CN112857959A - Preparation device and preparation method of coal ash slag sample - Google Patents
Preparation device and preparation method of coal ash slag sample Download PDFInfo
- Publication number
- CN112857959A CN112857959A CN202110084033.9A CN202110084033A CN112857959A CN 112857959 A CN112857959 A CN 112857959A CN 202110084033 A CN202110084033 A CN 202110084033A CN 112857959 A CN112857959 A CN 112857959A
- Authority
- CN
- China
- Prior art keywords
- sample
- crucible
- coal ash
- temperature
- corundum tube
- 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.)
- Pending
Links
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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)
- Sampling And Sample Adjustment (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The invention provides a preparation device and a preparation method of a coal ash slag sample, which comprises a high-temperature furnace, a sample stage, a thermocouple, a lifting device, a gas control system, a control module, an alundum tube and a crucible, wherein the sealing effect is realized on the upper surfaces of the alundum tube and the lifting device, the crucible comprises a protective crucible and a sample crucible, and the protective crucible is sleeved outside the sample crucible and is higher than the sample crucible so as to prevent the sample from being sprayed out to pollute the sample stage under the high-temperature melting condition; meanwhile, the high-temperature melting of the sample under a specific atmosphere condition can be realized, the method can be used for preparing high-temperature quenching slag or viscosity determination samples, and the workload in the test preparation process is reduced; in addition, the sample can be uniformly kept all the time in the pre-melting process by pretreating the sample, and simultaneously, the introduction of new impurities is avoided in the slag taking process, so that the precision of the test result is improved.
Description
Technical Field
The invention relates to the field of coal gasification, in particular to a preparation device and a preparation method of a coal ash residue sample.
Background
The melting characteristic and the viscosity-temperature characteristic of the coal ash are key factors for determining the long-period stable operation of the entrained flow gasifier, and the viscosity-temperature characteristic is the most important parameter for quantitatively describing the flow property of the coal ash at high temperature and is also an important basis for determining the operating temperature of the liquid slag-off gasifier. For the slag tapping gasifier, the viscosity of the coal ash must be controlled within a proper range, the slag plugging at the slag tapping hole is easily caused by too high viscosity, and the purpose of protecting the water-cooled wall by slag resistance is difficult to achieve by too low viscosity. Therefore, the accurate measurement of the viscosity of the coal ash and the research on the structural change of the coal ash at high temperature have important significance for guiding the safe and stable operation of the gasification furnace.
At present, the preparation process for measuring the viscosity of the coal ash generally needs to dry, crush, screen, ash, pre-melt and remove slag from a coal ash sample. The workload of the process is huge, and the accuracy of sample testing is directly influenced by the most key operation steps of pre-melting and slag taking before measurement. The pre-melting is to put a proper amount of a coal ash sample into a crucible, melt the coal ash sample by using high temperature, remove moisture and volatile components in the coal ash sample, and thus melt the coal ash sample into a uniform liquid phase at a set temperature; the slag taking is generally realized by breaking a crucible which is pre-melted and is filled with a coal ash sample, so that the coal ash sample is taken out. Through the operation, if the pre-melting process is not uniform, the coal ash sample is not representative easily during the test, so that the deviation of the later test result is caused, and the accuracy is low; in addition, crucible materials are easy to mix into the coal ash sample in the slag taking process, and the deviation of the later-period measurement result is easy to increase.
Disclosure of Invention
In order to solve the defects and shortcomings of the prior art, the preparation device and the preparation method of the coal ash slag sample are provided, so that the problems of large workload of a coal ash viscosity determination preparation process, non-uniform sample in a pre-melting process and low test accuracy caused by easy introduction of impurities in a slag taking process can be solved.
