CN101280433B - Connection method and alloy material of titanium-based noble metal electrode and cathode in electrolysis device - Google Patents
Connection method and alloy material of titanium-based noble metal electrode and cathode in electrolysis device Download PDFInfo
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- 239000010936 titanium Substances 0.000 title claims abstract description 36
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000005868 electrolysis reaction Methods 0.000 title claims abstract description 30
- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 14
- 239000000956 alloy Substances 0.000 title claims abstract description 12
- 239000010949 copper Substances 0.000 claims abstract description 40
- 229910052802 copper Inorganic materials 0.000 claims abstract description 38
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910000978 Pb alloy Inorganic materials 0.000 claims abstract description 28
- 239000011133 lead Substances 0.000 claims abstract description 26
- 229910000679 solder Inorganic materials 0.000 claims abstract description 18
- 229910052718 tin Inorganic materials 0.000 claims abstract description 17
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002131 composite material Substances 0.000 claims abstract description 8
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 5
- 229910052751 metal Inorganic materials 0.000 claims abstract description 5
- 239000002184 metal Substances 0.000 claims abstract description 5
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000007598 dipping method Methods 0.000 claims abstract 2
- 229910020220 Pb—Sn Inorganic materials 0.000 claims description 9
- 238000007654 immersion Methods 0.000 claims description 9
- 238000003466 welding Methods 0.000 claims description 9
- 239000007769 metal material Substances 0.000 claims description 6
- 229910020935 Sn-Sb Inorganic materials 0.000 claims description 5
- 229910008757 Sn—Sb Inorganic materials 0.000 claims description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 24
- 238000005265 energy consumption Methods 0.000 abstract description 7
- 238000012423 maintenance Methods 0.000 abstract description 6
- 238000005476 soldering Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 description 23
- 230000015572 biosynthetic process Effects 0.000 description 21
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 12
- 238000005516 engineering process Methods 0.000 description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000001384 succinic acid Substances 0.000 description 5
- 230000002378 acidificating effect Effects 0.000 description 4
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 4
- 239000008151 electrolyte solution Substances 0.000 description 4
- 229940021013 electrolyte solution Drugs 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- ZACYQVZHFIYKMW-UHFFFAOYSA-N iridium titanium Chemical compound [Ti].[Ir] ZACYQVZHFIYKMW-UHFFFAOYSA-N 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 239000010406 cathode material Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229910020816 Sn Pb Inorganic materials 0.000 description 1
- 229910001128 Sn alloy Inorganic materials 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000012993 chemical processing Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Abstract
本发明提供了一种电解装置中钛基贵金属电极与阴极连接方法，所述方法为：以铜棒表面包覆钛层的钛/铜复合棒为极耳，所述钛/铜复合棒端部为裸露的铜棒，对裸露的铜棒表面处理得到洁净的铜表面，干燥后，180～300℃下对铜表面进行浸锡处理，浸锡处理后用铅或铅合金焊料将铜棒与阴极焊接；所述铅或铅合金焊料表达式为Pb-xSb-yAg-zM，M为Cu、Sn、Bi中的一种或多种，x、y、z为Sb、Ag、M与Pb的质量之比，x＝0～0.2；y＝0～0.2；z＝0～0.1，所述的阴极为金属或合金制成。本发明具有连接可靠、接触电阻小、槽电压低等优点，能大幅度减少电解生产中的能耗，降低生产成本；而且连接可靠，能减少生产过程中设备维修时间，保证电解生产过程的可靠连续进行。The invention provides a method for connecting a titanium-based noble metal electrode and a cathode in an electrolysis device. The method is as follows: a titanium/copper composite rod coated with a titanium layer on the surface of a copper rod is used as a tab, and the end of the titanium/copper composite rod is It is a bare copper rod, and the surface of the bare copper rod is treated to obtain a clean copper surface. After drying, the copper surface is dipped in tin at 180-300 ° C. After the tin dipping treatment, the copper rod and the cathode are connected with lead or lead alloy solder. Soldering; the expression of the lead or lead alloy solder is Pb-xSb-yAg-zM, M is one or more of Cu, Sn, Bi, and x, y, z are the quality of Sb, Ag, M and Pb Ratio, x=0-0.2; y=0-0.2; z=0-0.1, the cathode is made of metal or alloy. The invention has the advantages of reliable connection, small contact resistance, low cell voltage, etc., can greatly reduce energy consumption in electrolysis production, and reduce production cost; moreover, the connection is reliable, can reduce equipment maintenance time in the production process, and ensure the reliability of the electrolysis production process Continuously.
