Mesophase pitch softening point measuring device
The device addresses inaccuracies in mesophase asphalt softening point determination by using a signal hole and ambient light detector to measure light intensity changes, ensuring precise and repeatable results in an inert gas environment.
Patent Information
- Application Number
- CN202420605581.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-03-27
- Publication Date
- 2024-12-13
- Estimated Expiration
- 2034-03-27
AI Technical Summary
Existing methods for determining the softening point of mesophase asphalt are inaccurate and prone to subjective errors due to oxidation and manual judgment, leading to poor repeatability.
A device that uses a signal hole and ambient light detector to detect light intensity changes when mesophase asphalt drips out during heating, eliminating the need for manual judgment and ensuring accurate measurement in an inert gas environment.
The device provides precise and repeatable softening point measurements by detecting light intensity changes, avoiding oxidation and subjective errors, thereby improving measurement accuracy and standardization.
Smart Images
Figure CN222166923U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of asphalt softening point testing, in particular to a mesophase asphalt softening point measuring device. Background Art
[0002] Mesophase pitch is a nematic liquid crystal material formed by high-temperature polymerization of aromatic hydrocarbons. It has the advantages of high carbon yield, high graphitization, and strong processability. There are many types of asphalt raw materials, and the common ones are petroleum asphalt, coal asphalt, and naphthalene asphalt. Mesophase pitch is an excellent raw material for preparing high-performance mesophase pitch-based carbon fibers. Carbon fiber is a fibrous material with a carbon content of more than 90% formed by carbonization and graphitization of organic polymers or asphalt-based materials. It is called the "king of new materials" because of its remarkable excellent properties such as high modulus, high strength, low density, chemical corrosion resistance, high temperature resistance and good fiber fineness. In the preparation process of carbon fiber, spinning temperature and pre-oxidation temperature are very critical process parameters. The determination of these two parameters needs to be based on the softening point temperature of the mesophase pitch. Therefore, it is necessary to accurately determine the softening point to provide a reference for the subsequent process.
[0003] The softening point of mesophase asphalt can be determined by referring to "GBT 4507-2014 Asphalt Softening Point Determination Method Ring and Ball Method" and "GBT2294-2019 Coking Solid Product Softening Point Determination Method". However, the softening point of mesophase asphalt is usually greater than 200°C. If the above two methods are used for determination, it cannot be accurately measured. One is because the temperature of the heating medium cannot reach the softening point temperature, and the other is that the asphalt sample is easily oxidized at high temperature. In this case, the measured softening point will be high. Utility model patent CN216792081 U introduces a test device for the softening point of high-softening-point mesophase asphalt. The principle is to heat it in an inert atmosphere and pierce the asphalt with a steel needle rod. When the asphalt becomes soft and begins to stick to the steel needle, the temperature at this time is recorded as the softening point. This method can provide a relatively high heating temperature while avoiding oxidation of the sample. However, the determination standard of the softening point temperature has certain subjective factors. Different operators may have different definitions of "soft" and "sticking", which may result in poor repeatability or inaccuracy of the obtained data.
[0004] It should be noted that the above introduction to the technical background is only for the convenience of providing a clear and complete description of the technical solutions of the present application and for the convenience of understanding by those skilled in the art. It cannot be considered that the above technical solutions are well known to those skilled in the art simply because they are described in the background technology section of the present application. Utility Model Content
[0005] The purpose of the utility model is to overcome the deficiencies of the prior art and to provide a device for determining the softening point of an intermediate phase asphalt. A signal hole and an ambient light detector corresponding to the signal hole are arranged below the sample cup. When the asphalt is heated and softened and drips out, the change in light intensity will be detected by the ambient light detector, thereby determining that the current temperature point is the softening point of the asphalt, thereby avoiding subjective errors in manual judgment.
