vessel 11 being suspended below the weighing means 30.
In the prior art, when the processed sample amount is larger, a larger temperature gradient exists inside and outside the sample, and particularly, the phenomenon of temperature nonuniformity of the sample is more obvious under the condition of higher temperature rising rate. In view of this, the heating device of the thermogravimetric apparatus provided by the present invention includes a first heating device 21 surrounding the outer sidewall 12 and a second heating device 22 fixedly connected to the first heating device 21 and disposed inside the inner sidewall 17, so that the samples at different positions are heated by the first heating device 21 and the second heating device 22, respectively, thereby reducing the temperature gradient of the samples at different positions and making the temperature distribution uniform.
In order to ensure that the weighing device 30 can smoothly collect data of weight change of the container 11, a first gap exists between the outer side wall 12 of the container 11 and the first heating device 21, and a second gap exists between the inner side wall 17 of the container 11 and the second heating device 22, wherein the first gap and the second gap can be between 5mm and 10 mm. Further, to expand the applicability of the thermal gravimetric device provided by the present invention, the heating means comprises third heating means 23 disposed at intervals below the outer bottom wall 16. It will be appreciated that when the third heating means 23 are provided, the bottom of the pick-and-place unit is preferably located at a distance from the outer bottom wall 16 of the container 11, reaching the thermostatic zone.
In addition, in order to realize automatic control, the thermogravimetric equipment in the present invention comprises a controller and a display electrically connected to the controller, wherein the controller is used for being electrically connected to the air source, the first heating device 21, the second heating device 22 and the third heating device 23 respectively. It will be appreciated that the thermogravimetric apparatus of the present invention also includes product separation means to separate the products. The working temperature of the heating device in the invention can reach 1100 ℃ (effective constant temperature region), and different temperature-raising programs are set in the controller to provide temperature-controlling modes (such as temperature-raising speed, constant temperature section, final temperature, atmosphere and the like) of various programs for sample reaction, so that samples at different positions can reach the same temperature at the same time. In the whole reaction process, data such as temperature, quality, pressure, flow and the like can be displayed in real time through the display, so that drawing can be performed according to the data and the data can be recorded in the background, the recording frequency can be 1-600 s, and the adjustment can be performed according to actual conditions. In addition, the flow rate of the supplied gas may be controlled by a controller, so that different gases may be accurately supplied for the reaction.
Wherein, a first thermocouple 61 electrically connected with the controller is arranged in the first heating device 21 and/or the second heating device 22 (for example, the first thermocouple 61 is arranged near the side wall of the first heating device 21 and/or the second heating device 22 to monitor, record and control the wall temperature of the first heating device 21 and/or the second heating device 22 in real time), a second thermocouple 62 for detecting the temperature of the reaction sample in real time is arranged in the container 11 (for example, as shown in fig. 4, the second thermocouple 62 can be arranged in the middle of the sample to monitor and record the temperature of the central point of the sample in real time), and the second thermocouple 62 is electrically connected with the controller, so that the heat conducting performance of the sample can be examined by comparing the two temperature values. Generally, the first thermocouple 61 and the second thermocouple 62 measure in the range of 0 to 1300 ℃ with a measurement accuracy of 0.1 ℃.
In addition, the thermogravimetric equipment comprises a lifting device capable of horizontally rotating, and the lifting device is electrically connected with the controller, so that the mechanical automatic operation without human intervention can be realized, and the taking and the placing of the container 11 at the beginning and the end of the experiment are facilitated. The container 11 electric lifting device can be located at one side of the heating device, for example, the lifting mechanism can include a motor and a lifting screw rod connected with the container 11 (specifically, the container 11 can have a bracket, and the bracket is connected with the lifting screw rod), so that the motor can drive the lifting screw rod to drive the bracket of the container 11 to move, and then the container 11 is driven to lift up and down or rotate horizontally, and the automatic taking and placing of the high-temperature container 11 when the experiment is finished are facilitated.
The container 11 and the weighing device 30 may be connected in various manners, and in this embodiment, the container 11 is provided with a suspension member for suspending the container 11 below the weighing device 30 (for example, the suspension member may be a wire rope and a lifting lug, the lifting lug is fixed on the container, one end of the wire rope is connected with the lifting lug, and the other end of the wire rope is connected with the weighing device 30), and the weighing device 30 is electrically connected with the controller. For example, the weighing device can be an electronic balance, the measuring range of the electronic balance is 0-10 kg, and the measuring precision is 0.01 g. Further, the thermogravimetric apparatus includes a support plate for supporting the weighing device 30, which can horizontally rotate and horizontally move, so that the taking and placing of the container can be facilitated.