Description
(一)技术领域(1) Technical field
本发明涉及一种电解装置中钛基贵金属电极与阴极连接方法，以及用于连接钛基贵金属电极与阴极的合金材料，适用于采用酸性或中性电解液的电解合成体系，尤其适合于工业化规模生产丁二酸的电解装置中的钛铱电极与铅或铅合金电极之间的连接。The invention relates to a method for connecting a titanium-based noble metal electrode and a cathode in an electrolysis device, and an alloy material used for connecting a titanium-based noble metal electrode and a cathode, which is suitable for an electrolytic synthesis system using an acidic or neutral electrolyte, and is especially suitable for an industrial scale Connection between titanium-iridium electrodes and lead or lead alloy electrodes in electrolysis plants for the production of succinic acid.
(二)背景技术(2) Background technology
电解合成是采用直流电解手段在电极表面进行电化学反应而生成新物质的一种合成技术，与传统的化学合成方法相比，电解法合成化学物质，利用电子作为清洁的反应剂，反应控制方便，反应选择性高，反应在常温常压下进行，合成条件温和，无需特殊的加热或加压设备，反应装置通用性好，具有许多常规化学合成方法无法相比的优点。更重要的是，采用电解法合成化学物质，产物分离和精致容易，产物纯度高，对环境的污染大幅度降低，很多体系可实现完全无污染，因此是一种对环境友好的绿色清洁合成技术。虽然电解合成通常需要消耗较多的电能，但从未来长远考虑，电能将成为未来化学加工的主要能源，结合越来越严重的环境问题，电解合成技术无疑是一种高效率的化学合成方法。Electrolytic synthesis is a synthesis technology that uses direct current electrolysis to perform electrochemical reactions on the electrode surface to generate new substances. Compared with traditional chemical synthesis methods, electrolytic synthesis of chemical substances uses electrons as clean reactants, and the reaction control is convenient. , the reaction selectivity is high, the reaction is carried out at normal temperature and pressure, the synthesis conditions are mild, no special heating or pressurization equipment is required, the reaction device is versatile, and has many advantages that cannot be compared with conventional chemical synthesis methods. More importantly, chemical substances are synthesized by electrolysis, the product is easy to separate and refine, the product is high in purity, and the pollution to the environment is greatly reduced. Many systems can be completely pollution-free, so it is an environmentally friendly green and clean synthesis technology . Although electrolytic synthesis usually consumes a lot of electric energy, in the long run, electric energy will become the main energy source for chemical processing in the future. Combined with increasingly serious environmental problems, electrolytic synthesis technology is undoubtedly a high-efficiency chemical synthesis method.
近20年来，美国、日本和欧盟各国对电解合成工艺的开发和应用非常活跃，迄今达到工业化生产或中试阶段的电解合成产品已逾百种，其中医药、香料、农药等高附加值的精细化学品的电解合成是主要的开发方向，相关的专利数在近年也大幅度上升。据估计，利用电解合成技术可以制备的有机产品可达八千种以上，表明了电解合成工艺的广阔发展空间。In the past 20 years, the United States, Japan and the European Union have been very active in the development and application of electrolytic synthesis technology. So far, more than 100 kinds of electrolytic synthesis products have reached the stage of industrial production or pilot test, including pharmaceuticals, spices, pesticides and other high value-added fine products. The electrolytic synthesis of chemicals is the main development direction, and the number of related patents has also increased significantly in recent years. It is estimated that more than 8,000 kinds of organic products can be prepared by electrolytic synthesis technology, which shows the broad development space of electrolytic synthesis technology.