[0006] In order to achieve the above-mentioned purpose, the utility model provides a device for determining the softening point of an intermediate phase asphalt, comprising a glove box, a heating device and a sample tube, the glove box being provided with a glove box door and operating gloves, and characterized in that the heating device is installed in the glove box, a sample bin corresponding to the sample tube is provided in the heating device, the sample tube comprises a tube body and a sample cup, the sample cup is fixedly or detachably connected in the cavity of the tube body, a signal hole is provided on the tube wall of the tube body, a small hole is provided at the bottom of the sample cup, the signal hole is arranged directly below the small hole, a through hole corresponding to the signal hole is provided in the sample bin, an ambient light sensor is provided in the through hole to monitor the change of the light signal in the signal hole, and a steel ball is movably provided in the sample cup.
[0007] Furthermore, one end of the glove box is fixedly connected to a transition cabin, the transition cabin communicates with the inner and outer sides of the glove box, and both ends of the transition cabin are hinged with cabin doors.
[0008] Furthermore, the transition cabin is connected to a vacuum pump.
[0009] Furthermore, the glove box and the transition cabin are respectively connected to inert gas cylinders through pipelines, and the pipelines are provided with stop valves.
[0010] Furthermore, a first pressure gauge is provided on the output port of the inert gas cylinder, and a second pressure gauge is provided on the transition cabin.
[0011] Furthermore, the glove box is connected to the liquid sealing tank through a pipeline.
[0012] Furthermore, the upper end of the tube body is fixedly or detachably connected to a handle.
[0013] The above solution of the utility model has the following beneficial effects:
[0014] The utility model provides a mesophase asphalt softening point measuring device. The entire asphalt softening point testing process is completed in a glove box in an inert gas environment. When testing high softening point asphalt, the sample will not be oxidized, and the softening point will not change due to oxidation.
[0015] The device sets a signal hole and an ambient light detector corresponding to the signal hole under the sample cup. When the asphalt is heated and softened and drips out, the ambient light detector will detect the change in light intensity. When the ambient light detector detects the change, it records the heating temperature, thereby recording the current temperature as the asphalt softening point. No manual auxiliary judgment is required, avoiding subjective errors in manual judgment, and improving the accuracy and standardization of measurement.
[0016] Other beneficial effects of the present invention will be described in detail in the subsequent specific implementation sections. BRIEF DESCRIPTION OF THE DRAWINGS
[0017] Figure 1 It is a schematic diagram of the overall structure of the utility model;
[0018] Figure 2 This is a cross-sectional view of the sample tube structure of the utility model.
[0019] [Description of Reference Numerals]
[0020] 1-glove box door; 2-glove box; 3-operating gloves; 4-heating device; 5-sample tube; 6-sample chamber; 7-transition chamber; 8-first stop valve; 9-cabin door; 10-vacuum pump; 11-first pressure gauge; 12-liquid seal tank; 13-inert gas cylinder; 14-handle; 15-steel ball; 16-sample cup; 17-signal hole; 18-tube body; 19-second pressure gauge. DETAILED DESCRIPTION
[0021] In order to make the purpose, technical scheme and advantages of the utility model clearer, the utility model is further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the utility model and are not used to limit the utility model. The various specific technical features and embodiments described in the specific implementation methods can be combined in any suitable manner without contradiction. For example, different implementation methods can be formed by combining different specific technical features / embodiments. In order to avoid unnecessary repetition, the various possible combinations of the specific technical features / embodiments in the utility model will not be described separately.
[0022] It should be noted that the terms "set" and "connect" should be understood in a broad sense. For example, they can be directly set, installed, and connected, or they can be indirectly set and connected through a central component or a central structural member. In addition, the orientations or positional relationships indicated by "center", "up", "down", "left", "right", "vertical", "horizontal", "inside", "outside", etc. in the present utility model are based on the orientations or positional relationships shown in the drawings or the conventional placement state or use state, and are only for the convenience of describing the present utility model and simplifying the description, and do not indicate or imply that the structural members, features, devices or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as limiting the present utility model.
[0023] like Figures 1-2 As shown, this embodiment provides a device for determining the softening point of mesophase pitch, including a glove box 2, a heating device 4 and a sample tube 5. The heating device 4 is installed in the glove box 2. The glove box 2 is a sealed chamber. The glove box 2 is provided with a glove box door 1 and operating gloves 3. The glove box door 1 facilitates the installation, maintenance and cleaning of the heating device 4 and other structures in the glove box 2. The operating gloves 3 are used for manual direct operation of the equipment in the glove box 2 in a sealed state. A sample chamber 6 corresponding to the sample tube 5 is provided in the heating device 4. The sample tube 5 can be heated by inserting it into the sample chamber 6.
