CN1552788A - A high-temperature conductive bonding material for aluminum electrolysis - Google Patents
A high-temperature conductive bonding material for aluminum electrolysis Download PDFInfo
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000005868 electrolysis reaction Methods 0.000 title claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 57
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 42
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- RHZUVFJBSILHOK-UHFFFAOYSA-N anthracen-1-ylmethanolate Chemical compound C1=CC=C2C=C3C(C[O-])=CC=CC3=CC2=C1 RHZUVFJBSILHOK-UHFFFAOYSA-N 0.000 claims description 8
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- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 description 2
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Abstract
Description
技术领域：Technical field:
本发明与铝电解有关，特别涉及铝电解碳素阳极、碳素阴极、惰性阳极、TiB2可润湿性阴极的连接，以及它们与金属导体连接用的高温导电粘结材料，它还适用于其他高温环境下材料间的导电连接。The present invention is related to aluminum electrolysis, in particular to the connection of aluminum electrolytic carbon anode, carbon cathode, inert anode, TiB2 wettable cathode, and their high-temperature conductive bonding materials for connecting with metal conductors, and it is also applicable to Conductive connection between materials in other high temperature environments.
背景技术：Background technique:
目前，铝电解采用的阴、阳极材料都是碳素材料。阳极碳块与导电钢棒间由磷生铁浇铸粘结；连续式预焙阳极间采用碳质糊料粘结；阴极炭块和阴极导电钢棒间采用炭质糊料捣固或磷生铁浇铸粘结；从而使炭块与炭块或钢棒间紧密连接并起到导电作用。At present, the cathode and anode materials used in aluminum electrolysis are all carbon materials. The anode carbon block and the conductive steel rod are bonded by casting phosphorus pig iron; the continuous prebaked anode is bonded by carbon paste; the cathode carbon block and the cathode conductive steel rod are bonded by carbon paste or phosphorus pig iron casting knot; so that the carbon block and the carbon block or steel rod are closely connected and play a conductive role.
采用碳素阳极和碳素阴极的现行熔盐铝电解工艺存在能耗高、碳耗大、成本高、环境污染严重、生产不稳定等问题。采用惰性阳极和TiB2可润湿性阴极的新型电解槽及其电解新工艺，可望解决上述问题，改革现有生产工艺，实现铝电解生产过程的低能耗，无污染和低成本等目标。然而惰性阳极材料主要有金属氧化物陶瓷、合金阳极和金属陶瓷三类，其中，除合金阳极外，金属氧化物陶瓷和金属陶瓷惰性阳极都存在与金属导杆连接困难的问题；TiB2可润湿性阴极可分为TiB2涂层、TiB2-C复合材料和TiB2基复合陶瓷三类，其中TiB2-C复合材料和TiB2基复合陶瓷也存在与金属导杆连接困难这一难题。The current molten salt aluminum electrolysis process using carbon anode and carbon cathode has problems such as high energy consumption, high carbon consumption, high cost, serious environmental pollution, and unstable production. The new electrolytic cell and its new electrolysis process using inert anode and TiB2 wettable cathode are expected to solve the above problems, reform the existing production process, and achieve the goals of low energy consumption, no pollution and low cost in the aluminum electrolysis production process. However, inert anode materials mainly include metal oxide ceramics, alloy anodes and cermets. Among them, except alloy anodes, metal oxide ceramics and cermet inert anodes have the problem of difficulty in connecting with metal guide rods; TiB 2 can wet Wet cathodes can be divided into three categories: TiB 2 coatings, TiB 2 -C composite materials and TiB 2 based composite ceramics, among which TiB 2 -C composite materials and TiB 2 based composite ceramics also have the difficulty of connecting with metal guide rods .
