CN103484898A - 一种真空高温连续电解炉系统及电解方法 - Google Patents
一种真空高温连续电解炉系统及电解方法 Download PDFInfo
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- CN103484898A CN103484898A CN201310469923.7A CN201310469923A CN103484898A CN 103484898 A CN103484898 A CN 103484898A CN 201310469923 A CN201310469923 A CN 201310469923A CN 103484898 A CN103484898 A CN 103484898A
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- vacuum
- furnace
- electrode
- electrolysis
- temperature continuous
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- 238000010438 heat treatment Methods 0.000 claims abstract description 35
- 238000007599 discharging Methods 0.000 claims abstract description 33
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 23
- 239000010439 graphite Substances 0.000 claims abstract description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical compound 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[C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000007789 sealing Methods 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 239000000498 cooling water Substances 0.000 claims abstract description 10
- 229910052751 metal Inorganic materials 0.000 claims abstract description 9
- 239000002184 metal Substances 0.000 claims abstract description 9
- 239000012535 impurity Substances 0.000 claims abstract description 5
- 230000000875 corresponding Effects 0.000 claims abstract description 4
- 238000005868 electrolysis reaction Methods 0.000 claims description 47
- 239000000463 material Substances 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 21
- 238000001816 cooling Methods 0.000 claims description 18
- 241000005139 Lycium andersonii Species 0.000 claims description 14