[0024] The sample tube 5 includes a tube body 18 and a sample cup 16. The sample cup 16 is fixedly installed in the cavity of the tube body 18. In other embodiments, the sample cup 16 can also be detachably installed in the tube body 18. Preferably, the tube body 18 is made of a transparent material, such as a glass test tube, so that the reaction in the tube body 18 can be easily observed. A signal hole 17 is provided on the tube wall of the tube body 18, and a small hole is provided at the bottom of the sample cup 16. The small hole is used for the asphalt sample to flow out from the bottom of the sample cup 16 after softening. The signal hole 17 is arranged directly below the small hole at the bottom of the sample cup 16. The sample chamber 6 is provided with a through hole corresponding to the signal hole 17. An ambient light sensor is arranged in the through hole to monitor the change of the light signal in the signal hole 17. Specifically, a light source can be arranged at the first end of the through hole, and an ambient light sensor (not shown in the figure) can be installed at the second end of the through hole. The position of the through hole is aligned with the position of the signal hole 17. Furthermore, a steel ball 15 is movably arranged in the sample cup 16, and the steel ball 15 is used to increase the pressure on the asphalt sample, so that the softened asphalt sample can drip smoothly from the bottom of the sample cup 16; the upper end of the tube body is fixedly connected to the handle 14, and the handle 14 can be convenient for the operator to hold, especially when the temperature of the heated tube body 18 is relatively high, the handle 14 can prevent the operator from being scalded.
[0025] In this embodiment, one end of the glove box 2 is fixedly connected to the transition cabin 7, which connects the inner and outer sides of the glove box 2. Both ends of the transition cabin 7 are hinged with hatches 9. When the hatches 9 at both ends are closed, the transition cabin 7 is an independent closed space for inert gas replacement; after opening the hatches 9 at both ends, the asphalt sample can be sent into the glove box 2.
[0026] Furthermore, the transition cabin 7 is connected to a vacuum pump 10. When the hatches 9 are all closed, the vacuum pump 10 can evacuate the transition cabin 7. When the hatch 9 located outside the transition cabin 7 is closed and the hatch 9 located inside is opened, the transition cabin 7 is connected to the inside of the glove box 2. At this time, the vacuum pump 10 can evacuate the transition cabin 7 and the glove box 2 at the same time. At the same time, the glove box 2 and the transition cabin 7 are respectively connected to the inert gas cylinder 13 through a pipeline. The gas in the inert gas cylinder 13 is an inert gas. The inert gas can be one of nitrogen and a rare gas. In this embodiment, nitrogen is preferably used. A stop valve 8 is provided on the pipeline to control whether the inert gas is passed into the glove box 2. A first pressure gauge 11 is provided on the output port of the inert gas cylinder 13 to monitor the output pressure of the inert gas. A second pressure gauge 19 is provided on the transition cabin 7 to monitor the pressure in the transition cabin 19.
[0027] Furthermore, the glove box 2 is connected to the liquid seal tank 12 through a pipeline. The liquid seal tank 12 contains water as a liquid seal liquid, which can discharge part of the exhaust gas generated during the heating of the asphalt sample and adjust the pressure balance inside the glove box 2, and can also prevent the external air from flowing back into the glove box 2. A switch valve is provided on the pipeline between the glove box 2 and the liquid seal tank 12, which is used to close the glove box 2 when exhausting air.