电解槽是电解合成的关键技术之一，选择和设计结构紧凑、工作可靠、加工容易、成本低廉的电解槽，是电解合成工艺成功的可靠保证。目前已经在工业生产上采用的电解槽已经有很多类型，取得成功的也不在少数。无论哪种类型的电解槽，其中的阳极和阴极之间的连接虽然从表面看是一个并不重要的小问题，但在实际生产中，电极之间的连接却非常重要，可靠的连接不仅能保证电解过程的连续顺利进行，减少设备检修和维护，同时能大幅度降低工业槽电压，减少生产成本。尤其对采用酸性电解质溶液的合成体系，更是如此。The electrolytic cell is one of the key technologies of electrolytic synthesis. Selecting and designing an electrolytic cell with compact structure, reliable operation, easy processing and low cost is a reliable guarantee for the success of the electrolytic synthesis process. There are many types of electrolyzers that have been used in industrial production at present, and there are not a few of them that have achieved success. Regardless of the type of electrolytic cell, although the connection between the anode and the cathode is an unimportant small problem on the surface, in actual production, the connection between the electrodes is very important. Reliable connections can not only Ensure the continuous and smooth electrolysis process, reduce equipment overhaul and maintenance, and at the same time greatly reduce the voltage of the industrial tank and reduce production costs. This is especially true for synthesis systems using acidic electrolyte solutions.
对目前已经实现工业化生产的一些化工产品，如丁二酸，其电解合成采用硫酸水溶液作为电解质溶液，反应温度在50～80℃，这样的合成条件对一般金属材料的腐蚀性很强，因此阳极采用耐腐蚀性高的钛基Ir/Ti涂层电极，而负极采用耐酸腐蚀的铅或铅合金。目前钛电极和铅电极的连接一般采用机械方式连接，即采用螺钉紧固的方法将钛电极和铅电极连接在一起。由于钛电极导电性差，且表面生成一层近乎绝缘的致密氧化物层，因此机械方法连接处电阻很大，实际电解过程中连接处电压降很大，发热严重，不仅增加了电解电耗，而且由于发热经常导致铅电极熔化，电极连接失效，使电解生产过程中断，增加了维修的困难。For some chemical products that have been industrialized at present, such as succinic acid, the electrolytic synthesis uses sulfuric acid aqueous solution as the electrolyte solution, and the reaction temperature is 50-80°C. Such synthesis conditions are very corrosive to general metal materials, so the anode A titanium-based Ir/Ti coated electrode with high corrosion resistance is used, while the negative electrode is made of acid-resistant lead or lead alloy. At present, the titanium electrode and the lead electrode are generally connected by mechanical means, that is, the titanium electrode and the lead electrode are connected together by screw fastening. Due to the poor conductivity of the titanium electrode and the formation of a dense oxide layer that is nearly insulating on the surface, the resistance of the mechanical connection is very large. In the actual electrolysis process, the voltage drop at the connection is large and the heat is serious. Due to heat, the lead electrode is often melted, and the electrode connection fails, which interrupts the electrolytic production process and increases the difficulty of maintenance.
针对电解合成生产中实际存在的问题，本发明提出了一种电解装置中贵金属电极与其它电极的连接方法，对不同类型的电解装置均适用。尤其对采用中性或酸性电解质溶液的体系，采用本发明的电极连接方法，具有连接可靠、操作简单、接触电阻小等优点，能可靠的将钛基贵金属电极与一般的阴极材料连接在一起，且电极之间的连接电阻小，能大幅度降低接触电阻，减少电解生产中的能耗，降低成本；而且连接可靠，能减少生产过程中设备维修时间，保证电解生产过程的可靠连续进行。Aiming at the problems actually existing in electrolytic synthesis production, the present invention proposes a connection method between noble metal electrodes and other electrodes in an electrolytic device, which is applicable to different types of electrolytic devices. Especially for systems using neutral or acidic electrolyte solutions, the electrode connection method of the present invention has the advantages of reliable connection, simple operation, small contact resistance, etc., and can reliably connect titanium-based noble metal electrodes with general cathode materials. And the connection resistance between the electrodes is small, which can greatly reduce the contact resistance, reduce the energy consumption in the electrolysis production, and reduce the cost; and the connection is reliable, which can reduce the maintenance time of the equipment in the production process and ensure the reliable and continuous operation of the electrolysis production process.
(三)发明内容(3) Contents of the invention
本发明目的是提供一种电解装置中钛基贵金属电极与阴极连接方法，以大幅度降低接触电阻、降低能耗，并保证电解生产过程的可靠连续进行。The purpose of the present invention is to provide a method for connecting titanium-based noble metal electrodes and cathodes in an electrolysis device, so as to greatly reduce contact resistance, reduce energy consumption, and ensure reliable and continuous electrolysis production process.
