CN112858079B - Method for detecting infiltration performance of asphalt for carbon - Google Patents
Method for detecting infiltration performance of asphalt for carbon Download PDFInfo
- Publication number
- CN112858079B CN112858079B CN202110094565.0A CN202110094565A CN112858079B CN 112858079 B CN112858079 B CN 112858079B CN 202110094565 A CN202110094565 A CN 202110094565A CN 112858079 B CN112858079 B CN 112858079B
- Authority
- CN
- China
- Prior art keywords
- asphalt
- sample
- raw material
- carbon
- heating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
- G01N5/02—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by absorbing or adsorbing components of a material and determining change of weight of the adsorbent, e.g. determining moisture content
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Coke Industry (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The invention relates to aThe method for detecting the infiltration performance of the asphalt for carbon comprises the following steps: 1) Preparing a powdered asphalt sample and a powdered carbonaceous raw material sample; 2) Taking the weight as m 1 Is spread on a sample of asphalt with a weight m 2 Heating the container, and then taking an excessive carbonaceous raw material sample and flatly paving the excessive carbonaceous raw material sample above the asphalt sample; 3) Heating the heating container to the detection temperature, keeping the temperature for a period of time, and cooling; 4) After the heating container is completely cooled, pouring out the carbon raw material sample which is not infiltrated in the heating container, and weighing the total weight m of the heating container and the infiltrated substance 3 Calculating the infiltration rate = (m) 3 ‑m 2 ‑m 1 ）/m 1 . Compared with the prior art, the detection method has the advantages of simplicity, practicability, good parallelism and repeatability of the detection result, high precision, easy formation of evaluation standard, and effective control of the asphalt quality, thereby improving the performance of the carbon material.
Description
Technical Field
The invention relates to a method for detecting the infiltration performance of asphalt for carbon, belonging to the technical field of carbon.
Background
The asphalt is an important raw material in the preparation of the carbon material, plays a role of a binder in the preparation of the carbon material, and plays a role in determining the performance of the carbon material by the quality of the asphalt. In the kneading process of preparing the carbon material, whether the asphalt can be uniformly spread on the surface of coke particles or not has important influence on the wetting of aggregate coke and the plasticity of a paste, on the liquid migration of the asphalt in the forming process and the early stage of roasting and on the strength of a finished carbon material. Therefore, how to accurately evaluate the wetting performance of the asphalt and select high-quality asphalt with good wetting performance is very important for improving the quality of the carbon material.
In the text of the wettability of coal pitch to coke and the effect of the coal pitch in the preparation of nuclear graphite (No. 4 of 2013), a method for determining the wettability coefficient by a coking experiment is provided, which comprises the steps of filling coke with a certain granularity into a measuring cylinder, vibrating, adding a layer of pitch with the granularity of 1-2mm on the coke, heating, taking out, weighing the bonded coke and pitch, and calculating the wettability coefficient. When a standard amount of coke is used, it can be used to describe the asphalt wettability; the wettability of the coke can also be measured when a standard amount of pitch is used.
The method is simple and easy to implement, but through actual operation, the problems of low detection result precision and poor parallelism, repeatability and reproducibility are found, so that the corresponding evaluation standard is difficult to establish.
Disclosure of Invention
Aiming at the problems, the invention provides a method for detecting the infiltration performance of asphalt for carbon, which has the specific scheme that:
a method for detecting the infiltration performance of asphalt for carbon comprises the following steps:
1) Preparing a powdered asphalt sample and a powdered carbonaceous raw material sample;
2) Taking the weight as m 1 Is spread on a sample of asphalt with a weight m 2 Heating the container, and then taking an excessive carbonaceous raw material sample and flatly paving the excessive carbonaceous raw material sample above the asphalt sample;
3) Heating the heating container to the detection temperature, keeping the temperature for a period of time, and then cooling;
4) After the heating container is completely cooled, pouring out the carbon raw material sample which is not infiltrated in the heating container, and weighing the total weight m of the heating container and the infiltrated substance 3 Calculating the infiltration rate = (m) 3 -m 2 -m 1 ）/m 1 。
The heating container in the scheme adopts a container with regular shape, uniform volume in the height direction and uniform heat conducting property, such as a glass measuring cylinder and a square porcelain boat.