[0028] When using the intermediate phase asphalt softening point measuring device provided by the utility model, first open the hatch 9 on the inner side of the transition cabin 7, close the hatch 9 on the outer side of the transition cabin 7, open the vacuum pump 10 to evacuate the air, and stop evacuating the air when the pressure displayed by the second pressure gauge 19 reaches -0.1MPa, then open the valve of the inert gas bottle 13 and the stop valve 8, input inert gas into the glove box 2, and repeatedly evacuate and pass the inert gas three times to completely replace the air in the glove box 2 with inert gas; then put the asphalt sample into the sample cup 16 for compaction and flatten the surface, place the steel ball 15 on the upper surface of the asphalt sample in the sample cup 16, close the hatch 9 on the inner side of the transition cabin 7, open the hatch 9 on the outer side of the transition cabin 7, and put the sample into the sample cup 16. The sample cup 16 is placed in the transition chamber 7, and then the outer hatch 9 of the transition chamber 7 is closed and the air in the transition chamber 7 is replaced by the above-mentioned exhaust-pass inert gas. After the replacement is completed, the operator opens the inner hatch 9 of the transition chamber 7 through the operating gloves 3, takes out the sample cup 16 and puts it into the sample chamber 6, turns on the heating device 4, and starts heating at a heating rate of 1°C / min. When the asphalt sample is heated and softened, it drips out from the small hole at the bottom of the sample cup 16. The dripping asphalt will instantly change the light intensity value detected by the ambient light sensor when passing through the signal hole 17. When the light intensity change is detected, the ambient light sensor will send a signal to remind the operator to record the heating temperature at this time, which is the softening point of the asphalt sample to be tested. Repeat three times and take the average value. Of course, in other embodiments, the control device can also be used to directly obtain the heating temperature of the heating device 4, that is, when the ambient light sensor detects a change in light intensity, it sends a signal to the control system to directly read the heating temperature of the heating device 4, and the test is completed.
[0029] Example 2
[0030] The test device and method provided in Example 1 were used to perform three parallel tests on three different asphalt samples, and the test results are shown in Table 1.
[0031] Table 1 Softening point of mesophase pitch
[0032]
[0033] It can be seen from the results in Table 1 that the softening point of asphalt samples tested by the measuring device provided by the utility model has good repeatability and small deviation in the test results.
[0034] The above is a preferred embodiment of the present invention. It should be pointed out that, for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as the protection scope of the present invention.
Claims
1. A device for measuring the softening point of mesophase pitch, comprising a glove box (2), a heating device (4) and a sample tube (5), wherein the glove box (2) is provided with a glove box door (1) and operating gloves (3), characterized in that: The heating device (4) is installed in the glove box (2). A sample chamber (6) corresponding to the sample tube (5) is provided in the heating device (4). The sample tube (5) comprises a tube body (18) and a sample cup (16). The sample cup (16) is fixedly or detachably connected in the cavity of the tube body (18). A signal hole (17) is provided on the tube wall of the tube body (18). A small hole is provided at the bottom of the sample cup (16). The signal hole (17) is arranged directly below the small hole. A through hole corresponding to the signal hole (17) is provided in the sample chamber (6). An ambient light sensor is provided in the through hole to monitor changes in light signals in the signal hole (17). A steel ball (15) is movably provided in the sample cup (16).
2. The device for measuring the softening point of mesophase pitch according to claim 1, characterized in that: One end of the glove box (2) is fixedly connected to a transition cabin (7), the transition cabin (7) communicates with the inner and outer sides of the glove box (2), and both ends of the transition cabin (7) are hinged with cabin doors (9).
3. The device for measuring the softening point of mesophase pitch according to claim 2, characterized in that: The transition chamber (7) is connected to a vacuum pump (10).
4. The device for measuring the softening point of mesophase pitch according to claim 2, characterized in that: The glove box (2) and the transition chamber (7) are respectively connected to an inert gas cylinder (13) via pipelines, and a stop valve (8) is provided on the pipelines.
5. The device for measuring the softening point of mesophase pitch according to claim 4, characterized in that: A first pressure gauge (11) is provided on the output port of the inert gas cylinder (13), and a second pressure gauge (19) is provided on the transition cabin (7).
6. The device for measuring the softening point of mesophase pitch according to claim 1, characterized in that: The glove box (2) is connected to the liquid sealing tank (12) via a pipeline.
7. The device for measuring the softening point of mesophase pitch according to claim 1, characterized in that: The upper end of the tube body (18) is fixedly or detachably connected to the handle (14).