A pyrolysis analyzer for chemical experiments and its working method

Abstract

The present invention relates to the field of chemical experimental equipment, and particularly to a pyrolysis analyzer and a working method for chemical experiments, including a chemical reaction chamber and a controllable heating furnace arranged in the chemical reaction chamber. An observation window and an access door for placing samples are arranged on the side of the chemical reaction chamber. A central computer is integrally arranged in the chemical reaction chamber, and the central computer is responsible for collecting and analyzing data in the controllable heating furnace. A rotary workbench for placing samples and an auxiliary heating mechanism are arranged in the controllable heating furnace, and the auxiliary heating mechanism is used to perform a full - aspect and uniform heating operation on the samples. A weight sensor is integrated in the rotary workbench, which solves the technical problems that in the process of chemical experiments with existing pyrolysis analyzers, the samples are unevenly heated, resulting in insufficient thermal decomposition, redox, and adsorption - desorption processes of the samples.

Description

Technical Field

[0001] The present invention relates to the field of chemical experimental equipment, and particularly to a pyrolysis analyzer and a working method for chemical experiments. Background Art

[0002] A pyrolysis analyzer is an instrument used to analyze the mass change of materials under programmed temperature control. Its working principle is to observe the change of the sample's mass with temperature or time during the heating, constant temperature, or cooling process to study the thermal stability and components of the material. During use, the sample is placed in a furnace with controllable temperature. As the temperature changes, the sample will undergo pyrolysis, redox, adsorption and desorption reactions, resulting in a change in its mass. The instrument measures the mass change of the sample in real time through a high-precision balance and records the corresponding temperature and time information to obtain a thermogravimetric curve. By analyzing the sample through the thermogravimetric curve, the thermal stability, decomposition temperature, reaction kinetic parameters, etc. of the material can be determined.

[0003] The invention patent with the Chinese patent application number 201910304010.7 discloses a thermal desorption analyzer with a low-temperature adsorption function, including an axial flow fan, a radiator, a heat preservation box, a refrigeration sheet, a cold storage sheet, a six-way valve, a driving motor, a carrier gas flow controller, a secondary adsorption tube, a primary adsorption tube, a primary heating body, a purge gas flow controller, a vent pipe, a detection device, and a heating wire. A radiator is provided on the axial flow fan, a heat preservation box is provided on the axial flow fan, a refrigeration sheet and a cold storage sheet are provided in the heat preservation box, and the cold storage sheet is arranged on the refrigeration sheet. The above technical solution is used to make a thermal desorption analyzer with a low-temperature adsorption function. The use of the secondary thermal desorption technology makes the peak shape relatively sharp and improves the detection limit. Since the secondary desorption device has the advantages of small volume, low-temperature concentration, and rapid heating, the systematic error is reduced, the unit concentration increases, and the detection limit is greatly improved. The technical solution proposed by the above invention improves the detection limit and reduces the systematic error through the improvement of the structure and components. However, in the actual use process, it is difficult to achieve uniform heating due to the various shapes of the samples, that is, the processes of pyrolysis, redox, adsorption and desorption, etc. will all be affected. Summary of the Invention

[0004] Therefore, in view of the above problems, the present invention proposes a pyrolysis analyzer and a working method for chemical experiments, which solve the technical problem that the existing pyrolysis analyzer causes insufficient pyrolysis, redox, and adsorption and desorption processes of the sample due to uneven heating of the sample during the chemical experiment process.

[0005] To achieve the above object, the present invention adopts the following technical solutions: A pyrolysis analyzer for chemical experiments, comprising a chemical reaction chamber and a controllable heating furnace arranged inside the chemical reaction chamber. An observation window and an access door for placing samples are arranged on the side surface of the chemical reaction chamber. A central computer is integrally arranged inside the chemical reaction chamber, and the central computer is responsible for collecting and analyzing the data inside the controllable heating furnace. An electronic display screen is arranged on the chemical reaction chamber, and the electronic display screen is electrically connected to the central computer and is responsible for data display. The access door is in through connection with the controllable heating furnace. A rotating workbench for placing samples and an auxiliary heating mechanism are arranged inside the controllable heating furnace. The auxiliary heating mechanism performs a full - aspect and uniform heating operation on the samples, and a weight sensor is integrated inside the rotating workbench.