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titan oxide Chemical group 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O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 10
- 238000009413 insulation Methods 0.000 claims description 9
- WUKWITHWXAAZEY-UHFFFAOYSA-L Calcium fluoride Chemical compound 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- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminum Chemical compound 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Abstract
本发明公开一种真空高温连续电解炉系统及电解方法，主要由电解室，以及以电解室为核心而设置的真空系统、加料系统、出料系统、电极升降系统、电气控制系统、循环冷却水系统、加热系统组成。其中电解室主要由炉壳、隔热屏、石墨发热体和熔池依次由外到内围设而成，炉壳上盖有炉盖；熔池的底部设置有高、低位两个出料口，分别对应纯净熔融金属液的液位和杂质熔液的液位；在炉盖上的电极入口处与电极升降系统之间连接波纹管，实现动密封。安装在电极升降系统上的电极穿过波纹管伸入到熔池中。本发明动态密封性好，保温性好，可实现高真空度、高温电解，可用此炉进行钛金属的电解熔炼，这种电解方法还适用于其它难熔金属的冶炼。
Description
—种真空高温连续电解炉系统及电解方法技术领域
[0001] 本发明涉及一种电解工艺及设备，尤其是关于一种在真空、高温条件下的连续电解难熔金属的电解炉系统及方法。
背景技术
[0002] 真空高温连续电解炉主要用于钛与钛基合金，以及某些有色金属及其合金的熔炼。它是在真空状态下，利用热阻加热进行熔化并采用电解还原的原理由含钛的原料还原制备和冶炼、浇铸成型。该炉除具备一般高温真空炉的特点以外，还在电解系统，密封系统，加料、出料系统等方面均有要求，需要在不破坏真空度条件下进行连续加料、测温、电解熔炼、出料、铸锭冷却及出锭，实现难熔金属及其合金的连续生产。
[0003] 现有的炉子主要为电解铝工业炉，温度一般低于1000°C，且炉膛为开放式结构，不能满足电解钛金属的真空高温连续电解炉的技术要求。另外，出料系统简单，不能进行分层出料。
发明内容
[0004] 本发明着重在于解决大于1800°C高温密闭条件下连续电解制备高熔点金属及合金的问题，并为此提出一种真空高温连续电解炉系统，特殊的炉体结构设计以及便捷的工艺，使本发明具有高效成本低的优势。
[0005] 为实现上述目的，本发明采取以下技术方案:一种真空高温连续电解炉系统，主要由电解室，以及以电解室为核心而设置的真空系统、加料系统、出料系统、电极升降系统、电气控制系统、循环冷却水系统、加热系统组成，其特征在于:所述电解室主要由炉壳、隔热屏、石墨发热体和熔池依次由外到内围设而成，所述炉壳上盖有炉盖；所述熔池的外侧面与发热体距离5-lOcm，在所述熔池的底部设置有高、低位两个出料口，分别对应纯净熔融金属液的液位和杂质熔液的液位；在所述炉盖上的电极入口处，设置有密封连接的波纹管，所述波纹管的上端密封连接于所述电极升降系统上，安装在所述电极升降系统上的电极穿过所述波纹管伸入到所述熔池中，随电极升降系统的升降而升降。
[0006] 所述炉壳及炉盖的外围设置有水冷套；所述炉盖与炉壳之间设置有高温密封圈。
[0007] 所述出料系统包括一连杆，由电解室外伸入，连杆下端带封头，正对着所述出料口，通过抽动连杆控制封头与出料口的开度，所述封头比出料口的尺寸大；所述出料系统还包括出料管，连接在所述出料口的下部，所述出料管下方放置接料坩埚，接料坩埚位于冷却的出料仓内。
[0008] 所述加料系统包括螺旋进料装置、进料管，和连接于所述螺旋进料装置与进料管之间的闸阀。
[0009] 进一步，所述出料管的外围设加热装置。