The invention will be verified by the following specific examples:
in this embodiment, thermogravimetric analysis is performed on a 500g coal sample, the particle size of raw coal is 3-6mm, the heating rate is 15 ℃/min, and the final temperature is 600 ℃, and the method is specifically realized by the following steps:
1) selecting a container 11 with the specification of an inner side wall 17 being 130 mm multiplied by 475mm, selecting a taking and placing part 40 with the hole size being 2mm, loading a sample into the taking and placing part 40, then placing the sample into an outer side wall 12 of the container 11, then placing the sample into the inner side wall 17, so that the taking and placing part 40 with the sample is positioned in the space 13, and finally connecting the inner side wall 17 and the outer side wall 12 through a flange and sealing the inner side wall 17 and the outer side wall 12 through a graphite gasket;
2) placing the container in the first heating device 21, connecting the air inlet pipe 80, and setting the first thermocouple 61 and the second thermocouple 62 according to the above to monitor, record and control the wall temperature of the first heating device 21 and the second heating device 22 and the temperature of the central point of the sample in real time;
3) the second heating device 22 is placed in the inner side wall 17 of the container 11 through an electric lifting device capable of horizontally rotating, and the position of the second heating device is finely adjusted through rotation, so that the inner side wall 17 is prevented from contacting with the second heating device 22; it should be noted that the second heating device 22 can be put in by the electric lifting device when the container 11 is installed and is not lifted;
4) suspending the container 11 below the weighing device 30 by means of a suspension loop or lifting lug and adjusting the position of the container 11 so as to avoid the container 11 coming into contact with the first heating device 21;
5) weighing the sample and the initial weight of the container 11 by a weighing device 30;
6) setting a temperature-raising program, a heating speed, a retention time, a final temperature and a flow rate of reaction gas by a controller;
7) starting the experiment, automatically heating the first heating device 21 and the second heating device 22 at a set speed, and recording the weight loss condition of the sample by a display until the experiment is finished and obtaining a TG curve and a temperature-time curve as shown in FIG. 6;
the test data in fig. 6 shows that the temperature programmed control of the thermogravimetric equipment of the present invention is accurate, and compared with the prior art, the TG curve is reasonable, so that the thermogravimetric equipment of the present invention can realize the thermogravimetric test of a large sample.
One of the differences between the present embodiment and embodiment 1 is that: the bottom of the inner side wall 17 is fixedly connected to the inner surface of the outer bottom wall 16, and it is also understood that the inner bottom wall 18 is coincident with the outer bottom wall 16, and in this case, the space 13 formed by the container 11 is only closed by an annular top cover, and meanwhile, in this embodiment, the gas distributor 50 may be in an annular structure. Of course, in the present embodiment, the pick-and-place unit 40 may have a concave shape in a section along the longitudinal direction of the reactor assembly, or the pick-and-place unit 40 may have a ring shape in a section perpendicular to the longitudinal direction of the reactor assembly.
Other features in this embodiment are similar or identical to those in embodiment 1 and will not be repeated here.
The thermogravimetric equipment provided by the invention can be suitable for the situation that the sample handling amount is large, in the reaction, the solid sample is in a thin layer state in the container 11 (specifically in the taking and placing component 40), so that the solid sample is completely contacted with the gas, the reaction is sufficient, and the heat transfer resistance is small because the taking and placing component 40 is closely attached to the space 13 of the container 11. Moreover, since the heating devices such as the first heating device and the second heating device are disposed outside and inside the container 11 in the present invention, the temperature gradient of the sample to be measured at different positions is extremely small, and the temperature distribution is uniform. In conclusion, the invention can realize the condition of the thermal weight loss change and the material heat conductivity of the large-mass sample under the conditions of different heating rates, different final temperatures, different heating processes and different gases (including nitrogen, carbon monoxide and carbon dioxide), is more close to the industrial actual process than the conventional common thermal weight device, and can better meet the requirement of the thermal weight loss analysis of the material in the technical industrial process.