[0006] Further, anti - seismic feet are arranged at the four corners of the bottom surface of the chemical reaction chamber.

[0007] Further, the rotating workbench can rotate 360° along its own axis direction, and the rotation mode is uniform rotation driven by a motor.

[0008] Further, a constant - temperature heating device is arranged inside the controllable heating furnace. The constant - temperature heating device is arranged around the inner surface of the controllable heating furnace. The constant - temperature heating device includes a first electric heating rod and a second electric heating rod. The first electric heating rod and the second electric heating rod are arranged at intervals. The first electric heating rod is arranged in a state perpendicular to the horizontal plane, and the second electric heating rod can rotate around its own mid - point, generating a circulating air flow during the rotation process.

[0009] Further, the auxiliary heating mechanism includes a third electric heating rod arranged at the center position of the rotating workbench, an inclination adjustment device arranged on the rotating workbench, and an inclined heating device arranged on the inner top surface of the controllable heating furnace. The inclination adjustment device is used to adjust the inclination angle of the sample, and the inclined heating device is used to uniformly heat the inside of the sample.

[0010] Further, the inclination adjustment device includes a first annular support ring, a second annular support ring, and a plurality of movable support columns arranged between the first annular support ring and the second annular support ring. The first annular support ring and the second annular support ring are arranged around the third electric heating rod. The first annular support ring and the second annular support ring are concentrically arranged. The movable support columns can move up and down along their own axis directions, and their up - and - down movement modes are driven by a driving motor for lifting and lowering, and the lifting and lowering of each movable support column are independent of each other.

[0011] Further, in the vertical direction, the height of the first annular support ring is lower than the height of the second annular support ring, and the difference between the two is 3 - 5 cm.

[0012] Furthermore, the inclined heating device includes a rotating disk arranged on the top surface of the controllable heating furnace and a fourth electric heating rod rotatably arranged on the rotating disk. The rotating disk can rotate 360° along its own axial direction, and the fourth electric heating rod rotates along with the rotating disk. The fourth electric heating rod can move horizontally in the horizontal direction, approaching or moving away from the center of the rotating disk, and the fourth electric heating rod can extend and retract up and down along its own axial direction in the vertical direction, approaching or moving away from the rotating workbench.

[0013] Furthermore, an arc-shaped receiving portion is provided at the free end of the third electric heating rod, and a sliding ball is provided at the free end of the fourth electric heating rod, and the sliding ball cooperates with the arc-shaped receiving portion.

[0014] A working method, using a pyrolysis analyzer for chemical experiments, comprises the following steps:

[0015] S1. Sample placement: Place the sample to be tested on the tilt adjustment device on the rotating workbench through the access door;

[0016] S2, sample position adjustment; adjust the movable support column so that each movable support column is in the same horizontal plane and the horizontal height is lower than the first annular support ring, and align the ring opening of the sample with the movable support column for placement;

[0017] S3, heating and pyrolysis: the equipment starts to heat and pyrolyze the sample;

[0018] S3.1, initial pyrolysis; the first electric heating rod and the second electric heating rod are powered on for heating, wherein the second electric heating rod rotates synchronously during the heating process, so that the hot air flow in the controllable heating furnace circulates;

[0019] S3.2, re-pyrolysis; the fourth electric heating rod moves downward to the end to cooperate with the third electric heating rod, and the rotating disk starts to rotate, and the fourth electric heating rod rotates with it, and the horizontal position of the fourth electric heating rod is adjusted, intermittently approaching or moving away from the center of the rotating disk, at this time, the movable support column is raised and lowered to make the sample tilted at different angles, and cooperates with the fourth electric heating rod to evenly pyrolyze the inside of the sample;

[0020] S4. Data analysis.