In the invention, the heat transfer performance of the heating container has influence on the temperature rising speed of the asphalt, and further influences the infiltration rate, so that the heating container with the same specification is selected when the reproducibility experiment comparison is carried out. The detection temperature is determined according to the kneading temperature of the corresponding kneading process so as to accurately reflect the wetting performance of the asphalt during kneading. The constant temperature time is related to the weight of the asphalt sample, and when the sampling amount is large, the constant temperature time is prolonged to ensure that the asphalt sample completely soaks the carbonaceous raw material sample.
Wherein the excessive carbonaceous feedstock sample is a carbonaceous feedstock sample that can be completely infiltrated relative to the pitch sample, and if the measured infiltration rate of a certain modified pitch sample is less than 2.0 through multiple experiments, the excessive carbonaceous feedstock sample is selected as a sample whose weight is 2 times the weight of the pitch sample.
The asphalt sample can be various low-temperature asphalt, medium-temperature asphalt, high-temperature asphalt and modified asphalt, and the carbonaceous raw material sample can be various calcined petroleum coke, asphalt coke, metallurgical coke and calcined anthracite.
In the invention, the granularity of the asphalt sample in the step 1) is 1-2mm. This size range allows for uniform spreading of the asphalt sample.
In the invention, the granularity of the carbonaceous raw material sample in the step 1) is 40-60 meshes. The particle size range is consistent with the particle size range of the carbonaceous raw material sample for powder specific resistance detection, pores of the carbonaceous raw material sample are fully exposed in the particle size range, the particle size is uniform, and the uniformity of particle properties is good.
As a specific embodiment of the present invention, m is selected 1 1 to 2g, and the temperature is detected to be 160 to 200 ℃ in the step 3), and the constant temperature time is 1 hour. The detection temperature is suitable for the kneading temperature of the kneading process when most carbon materials are prepared. At m 1 When the temperature is 1 to 2g, the complete infiltration of the asphalt sample to the carbonaceous raw material sample can be ensured by keeping the temperature for 1 hour.
As a specific application of the invention, the asphalt sample is modified asphalt, the carbonaceous raw material sample is a calcined petroleum coke sample of 40-60 meshes, and the tap density of the calcined petroleum coke sample is 0.78-0.82g/cm 3 (ii) a M is 1 1 to 2g, the detection temperature is 180 ℃, and the constant temperature time is 1 hour; and when the detection result is not less than 1.5, judging that the infiltration performance of the modified asphalt is qualified.
The method has the advantages of simplicity, practicability, good parallelism and repeatability of detection results, high precision, easy formation of evaluation standards and effective control of the asphalt quality compared with the prior art, thereby improving the performance of the carbon material.
Detailed Description
The following examples are for illustrative purposes only and are not intended to limit the scope of the present invention.
Comparative example 1
According to the method mentioned in the prior art, firstly, the sampled calcined petroleum coke is sequentially dried, crushed and screened to obtain a calcined petroleum coke sample of 40-60 meshes; and drying, crushing and screening the sampled modified asphalt sample in sequence to obtain a modified asphalt sample with the thickness of 1-2mm. Taking a measuring cylinder with the volume of 10ml, firstly filling 50g of calcined petroleum coke sample, compacting, and scraping the upper surface of the calcined petroleum coke sample; and then 10g of modified asphalt sample is filled above the calcined petroleum coke sample, and the asphalt sample completely covers the calcined petroleum coke sample and is uniformly spread. And (3) putting the measuring cylinder into an oven, heating to 180 ℃, preserving the heat for 2 hours, cooling, taking out the sample from the measuring cylinder, weighing the mass m of the coke, and calculating the infiltration rate = (m-10)/10.
According to the method, 5 groups of parallel samples are arranged for each detection, the detection is carried out for 5 times in total, and the detection results are as follows:
as can be seen from the table above, the detection results of the parallel samples in the same batch are very different, the detection results of different batches are also very different, the detection precision is very low, and the asphalt infiltration performance cannot be accurately evaluated.
