CN117626357A - 一种铝电解槽新型侧壁材料的制备方法 - Google Patents
一种铝电解槽新型侧壁材料的制备方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 73
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 34
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000005868 electrolysis reaction Methods 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000002699 waste material Substances 0.000 claims abstract description 20
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 18
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 18
- 239000011734 sodium Substances 0.000 claims abstract description 18
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 15
- 238000004821 distillation Methods 0.000 claims abstract description 14
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 12
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 8
- 239000002002 slurry Substances 0.000 claims abstract description 8
- 239000000853 adhesive Substances 0.000 claims abstract description 7
- 230000001070 adhesive effect Effects 0.000 claims abstract description 7
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- 238000003825 pressing Methods 0.000 claims abstract description 7
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- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 229910052810 boron oxide Inorganic materials 0.000 claims description 5
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052731 fluorine Inorganic materials 0.000 claims description 5
- 239000011737 fluorine Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 4
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical group [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 229910052845 zircon Inorganic materials 0.000 claims description 3
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims description 3
- 239000000292 calcium oxide Substances 0.000 claims description 2
- 235000012255 calcium oxide Nutrition 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- RGPUVZXXZFNFBF-UHFFFAOYSA-K diphosphonooxyalumanyl dihydrogen phosphate Chemical compound [Al+3].OP(O)([O-])=O.OP(O)([O-])=O.OP(O)([O-])=O RGPUVZXXZFNFBF-UHFFFAOYSA-K 0.000 claims description 2
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- 229910052799 carbon Inorganic materials 0.000 abstract description 21
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- 239000000126 substance Substances 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