[0021] By adopting the above technical solution, the beneficial effects of the present invention are:

[0022] 1. The present invention improves and innovates in two aspects: the fixation and heating of samples in a controllable heating furnace, ensuring that during the use of the pyrolysis analyzer, the shape of the sample and the shape of the heating device can be changed. By combining the two, the sample is evenly heated during pyrolysis analysis, thereby achieving more accurate analysis data. Specifically, the present invention is provided with a rotating workbench in the controllable heating furnace. During operation, the rotating workbench rotates 360° along its own axis to drive the workpiece to rotate, thus achieving preliminary omnidirectional uniform heating. At the same time, an auxiliary heating mechanism is provided in the present invention to cooperate with the work.

[0023] 2. In the present invention, anti-vibration feet are provided at the lower bottom surface of the chemical reaction box. The purpose of setting the anti-vibration feet is to prevent the vibration generated during the operation of the equipment itself from being transmitted to the ground, resulting in equipment displacement, and to prevent the vibration generated on the ground from being conducted to the equipment, resulting in deviation of chemical test results.

[0024] 3. In the present invention, a constant temperature heating device is provided in the controllable heating furnace. Through the constant temperature heating device, the constant temperature of the specified temperature in the controllable heating furnace can be maintained, meeting the requirement of constant temperature pyrolysis of the sample. The constant temperature heating device includes a first electric heating rod and a second electric heating rod. The first electric heating rod, as the main heating structure, plays a major heating effect. The second electric heating rod is rotatably arranged, and during its own heating process, it can synchronously rotate itself. During the rotation process, air flow will be generated, and the generated air flow will further drive the hot air flow in the controllable heating furnace to circulate. On the one hand, it improves the pyrolysis efficiency, and on the other hand, it ensures the temperature constancy in each area of the controllable heating furnace.

[0025] 4. In the present invention, an auxiliary heating mechanism is provided. The auxiliary heating mechanism mainly achieves the optimal effect of uniform heating through the mutual cooperation of the tilt adjustment device and the tilt heating device. The first annular support ring and the second annular support ring in the tilt adjustment device are used for internal and external positioning of the sample, and the movable support columns arranged in the first annular support ring and the second annular support ring are mainly used to provide support for the sample. The provided movable support columns can move up and down along the vertical direction, and can drive the sample to tilt during the up and down movement. At the same time, the gap distance between the first annular support ring and the second annular support ring is greater than the wall thickness of the sample itself, aiming to ensure that the sample will not interfere when driven by the movable support columns to tilt. In the present invention, the vertical height of the first annular support ring is lower than the vertical height of the second annular support ring, also to ensure that the sample will not interfere during the tilting process. At the same time, each movable support column in the present invention moves up and down independently, ensuring that the angle and state of the sample are more controllable during the tilting process.

[0026] 5. The inclined heating device in the present invention is matched with the inclined adjustment device, which can uniformly heat the inside of the sample. Specifically, the fourth electric heating rod moves downward to cooperate with the third electric heating rod. When the sample is rotated by the rotating worktable, the fourth electric heating rod also rotates with the rotation of the rotating disk, and the rotation direction of the fourth electric heating rod and the sample can be the same or opposite. The two work together to improve the pyrolysis efficiency on the one hand, and ensure uniform heating inside and outside the sample on the other.