The device for preparing the coal ash slag sample comprises a high-temperature furnace, a sample table, a thermocouple, a lifting device, a gas control system and a control module, and is characterized in that: still including corundum tube and crucible, the one end of corundum tube is sealed, and the other end is opened, the blind end of corundum tube inlays in the zone of heating of high temperature furnace, the open end of corundum tube extends the zone of heating of high temperature furnace, and with elevating gear's elevating platform upper surface passes through the sealed cooperation of flange to realize sealed effect, the crucible is including protection crucible and sample crucible, protection crucible cover is in the sample crucible outside and is higher than the sample crucible, in order to avoid the sample to spout out dirty sample platform behind the high temperature melting, the central point that the sample platform was placed to the crucible puts, the thermocouple is fixed in the central point of sample platform puts, and contacts with the bottom of crucible to realize the real-time supervision of sample temperature, the sample platform is fixed in elevating gear's elevating platform central point and puts.
As a further improvement of the above scheme, the material of the protective crucible and the sample crucible is one of alumina, zirconia, molybdenum and graphite.
A preparation method of a coal ash sample is characterized by comprising the following steps: the method comprises the following steps:
uniformly mixing coal ash and dextrin solution to obtain a coal ash mixture;
secondly, putting the sample crucible into a protective crucible, pressing the coal ash mixture into a cylindrical sheet or directly putting the cylindrical sheet into the sample crucible;
placing the crucible at the central position of the sample table, and adjusting the height of the lifting table by using the lifting device until the open end of the corundum tube is flush with the lifting table of the lifting device, so that the sample table is sealed in the corundum tube;
regulating a gas control system to introduce gas into the corundum tube according to the experimental requirements, and setting the corundum tube to be in a specific gas atmosphere;
step five, heating the high-temperature furnace through the control module according to the experimental requirements to melt the coal ash mixture;
step six, when the thermocouple monitors that the temperature of the sample reaches the target temperature, keeping the temperature for a certain period of time to ensure the melting of the coal ash mixture;
and step seven, rapidly lowering the sample table through the lifting device, taking the sample crucible out of the protective crucible, and chilling or cooling the sample crucible by using ice water to obtain the coal ash sample.
As a further improvement of the scheme, the time length in the sixth step is not less than 5 min.
As a further improvement of the above scheme, the coal ash sample in the seventh step is one of high-temperature quenching slag and a viscosity measurement sample.
The invention has the beneficial effects that:
compared with the prior art, the preparation device and the preparation method of the coal ash slag sample can realize high-temperature melting of coal ash under a specific atmosphere condition, can be used for preparing high-temperature quenching slag or viscosity determination samples, and reduce workload in a test preparation process; in addition, the sample can be uniformly kept all the time in the pre-melting process by pretreating the sample, and simultaneously, the introduction of new impurities is avoided in the slag taking process, so that the precision of the test result is improved.
Drawings
FIG. 1 is a diagram of an apparatus of the present invention;
FIG. 2 is a view showing the internal structure of the apparatus of the present invention;
FIG. 3 is a schematic view of a crucible of the present invention;
FIG. 4 is a schematic diagram of the high-temperature quenched slag prepared by the method of the invention;
FIG. 5 is a schematic view of a sample for viscosity measurement prepared by the method of the present invention.
Wherein: 1-high temperature furnace, 2-sample stage, 3-thermocouple, 4-lifting device, 5-gas control system, 6-control module, 7-corundum tube, 8-crucible, 9-protective crucible and 10-sample crucible.
Detailed Description
The following detailed description of embodiments of the invention is provided in connection with the accompanying drawings,
example 1
As shown in fig. 1 to 3, a coal ash sample preparation device comprises a high temperature furnace 1, a sample table 2, a thermocouple 3, a lifting device 4, a gas control system 5 and a control module 6, and is characterized in that: the device is characterized by further comprising a corundum tube 7 and a crucible 8, wherein one end of the corundum tube 7 is closed, the other end of the corundum tube 7 is open, the closed end of the corundum tube 7 is embedded in a heating area of the high-temperature furnace 1, the open end of the corundum tube 7 extends out of the heating area of the high-temperature furnace 1 and is in sealing fit with the upper surface of a lifting platform of the lifting device 4 through a flange to achieve a sealing effect, the crucible 8 comprises a protective crucible 9 and a sample crucible 10, the protective crucible 9 is sleeved outside the sample crucible 10 and is higher than the sample crucible 10 to prevent a sample from being sprayed out to pollute the sample platform 2 under high-temperature melting, the crucible 8 is placed at the central position of the sample platform 2, the thermocouple 3 is fixed at the central position of the sample platform 2 and is in contact with the bottom of the crucible 8 to achieve real-time monitoring of the sample temperature, the sample platform 2 is fixed at, the protective crucible 9 and the sample crucible 10 are made of one of alumina, zirconia, molybdenum and graphite.