The preferred embodiments of the present invention have been described in detail with reference to the accompanying drawings, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various features described in the above embodiments may be combined in any suitable manner without departing from the scope of the invention. The invention is not described in detail in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (10)
1. A reactor assembly for a thermal gravimetric system characterized in that it comprises a container (11) having at least two walls, the space (13) between adjacent walls of the container (11) being closable and intended for placing a sample to be measured; the vessel (11) comprising an outer bottom wall (16), an outer side wall (12) extending upwardly from the outer bottom wall (16) and an inner side wall (17) located inwardly of the outer side wall, the inner and outer side walls (17, 12) being spaced apart in a direction perpendicular to the longitudinal direction of the reactor assembly to form at least a part of the space (13); the vessel (11) further comprising an inner bottom wall (18), the inner bottom wall (18) being located at the bottom of the inner side wall (17) and being fixedly connected to the inner side wall (17), the inner bottom wall (18) and the outer bottom wall (16) being arranged at a distance longitudinally of the reactor assembly to form at least a part of the space (13);
the reactor assembly comprises a pick-and-place component (40) which can be placed in the space (13), wherein the pick-and-place component (40) is used for enabling a sample to be tested to be in or out of a constant temperature area in the space (13);
the taking and placing component (40) is a screen component with a hole structure;
the screen parts comprise a first screen part (41) which is tightly sleeved outside the inner side wall (17) in a fitting manner and a second screen part (42) which can be connected with the first screen part (41) and is sleeved outside the first screen part (41), and the second screen part (42) is tightly fitted with the outer side wall (12);
the first screen member (41) and the second screen member (42) each have a bottom wall and a side wall extending upwardly from the bottom wall, the bottom wall of the first screen member (41) and the bottom wall of the second screen member (42) being spaced longitudinally of the reactor assembly.
2. The reactor assembly for hot thermal plants according to claim 1, characterized in that it further comprises a flange for connecting the inner side wall (17) with the outer side wall (12) and closing the space (13) from the top.
3. The reactor assembly for thermal gravimetric plants according to claim 1, characterized in that a bottom portion of said inner side wall (17) is fixedly connected to an inner surface of said outer bottom wall (16).
4. The reactor assembly for thermal gravimetric plants according to claim 1, characterized in that said outer side wall (12) and said inner side wall (17) of said vessel (11) are both formed as a cylindrical structure, the annular space between said outer side wall (12) and said inner side wall (17) being formed as at least a part of said space (13).
5. The reactor assembly for thermal gravimetric plants according to claim 1, characterized in that said pick-and-place means (40) comprise an inner perimetral wall, an outer perimetral wall and an annular bottom wall connecting bottom ends of said inner and outer perimetral walls, arranged coaxially.
6. The reactor assembly for thermal gravimetric plants according to claim 5, characterized in that said annular bottom wall and said outer bottom wall (16) are arranged at a distance along the longitudinal direction of said reactor assembly to place said sample to be tested in a thermostatic zone in said space (13).
7. The reactor assembly for thermal gravimetric plants according to claim 1, characterized in that it comprises a gas inlet tube (80) and a gas distributor (50) arranged in said space (13) and located below said pick-and-place member (40), one end of said gas inlet tube (80) being intended to communicate with a gas source, the other end of said gas inlet tube (80) extending into said gas distributor (50).
8. A thermal gravimetric system characterized in that it comprises a reactor assembly according to any one of claims 1 to 7, heating means for heating said containers (11) and weighing means (30) connected to said containers (11), and in that the containers (11) are suspended below said weighing means (30).
9. The thermal gravimetric device by claim 8, characterized in that said heating means comprise first heating means (21) arranged around said outer lateral wall (12) and second heating means (22) fixedly connected to said first heating means (21) and arranged inside said inner lateral wall (17).
10. The thermal gravimetric apparatus by claim 8 or 9, characterized in that said heating means comprise third heating means (23) arranged spaced below said outer bottom wall (16).
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| CN113433022B (en) * | 2021-05-21 | 2022-05-31 | 中国科学院金属研究所 | Thermogravimetric analysis system capable of realizing high-precision initial-stage stable measurement |
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Address after: 100011 Beijing Dongcheng District, West Binhe Road, No. 22 Patentee after: CHINA ENERGY INVESTMENT Corp.,Ltd. Patentee after: Beijing low carbon clean energy research institute Address before: 100011 Shenhua building, 22 West Binhe Road, Dongcheng District, Beijing Patentee before: SHENHUA GROUP Corp.,Ltd. Patentee before: Beijing low carbon clean energy research institute |