[0027] 6. The end of the fourth electric heating rod in the present invention can move close to or away from the center of the rotating disk during the rotation process, ensuring that the vertical angle can be offset during the rotation to adapt to the deflection of the sample. In the present invention, an arc-shaped receiving portion is provided at the free end of the third electric heating rod, and a sliding ball is provided at the free end of the fourth electric heating rod. When the third electric heating rod and the fourth electric heating rod cooperate with each other, the friction force can be reduced when the two rotate relative to each other, making the rotation smoother. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Other features, objects and advantages of the present invention will become more apparent from the detailed description of non-limiting embodiments made with reference to the following drawings:

[0029] Figure 1 It is a schematic diagram of the overall structure of the present invention;

[0030] Figure 2 for Figure 1 Enlarged view of point A in the middle;

[0031] Figure 3 It is a schematic diagram of the front structure of the present invention;

[0032] Figure 4 It is a schematic diagram of the internal structure of the present invention;

[0033] Figure 5 This is a schematic diagram of the top view of the rotary table of the present invention;

[0034] Figure 6 for Figure 5 Section view at BB in the middle;

[0035] Figure 7 It is a schematic diagram of the structure of the rotating disk in the present invention when viewed from above;

[0036] Figure 8 It is a flow chart of the working method in the present invention. DETAILED DESCRIPTION

[0037] To make the technical means, creative features, achieved purposes and effects of the present invention easy to understand, the present invention will be further described below in conjunction with specific embodiments.

[0038] Please refer to Figures 1-8 , the present invention provides a pyrolysis analyzer for chemical experiments, including a chemical reaction chamber 1 and a controllable heating furnace 2 disposed in the chemical reaction chamber 1. An observation window 3 and an access door 4 for placing samples are provided on the side surface of the chemical reaction chamber 1. A central computer is integrally disposed in the chemical reaction chamber 1. The central computer is responsible for collecting and analyzing data in the controllable heating furnace 2. An electronic display screen 11 is provided on the chemical reaction chamber 1. The electronic display screen 11 is electrically connected to the central computer and is responsible for data display. The access door 4 and the controllable heating furnace 2 communicate with each other. A rotary worktable 6 for placing samples and an auxiliary heating mechanism are provided in the controllable heating furnace 2. The auxiliary heating mechanism performs a full - aspect and uniform heating operation on the sample. A weight sensor 61 is integrated in the rotary worktable 6. In this embodiment, it is a two - station structure, that is, there are two identical stations for sample pyrolysis, and the data are respectively displayed on the electronic display screen 11. The two stations are completely the same;

[0039] Anti - seismic feet 5 are provided at the four corners of the bottom surface of the chemical reaction chamber 1. Among them, the anti - seismic feet 5 provide shock - absorbing effects through built - in high - strength springs. Its structure is well - known and will not be elaborated here.

[0040] The rotary worktable 6 can rotate 360° along its own axis direction, and the rotation mode is uniform rotation driven by a motor. A constant - temperature heating device is provided in the controllable heating furnace 2. The constant - temperature heating device is disposed around the inner surface of the controllable heating furnace 2. The constant - temperature heating device includes a first electric heating rod 21 and a second electric heating rod 22. The first electric heating rod 21 and the second electric heating rod 22 are arranged at intervals. The first electric heating rod 21 is arranged perpendicular to the horizontal plane. The second electric heating rod 22 can rotate around its own mid - point. During the rotation process, a circulating air flow is generated, and the generated air flow drives the heat flow in the controllable heating furnace 2 to circulate, ensuring constant - temperature heating in the controllable heating furnace 2.

[0041] The auxiliary heating mechanism includes a third electric heating rod 71 disposed at the central position of the rotary table, an inclination adjusting device 72 disposed on the rotary table 6, and an inclined heating device 73 disposed on the inner top surface of the controllable heating furnace 2. The inclination adjusting device 72 is used to adjust the inclination angle of the sample, and the inclined heating device 73 is used to uniformly heat the inside of the sample. The inclination adjusting device 72 includes a first annular support ring 721, a second annular support ring 722, and a plurality of movable support columns 723 disposed between the first annular support ring 721 and the second annular support ring 722. The first annular support ring 721 and the second annular support ring 722 are disposed around the third electric heating rod 71, and the first annular support ring 721 and the second annular support ring 722 are concentrically arranged. The movable support columns 723 can be lifted and lowered along their own axial directions, and their up and down lifting methods are driven by a driving motor. The lifting and lowering of each movable support column 723 are independent of each other. Vertically, the height of the first annular support ring 721 is lower than the height of the second annular support ring 722, and the difference between the two is 5 cm.