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- 230000003628 erosive effect Effects 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
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- 238000009825 accumulation Methods 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- RHZUVFJBSILHOK-UHFFFAOYSA-N anthracen-1-ylmethanolate Chemical compound C1=CC=C2C=C3C(C[O-])=CC=CC3=CC2=C1 RHZUVFJBSILHOK-UHFFFAOYSA-N 0.000 description 1
- 239000003830 anthracite Substances 0.000 description 1
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- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- -1 compound calcium fluoride Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
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- 238000002407 reforming Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/06—Electrolytic production, recovery or refining of metals by electrolysis of melts of aluminium
- C25C3/08—Cell construction, e.g. bottoms, walls, cathodes
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
本发明公开了一种铝电解槽新型侧壁材料的制备方法，属于铝电解槽技术领域。该方法包括：(1)将废旧碳化硅结合氮化硅耐火块破碎为粒径5mm以下的球形颗粒物或针状颗粒物；(2)破碎后物料中加入除钠剂，快速搅拌0.5～2h形成浆液，泵送至蒸馏釜中，控制蒸馏温度为300～700℃，以去除金属钠的残留；蒸馏釜内物料经压滤处理后烘干，得到干料；(3)将干料35～40份、黏结剂7～8份和碳粉1～3份混合并在150～260℃加热，然后放入成型模腔内焙烧后，即得到所述侧壁材料。该侧壁材料能满足和适应低温低耗电解技术侧部热平衡需求，同时解决废侧部炭块资源闲置及对环境造成的危害等问题，实现废旧侧部炭块资源化循环利用。
Description
技术领域
本发明涉及铝电解槽技术领域，具体涉及一种铝电解槽新型侧壁材料的制备方法。
背景技术
电解槽既是金属铝冶炼最为关键的设备，也是盛装铝液的重要容器。铝电解槽由多种不同材质、规格的材料按施工工艺砌筑而成。在电解槽中，侧部炭块是用于调节热平衡的重要组成部分。目前用于铝电解槽侧部炭块材质分为两大类，分别是碳质材料和氮化硅结合碳化硅材质。氮化硅结合碳化硅材料因其优异的高温力学性能、高的热传导率、散热快、抗化学侵蚀、抗氧化等特性，是目前大部分铝企电解槽侧部结构的首选材料；其较高的导温系数和超强的耐腐蚀性能，能够成功解决大型槽热量过剩的电解热平衡难题。对于前期在较高电压环境下生产热收入大于支出的槽型非常有利；但是，随着国家对铝电解行业节能减排日益严峻的要求，电解低能耗技术和能源利用率不断提升的要求下，低电压低电耗生产的电解槽是各大铝企升级改造的方向。此种类型的电解槽由于热量收入减小，为保持槽内热平衡，侧部需要保温功能，而氮化硅结合碳化硅材质炭块电解槽散热造成大量的能耗空耗，侧部热量散失的弊端日益显现，更成为低能耗电解槽需要熔池保温的技术障碍。
再者来说，经过长期铝冶炼过程的槽衬材料由于受熔盐的化学侵蚀、氧化、高温、渗透等作用及日常的管理水平等因素的影响，电解槽的使用寿命远远小于其设计寿命。当电解槽达到使用寿命或破损时，需要将原有内衬材料刨除，替换新的内衬材料，而被刨除的侧部炭块因没有合适的处理方法，基本处于堆弃状态。碳化硅结合氮化硅材料导温系数远高于碳质材质材料。目前侧部炭块的处理方法的弊端：一是随着电解槽更新换代的速度，需要空间及场地堆放，占用各种资源。二是从本质上，无适当的处理方法，堆放易造成资源的浪费。
针对上述氮化硅结合碳化硅材质炭块电解槽的弊端，少部分铝企电解槽侧部结构材料使用以无烟煤为主要原料生产的普通炭块或无定形炭块、石墨炭块、半石墨质炭块结构材料等。一般铝电解温度在920～950℃左右，电解槽侧部结构不仅要具有耐高温耐腐蚀、抗氧化性能，而且要求可以调整电解热平衡，以形成正常槽帮满足生产需要。但传统电解生产受材料制造、生产工艺等技术限制，均采用槽底保温、侧部散热的槽型，采用较厚碳质侧部碳块用于加强散热，造成侧部漏电严重，电能消耗增大。这类材料最致命的缺点是容易被高温的冰晶石电解质浸蚀，金属钠的嵌入使碳晶格的层间距增大，导致体积膨胀，强度降低。