Example 2
As shown in fig. 4, a preparation method of a coal ash sample comprises the following steps:
uniformly mixing coal ash and dextrin solution to obtain a coal ash mixture;
secondly, putting a sample crucible 10 made of alumina into a protective crucible 9 made of zirconia, and directly putting the coal ash mixture into the sample crucible 10;
placing the crucible 8 at the center of the sample table 2, and adjusting the height of the lifting table by using the lifting device 4 until the open end of the corundum tube 7 is flush with the lifting table of the lifting device 4, so that the sample table 2 is sealed in the corundum tube 7;
regulating the gas control system 5 to introduce gas into the corundum tube 7 according to the experimental requirements, and setting the interior of the corundum tube 7 to be a specific gas atmosphere;
step five, heating the high-temperature furnace 1 through the control module 6 according to the experiment requirement to melt the coal ash mixture;
step six, when the thermocouple 3 monitors that the temperature of the sample reaches the target temperature, keeping the temperature for 10min to ensure the melting of the coal ash mixture;
and step seven, rapidly lowering the sample table 2 through the lifting device 4, taking the sample crucible 10 out of the protective crucible 9, and putting the sample crucible into ice water for chilling treatment to obtain high-temperature chilled slag.
Example 3
As shown in fig. 5, a preparation method of a coal ash sample comprises the following steps:
uniformly mixing coal ash and dextrin solution to obtain a coal ash mixture;
secondly, putting a sample crucible 10 made of molybdenum into a protective crucible 9 made of graphite, pressing the coal ash mixture into a cylindrical sheet, and putting the cylindrical sheet into the sample crucible 10;
placing the crucible 8 at the center of the sample table 2, and adjusting the height of the lifting table by using the lifting device 4 until the open end of the corundum tube 7 is flush with the lifting table of the lifting device 4, so that the sample table 2 is sealed in the corundum tube 7;
regulating the gas control system 5 to introduce gas into the corundum tube 7 according to the experimental requirements, and setting the interior of the corundum tube 7 to be a specific gas atmosphere;
step five, heating the high-temperature furnace 1 through the control module 6 according to the experiment requirement to melt the coal ash mixture;
step six, when the temperature of the sample monitored by the thermocouple 3 reaches the target temperature, preserving the heat for 20min to ensure the melting of the coal ash mixture;
and step seven, rapidly lowering the sample table 2 through the lifting device 4, taking the sample crucible 10 out of the protective crucible 9, and cooling to obtain a viscosity determination sample.
The above embodiments are not limited to the technical solutions of the embodiments themselves, and the embodiments may be combined with each other into a new embodiment. The above embodiments are only for illustrating the technical solutions of the present invention and are not limited thereto, and any modification or equivalent replacement without departing from the spirit and scope of the present invention should be covered within the technical solutions of the present invention.
Claims (5)
1. The utility model provides a preparation facilities of coal ash sediment sample, including high temperature furnace (1), sample platform (2), thermocouple (3), elevating gear (4), gas control system (5) and control module (6), its characterized in that: the device is characterized by further comprising a corundum tube (7) and a crucible (8), wherein one end of the corundum tube (7) is closed, the other end of the corundum tube is open, the closed end of the corundum tube (7) is embedded in a heating area of the high-temperature furnace (1), the open end of the corundum tube (7) extends out of the heating area of the high-temperature furnace (1) and is in sealing fit with the upper surface of a lifting platform of the lifting device (4) through a flange to achieve a sealing effect, the crucible (8) comprises a protective crucible (9) and a sample crucible (10), the protective crucible (9) is sleeved outside the sample crucible (10) and is higher than the sample crucible (10) to prevent a sample from being sprayed out to contaminate the sample platform (2) under high-temperature melting, the crucible (8) is placed at the central position of the sample platform (2), the thermocouple (3) is fixed at the central position of the sample platform (2) and is in contact with the bottom of, the sample stage (2) is fixed at the center of the lifting stage of the lifting device (4).
2. The apparatus for preparing a soot ash sample according to claim 1, wherein: the protective crucible (9) and the sample crucible (10) are made of one of alumina, zirconia, molybdenum and graphite.
3. A preparation method of a coal ash sample is characterized by comprising the following steps: the method comprises the following steps:
uniformly mixing coal ash and dextrin solution to obtain a coal ash mixture;
secondly, putting the sample crucible (10) into a protective crucible (9), pressing the coal ash mixture into a cylindrical sheet or directly putting the cylindrical sheet into the sample crucible (10);
thirdly, placing the crucible (8) at the central position of the sample platform (2), and adjusting the height of the lifting platform by using the lifting device (4) until the open end of the corundum tube (7) is flush with the lifting platform of the lifting device (4), so that the sample platform (2) is sealed in the corundum tube (7);
regulating a gas control system (5) to introduce gas into the corundum tube (7) according to the experimental requirements, and setting the interior of the corundum tube (7) to be in a specific gas atmosphere;
step five, heating the high-temperature furnace (1) through a control module (6) according to the experiment requirement to melt the coal ash mixture;
step six, when the thermocouple (3) monitors that the temperature of the coal ash mixture reaches the target temperature, keeping the temperature for a certain period of time to ensure the melting of the coal ash mixture;
and seventhly, rapidly lowering the sample table (2) through the lifting device (4), taking the sample crucible (10) out of the protective crucible (9), and chilling or cooling with ice water to obtain a coal ash sample.
4. The method for preparing a coal ash sample according to claim 3, which is characterized in that: the time length in the sixth step is not less than 5 min.
5. The method for preparing a coal ash sample according to claim 3, which is characterized in that: and the coal ash sample in the seventh step is one of high-temperature quenching slag and a viscosity measurement sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110084033.9A CN112857959A (en) | 2021-01-21 | 2021-01-21 | Preparation device and preparation method of coal ash slag sample |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110084033.9A CN112857959A (en) | 2021-01-21 | 2021-01-21 | Preparation device and preparation method of coal ash slag sample |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112857959A true CN112857959A (en) | 2021-05-28 |
Family
ID=76009079
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110084033.9A Pending CN112857959A (en) | 2021-01-21 | 2021-01-21 | Preparation device and preparation method of coal ash slag sample |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112857959A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113466322A (en) * | 2021-06-17 | 2021-10-01 | 新疆众和股份有限公司 | Method for detecting pollution degree of contact material for high-purity aluminum smelting on aluminum liquid |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN203323554U (en) * | 2013-05-17 | 2013-12-04 | 合肥科晶材料技术有限公司 | Liftable type vacuum high-temperature furnace |
| CN105092631A (en) * | 2015-08-07 | 2015-11-25 | 欧优科学仪器南京有限公司 | Thermal analysis method for testing high-activity element alloy material through seal crucible |
| EP2966039A1 (en) * | 2014-07-08 | 2016-01-13 | PANalytical B.V. | Preparation of samples for XRF using flux and platinum crucible |
| CN208334187U (en) * | 2018-05-30 | 2019-01-04 | 上海宝钢工业技术服务有限公司 | Graphite set crucible for oxygen-nitrogen analyzer |
| CN110501261A (en) * | 2019-09-26 | 2019-11-26 | 煤炭科学技术研究院有限公司 | A kind of measurement device of high-temperature coal ash viscosity |
| CN110702560A (en) * | 2019-10-14 | 2020-01-17 | 中国科学院山西煤炭化学研究所 | Device and method for measuring viscosity-temperature characteristics of coal ash slag in presence of high-temperature steam |
-
2021
- 2021-01-21 CN CN202110084033.9A patent/CN112857959A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN203323554U (en) * | 2013-05-17 | 2013-12-04 | 合肥科晶材料技术有限公司 | Liftable type vacuum high-temperature furnace |
| EP2966039A1 (en) * | 2014-07-08 | 2016-01-13 | PANalytical B.V. | Preparation of samples for XRF using flux and platinum crucible |
| CN105092631A (en) * | 2015-08-07 | 2015-11-25 | 欧优科学仪器南京有限公司 | Thermal analysis method for testing high-activity element alloy material through seal crucible |
| CN208334187U (en) * | 2018-05-30 | 2019-01-04 | 上海宝钢工业技术服务有限公司 | Graphite set crucible for oxygen-nitrogen analyzer |
| CN110501261A (en) * | 2019-09-26 | 2019-11-26 | 煤炭科学技术研究院有限公司 | A kind of measurement device of high-temperature coal ash viscosity |
| CN110702560A (en) * | 2019-10-14 | 2020-01-17 | 中国科学院山西煤炭化学研究所 | Device and method for measuring viscosity-temperature characteristics of coal ash slag in presence of high-temperature steam |
Non-Patent Citations (1)
| Title |
|---|
| 沿杰峰 等: "RSV-1600 型旋转高温黏度仪在煤灰黏度检测中的应用", 《大氮肥》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113466322A (en) * | 2021-06-17 | 2021-10-01 | 新疆众和股份有限公司 | Method for detecting pollution degree of contact material for high-purity aluminum smelting on aluminum liquid |
| CN113466322B (en) * | 2021-06-17 | 2022-10-14 | 新疆众和股份有限公司 | Method for detecting pollution degree of contact material for high-purity aluminum smelting on aluminum liquid |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN201145676Y (en) | Iron ore melting dripping test device | |
| CN112857959A (en) | Preparation device and preparation method of coal ash slag sample | |
| CN105588781B (en) | A kind of device and method for measuring field trash rate of dissolution in metallurgy clinker | |
| CN109298016B (en) | Experimental device for simulating iron layer of blast furnace hearth | |
| US11919814B2 (en) | Method for simulating intraplate volcanism | |
| Osugi et al. | Effect of oxidation state of iron ions on the viscosity of alkali silicate melts | |
| CN113336420B (en) | Molten glass stirring control system and method for laboratory | |
| CN201583480U (en) | Slag resistance test apparatus for refractory materials | |
| CN109612274B (en) | Alloy sample preparation device and method | |
| AU2012302126B2 (en) | Preparation of inorganic samples by fusion | |
| CN113624794A (en) | Test device and method for evaluating molten iron corrosion resistance of blast furnace carbon brick | |
| Meng et al. | Mould Slag Property Measurements To Characterize Cc Mould–Shell Gap Phenomena | |
| CN207709073U (en) | A kind of device melting sample for experimental glass | |
| Noel | Alternative to the Conradson carbon residue test | |
| CN109748481A (en) | A kind of method and apparatus melting sample for experimental glass | |
| CN211503694U (en) | Simulation test furnace for detecting real-time temperature in service process of steel ladle ventilating plug | |
| CN208833643U (en) | A kind of system for detecting clinker respond | |
| CN220751790U (en) | Melting device for hot melt marking paint laboratory | |
| CN110702560A (en) | Device and method for measuring viscosity-temperature characteristics of coal ash slag in presence of high-temperature steam | |
| CN100457275C (en) | A low-temperature carbonization device using microwave | |
| CN214830590U (en) | Continuous refining furnace system with shaft furnace for online detection of oxygen content of copper liquid | |
| CN108693210A (en) | Cooling wall cooling rate and thermal shock relation test equipment and test method | |
| CN108896477B (en) | System for detecting slag reaction capacity based on electric signal change | |
| CN117128910A (en) | Method for detecting corrosion thickness of refractory material of tank wall of kiln | |
| CN109187182A (en) | A method of for detecting clinker reactivity worth |
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 | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210528 |