The analysis reason is that because the asphalt sample is placed above the calcined petroleum coke sample, after being heated, the asphalt is gradually melted into liquid and gradually infiltrates into the calcined petroleum coke sample layer from top to bottom to infiltrate the calcined petroleum coke. However, the calcined petroleum coke sample layer is full of air, even after the calcined petroleum coke sample layer is vibrated, the air content of the calcined petroleum coke sample layer is high, an airtight sealing layer is formed above the calcined petroleum coke sample layer after the asphalt is melted into a liquid state, the air in the calcined petroleum coke sample layer is prevented from being discharged, the liquid asphalt is inevitably influenced by air pressure resistance in the downward infiltration process, the influence degree of the factor is uncontrollable, the liquid asphalt cannot evenly infiltrate the calcined petroleum coke sample, and local asphalt is concentrated. In addition, asphalt infiltrates the calcined petroleum coke sample and infiltrates the measuring cylinder wall, and due to the influence factor, the infiltration depth of different sample groups on the measuring cylinder wall has a large difference, and the actual asphalt infiltration amount of the calcined petroleum coke can be influenced. During the heating process, it was clearly observed that bubbles were expelled after the bitumen melted. The shape of the coke taken out is irregular, a large cavity exists in the middle of some sample coke compositions, and the edge part is thick; some sample groups had thin edges and thick middle parts of the coke.
In addition, this method requires weighing the sinter after cooling. During operation, the coked objects need to be completely taken out, and because the asphalt wets the wall of the measuring cylinder, the coked objects are firmly bonded with the wall of the measuring cylinder after cooling, and a larger external force is needed when the coked objects are taken out. This operation necessarily results in the shedding of a portion of the char, firstly resulting in a weighable char weight that is significantly lower than the actual char weight; secondly, the falling amount of the coking object is uncontrollable in each operation, so that the detection result is low in precision.
Example 1
Taking 50g of the calcined petroleum coke sample and 10g of the modified asphalt sample in the comparative example 1, taking a 10ml measuring cylinder as a heating container, firstly weighing the weight m of the measuring cylinder 2 Uniformly spreading the modified asphalt sample on the bottom of the measuring cylinder to keep the surface of the modified asphalt sample flat, and adding the calcined petroleum coke sample above the modified asphalt sample. Putting the measuring cylinder into an oven, heating to 180 ℃, preserving heat for 2 hours, cooling, naturally taking out the uncoked loose calcined petroleum coke from the measuring cylinder, and weighing the residual coke and the total weight m of the measuring cylinder 3 Calculating the infiltration rate = (m) 3 -m 2 -10）/10。
According to the method, 5 groups of parallel samples are set for each detection, the detection is carried out for 5 times, and the detection results are as follows:
as can be seen from the table, the detection results of the parallel samples in the same batch and the parallel samples in different batches have a difference of only 0.01, and the accuracy is far higher than that of the method in the prior art.
In principle, compared with a comparative example, the method changes the vertical position relation of the asphalt sample and the calcined petroleum coke sample, the asphalt sample is infiltrated at the bottom and the asphalt is infiltrated at the upper part after melting, air in the calcined petroleum coke sample can be freely discharged towards the upper part, the influence of air resistance on the asphalt infiltration process is solved, the asphalt is evenly infiltrated towards the calcined petroleum coke layer, the infiltration degree of the asphalt on the measuring cylinder wall is consistent, and the influence of the factor is also eliminated. After cooling, the coked petroleum coke is positioned at the upper part, the coked material at the bottom is adhered to the wall of the measuring cylinder, and when weighing, the coked petroleum coke is only required to be naturally poured out, and then the coked material and the measuring cylinder are weighed integrally, so that the influence of falling of the coked material due to the action of external force is eliminated. Finally, the coke at the bottom of the measuring cylinder can be observed to be regular round cakes with uniform thickness, and the method can also prove that asphalt can uniformly infiltrate calcined petroleum coke without being obviously influenced by external factors when being detected by the method.
Example 2
This embodiment is used to verify the effect of the heating time on the test results,
taking 1g of asphalt sample without changing other conditions, keeping the temperature of the asphalt sample for 30min, 1h, 1.5h and 2h after the temperature of the asphalt sample is increased to 180 ℃, and detecting results are as follows:
it can be seen that, after the holding time reaches 1 hour, the detection result value is stable and unchanged, and the holding time is 1 hour when the amount of the asphalt sample is 1 g.