发明内容：Invention content:
本发明的目的就是开发出具有良好导电性，粘结强度高的可用于惰性阳极和TiB2可润湿性阴极与相应金属导杆连接的高温导电粘结材料，取代目前所用的阳极炭块与阳极钢爪(棒)连接用浇铸磷生铁或炭质糊料、连续式预焙阳极炭块粘结用炭质糊料、阴极炭块与阴极炭块连接用粘结剂、阴极炭块与阴极钢棒连接用浇铸磷生铁或炭质捣固糊等；用作惰性阳极与阳极导杆的连接，TiB2可润湿性阴极与阴极钢棒的连接用高温导电粘结材料；用它处理的电极在铝电解工艺过程中生产稳定、能耗降低、环境污染减小。The purpose of the present invention is to develop a high-temperature conductive bonding material with good conductivity and high bonding strength that can be used for the connection of the inert anode and the wettable cathode of TiB with the corresponding metal guide rod, to replace the currently used anode carbon block and Cast phosphorus pig iron or carbon paste for anode steel claw (rod) connection, carbon paste for continuous prebaked anode carbon block bonding, binder for cathode carbon block and cathode carbon block connection, cathode carbon block and cathode Cast phosphorus pig iron or carbon tamping paste for steel rod connection; used for connection between inert anode and anode guide rod, high-temperature conductive bonding material for connection between TiB 2 wettable cathode and cathode steel rod; treated with it The production of the electrode is stable during the aluminum electrolysis process, the energy consumption is reduced, and the environmental pollution is reduced.
本发明所设计的铝电解用高温导电粘结材料其特征在于：糊料配方如表1所示。The high-temperature conductive bonding material for aluminum electrolysis designed in the present invention is characterized in that the paste formula is shown in Table 1.
表1 铝电解用高温导电粘结材料的糊料配方
上述高温导电粘结材料的糊料配方包括导电功能材料粉末、树脂粘结剂、固化剂、溶剂、增强添加剂和其它添加剂等，其中The paste formula of the above-mentioned high-temperature conductive bonding material includes conductive functional material powder, resin binder, curing agent, solvent, reinforcing additive and other additives, etc., wherein
I.导电功能材料粉末为下述三种中的至少一种：I. Conductive functional material powder is at least one of the following three types:
①金属粉末：包括Cu、Fe、Ni、Co、Cr、Mn、Ti、Nb、Ta、W、Mo、Ti、Ag、Au、Pt金属粉末；① Metal powder: including Cu, Fe, Ni, Co, Cr, Mn, Ti, Nb, Ta, W, Mo, Ti, Ag, Au, Pt metal powder;
②导电陶瓷粉末：包括TiB2、ZrB2、TiC、ZrC粉末；②Conductive ceramic powder: including TiB 2 , ZrB 2 , TiC, ZrC powder;
③石墨粉和其它炭质粉末：包括石油焦、冶金焦、沥青焦、煅后无烟煤粉末；③Graphite powder and other carbonaceous powders: including petroleum coke, metallurgical coke, pitch coke, calcined anthracite powder;
且分三种不同粒度，粒径分别为：小于10μm、10～149μm和149～250μm；And it is divided into three different particle sizes, the particle sizes are: less than 10 μm, 10-149 μm and 149-250 μm;
II.树脂粘结剂为呋喃树脂、酚醛树脂、E51环氧树脂、E44环氧树脂、E42环氧树脂中的至少一种；II. The resin binder is at least one of furan resin, phenolic resin, E 51 epoxy resin, E 44 epoxy resin, E 42 epoxy resin;
III.固化剂为乙酸丁脂、对甲苯磺酸、磷酸乙脂、硫酸乙脂和无机酸，包括H2SO4、H3PO4中的至少一种；III. The curing agent is butyl acetate, p-toluenesulfonic acid, ethyl phosphate, ethyl sulfate and inorganic acid, including at least one of H 2 SO 4 and H 3 PO 4 ;
IV.溶剂为乙醇和丙酮中的至少一种；IV. solvent is at least one in ethanol and acetone;
V.增强添加剂包括碳纤维和碳纤维粉等；V. Reinforcing additives include carbon fiber and carbon fiber powder, etc.;
其它添加剂为煤焦油和氧化沥青粉中的至少一种。Other additives are at least one of coal tar and oxidized pitch powder.