[0042] The inclined heating device 73 includes a rotating disk 731 disposed on the inner top surface of the controllable heating furnace 2, and a fourth electric heating rod 732 rotatably disposed on the rotating disk 731. The rotating disk 731 can rotate 360° along its own axis direction, and the fourth electric heating rod 732 rotates following the rotation of the rotating disk 731. Horizontally, the fourth electric heating rod 732 can move horizontally, approaching or moving away from the center of the rotating disk 731. Vertically, the fourth electric heating rod 732 can be telescoped along its own axis direction, approaching or moving away from the rotary table 6. An arc-shaped receiving portion 711 is provided at the free end of the third electric heating rod 71, and a sliding ball 7321 is provided at the free end of the fourth electric heating rod 732. The sliding ball 7321 cooperates with the arc-shaped receiving portion 711.

[0043] This embodiment synchronously proposes a working method of the above pyrolysis analyzer. A working method of a pyrolysis analyzer for chemical experiments includes the following steps:

[0044] S1. Sample placement: Place the sample to be detected on the inclination adjusting device 72 on the rotary table 6 through the access door 4.

[0045] S2. Sample position adjustment: Adjust the movable support columns 723 so that all the movable support columns 723 are on the same horizontal plane and the horizontal height is lower than that of the first annular support ring 721, and place the sample with the ring opening aligned with the movable support columns 723.

[0046] S3. Heating and pyrolysis: Start the equipment to heat and pyrolyze the sample.

[0047] S3.1, Initial pyrolysis: The first electric heating rod 21 and the second electric heating rod 22 are energized for heating. During the self-heating process of the second electric heating rod 22, it rotates synchronously by itself, causing the internal hot air flow in the controllable heating furnace 2 to circulate.

[0048] S3.2, Re-pyrolysis: The fourth electric heating rod 732 moves downward to the end to cooperate with the third electric heating rod 71. At the same time, the rotating disk 731 starts to rotate, and the fourth electric heating rod 732 rotates accordingly. Moreover, the horizontal position of the fourth electric heating rod 732 is adjusted to approach or move away from the center of the rotating disk 731 intermittently. At this time, the movable support column 723 moves up and down to tilt the sample at different angles, and cooperates with the fourth electric heating rod 732 to pyrolyze the inside of the sample evenly.

[0049] S4, Data analysis.

[0050] The above has shown and described the basic principles, main features and advantages of the present invention. For those skilled in the art, it is obvious that the present invention is not limited to the details of the above exemplary embodiments, and without departing from the spirit or basic features of the present invention, the present invention can be implemented in other specific forms. Therefore, from any point of view, the embodiments should be regarded as exemplary and non-limiting. The scope of the present invention is defined by the appended claims rather than the above description. Therefore, all changes falling within the meaning and scope of the equivalent elements of the claims are intended to be included in the present invention. Any reference signs in the claims should not be regarded as limiting the claimed rights.