本发明采用的技术方案是：The technical scheme adopted in the present invention is:
一种电解装置中钛基贵金属电极与阴极连接方法，所述方法为：以铜棒表面包覆钛层的钛/铜复合棒为极耳，所述钛/铜复合棒端部为裸露的铜棒，对裸露的铜棒表面处理得到洁净的铜表面，干燥后，180～300℃下对铜表面进行浸锡处理，浸锡处理后用铅或铅合金焊料将铜棒与阴极焊接；所述铅或铅合金焊料表达式为Pb-xSb-yAg-zM，其中M为Cu、Sn、Bi中的一种或多种，x、y、z为Sb、Ag、M与Pb的质量之比，x＝0～0.2；y＝0～0.2；z＝0～0.1，所述的阴极为金属或合金制成。A method for connecting a titanium-based noble metal electrode to a cathode in an electrolysis device, the method comprising: using a titanium/copper composite rod covered with a titanium layer on the surface of a copper rod as a tab, and the end of the titanium/copper composite rod is bare copper Rod, the exposed copper rod surface is treated to obtain a clean copper surface, after drying, the copper surface is subjected to immersion tin treatment at 180-300 °C, and after the tin immersion treatment, the copper rod and the cathode are welded with lead or lead alloy solder; The expression of lead or lead alloy solder is Pb-xSb-yAg-zM, where M is one or more of Cu, Sn, Bi, and x, y, z are the mass ratios of Sb, Ag, M to Pb, x=0-0.2; y=0-0.2; z=0-0.1, the cathode is made of metal or alloy.
所述的阴极采用的金属材料或合金为常见用于阴极的金属材料或合金材料：铅或铅合金、不锈钢、镍、铁或铜及其它金属材料，对于铅或者铅合金电极，可直接进行焊接处理，采用其他的金属材料作为阴极，则可采用与阳极同样的浸锡处理后，再进行焊接。The metal material or alloy used in the cathode is a metal material or alloy material commonly used in the cathode: lead or lead alloy, stainless steel, nickel, iron or copper and other metal materials, for lead or lead alloy electrodes, can be directly welded If other metal materials are used as the cathode, the same immersion tin treatment as the anode can be used before welding.
所述极耳的结构如附图1所示，可直接向钛合金制造企业定制，也可利用现有钛/铜复合棒，进行机械加工刨去钛/铜复合棒头部的钛层，露出里面的紫铜。The structure of the tab is shown in Figure 1, which can be directly customized to the titanium alloy manufacturing enterprise, or the existing titanium/copper composite rod can be used to machine the titanium layer on the head of the titanium/copper composite rod to expose Copper inside.
本发明方法对不同类型的电解装置均适用。尤其对采用中性或酸性电解质溶液的体系，采用本发明的电极连接方法，具有连接可靠、操作简单、接触电阻小等优点，能可靠的将钛基贵金属电极与一般的阴极材料连接在一起，且电极之间的连接电阻小，能大幅度降低接触电阻，减少电解生产中的能耗，降低成本；而且连接可靠，能减少生产过程中设备维修时间，保证电解生产过程的可靠连续进行。The method of the invention is applicable to different types of electrolysis devices. Especially for systems using neutral or acidic electrolyte solutions, the electrode connection method of the present invention has the advantages of reliable connection, simple operation, small contact resistance, etc., and can reliably connect titanium-based noble metal electrodes with general cathode materials. And the connection resistance between the electrodes is small, which can greatly reduce the contact resistance, reduce the energy consumption in the electrolysis production, and reduce the cost; and the connection is reliable, which can reduce the maintenance time of the equipment in the production process and ensure the reliable and continuous operation of the electrolysis production process.
所述浸锡处理为浸纯锡或市售常规的Pb-Sn或Pb-Sn-Sb焊料。The immersion tin treatment is pure tin or commercially available conventional Pb-Sn or Pb-Sn-Sb solder.
所述焊接利用焊接模具进行，将裸露的铜棒、阴极分别和焊接模具焊接，再往模具中倒入熔化的铅或铅合金焊料，加热使铅或铅合金焊料熔化均匀，冷却后除去模具。The welding is carried out by using a welding mold, welding the exposed copper rod and cathode to the welding mold respectively, pouring molten lead or lead alloy solder into the mold, heating to melt the lead or lead alloy solder evenly, and removing the mold after cooling.