本发明的发明的优点和积极效果表现在：The advantages and positive effects of the invention of the present invention are as follows:
高温导电粘结材料具备良好的粘结强度、导电性、高温力学性能和抗热冲击性能。The high-temperature conductive bonding material has good bond strength, electrical conductivity, high-temperature mechanical properties and thermal shock resistance.
高温导电粘结材料实现了常温下固化，免去了高温固化所需的加热设备及人力物力，降低了应用成本，广泛应用于铝电解生产等高温条件下各种高温导电材料间的连接及其与金属导体间的连接。The high-temperature conductive bonding material can be cured at room temperature, eliminating the need for heating equipment, manpower and material resources required for high-temperature curing, and reducing application costs. It is widely used in the connection of various high-temperature conductive materials and their connection to metal conductors.
高温导电粘结材料分别针对铝电解用阳极炭块、阴极炭块、金属氧化物陶瓷惰性阳极、金属陶瓷惰性阳极、TiB2可润湿性阴极：包括TiB2-C复合材料和TiB2基复合陶瓷、阳极钢爪或导杆和阴极钢棒等高温导电材料的物理化学特性而配备；根据具体应用对象调整其热膨胀性能，保持良好的与被粘结高温导电材料的热匹配性，保证了粘结材料在高温使用过程中，不分层、不开裂、不脱落，生产稳定，能耗降低，环境污染减少。High-temperature conductive bonding materials are respectively aimed at anode carbon blocks, cathode carbon blocks, metal oxide ceramic inert anodes, cermet inert anodes, and TiB 2 wettable cathodes for aluminum electrolysis: including TiB 2 -C composite materials and TiB 2 based composites It is equipped according to the physical and chemical properties of high-temperature conductive materials such as ceramics, anode steel claws or guide rods and cathode steel rods; adjust its thermal expansion performance according to specific application objects, maintain good thermal matching with the high-temperature conductive materials to be bonded, and ensure adhesion. In the process of high temperature use, the junction material will not delaminate, crack or fall off, and the production is stable, energy consumption is reduced, and environmental pollution is reduced.
具体实施方式：Detailed ways:
实施例1：一种连续式预焙阳极碳块连接用高温导电粘结材料。高温导电粘结材料的糊料配方见表2。Embodiment 1: A high-temperature conductive bonding material for connecting continuous prebaked anode carbon blocks. The paste formula of the high temperature conductive bonding material is shown in Table 2.
表2 连续式预焙阳极碳块连接用高温导电粘结材料的糊料配方实例
将表2中的各物料混合成糊料，连接连续式预焙阳极炭块，炭块间粘结强度为3MPa，大于铝电解用预焙阳极炭块的抗拉强度；随着温度的升高，粘结材料的电阻率急剧下降，25℃下电阻率为5×10-3Ωm，150℃下电阻率为3×10-4Ωm，400℃下电阻率为4×10-5Ωm(与相同条件下预焙阳极炭块的电阻率相当)，800℃下电阻率为1.9×10-5Ωm，低于相同条件下预焙阳极炭块的电阻率；连续式预焙阳极炭块在使用条件下的导电性能良好，连接处无裂纹，不脱落。Mix the materials in Table 2 into a paste, connect the continuous prebaked anode carbon blocks, the bond strength between the carbon blocks is 3MPa, which is greater than the tensile strength of the prebaked anode carbon blocks for aluminum electrolysis; with the increase of temperature , the resistivity of the bonding material drops sharply, the resistivity at 25°C is 5×10 -3 Ωm, the resistivity at 150°C is 3×10 -4 Ωm, and the resistivity at 400°C is 4×10 -5 Ωm (compared to Under the same conditions, the resistivity of prebaked anode carbon blocks is equivalent), and the resistivity at 800 ° C is 1.9×10 -5 Ωm, which is lower than that of prebaked anode carbon blocks under the same conditions; continuous prebaked anode carbon blocks are used The electrical conductivity under the condition is good, there is no crack at the connection, and it does not fall off.
