Pyrolysis analyzer for chemical experiment and working method

Abstract

The invention relates to the field of chemical experiment equipment, in particular to a pyrolysis analyzer for chemical experiments and a working method.The pyrolysis analyzer comprises a chemical reaction box and a controllable heating furnace arranged in the chemical reaction box, and an observation window and a door for containing samples are arranged on the side face of the chemical reaction box; a central computer is integrally arranged in the chemical reaction box, the central computer is responsible for collecting, analyzing and processing data in the controllable heating furnace, a rotary worktable for placing a sample and an auxiliary heating mechanism are arranged in the controllable heating furnace, and the sample is uniformly heated in all aspects through the auxiliary heating mechanism. And a weight sensor is integrated in the rotary worktable. The technical problem that a sample is not fully subjected to thermal decomposition, oxidation reduction and adsorption desorption due to non-uniform heating of the sample in the chemical experiment process of an existing pyrolysis analyzer is solved.

Description

Technical Field

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

[0002] The pyrolysis analyzer is an instrument used to analyze the mass change of materials under program-controlled temperature. Its working principle is to study the thermal stability and composition of materials by observing the changes in the mass of samples with temperature or time during the process of heating, constant temperature or cooling. During use, the sample is placed in a temperature-controlled furnace. As the temperature changes, the sample will undergo thermal decomposition, oxidation-reduction, adsorption-desorption and other reactions, causing its mass to change. 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 of Chinese patent application No. 201910304010.7 discloses a thermal analyzer with low-temperature adsorption function, including an axial flow fan, a radiator, an insulation box, a refrigeration sheet, a cold storage sheet, a six-way valve, a drive 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. The axial flow fan is provided with a radiator, and the axial flow fan is provided with an insulation box. The insulation box is provided with a refrigeration sheet and a cold storage sheet, and the cold storage sheet is provided on the refrigeration sheet. A thermal analyzer with low-temperature adsorption function is made by adopting the above technical scheme. The secondary thermal analysis technology is used to make the peak shape sharper and improve the detection limit. Since the secondary analysis device has the advantages of small size, low-temperature concentration and rapid heating, the system error is reduced, the unit concentration is increased, and the detection limit is greatly improved. The technical solution proposed by the above invention improves the detection limit and reduces the system error through the improvement of structure and components, but in actual use, it is difficult to achieve uniform heating due to the different sample forms, that is, the processes of thermal decomposition, oxidation-reduction, adsorption analysis, etc. will be affected. Summary of the invention

[0004] Therefore, in response to the above problems, the present invention proposes a pyrolysis analyzer and a working method for chemical experiments, which solves the technical problem that the existing pyrolysis analyzer heats the sample unevenly during the chemical experiment, resulting in insufficient thermal decomposition, oxidation-reduction and adsorption analysis of the sample.

[0005] To achieve the above-mentioned purpose, the present invention adopts the following technical scheme: a pyrolysis analyzer for chemical experiments, comprising 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 entry 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 entry and exit door and the controllable heating furnace are interconnected, the controllable heating furnace is provided with a rotating workbench and an auxiliary heating mechanism for placing samples, the samples are heated uniformly in all aspects by the auxiliary heating mechanism, and a weight sensor is integrated in the rotating workbench.

[0006] Furthermore, anti-vibration feet are arranged on the four corners of the lower bottom surface of the chemical reaction box.

[0007] Furthermore, the rotating worktable can rotate 360° along its own axis, and the rotation method is to rotate at a constant speed driven by a motor.

[0008] Furthermore, 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. 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, and the first electric heating rod is arranged in a state perpendicular to the horizontal plane. The second electric heating rod can rotate along its own midpoint, and a circulating airflow is generated during the rotation.

[0009] Furthermore, the auxiliary heating mechanism includes a third electric heating rod arranged at the center position 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. 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.

[0010] Furthermore, 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 axial 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.

[0011] Furthermore, 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: S1. Sample placement: Place the sample to be tested on the tilt adjustment device on the rotating workbench through the access door; 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; 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.

[0015] By adopting the above technical solution, the beneficial effects of the present invention are: 1. The present invention improves and innovates the sample fixation and heating in the controllable heating furnace, thereby ensuring that the pyrolysis analyzer can achieve the change of sample shape and the shape of the heating device during use. Through the combination of the two, the sample is heated evenly during pyrolysis analysis, thereby achieving a more accurate analysis data effect. Specifically, the present invention is provided with a rotating worktable in the controllable heating furnace. During operation, the rotating worktable rotates 360° along its own axis to drive the workpiece to rotate, thereby achieving preliminary all-round uniform heating. At the same time, the present invention is provided with an auxiliary heating mechanism to cooperate with the work.