Example 3
The present example is used to verify the difference of the results of measuring the infiltration rate of different qualities of asphalt. In particular, in a certain factory for preparing the prebaked anode, petroleum coke raw materials are not adjusted in a production period, corresponding process parameters are not changed, and modified asphalt of the factory 1, the factory 2 and the factory 3 is respectively adopted for production. When the asphalt of the manufacturer 1 and the manufacturer 2 is used for production, the paste after kneading has good plasticity, the produced product has no crack, and the asphalt consumption is kept at 15%. When the asphalt of manufacturer 3 is used for production, the plasticity of the paste becomes poor after kneading, the crack rate of the product is increased, and the problem is improved after the asphalt amount is adjusted to 15.2%.
Sampling the modified asphalt of the three manufacturers, and taking the tap density of 0.78 to 0.82g/cm 3 The petroleum coke calcined at 40 to 60 meshes is used as a standard sample, and the method of the embodiment 2 is used for detecting the infiltration performance, and the result is as follows:
as can be seen from the above results, the results of the asphalt wettability test of manufacturer 3 were significantly lower than those of manufacturers 1 and 2, and corresponded to the performance of the kneading step. Therefore, the asphalt having the wettability test value of less than 1.50 is judged to be defective.
Claims (5)
1. The method for detecting the infiltration performance of the asphalt for the carbon is characterized by comprising the following steps of:
1) Preparing a powdered asphalt sample and a powdered carbonaceous raw material sample;
2) Taking the weight as m 1 Is spread on a sample of asphalt of weight m 2 Heating the container, and then taking an excessive carbonaceous raw material sample and flatly paving the excessive carbonaceous raw material sample above the asphalt sample;
3) Heating the heating container to the detection temperature, keeping the temperature for a period of time, and then cooling;
4) After the heating container is completely cooled, pouring out the carbon raw material sample which is not soaked in the heating container, and weighing the total weight m of the heating container and the soaked substance 3 Calculating the infiltration rate = (m) 3 -m 2 -m 1 ）/m 1 。
2. The method for detecting the wettability of carbon with pitch according to claim 1, wherein: the particle size of the asphalt sample is 1-2mm.
3. The method for detecting the wettability of carbon with pitch according to claim 1, wherein: the particle size of the carbonaceous raw material sample is 40-60 meshes.
4. The method for detecting the wettability of the pitch for carbon according to claim 1, wherein: m is a unit of 1 1 to 2g, and the temperature is detected to be 160 to 200 ℃ in the step 3), and the constant temperature time is 1 hour.
5. The method for detecting the wettability of carbon with pitch according to claim 1, wherein: the asphalt sample is modified asphalt, the carbonaceous raw material sample is a calcined petroleum coke sample of 40-60 meshes, and the tap density of the calcined petroleum coke sample is 0.78-0.82g/cm 3 (ii) a M is 1 1 to 2g, the detection temperature is 180 ℃, and the constant temperature time is 1 hour; and when the detection result is not less than 1.5, judging that the infiltration performance of the modified asphalt is qualified.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110094565.0A CN112858079B (en) | 2021-01-25 | 2021-01-25 | Method for detecting infiltration performance of asphalt for carbon |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110094565.0A CN112858079B (en) | 2021-01-25 | 2021-01-25 | Method for detecting infiltration performance of asphalt for carbon |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112858079A CN112858079A (en) | 2021-05-28 |
| CN112858079B true CN112858079B (en) | 2022-12-06 |
Family
ID=76008326
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110094565.0A Active CN112858079B (en) | 2021-01-25 | 2021-01-25 | Method for detecting infiltration performance of asphalt for carbon |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112858079B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4426160A (en) * | 1980-12-30 | 1984-01-17 | Huiles, Goudrons Et Derives | Device for measuring the deformation of a material under the influence of heat and its application to the determination of the wetting power of pitches |
| RU2013102000A (en) * | 2013-01-17 | 2014-07-27 | Открытое акционерное общество "Авиационная корпорация "Рубин" (ОАО "АК "Рубин") | METHOD FOR DETERMINING THE DEGREES OF IMPREGNATION OF CARBON FIBER HARNESSES BY FIRES AND INSTALLATION FOR ITS IMPLEMENTATION |