[0051] In addition, it should be understood that although this specification is described according to the embodiments, not every embodiment only contains an independent technical solution. This narrative way of the specification is only for clarity. Those skilled in the art should regard the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A pyrolysis analyzer for chemical experiments, characterized in that: It comprises a chemical reaction box and a controllable heating furnace arranged in the chemical reaction box, the side of the chemical reaction box is provided with an observation window and an entrance and exit door for placing samples, the chemical reaction box is integrated with a central computer, the central computer is responsible for collecting and analyzing the data in the controllable heating furnace, the chemical reaction box is provided with an electronic display screen, the electronic display screen is electrically connected to the central computer and is responsible for data display, the entrance and exit door and the controllable heating furnace are mutually connected, a rotating workbench and an auxiliary heating mechanism for placing samples are provided in the controllable heating furnace, the samples are uniformly heated in all aspects by the auxiliary heating mechanism, and a weight sensor is integrated in the rotating workbench; The chemical reaction box has anti-vibration feet arranged at the four corners on the bottom surface thereof; The rotating table can rotate 360° along its own axis, and the rotation mode is to rotate at a constant speed driven by a motor; A constant temperature heating device is arranged in the controllable heating furnace, and the constant temperature heating device is arranged around the inner surface of the controllable heating furnace, and the constant temperature heating device includes a first electric heating rod and a second electric heating rod, the first electric heating rod and the second electric heating rod are arranged at intervals, the first electric heating rod is arranged in a state perpendicular to the horizontal plane, and the second electric heating rod can rotate along its own midpoint, and a circulating airflow is generated during the rotation process; The auxiliary heating mechanism includes a third electric heating rod arranged at the center of the rotating worktable, a tilt adjustment device arranged on the rotating worktable, and a tilt heating device arranged on the top surface of the controllable heating furnace, wherein the tilt adjustment device is used to adjust the tilt angle of the sample, and the tilt heating device is used to uniformly heat the inside of the sample; The tilt adjustment device includes a first annular support ring, a second annular support ring, and a plurality of movable support columns arranged between the first annular support ring and the second annular support ring, the first annular support ring and the second annular support ring are arranged around the third electric heating rod, the first annular support ring and the second annular support ring are arranged concentrically, and the movable support column can be lifted up and down along its own axis direction, and the lifting and lowering method is driven by a driving motor, and the lifting and lowering of each movable support column is independent of each other.

2. A pyrolysis analyzer for chemical experiments according to claim 1, characterized in that: In the vertical direction, the height of the first annular support ring is lower than the height of the second annular support ring, and the difference between the two is 3-5 cm.

3. A pyrolysis analyzer for chemical experiments according to claim 2, characterized in that: The inclined heating device includes a rotating disk arranged on the top surface of the controllable heating furnace and a fourth electric heating rod rotatably arranged on the rotating disk. The rotating disk can rotate 360° along its own axial direction, and the fourth electric heating rod rotates along with the rotating disk. The fourth electric heating rod can move horizontally in the horizontal direction, approaching or moving away from the center of the rotating disk. In the vertical direction, the fourth electric heating rod can extend and retract up and down along its own axial direction, approaching or moving away from the rotating workbench.

4. A pyrolysis analyzer for chemical experiments according to claim 3, characterized in that: The free end of the third electric heating rod is provided with an arc-shaped receiving portion, and the free end of the fourth electric heating rod is provided with a sliding ball, and the sliding ball cooperates with the arc-shaped receiving portion.

5. A working method, using the pyrolysis analyzer for chemical experiments as claimed in claim 4, characterized in that: The following steps are involved: S1. Sample placement; Place the sample to be tested through the access door on the tilt adjustment device on the rotating workbench; S2, sample position adjustment; Adjust the movable support columns so that all movable support columns are on the same horizontal plane and their horizontal height is lower than the first annular support ring, and align the ring opening of the sample with the movable support column for placement; S3, heating and pyrolysis: the equipment starts to heat and pyrolyze the sample; S3.1, initial pyrolysis; the first electric heating rod and the second electric heating rod are powered on for heating, wherein the second electric heating rod rotates synchronously during the heating process, so that the hot air flow in the controllable heating furnace circulates; S3.2, re-pyrolysis; the fourth electric heating rod moves downward to the end to cooperate with the third electric heating rod, and the rotating disk starts to rotate, and the fourth electric heating rod rotates with it, and the horizontal position of the fourth electric heating rod is adjusted, intermittently approaching or moving away from the center of the rotating disk, at this time, the movable support column is raised and lowered to make the sample tilted at different angles, and cooperates with the fourth electric heating rod to evenly pyrolyze the inside of the sample; S4. Data analysis.

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