[0016] 2. In the present invention, anti-seismic feet are provided at the bottom surface of the chemical reaction box. The purpose of providing the anti-seismic feet is to prevent the vibration generated during the operation of the equipment itself from being transmitted to the ground and causing the equipment to shift, and to prevent the vibration generated by the ground from being transmitted to the equipment and causing deviations in chemical test results.

[0017] 3. In the present invention, a constant temperature heating device is provided in the controllable heating furnace. The constant temperature heating device can maintain a specified temperature in the controllable heating furnace at a constant temperature, thereby meeting the constant temperature pyrolysis requirement for the sample. The constant temperature heating device includes a first electric heating rod and a second electric heating rod. The first electric heating rod serves as a main heating structure and plays a main heating effect, while the second electric heating rod is arranged to rotate. During the self-heating process, airflow is generated during the rotation, and the generated airflow further drives the hot airflow in the controllable heating furnace to circulate. On the one hand, the pyrolysis efficiency is improved, and on the other hand, the temperature of each area in the controllable heating furnace is ensured to be constant.

[0018] 4. The present invention is provided with an auxiliary heating mechanism, wherein the auxiliary heating mechanism mainly achieves the optimal effect of uniform heating through the cooperation between 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 to position the sample inside and outside, and the movable support column arranged in the first annular support ring and the second annular support ring is mainly used to provide support for the sample. The movable support column can be lifted up and down in the vertical direction, and can drive the sample to tilt during the lifting and lowering process. 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, in order to ensure that there will be no interference when the sample is driven to tilt by the movable support column. 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 there will be no interference when the sample is tilted. At the same time, each movable support column in the present invention has independent up and down lifting activities, which ensures that the angle and state of the sample are more controllable during the tilting process.

[0019] 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.

[0020] 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

[0021] 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: Figure 1 It is a schematic diagram of the overall structure of the present invention; Figure 2 for Figure 1 Enlarged view of point A in the middle; Figure 3 It is a schematic diagram of the front structure of the present invention; Figure 4 It is a schematic diagram of the internal structure of the present invention; Figure 5 This is a schematic diagram of the top view of the rotary table of the present invention; Figure 6 for Figure 5 Section view at BB in the middle; Figure 7 It is a schematic diagram of the structure of the rotating disk in the present invention when viewed from above; Figure 8 It is a flow chart of the working method in the present invention. DETAILED DESCRIPTION

[0022] In order to make the technical means, creative features, objectives and effects achieved by the present invention easy to understand, the present invention is further explained below in conjunction with specific implementation methods.

[0023] See also Figure 1-Figure 8The present invention provides a pyrolysis analyzer for chemical experiments, comprising a chemical reaction box 1 and a controllable heating furnace 2 arranged in the chemical reaction box 1, an observation window 3 and an entrance door 4 for placing samples are arranged on the side of the chemical reaction box 1, a central computer is integrated in the chemical reaction box 1, the central computer is responsible for collecting and analyzing the data in the controllable heating furnace 2, an electronic display screen 11 is arranged on the chemical reaction box 1, the electronic display screen 11 is electrically connected to the central computer and is responsible for data display, the entrance door 4 and the controllable heating furnace 2 are interconnected, a rotating workbench 6 and an auxiliary heating mechanism for placing samples are arranged in the controllable heating furnace 2, the samples are uniformly heated in all aspects by the auxiliary heating mechanism, a weight sensor 61 is integrated in the rotating workbench 6, and in this embodiment, a double-station structure is used, that is, there are two identical stations for sample pyrolysis, and the data are displayed on the electronic display screen 11 respectively, and the two stations are exactly the same; The chemical reaction box 1 is provided with anti-vibration feet 5 at the four corners on the bottom surface thereof, wherein the anti-vibration feet 5 provide a shock absorbing effect by means of built-in high-strength springs, and its structure is well known and will not be described in detail here.

[0024] The rotating workbench 6 can rotate 360° along its own axial direction, and the rotation method is to rotate at a uniform speed through a motor drive. A constant temperature heating device is arranged in the controllable heating furnace 2, and the constant temperature heating device is arranged 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 in a state perpendicular to the horizontal plane. The second electric heating rod 22 can rotate along its own midpoint, and a circulating airflow is generated during the rotation. The generated airflow drives the heat flow in the controllable heating furnace 2 to circulate, thereby ensuring that the controllable heating furnace 2 maintains constant temperature heating.