[0010] 所述电极升降系统包括一电机或液压缸带动下的升降立柱，所述升降立柱上横向固定一导电横臂，所述导电横臂的端部连接一电极抱卡，所述电极抱卡抱紧所述电极。[0011] 所述真空系统主要包括进料真空泵、出料真空泵、电解室真空泵，使得所述电解室内真空度为 5 X 10-3-1 X KT1Pa15
[0012] 所述循环冷却水系统主要包括两部分，一是针对电极升降系统设置的纯水冷却装置系统，二是炉壳和炉盖水冷套及出料仓的冷却循环水系统，所述出料仓内设置有水冷制冷板，冷却过程将温度由大于1500°C降至500°C以下。
[0013] 所述加热系统采用电阻式加热方式，发热部件为石墨发热体。
[0014] 本发明还提供一种真空高温连续电解炉电解方法，其特征在于:
[0015] 第一步，将石墨电极安装到抱卡内，提高电极高度至高于电解熔池上沿，电极电气接通良好，各管路闸阀保持关闭，炉体密封良好；
[0016] 第二步，开启真空系统将炉内抽真空，真空度0.005Pa，开启入料闸阀使螺旋进料装置与加料管连通，增大加料真空泵真空度至0.1Pa，开始加料，加料完成后关闭入料闸阀；原料种类与配比如下:二氧化钛和氟化钙电解质球团，质量比2:1，电解质加入量为熔池容量的2/3 ；
[0017] 第三步，继续开启电解炉抽真空系统，炉真空度至IXKT1-SXKT3Pa ；
[0018] 第四步，开启热源系统，石墨发热体通电加热，控制300°C保温2小时后持续升温至1800°C，持续保温；
[0019] 第五步，调整电极升降装置，使石墨电极到达预定高度，设置电源输出电流l-30kA,电压0-5V，电解温度1800-1900°C条件下进行电解，电解50_900min，进入出料工序;
[0020] 第六步，加热出液管，使其出口处的温度达到1800-1900°C，控制导轨将接料坩埚定位至出料口，打开封头，使钛液通过出料管流入到接料坩埚中，出料完毕后，关闭出料口，将接料坩埚推进至水冷制冷板区域冷却至500°C以下后，打开冷却室的仓门取出接料坩埚和出锭。
[0021] 本发明由于采取以上技术方案，其具有以下优点:1、炉体结构设计考虑了炉体材料，密封，保温与传热，高温寿命，高温下投料、出料等相关问题，通过对炉体加发热体、隔热屏，对炉盖加密封圈，对炉体炉盖加水冷套，对电极加波纹管动态密封等措施，实现真空高温连续电解的需求。2、熔池的外侧面与发热体距离5-10cm是最佳的加热距离。3、在熔池内设置高低位出料口，实现不同层次的出料。尤其在生产钛金属的过程中，通过高温下以石墨电极为阳极，以二氧化钛原料为阴极，二氧化钛在氟化钙或者是氟化钙与氟化锂的混合熔盐中进行电解，二氧化钛被电解还原为液态的钛，由于密度的差异，钛沉到最底层，当累积的钛达到一定的量后，从高温炉底部出料。4、由于高温下氧阴离子扩散速度快，从而加速了脱氧速度，因而该方法电流效率高，电耗低，同时由于产品金属钛为液体，可使二氧化钛电解实现连续化，因此能够大幅度降低钛的生产成本，与传统工艺比较可节能50%，电流效率提高到90%以上；而杂质液体由高位出料口出料，可实现出料成分的有效分离。
附图说明
[0022] 图1是本装置的结构剖视图。
[0023] 图2是螺旋进料装置的结构示意图。
[0024] 1-带有水冷套的炉壳、2-带有水冷套的炉盖、3-隔热屏、4-石墨发热体、5-熔池、6-高位出料口、7-低位出料口、8-导流台、9-连杆、10-封头、11-出料管、12-接料坩埚、13-坩埚导轨、14-出料仓、15-入仓门、16-出仓门、17-制冷板、18-螺旋进料装置、19-闸阀、20-进料管、21-动力部分、22-导电横臂、23-电极抱卡、24-波纹密封管、25-升降立柱、26-电极、27-进料真空泵、28-出料真空泵、29-电解室真空泵、30-真空度/气流量(速)检测装置、31-真空排气口、32-尾气处理吸收塔、33-冷却机、34-冷却塔；
[0025] 181-料口、182-料管、183-螺旋叶片、184-电机、185-支座、186-手动转柄。
具体实施方式
[0026] 下面结合附图和实施例对本发明进行详细的描述。