本发明还涉及用于连接钛基贵金属电极与阴极的合金材料，所述合金材料作为焊料用于钛基贵金属电极与阴极的连接，所述的合金材料为多组分铅合金，表达式为Pb-xSb-yAg-zM，其中M为Cu、Sn、Bi中的一种或多种，x、y、z分别为Sb、Ag、M与Pb的质量之比，x＝0～0.2；y＝0～0.2；z＝0～0.1、x、y、z不同时为0。The present invention also relates to an alloy material used for connecting titanium-based noble metal electrodes and cathodes. The alloy material is used as solder for the connection between titanium-based noble metal electrodes and cathodes. The alloy material is a multi-component lead alloy, expressed as Pb -xSb-yAg-zM, wherein M is one or more of Cu, Sn, Bi, x, y, z are respectively the mass ratio of Sb, Ag, M and Pb, x=0～0.2; y= 0 to 0.2; z=0 to 0.1, x, y, and z are not 0 at the same time.
常用的，所述铅合金表达式为：Pb-xSb，x＝0.05～0.08；或者Pb-yAg，y＝0.005～0.01。优选的，所述铅合金表达式为：Pb-xSb-yAg，x＝0.05～0.08；y＝0.005～0.01。或者，所述铅合金表达式为：Pb-xSb-yAg-zM，x＝0.05～0.08；y＝0.005～0.01，z＝0.01～0.05，M为Cu、Sn中的一种或两种。Usually, the expression of the lead alloy is: Pb-xSb, x=0.05-0.08; or Pb-yAg, y=0.005-0.01. Preferably, the expression of the lead alloy is: Pb-xSb-yAg, x=0.05-0.08; y=0.005-0.01. Alternatively, the expression of the lead alloy is: Pb-xSb-yAg-zM, x=0.05-0.08; y=0.005-0.01, z=0.01-0.05, M is one or both of Cu and Sn.
更为优选的，所述铅合金表达式为：Pb-0.05Sb-0.005Ag-0.01Cu。或者，所述铅合金表达式为：Pb-0.05Sb-0.005Ag-0.01Cu-0.02Sn。More preferably, the expression of the lead alloy is: Pb-0.05Sb-0.005Ag-0.01Cu. Alternatively, the expression of the lead alloy is: Pb-0.05Sb-0.005Ag-0.01Cu-0.02Sn.
本发明和现有的机械连接方式相比，具有连接可靠、接触电阻小、槽电压低等优点，能大幅度减少电解生产中的能耗，降低生产成本；而且连接可靠，能减少生产过程中设备维修时间，保证电解生产过程的可靠连续进行。Compared with the existing mechanical connection method, the present invention has the advantages of reliable connection, small contact resistance, low cell voltage, etc., can greatly reduce energy consumption in electrolytic production, and reduce production cost; Equipment maintenance time, to ensure reliable and continuous electrolysis production process.
(四)附图说明(4) Description of drawings
图1为本发明的贵金属电极上导电Ti/Cu极耳结构示意图；1为螺孔，2为铜，3为钛；Fig. 1 is a schematic diagram of the conductive Ti/Cu tab structure on the noble metal electrode of the present invention; 1 is a screw hole, 2 is copper, and 3 is titanium;
图2为本发明的金属电极的导电Ti/Cu极耳与铅或铅合金电极的连接示意图；4为铅或铅合金焊接层，5为钛基贵金属极耳，6为阴极极耳。Fig. 2 is the connection diagram of the conductive Ti/Cu tab of the metal electrode of the present invention and the lead or lead alloy electrode; 4 is the lead or lead alloy welding layer, 5 is the titanium-based noble metal tab, and 6 is the cathode tab.
(五)具体实施方式(5) Specific implementation methods
下面结合具体实施例对本发明进行进一步描述，但本发明的保护范围并不仅限于此：The present invention is further described below in conjunction with specific embodiment, but protection scope of the present invention is not limited thereto:
实施例1：Example 1:
某企业无隔膜电解合成丁二酸的电解装置，由40单元槽串联，阳极采用钛铱电极，阴极采用铅合金电极(Pb-0.08Sb-0.005Ag电极)，电解合成丁二酸时，电解液为饱和丁二酸的6％硫酸溶液，电解液温度为50-60℃，电流密度为600A/m2。An enterprise’s electrolytic device for the electrolytic synthesis of succinic acid without a diaphragm consists of 40 unit cells in series, the anode uses a titanium iridium electrode, and the cathode uses a lead alloy electrode (Pb-0.08Sb-0.005Ag electrode). When electrolytically synthesizing succinic acid, the electrolyte It is a 6% sulfuric acid solution of saturated succinic acid, the temperature of the electrolyte is 50-60°C, and the current density is 600A/m 2 .