实施例2：一种惰性阳极与金属导杆连接用高温导电粘结材料。Embodiment 2: A high-temperature conductive bonding material for connecting an inert anode to a metal guide rod.
表3惰性阳极与金属导杆连接用高温导电粘结材料的糊料配方实例
将表3中的各物料混合成糊料，涂抹于含10wt％Ni的NiFe2O4/Ni金属陶瓷惰性阳极与不锈钢导杆的连接处，室温固化2h后，即具备良好的粘结强度；然后将惰性阳极试样悬挂于试验铝电解槽上方，在高温电阻炉内随同试验电解槽一起升温到970℃，在此升温过程中高温导电粘结材料的粘结剂发生炭化；待电解质熔化后，将惰性阳极插入电解质，1A/cm2下通电电解10h，同时测试电解槽的槽电压。在整个电解过程中，槽电压基本恒定在2.7V，说明所用高温导电粘结材料的导电性能良好。电解完成后，直接取出阳极试样在空气中冷却，结果发现金属陶瓷惰性阳极与不锈钢导杆的连接处无裂纹，不脱落，表明所用高温导电粘结材料具有良好的粘结强度、抗热震性和高温力学性能。Mix the materials in Table 3 into a paste, apply it on the joint of the NiFe 2 O 4 /Ni cermet inert anode containing 10wt% Ni and the stainless steel guide rod, and after curing at room temperature for 2 hours, it has good bonding strength; Then hang the inert anode sample above the test aluminum electrolytic cell, and heat it up to 970°C together with the test electrolytic cell in the high-temperature resistance furnace. During this heating process, the binder of the high-temperature conductive bonding material is carbonized; after the electrolyte is melted , Insert the inert anode into the electrolyte, conduct electrolysis at 1A/cm 2 for 10 hours, and test the cell voltage of the electrolytic cell at the same time. During the whole electrolysis process, the cell voltage was basically constant at 2.7V, which indicated that the high-temperature conductive bonding material used had good conductivity. After the electrolysis was completed, the anode sample was directly taken out and cooled in the air. It was found that there was no crack at the connection between the cermet inert anode and the stainless steel guide rod, and it did not fall off, indicating that the high-temperature conductive bonding material used had good bonding strength and thermal shock resistance. and high temperature mechanical properties.
实施例3：一种阴极炭块与阴极钢棒连接用高温导电粘结材料。Embodiment 3: A high-temperature conductive bonding material for connecting cathode carbon blocks and cathode steel rods.
表4 阴极炭块与阴极钢棒连接用高温导电粘结材料的糊料配方实例
将表4中的各物料混合成糊料，用于阴极炭块与阴极钢棒的连接，室温固化2h后，用于铝电解槽的砌筑。铝电解槽焙烧启动和正常生产过程中，阴极电流分布均匀，未见阴极钢棒发红，阴极钢棒与阴极母线连接处的温度为100～250℃，表明所用高温导电粘结材料的导电性能良好，使用条件下材料内部无裂纹、分层等缺陷。Mix the materials in Table 4 into a paste, which is used for the connection of the cathode carbon block and the cathode steel rod. After curing at room temperature for 2 hours, it is used for the masonry of the aluminum electrolytic cell. During the firing start-up and normal production process of the aluminum electrolytic cell, the cathode current distribution is uniform, no redness of the cathode steel rod is seen, and the temperature at the junction of the cathode steel rod and the cathode bus bar is 100-250 ° C, indicating the conductivity of the high-temperature conductive bonding material used Good, there are no cracks, delamination and other defects inside the material under the conditions of use.
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