[0027] 如图1所示，本发明电解炉设备主要由电解室、真空系统、加料系统、出料系统、电极升降系统、电气控制系统、循环冷却水系统、加热系统等几部分组成。工作最高温度可达2000°C，最大冷态真空度达30Pa，采用熔盐电解还原工艺金属氧化物为金属并排出液态金
属铸锭。
[0028] 1、电解室
[0029] 在该发明中，电解室主要包括带有水冷套的炉壳1、带有水冷套的炉盖2、隔热屏
3、石墨发热体4和熔池5构成，炉壳1、隔热屏3、石墨发热体4和熔池5依次由外到内层围设置，可为方形也可为圆形结构。其中，带有水冷套的炉壳1，由具有良好焊接性能的轧制钢板加工而成，为防止加热不均匀引起变形和保护密封圈，在炉壳的四周焊接有水冷套。带有水冷套的炉盖2与带有水冷套的炉壳I通过法兰连接，中间有高温密封圈，可以保证电解室的密封；在炉盖2上设置有进料口、出料连杆口、电极口、出气口等，与其相应连接件都为密封连接。为了防止热辐射造成炉盖过热和变形，以及保护密封元件，在炉盖的上表面焊接有冷却水套。熔池5位于电解室的中心，由石墨材料制成，用做高温熔盐电解用的电解池，在电解的过程中兼做熔盐电解用的阴极。熔池5的外侧面与发热体4距离5-lOcm，发热体4也由石墨材料制成。为了进一步地减少炉壁的散热损失和蓄热损失，提高炉子的热效率，在发热体4的四周设置有石墨隔热屏3，其主要作用是隔热、保温及减少热损失。
[0030] 2、出料系统
[0031] 在熔池5的底部，设置有出料口，对着所述出料口的位置设置有出料系统，本装置中，出料系统设置有高、低位两个出料口 6、7，连杆9，封头10，出料管11，接料坩埚12，坩埚导轨13，出料仓14，入仓门15，出仓门16，制冷板17组成。高、低位出料口 6、7分别用于出不同层面的熔料，高位出料口 6是通过在熔池底部原有低位出料口上加装一导流台8而形成(如图1所示)，导流台即为一凸台。连杆9由电解室外伸入，杆下端带封头10，正对着出料口，抽动连杆9可以改变封头10与出料口的开度。封头10比出料口的尺寸大，当封头全部落在出料口处时，可以堵死出料口。出料管11连接在出料口的下部，出料管外可设加热装置，以便熔融液流出时顺畅，而出料仓14内是冷的。出料管下方放置接料坩埚12，位于出料仓14内，接料坩埚12滑动设置在坩埚导轨13上利于接料坩埚移动和停止，由入仓门15进，由出仓门16出，制冷板17置于出仓门16的前方，用于给坩埚降温，快速吸收熔料辐射热和坩埚底部传导热，使物料成锭凝固，一般为水冷板方式。
[0032] 3、加料系统
[0033] 加料系统包括螺旋进料装置18、闸阀19、进料管20。颗粒状物料经由螺旋进料装置18进料，螺旋进料装置下接闸阀19，闸阀19下接进料管20，进料管20插入到电解室中，进料最大速度控制为500kg/h。螺旋进料装置18的详细结构如图2所示，螺旋进料装置为传统螺旋进料器，包括料口 181、料管182、螺旋叶片183、电机184、支座185、手动转柄186等，该装置属于现有技术。
[0034] 4、电极升降系统
[0035] 电极升降系统包括动力部分21、导电横臂22、电极抱卡23、波纹密封管24四个主要部分。电极升降系统动力部分主要为电机或液压缸带动下的升降立柱25。升降立柱25上固定一导电横臂22，导电横臂22的端部连接电极抱卡23，电极抱卡23抱紧一电极26，电极26穿过波纹密封管24伸入到电解室中。波纹密封管24上端密封连接在导电横臂22上，下端密封连接在炉盖2上，当电极26在导电横臂22的带动下升降时，波纹密封管24弹性伸缩，实现电极的动态密封。在导电横臂中，设置有封闭的水冷却管路。
[0036] 波纹密封管24采用耐温压波纹管材料，连接加热炉电极口与导电抱卡，实现整体密封。
[0037] 5、真空系统与真空度的获得
[0038] 电解炉整体密封，真空环境由多台持续运转的真空泵获得，制造电解室的真空度。主要包括进料真空泵27、出料真空泵28、电解室真空泵29，进料真空泵主要用于加料过程中补进的空气进行排空，出料真空泵主要用于出料操作时对出料仓进行抽真空、电解室真空泵用于电解前期和电解过程中反应产生气体时气体的排出。各真空系统附属设计有真空度/气流量(速)检测装置30、真空排气口 31、尾气处理吸收塔32等。设备启动运行初气体经排气口 31排出，后期电解过程尾气经由吸收塔排空。本设备为多封口系统，加料口、电极口等均采用机械密封结构，可满足批量化生产的要求。设备从大气压到0.01Pa时所用的时间保证在8-10min，设计真 空度要求为5 X 10-3-1 X IO^1Pa0