采用机械方式连接钛铱电极和铅合金电极，其中钛电极的每个电极极耳采用4个
采用本发明的连接方式，将钛铱电极的极耳头部刨去表面的钛，露出其中的紫铜，清洗后对铜表面进行浸纯锡处理，然后采用本发明的方法将钛电极和铅合金电极用Pb-0.05Sb-0.005Ag焊料进行焊接(参见图1、图2)。电极连接好后，在同样的条件下进行连续电解生产，电解过程中单槽电压为2.5～3.0V，总槽电压100～120V，电解直流电能耗约为2000～2100度/吨丁二酸。电解生产过程中，电极连接处的温度最高不超过80℃，一般为室温，电解过程中由于电极发热而经常导致电极连接失效现象完全消除，本发明的电极连接方式可保证电解连续运行一年以上。Using the connection method of the present invention, the titanium on the surface of the lug head of the titanium-iridium electrode is planed off to expose the red copper therein, and after cleaning, the copper surface is treated with immersion in pure tin, and then the titanium electrode and the lead alloy are separated by the method of the present invention. The electrodes are soldered with Pb-0.05Sb-0.005Ag solder (see Figure 1, Figure 2). After the electrodes are connected, continuous electrolytic production is carried out under the same conditions. During the electrolysis process, the single cell voltage is 2.5-3.0V, the total cell voltage is 100-120V, and the electrolytic direct current energy consumption is about 2000-2100 degrees/ton succinic acid. During the electrolysis production process, the maximum temperature at the electrode connection does not exceed 80°C, which is generally room temperature. During the electrolysis process, the electrode connection failure phenomenon often caused by the heating of the electrodes is completely eliminated. The electrode connection method of the present invention can ensure the continuous operation of the electrolysis for more than one year .
采用不同焊料进行焊接时，其结果与上类似，如下表所示(浸锡合金Pb-Sn焊料和Pb-Sn-Sb焊料中，各金属为等质量)：When different solders are used for soldering, the results are similar to the above, as shown in the following table (in the tin-immersion alloy Pb-Sn solder and Pb-Sn-Sb solder, each metal is of equal mass):
*指在600A/m2的连续电解条件下，电解液为饱和丁二酸的6％硫酸溶液，电解液温度为50-60℃。*Indicates that under the condition of continuous electrolysis of 600A/m 2 , the electrolyte is a 6% sulfuric acid solution of saturated succinic acid, and the temperature of the electrolyte is 50-60°C.
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| RU2711425C2 (en) * | 2018-01-31 | 2020-01-17 | Акционерное общество "Ордена Трудового Красного Знамени Научно-исследовательский физико-химический институт им. Л.Я. Карпова" (АО "НИФХИ им. Л.Я. Карпова") | Current lead device to electrode for electrolytic production of peroxide type oxidisers |
| CN112251768A (en) * | 2020-10-09 | 2021-01-22 | 浙江工业大学 | Graphite electrode system for industrial electrolytic production of succinic acid |
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| US4137144A (en) * | 1976-03-19 | 1979-01-30 | Hooker Chemicals & Plastics Corp. | Hollow bipolar electrolytic cell anode-cathode connecting device |
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| CN1608789A (en) * | 2003-10-22 | 2005-04-27 | 李志平 | High-strength silver-less soft brazing filler alloy |
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| US4137144A (en) * | 1976-03-19 | 1979-01-30 | Hooker Chemicals & Plastics Corp. | Hollow bipolar electrolytic cell anode-cathode connecting device |
| CN1095114A (en) * | 1994-04-29 | 1994-11-16 | 陈有孝 | High-energy density amorphous lead alloy sheet and manufacturing process and purposes |
| CN1110725A (en) * | 1995-03-17 | 1995-10-25 | 贵州省新材料研究开发基地 | Compound alloy anode for electrolytic production of metal manganes and its preparation method |
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