[0025] The auxiliary heating mechanism includes a third electric heating rod 71 arranged at the center of the rotating worktable, a tilt adjustment device 72 arranged on the rotating worktable 6, and a tilt heating device 73 arranged on the top surface of the controllable heating furnace 2. The tilt adjustment device 72 is used to adjust the tilt angle of the sample, and the tilt heating device 73 is used to uniformly heat the inside of the sample. The tilt adjustment device 72 includes a first annular support ring 721, a second annular support ring 722, and a plurality of movable support columns 723 arranged 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 arranged around the third electric heating rod 71, and the first annular support ring 721 and the second annular support ring 722 are arranged concentrically. The movable support column 723 can be lifted up and down along its own axis direction, and its lifting and lowering mode is driven by a driving motor. The lifting and lowering of each movable support column 723 are independent of each other. The height of the first annular support ring 721 in the vertical direction is lower than the height of the second annular support ring 722, and the difference between the two is 5 cm.

[0026] The inclined heating device 73 includes a rotating disk 731 arranged on the top surface of the controllable heating furnace 2, and a fourth electric heating rod 732 rotatably arranged on the rotating disk 731. The rotating disk 731 can rotate 360° along its own axial direction, and the fourth electric heating rod 732 rotates along with the rotating disk 731. The fourth electric heating rod 732 can move horizontally in the horizontal direction, approaching or moving away from the center of the rotating disk 731. In the vertical direction, the fourth electric heating rod 732 can be extended and retracted up and down along its own axial direction, approaching or moving away from the rotating workbench 6. The free end of the third electric heating rod 71 is provided with an arc-shaped receiving portion 711, and the free end of the fourth electric heating rod 732 is provided with a sliding ball 7321, and the sliding ball 7321 cooperates with the arc-shaped receiving portion 711.

[0027] This embodiment simultaneously proposes a working method of the above-mentioned pyrolysis analyzer, a working method of a pyrolysis analyzer for chemical experiments, comprising the following steps: S1, sample placement; placing the sample to be tested on the tilt adjustment device 72 on the rotating workbench 6 through the access door 4; S2, sample position adjustment; adjust the movable support column 723, so that each movable support column 723 is in the same horizontal plane and the horizontal height is lower than the first annular support ring 721, and align the ring opening of the sample with the movable support column 723 for placement; S3, heating and pyrolysis: the equipment starts to heat and pyrolyze the sample; S3.1, initial pyrolysis; the first electric heating rod 21 and the second electric heating rod 22 are powered on for heating, wherein the second electric heating rod 22 rotates synchronously during the heating process, so that the hot air flow in the controllable heating furnace 2 circulates; S3.2, re-pyrolysis; the fourth electric heating rod 732 moves downward to the end to cooperate with the third electric heating rod 71, and at the same time the rotating disk 731 starts to rotate, and the fourth electric heating rod 732 follows the rotation, and the horizontal position of the fourth electric heating rod 732 is adjusted, intermittently approaching or moving away from the center of the rotating disk 731, at this time the movable support column 723 is raised and lowered to make the sample tilted at different angles, and cooperates with the fourth electric heating rod 732 to perform uniform pyrolysis on the inside of the sample; S4. Data analysis.

[0028] The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention. It is obvious to those skilled in the art that the present invention is not limited to the details of the above exemplary embodiments, and the present invention can be implemented in other specific forms without departing from the spirit or basic features of the present invention. Therefore, no matter from which point of view, the embodiments should be regarded as exemplary and non-restrictive. The scope of the present invention is defined by the attached claims rather than the above description, and it is intended that all changes falling within the meaning and scope of the equivalent elements of the claims are included in the present invention. Any figure mark in the claims should not be regarded as limiting the claims involved.

[0029] In addition, it should be understood that although the present specification is described according to implementation modes, not every implementation mode contains only one independent technical solution. This description of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment may also be appropriately combined to form other implementation modes 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. 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, and the first electric heating rod is arranged in a state perpendicular to the horizontal plane. The second electric heating rod can rotate along its own midpoint, and a circulating airflow is generated during the rotation.

2. A pyrolysis analyzer for chemical experiments according to claim 1, characterized in that: The auxiliary heating mechanism includes a third electric heating rod arranged at the center position 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. 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.

3. A pyrolysis analyzer for chemical experiments according to claim 2, characterized in that: 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.

4. A pyrolysis analyzer for chemical experiments according to claim 3, 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.

5. A pyrolysis analyzer for chemical experiments according to claim 4, 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.

6. A pyrolysis analyzer for chemical experiments according to claim 5, 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.

7. A working method, using the pyrolysis analyzer for chemical experiments as claimed in claim 6, 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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