[0039] 6、电气控制系统
[0040] 设备采用数字化控制系统，操作简单，自动控制程度高。电气控制系统采用常规选择，包括人机操作界面、PLC控制系统，可实现与真空系统，电源系统，动力系统，测量系统等之间的电脑化自动控制。在生产过程中可调节电极升降，抱卡，密封定位，控制加热电压，时间，加热方式，工作方式等工艺参数，同时可以显示真空系统的工作状态、电源系统的工作状态、部件位置、报警状态等；系统设置了各种自动保护措施，为设备的可靠运行提供了安全保障。另外，由于在真空中，不同的热封材料其热封时间也有一定的差异，所以本系统采用数字控制热封时间，以及在热封装置中采用过热自动保护装置，防止热封材料被损坏。
[0041] 7、循环式冷却水系统
[0042] 冷却水系统主要包括两部分，一是针对导电横臂和抱卡电极的导电铜排设置的纯水冷却装置系统，主要由冷却机33提供冷却循环，并绝缘避免通电。二是加热炉整体水冷套与出料仓冷却循环水系统，通过外置冷却塔34对炉体钢件实现冷却保护。出料仓内设置有水冷制冷板17，快速吸收熔料表层和底部热量，在出仓前完成冷却。冷却过程将温度由大于1500°C降至500°C以下。
[0043] 8、加热系统
[0044] 本设备采用电阻式加热方式，发热部件为石墨发热体4。发热体4采用石墨连接件与外部导电铜排连接，接触部位铜排设计有水冷循环进行铜部件冷却。为了减少热辐射，在发热体4四周设置有多层石墨材质隔热屏3，避免造成对钢制炉体的辐射损伤。热源系统控制由数字化电气控制系统进行调节，通过程序化电流电压实现升温方式的变化。
[0045] 电解室炉盖有均匀分布的一个或多个电极口，电极米用一根或多根石墨电极，电极直径为100-700mm，电极从炉盖顶部上方插入炉中，工作时电极可分别独立调整。为保证炉内气氛和绝缘，电极与带有水冷套的炉盖之间有波纹管动态密封和绝缘装置。为了保证电解的连续进行，在电解室炉盖上均匀分布一个或多个加料管，加料管带有密封装置与炉盖密封，具有防止散热、防止漏气的功能。在电解室炉盖上设置液体钛出料连杆，通过气动装置实现液体钛出料装置的开启和关闭。熔液成分冶炼反应完全后，因物料比重差异较大和互不相溶，物料出现结构性分层，因此本设备将出料口设计为高低位出料，当执行高位放料操作时，打开高位出料口，将熔融钛液放出，当执行低位放料操作时，将打开低位出料口，将含有杂质的熔液放出。
[0046] 由于钛高温电解炉采用了全封闭设计，尾气从出气口排放，而该尾气含有少量含氟气体和固体氟化钙粉尘或者是氟化钙与氟化锂的混合粉尘。含氟气体对人体有伤害，并且氟化钙粉尘也会污染环境。本设备还包括为钛高温电解炉提供的一套尾气处理装置，该吸收系统操作简单，利于环保，对尾气中的含氟气体具有很好的吸收效果。
[0047] 一种利用此电解炉的真空高温电解方法是:
[0048] 第一步，安装电极与各部件密封。采用吊装工具将石墨电极安装到抱卡内，启动抱卡将电极接牢并保证电极电气接通良好。调整波纹管密封件，各管路闸阀等保持关闭。提高电极高度至高于电解熔池上沿。
[0049] 第二步，开启全设备真空系统将设备内部实现真空，真空度0.005Pa。开启入料闸阀使螺旋进料装置与加料管连通。增大加料真空泵真空度至0.1Pa，开始加料:将造粒并干燥后的颗粒经由加料口、螺旋进料装置加入到电解炉熔池内，完成后关闭入料闸阀。
[0050] 原料种类与配比举例如下:将制备好的二氧化钛、氟化钙电解质球团按质量比2:1比例加入熔池中，电解质加入量为熔池容量的2/3。
[0051] 第三步，继续开启电解炉抽真空至钛高温电解炉真空度I X KT1-SXKT3Pa,气体经由排气口排出。
[0052] 第四步，开启加热系统，石墨发热体通电加热，控制300°C保温2h后持续升温至1800°C，持续保温。
[0053] 第五步，调整电极升降装置，使石墨电极到达预定高度。设置电源输出电流l-30kA,电压0-5V，电解温度1800-1900°C条件下进行电解，电解50_900min，按工艺条件允许开始进入出料工序；