| CN109870379A (en) * | 2019-02-28 | 2019-06-11 | 蜂巢能源科技有限公司 | For detecting the detection device and wellability detection method of wellability |
| CN110286064A (en) * | 2019-08-05 | 2019-09-27 | 贵州大学 | A kind of mineral grain wetability measuring device and its measurement method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN211904980U (en) * | 2020-01-16 | 2020-11-10 | 济宁碳素集团有限公司 | System for measuring wettability of coal tar pitch to calcined coke aggregate |
-
2021
- 2021-01-25 CN CN202110094565.0A patent/CN112858079B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4426160A (en) * | 1980-12-30 | 1984-01-17 | Huiles, Goudrons Et Derives | Device for measuring the deformation of a material under the influence of heat and its application to the determination of the wetting power of pitches |
| RU2013102000A (en) * | 2013-01-17 | 2014-07-27 | Открытое акционерное общество "Авиационная корпорация "Рубин" (ОАО "АК "Рубин") | METHOD FOR DETERMINING THE DEGREES OF IMPREGNATION OF CARBON FIBER HARNESSES BY FIRES AND INSTALLATION FOR ITS IMPLEMENTATION |
| CN109870379A (en) * | 2019-02-28 | 2019-06-11 | 蜂巢能源科技有限公司 | For detecting the detection device and wellability detection method of wellability |
| CN110286064A (en) * | 2019-08-05 | 2019-09-27 | 贵州大学 | A kind of mineral grain wetability measuring device and its measurement method |
Non-Patent Citations (1)
| Title |
|---|
| 粉焦对沥青浸润和结焦体反应性的影响研究;张念炳等;《轻金属》;20180620(第06期);第44-46页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112858079A (en) | 2021-05-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103154200B (en) | Method for producing metallurgical coke | |
| KR101561748B1 (en) | Method for producing coke | |
| CN108046803B (en) | High-strength graphite product produced by adding asphalt coke and method | |
| CN103180414B (en) | Metallurgical coke production method | |
| CN101788441B (en) | Device and method for determining moisture content and size composition of sinter mixture | |
| CN112858079B (en) | Method for detecting infiltration performance of asphalt for carbon | |
| CN111116200A (en) | Carbon electrode with conical central hole and preparation method thereof | |
| CN101793643B (en) | Method for refining coke used for measuring coke optical texture | |
| CN113233898A (en) | Electrolytic aluminum prebaked anode and production process thereof | |
| CN107290511B (en) | Detection method for grading of cement stabilizing material | |
| Wilkening | Maintaining consistent anode density using varying carbon raw materials | |
| US3442989A (en) | Method of forming carbon-bonded silicon carbide bodies | |
| WO2012029984A1 (en) | Method for producing metallurgical coke | |
| US4197160A (en) | Process by means of which moulded coke can be obtained from non-cokable coals | |
| CN107176827A (en) | One kind prepares crucible refractory material powder | |
| Wilkening | Properties and behaviour of green anodes | |
| Mollaabbasi et al. | Rheological characterization of pitch and binder matrix with different concentrations of fine particles | |
| NO144709B (en) | CONTINUOUS SELF-BURNING ANODE AND PROCEDURE FOR MAINTENANCE OF SUCH ANODE | |
| JP4132710B2 (en) | Blast furnace coke strength estimation method | |
| Larsen et al. | Melting and densification of electrode paste briquettes in Søderberg electrodes | |
| CN112067455A (en) | High-temperature crushing value test method for coarse aggregate | |
| CN205115620U (en) | Plain positive pole of quick electrically conductive gradient charcoal | |
| CN117026304A (en) | Test method of cathode cold ramming paste for integral furnace building of aluminum electrolysis cell | |
| CN117658647A (en) | Cold ramming paste for integral furnace construction of aluminum electrolysis cell and preparation method thereof | |
| Murthy et al. | Comparative Studies on a High Temperature Coke Oven Coal Tar Pitch as a Binder in the Manufacture of Carbon Refractories and Compacts |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Han Jianhua Inventor after: Niu Jincai Inventor after: Wu Yanli Inventor before: Wu Yanli |
|
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20221110 Address after: 454,191 100m north of Xuelian Road West Section, Longxiang Street, Zhongzhan District, Jiaozuo City, Henan Province Applicant after: JIAOZUO ZHONGZHOU CARBON Co.,Ltd. Address before: Room 205-44, building 9, Science Park, Henan University of technology, 1365 Zhongyuan Road, urban rural integration demonstration zone, Jiaozuo City, Henan Province, 454150 Applicant before: Jiaozuo Junfei Jincai Technology Co.,Ltd. |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant |