WO2022121194A1 - Method for determining free radicals in high-temperature oxide melt - Google Patents
Method for determining free radicals in high-temperature oxide melt Download PDFInfo
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- WO2022121194A1 WO2022121194A1 PCT/CN2021/086323 CN2021086323W WO2022121194A1 WO 2022121194 A1 WO2022121194 A1 WO 2022121194A1 CN 2021086323 W CN2021086323 W CN 2021086323W WO 2022121194 A1 WO2022121194 A1 WO 2022121194A1
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- free radicals
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- 238000000034 method Methods 0.000 title claims abstract description 30
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 27
- 239000010431 corundum Substances 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 3
- 238000010791 quenching Methods 0.000 claims abstract description 3
- 150000003254 radicals Chemical class 0.000 claims description 24
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 6
- 230000000171 quenching effect Effects 0.000 abstract 1
- 239000000155 melt Substances 0.000 description 6
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 4
- 239000000292 calcium oxide Substances 0.000 description 4
- 239000002893 slag Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000004435 EPR spectroscopy Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 230000005291 magnetic effect Effects 0.000 description 1
- 238000010310 metallurgical process Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000009853 pyrometallurgy Methods 0.000 description 1
- 238000007348 radical reaction Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
- G01N25/48—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Definitions
- the invention belongs to the technical field of high-temperature melts, and particularly relates to a method for measuring free radicals of high-temperature oxide melts.
- slag is not only an inevitable product, but also has an important impact on the metallurgical process and the quality of its products.
- metallurgical slag there are many types of metallurgical slag, and the composition of the system is complex, but it is mainly a high-temperature melt composed of various oxides such as CaO, SiO 2 , Al 2 O 3 , MgO, FeO, Fe 2 O 3 , and MnO.
- slag structure namely molecular structure theory, ionic structure theory, ion-molecular coexistence theory and polymer theory. In this study, it was found that CaO-Al 2 O 3 oxide melts can generate free radicals at high temperature.
- EPMR electron paramagnetic resonance
- the present invention provides a free radical determination method of oxide high temperature melt with simple process and easy operation.
- section of the corundum crucible is a regular triangle, a square, a regular pentagon or a regular six
- the holding time is 0.1-10 hours.
- the difference in holding time of the two corundum crucibles is 0.5-2 hours.
- the height of the crucible is ⁇ 3 times the height of the oxide melt in the crucible.
- the Al 2 O 3 content in the corundum crucible is ⁇ 99.5 wt %, and the bulk density is ⁇ 3.8 g/cm 3 .
- the chemical bond breaking speed of the oxide mixture is very fast under the action of high temperature, and it may be homogenized and generate free radicals.
- CaO ionic bond will be homogenized under the action of high temperature to generate Ca and O, which is combined with Al 2 O in the corundum crucible. 3.
- Free radical reaction will be generated, releasing chemical energy to push the melt at the corners of the equilateral triangle corundum crucible to rise significantly. Free-radical determination of melts.
- the present invention has the following beneficial effects:
- the invention can carry out the determination of free radicals in high temperature oxide melt, and has the characteristics of simple process and easy operation.
- the oxide mixed powder containing 50wt% calcium oxide, 35wt% alumina and 15wt% silicon oxide to be tested is divided into two equal parts by mass, and placed in two corundum crucibles with the same cross-section of an equilateral triangle respectively.
- the two corundum crucibles were placed in a high-temperature furnace, then heated to 1600 °C for 0.1 hour and 0.6 hours, respectively, and then quenched.
- the oxide melts in the two corundum crucibles held for different times were measured at The relative average height difference at the three corners of the corundum crucible is about 4 mm, indicating that the oxide melt produced free radicals during the high temperature process.
- the height of the crucible is 3 times the height of the oxide melt in the crucible; the Al 2 O 3 content in the corundum crucible is 99.5 wt %, and the bulk density is 3.8 g/cm 3 .
- This embodiment can perform free radical determination in high temperature oxide melt, and has the characteristics of simple process and easy operation.
- the oxide mixed powder containing 40wt% calcium oxide, 40wt% alumina and 20wt% silicon oxide to be tested is divided into two equal parts by mass, and placed in two corundum crucibles with the same square cross section respectively And tamping, the two corundum crucibles were placed in a high-temperature furnace, and then heated to 1800 ° C for 8 hours and 10 hours, respectively, and then quenched, and the oxide melt in the two corundum crucibles held for different times was measured.
- the relative average height difference at the three corners of the crucible is about 15mm, indicating that the oxide melt produces free radicals during the high temperature process, and the oxide melt produces more free radicals during the high temperature process.
- the height of the crucible is 4 times the height of the oxide melt in the crucible; the Al 2 O 3 content in the corundum crucible is 99.8 wt %, and the bulk density is 4.0 g/cm 3 .
- the cross section of the corundum crucible may also be a regular pentagon, a regular hexagon or other symmetrical polygons.
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Abstract
A method for determining free radicals in a high-temperature oxide melt, comprising: firstly, equally dividing an oxide powder to be determined into two parts by mass, respectively placing same in two identical corundum crucibles having a polygon cross section and tamping same, placing both the corundum crucibles in a high-temperature furnace, then increasing the temperature to 1600℃ or more, and respectively maintaining the temperature for different times and then quenching; and measuring the relative average height difference of the oxide melt that has been maintained for different times at each corner of the corundum crucible, when a height difference exists, it indicates that the oxide produces free radicals during the high-temperature process, and a larger height difference indicates that the oxide melt produces more free radicals during the high-temperature process. The method can determine free radicals in a high-temperature oxide melt, and has the characteristics of a simple process and easy operation.
Description
相关申请的交叉引用CROSS-REFERENCE TO RELATED APPLICATIONS
本申请要求享有于2020年12月7日提交的名称为“一种高温氧化物熔体自由基的测定方法”的中国专利申请CN 202011418211.9的优先权，上述申请的全部内容通过引用并入本文中。This application claims to enjoy the priority of Chinese patent application CN 202011418211.9, which was filed on December 7, 2020 and is entitled "A Determination Method for High-Temperature Oxide Melt Radicals", the entire contents of which are incorporated herein by reference. .
本发明属于高温熔体技术领域，具体涉及一种高温氧化物熔体自由基的测定方法。The invention belongs to the technical field of high-temperature melts, and particularly relates to a method for measuring free radicals of high-temperature oxide melts.
在火法冶金过程中，熔渣既是其必然产物，又对冶金工艺及其产品品质具有重要影响。冶金熔渣类型较多，体系成分复杂，但主要是由各种氧化物如CaO、SiO
2、Al
2O
3、MgO、FeO、Fe
2O
3、MnO等组成的高温熔体。目前，熔渣结构理论主要有四种，分别为分子结构理论、离子结构理论、离子—分子共存理论和聚合物理论。本研究发现，CaO-Al
2O
3系氧化物熔体在高温下会产生自由基，然而，现阶段对自由基测定主要采用电子顺磁共振仪，基于自由基总磁矩的绝大部分(99％以上)的贡献来自电子自旋，直接检测物质原子或分子中所含的不配对电子，但仅在低温和常温等条件下开展检测，难以进行高温下氧化物熔体的自由基测定。
In the process of pyrometallurgy, slag is not only an inevitable product, but also has an important impact on the metallurgical process and the quality of its products. There are many types of metallurgical slag, and the composition of the system is complex, but it is mainly a high-temperature melt composed of various oxides such as CaO, SiO 2 , Al 2 O 3 , MgO, FeO, Fe 2 O 3 , and MnO. At present, there are four main theories of slag structure, namely molecular structure theory, ionic structure theory, ion-molecular coexistence theory and polymer theory. In this study, it was found that CaO-Al 2 O 3 oxide melts can generate free radicals at high temperature. However, at this stage, electron paramagnetic resonance (EPMR) is mainly used for the determination of free radicals, which is based on the vast majority of the total magnetic moment of free radicals ( The contribution of more than 99%) comes from the electron spin, and the unpaired electrons contained in the atoms or molecules of the substance are directly detected, but the detection is only carried out under the conditions of low temperature and normal temperature, and it is difficult to measure the free radicals of the oxide melt at high temperature.
发明内容SUMMARY OF THE INVENTION
本发明针对现有技术的缺陷，提供一种流程简单、易于操作的氧化物高温熔体的自由基测定方法。Aiming at the defects of the prior art, the present invention provides a free radical determination method of oxide high temperature melt with simple process and easy operation.
本发明所采用的技术方案具体为：The technical scheme adopted in the present invention is specifically:
将待测的氧化物粉体按质量等分成两份，分别置于两个相同的截面为多 边形的刚玉坩埚中并捣实，将所述两个刚玉坩埚均置于高温炉中，然后升温至1600℃以上，分别保温不同时间后淬冷；测量所述经不同时间保温的氧化物熔体在所述刚玉坩埚各个角处的相对平均高度差，若存在高度差则表明所述氧化物熔体在高温过程中产生了自由基，高度差越大表明该氧化物熔体在高温过程中产生自由基的越多。Divide the oxide powder to be tested into two equal parts by mass, place them in two corundum crucibles with the same polygonal cross-section and tamp them, place the two corundum crucibles in a high-temperature furnace, and then heat up to Above 1600°C, heat preservation for different times and then quench; measure the relative average height difference of the oxide melt held at different times at each corner of the corundum crucible, if there is a height difference, it indicates that the oxide melt Free radicals were generated during the high temperature process, and the larger the height difference, the more free radicals were generated in the oxide melt during the high temperature process.
进一步地，所述刚玉坩埚的截面为正三角形、正方形、正五边形或正六Further, the section of the corundum crucible is a regular triangle, a square, a regular pentagon or a regular six
边形。edge.
进一步地，所述保温时间为0.1-10小时。Further, the holding time is 0.1-10 hours.
进一步地，所述两个刚玉坩埚的保温时间差值为0.5-2小时。Further, the difference in holding time of the two corundum crucibles is 0.5-2 hours.
进一步地，所述坩埚的高度≥所述坩埚内氧化物熔体高度的3倍。Further, the height of the crucible is ≥ 3 times the height of the oxide melt in the crucible.
进一步地，所述刚玉坩埚中的Al
2O
3含量为≥99.5wt％，体积密度≥3.8g/cm
3。
Further, the Al 2 O 3 content in the corundum crucible is ≥99.5 wt %, and the bulk density is ≥3.8 g/cm 3 .
氧化物混合体在高温作用下化学键断裂速度非常快，可能发生均裂并生成自由基，如CaO离子键高温作用下发生均裂生成·Ca·和O，·其与刚玉坩埚中的Al
2O
3会产生自由基反应，释放化学能推动正三角形的刚玉坩埚的边角处的熔体显著上升，氧化物熔体中的自由基越多，其熔体上升高度越高，进而能够进行氧化物熔体的自由基测定。
The chemical bond breaking speed of the oxide mixture is very fast under the action of high temperature, and it may be homogenized and generate free radicals. For example, CaO ionic bond will be homogenized under the action of high temperature to generate Ca and O, which is combined with Al 2 O in the corundum crucible. 3. Free radical reaction will be generated, releasing chemical energy to push the melt at the corners of the equilateral triangle corundum crucible to rise significantly. Free-radical determination of melts.
本发明与现有技术相比具有如下有益效果：Compared with the prior art, the present invention has the following beneficial effects:
本发明能进行高温氧化物熔体中的自由基测定，具有流程简单和易于操作的特点。The invention can carry out the determination of free radicals in high temperature oxide melt, and has the characteristics of simple process and easy operation.
下面结合具体实施方式对本发明作进一步的描述：Below in conjunction with specific embodiment, the present invention is further described:
实施例1Example 1
本实施例中将待测的含50wt％氧化钙、35wt％氧化铝和15wt％氧化硅的氧化物混合粉体按质量等分成两份，分别置于两个相同的截面为正三角形的刚玉坩埚中并捣实，将这两个刚玉坩埚均置于高温炉中，然后升温至1600℃分别保温0.1小时和0.6小时后淬冷，测量保温不同时间的两个刚玉坩埚中的氧化物熔体在刚玉坩埚三个角处的相对平均高度差约为4mm，表明该氧化物熔体在高温过程中产生了自由基。In this example, the oxide mixed powder containing 50wt% calcium oxide, 35wt% alumina and 15wt% silicon oxide to be tested is divided into two equal parts by mass, and placed in two corundum crucibles with the same cross-section of an equilateral triangle respectively The two corundum crucibles were placed in a high-temperature furnace, then heated to 1600 °C for 0.1 hour and 0.6 hours, respectively, and then quenched. The oxide melts in the two corundum crucibles held for different times were measured at The relative average height difference at the three corners of the corundum crucible is about 4 mm, indicating that the oxide melt produced free radicals during the high temperature process.
在本实施例中，所述坩埚的高度为所述坩埚内氧化物熔体高度的3倍；所述刚玉坩埚中的Al
2O
3含量为99.5wt％，体积密度3.8g/cm
3。
In this embodiment, the height of the crucible is 3 times the height of the oxide melt in the crucible; the Al 2 O 3 content in the corundum crucible is 99.5 wt %, and the bulk density is 3.8 g/cm 3 .
本实施方式能进行高温氧化物熔体中的自由基测定，具有流程简单和易于操作的特点。This embodiment can perform free radical determination in high temperature oxide melt, and has the characteristics of simple process and easy operation.
实施例2Example 2
本实施例中将待测的含40wt％氧化钙、40wt％氧化铝和20wt％氧化硅的氧化物混合粉体按质量等分成两份，分别置于两个相同的截面为正方形的刚玉坩埚中并捣实，将这两个刚玉坩埚均置于高温炉中，然后升温至1800℃分别保温8小时和10小时后淬冷，测量保温不同时间的两个刚玉坩埚中的氧化物熔体在刚玉坩埚三个角处的相对平均高度差约为15mm，表明该氧化物熔体在高温过程中产生了自由基，且该氧化物熔体在高温过程中产生的自由基较多。In this example, the oxide mixed powder containing 40wt% calcium oxide, 40wt% alumina and 20wt% silicon oxide to be tested is divided into two equal parts by mass, and placed in two corundum crucibles with the same square cross section respectively And tamping, the two corundum crucibles were placed in a high-temperature furnace, and then heated to 1800 ° C for 8 hours and 10 hours, respectively, and then quenched, and the oxide melt in the two corundum crucibles held for different times was measured. The relative average height difference at the three corners of the crucible is about 15mm, indicating that the oxide melt produces free radicals during the high temperature process, and the oxide melt produces more free radicals during the high temperature process.
在本实施例中，所述坩埚的高度为所述坩埚内氧化物熔体高度的4倍；所述刚玉坩埚中的Al
2O
3含量为99.8wt％，体积密度4.0g/cm
3。
In this embodiment, the height of the crucible is 4 times the height of the oxide melt in the crucible; the Al 2 O 3 content in the corundum crucible is 99.8 wt %, and the bulk density is 4.0 g/cm 3 .
在其他实施方式中，所述刚玉坩埚的截面还可以为正五边形、正六边形或其他对称多边形。In other embodiments, the cross section of the corundum crucible may also be a regular pentagon, a regular hexagon or other symmetrical polygons.
应该指出，上述详细说明都是示例性的，旨在对本申请提供进一步的说明。除非另有指明，本文使用的所有技术和科学术语均具有与本申请所属技术领域的普通技术人员的通常理解所相同的含义。It should be noted that the above detailed description is exemplary and intended to provide further explanation for the present application. Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
需要注意的是，这里所使用的术语仅是为了描述具体实施方式，而非意图限制根据本申请所述的示例性实施方式。如在这里所使用的，除非上下文另外明确指出，否则单数形式也意图包括复数形式。此外，还应当理解的是，当在本说明书中使用术语“包含”和/或“包括”时，其指明存在特征、步骤、操作、器件、组件和/或它们的组合。It should be noted that the terminology used herein is for the purpose of describing specific embodiments only, and is not intended to limit the exemplary embodiments described in accordance with the present application. As used herein, the singular forms are also intended to include the plural forms unless the context clearly dictates otherwise. In addition, it should also be understood that when the terms "comprising" and/or "comprising" are used in this specification, they indicate the presence of features, steps, operations, devices, components, and/or combinations thereof.
此外，术语“包括”和“具有”以及他们的任何变形，意图在于覆盖不排他的包含。例如，包含了一系列步骤或单元的过程、方法、系统、产品或设备不必限于清楚地列出的那些步骤或单元，而是可包括没有清楚地列出的或对于这些过程、方法、产品或设备固有的其它步骤或单元。Furthermore, the terms "comprising" and "having", and any variations thereof, are intended to cover non-exclusive inclusion. For example, a process, method, system, product or device comprising a series of steps or units is not necessarily limited to those steps or units expressly listed, but may include steps or units not expressly listed or for such process, method, product or Other steps or units inherent to the device.
以上所述仅为本发明的优选实施例而已，并不用于限制本发明，对于本领域的技术人员来说，本发明可以有各种更改和变化。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and changes. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.
Claims (6)
- 一种高温氧化物熔体的自由基测定方法，其特征在于：A kind of free radical determination method of high temperature oxide melt is characterized in that:将待测的氧化物粉体按质量等分成两份，分别置于两个相同的截面为多边形的刚玉坩埚中并捣实，将所述两个刚玉坩埚均置于高温炉中，然后升温至1600℃以上，分别保温不同时间后淬冷；Divide the oxide powder to be tested into two equal parts by mass, place them in two corundum crucibles with the same polygonal cross-section and tamp them, place the two corundum crucibles in a high-temperature furnace, and then heat up to Above 1600℃, quench after holding for different time respectively;测量所述经不同时间保温的氧化物熔体在所述刚玉坩埚各个角处的相对平均高度差，若存在高度差则表明所述氧化物熔体在高温过程中产生了自由基，高度差越大表明该氧化物熔体在高温过程中产生自由基的越多。Measure the relative average height difference of the oxide melt held at different times at each corner of the corundum crucible. If there is a height difference, it means that the oxide melt has produced free radicals during the high temperature process. Larger indicates that the oxide melt generates more free radicals during high temperature.
- 根据权利要求1所述的一种高温氧化物熔体的自由基测定方法，其特征在于：所述刚玉坩埚的截面为正三角形、正方形、正五边形或正六边形。The method for measuring free radicals in a high temperature oxide melt according to claim 1, wherein the cross section of the corundum crucible is a regular triangle, a square, a regular pentagon or a regular hexagon.
- 根据权利要求1所述的一种高温氧化物熔体的自由基测定方法，其特征在于：所述保温时间为0.1-10小时。The method for measuring free radicals in a high temperature oxide melt according to claim 1, wherein the holding time is 0.1-10 hours.
- 根据权利要求1所述的一种高温氧化物熔体的自由基测定方法，其特征在于：所述两个刚玉坩埚的保温时间差值为0.5-2小时。The method for measuring free radicals in a high temperature oxide melt according to claim 1, wherein the difference in the holding time of the two corundum crucibles is 0.5-2 hours.
- 根据权利要求1所述的一种高温氧化物熔体的自由基测定方法，其特征在于：所述坩埚的高度≥所述坩埚内氧化物熔体高度的3倍。The method for measuring free radicals in a high temperature oxide melt according to claim 1, wherein the height of the crucible is ≥ 3 times the height of the oxide melt in the crucible.
- 根据权利要求1所述的一种高温氧化物熔体的自由基测定方法，其特征在于：所述刚玉坩埚中的Al 2O 3含量为≥99.5wt％，体积密度≥3.8g/cm 3。 The method for measuring free radicals in a high temperature oxide melt according to claim 1, wherein the Al 2 O 3 content in the corundum crucible is ≥99.5wt%, and the bulk density is ≥3.8g/cm 3 .
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