[0054] 第六步，出料时加热出液管，使其出口处的温度达到1800-1900°C。控制坩埚导轨将接料坩埚定位至出料口。打开封头，使钛液通过出料管流入到冷却室的接料坩埚中，出料完毕后，关闭出料口 ；将坩埚推进至水冷制冷板区域冷却至500°C以下后，打开冷却室的仓门取出接料坩埚和出锭。
Claims (10)
1.一种真空高温连续电解炉系统，主要由电解室，以及以电解室为核心而设置的真空系统、加料系统、出料系统、电极升降系统、电气控制系统、循环冷却水系统、加热系统组成，其特征在于: 所述电解室主要由炉壳、隔热屏、石墨发热体和熔池依次由外到内围设而成，所述炉壳上盖有炉盖；所述熔池的外侧面与石墨发热体距离5-lOcm保证最佳加热距离，在所述熔池的底部设置有高、低位两个出料口，分别对应纯净熔融金属液的液位和杂质熔液的液位； 在所述炉盖上的电极入口处，密封连接一动态波纹管，波纹管的上端密封连接到电极升降系统上，实现电极的动态密封，抱卡在所述电极升降系统上的电极穿过所述波纹管伸入到所述熔池中，随电极升降系统的升降而升降。
2.根据权利要求1所述的真空高温连续电解炉系统，其特征在于:所述炉壳及炉盖的外围设置有水冷套；所述炉盖与炉壳之间设置有高温密封圈。
3.根据权利要求1所述的真空高温连续电解炉系统，其特征在于:所述出料系统包括一连杆，由电解室外伸入，连杆下端带封头，正对着所述出料口，通过抽动连杆控制封头与出料口的开度，所述封头比出料口的尺寸大；所述出料系统还包括出料管，连接在所述出料口的下部，所述出料管下方放置接料坩埚，接料坩埚位于冷却的出料仓内。
4.根据权利要求3所述的真空高温连续电解炉系统，其特征在于:所述出料管的外围设置有加热装置。
5.根据权利要求1或2或3或4所述的真空高温连续电解炉系统，其特征在于:所述电极升降系统包括一电机或液压缸带动下的升降立柱，所述升降立柱上横向固定一导电横臂，所述导电横臂的端部连接一电极抱卡，所述电极抱卡抱紧所述电极。
6.根据权利要求1或2或3或4所述的真空高温连续电解炉系统，其特征在于:所述真空系统主要包括进料真空泵、出料真空泵、电解室真空泵，附属配有真空度/流量检测装置、真空排气口、尾气处理吸收塔。
7.根据权利要求1或2或3或4所述的真空高温连续电解炉系统，其特征在于:所述电气控制系统采用常规技术的人机操作界面和PLC控制系统。
8.根据权利要求1或2或3或4所述的真空高温连续电解炉系统，其特征在于:所述循环冷却水系统主要包括:针对电极升降系统设置的封闭冷却水管路，针对炉壳、炉盖设置的水冷套以及针对出料仓设置的循环冷却水系统，所述出料仓内设置有制冷板。
9.根据权利要求1或2或3或4所述的真空高温连续电解炉系统，其特征在于:所述加热系统采用电阻式加热方式，发热部件为所述石墨发热体。
10.利用权利要求1-9之一所述的真空高温连续电解炉的电解方法，其特征在于: 第一步，将石墨电极安装到抱卡内，提高电极高度至高于电解熔池上沿，电极电气接通良好，各管路闸阀保持关闭，炉体密封良好； 第二步，开启真空系统将炉内抽真空，真空度0.005Pa，开启入料闸阀使螺旋进料装置与加料管连通，增大加料真空泵真空度至0.1Pa，开始加料，加料完成后关闭入料闸阀；原料种类为二氧化钛和氟化钙电解质球团，配比为质量比2:1，且电解质加入量为熔池容量的2/3 ； 第三步，继续开启电解炉抽真空系统，炉真空度至I X 10^-5 X 10¾ ； 第四步，开启加热系统，石墨发热体通电加热，控制300°C保温2小时后持续升温至，1800°C，持续保温； 第五步，调整电极升降装置，使石墨电极到达预定高度，设置电源输出电流l-30kA，电压0-5V，电解温度1800-1900°C条件下进行电解，电解50-900分钟，进入出料工序； 第六步，同期加热出液管，使其出口处的温度达到1800-1900°C，控制导轨将接料坩埚定位至出料口下，打开封头，使电解液通过出料管流入到接料坩埚中，出料完毕后，关闭出料口，将接料坩埚推进至水冷制冷板 区域冷却至500°C以下后，打开冷却室的仓门取出接料坩埚和出锭。
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