发明内容
本发明的目的在于提供一种铝电解槽新型侧壁材料的制备方法，所制备的新型材料能够满足和适应低温低耗电解技术侧部热平衡需求，同时能够解决废侧部炭块资源闲置及对环境造成的危害等问题，实现废旧侧部炭块资源化循环利用。
为实现上述目的，本发明所采用的技术方案如下：
一种铝电解槽新型侧壁材料的制备方法，该方法包括如下步骤：
(1)将废旧碳化硅结合氮化硅耐火块破碎为粒径5mm以下的球形颗粒物或针状颗粒物，以便于浸湿溶解及缩短工艺反应时长；
(2)除钠和固氟：
在经步骤(1)破碎后的物料中加入除钠剂，快速搅拌形成浆液，控制反应时长(搅拌时间)0.5～2h；将反应后所得液体物料(浆液)泵送至蒸馏釜中，控制蒸馏温度为300～700℃，以去除金属钠的残留；蒸馏釜内物料经压滤处理后烘干，得到干料；
(3)准备侧壁材料的制备原材料，将各原材料混合，并在150～260℃加热，加热时间0.5～1h；将加热后的混合原材料放入成型模腔内焙烧后，即得到所需结构的铝电解槽新型侧壁材料。
进一步地，步骤(2)中，所述除钠剂为石灰水；或者，所述除钠剂为生石灰与水按4：(8-15)重量比例混合而成；破碎后的物料与除钠剂的重量比例为(6-13)：100。
进一步地，步骤(2)中，经压滤处理后所得固体物料在200～300℃温度区间内烘0.5～1h得到干料。
进一步地，步骤(3)中，所述原材料按重量份数计包括如下组分：
干料 35～40份；
黏结剂 7～8份；
碳粉 1～3份。
进一步地，步骤(3)中，所述黏结剂为磷酸二氢铝、铝溶胶和硅溶胶中的一种或几种。
进一步地，步骤(3)中，所述焙烧的温度为1200～1300℃，焙烧时间2～3小时。
进一步地，步骤(3)中，所述侧壁材料的制备原材料中还可含有其它添加剂1-2重量份，所述其它添加剂为氧化铝粉、锆英粉和氧化硼粉中的一种或几种。
本发明的设计机理如下：
本发明将废旧碳化硅结合氮化硅材料破碎后进行湿浸固氟，将全部的氟转化为稳定的化合物氟化钙，通过蒸馏去除钠，得到的粉料作为新侧壁材料的原料，并添加黏结剂与添加剂等，特定的添加剂(氧化铝粉、锆英粉、氧化硼粉)改善了材料的烧结性能与显微结构，并提高材料的抗性，最终“变废为宝”制备成用于电解槽侧壁结构材料。
本发明的优点及有益效果如下：
1、随着国家对铝电解行业节能减排日益严峻的要求，电解低能耗技术和能源利用率不断提升的要求下，氮化硅结合碳化硅材质炭块在电解槽中散热造成大量的能耗空耗，成为低能耗电解槽熔池保温的技术障碍。再者而言，没有适当的处理方法，刨槽后的废旧侧部结构体以堆弃为主。本发明制备了经济合理的新型侧衬材料，可实现废旧侧部资源重复再利用，减少危废堆存，减轻对环境的危害。
2、电解槽废旧侧部炭块经破碎、湿浸、蒸馏、压滤、烘干、成型等工序处理后，变废为宝，可以实现废旧资源100％重复再利用，将制得干料可作为新结构体成型的原材料及关键骨料，而且可以解决废侧部炭块资源闲置及对环境造成的危害等问题，提升废旧侧部炭块资源利用的经济价值。
3、因碳化硅砖的价格是普通炭素侧块的5倍及以上，铝企急需开发一种经济合理的新型侧衬材料。本发明恰可减少原材料的成本，减少电解固废堆积，改善环境，成型后的侧部炭块在性能上更能满足和适应低温低耗电解技术侧部热平衡需求。
具体实施方式：
本发明提供一种铝电解槽新型侧壁材料的制备方法，该方法中关键技术是先进行无害化、再进行资源化技术处理。以“变废为宝，资源利用”为目的，将废旧碳化硅结合氮化硅侧部材料经破碎、湿浸固氟、蒸馏去钠、压滤、烘干制成原料，添加碳粉和一种或几种黏结剂在高温下混捏成型得到所需结构的新材质。
实施例1：
本实施例为铝电解槽新型侧壁材料的制备方法，具体过程如下：
1、本实施例铝电解槽侧壁材料制备原料组成如下：
干料37重量份(干料中SiC为64％～75wt.％，Si3N4为16～18wt.％)，黏结剂(硅溶胶)7重量份，碳粉3重量份，氧化硼粉2重量份。
2、具体制备过程和各工艺参数：
①废旧碳化硅结合氮化硅耐火块破碎成5mm以下球形颗粒物或针状颗粒物；②在破碎后的物料中加入饱和石灰水中，破碎后的物料与饱和石灰水的重量比例为10：100，快速搅拌形成浆液，控制反应时长1h；③将浆液泵送至蒸馏釜去除钠，控制蒸馏温度在500℃之间，蒸馏后进行压滤；④在250℃烘0.5～1h，得到干料；⑤将干料、黏结剂、碳粉和氧化硼粉混合放入混捏锅加热，加热温度控制在220℃；⑥将加热后物料放入成型模腔内在1250℃焙烧2.5小时焙烧成所需形状的侧部结构体。
实施例2：
与实施例1不同之处在于：
干料40重量份(干料中SiC为64％～75wt.％，Si3N4为16～18wt.％)，黏结剂(铝溶胶)8重量份，碳粉1重量份，氧化铝粉2重量份。
对以上实施例1-2生成产品进行分析鉴定，证明生成的产品就是发明目的要得到的化工产品或冶金产品，如表1。
表1性能测试
Claims (7)
1.一种铝电解槽新型侧壁材料的制备方法，其特征在于：该方法包括如下步骤：
(1)将废旧碳化硅结合氮化硅耐火块破碎为粒径5mm以下的球形颗粒物或针状颗粒物，以便于浸湿溶解及缩短工艺反应时长；
(2)除钠和固氟：
在经步骤(1)破碎后的物料中加入除钠剂，快速搅拌形成浆液，控制反应时长为0.5～2h；将反应后所得浆液泵送至蒸馏釜中，控制蒸馏温度为300～700℃，以去除金属钠的残留；蒸馏釜内剩余物料经压滤处理后烘干，得到干料；
(3)准备侧壁材料的制备原材料，将各原材料混合，并在150～260℃加热，加热时间0.5～1h；将加热后的混合原材料放入成型模腔内焙烧后，即得到所需结构的铝电解槽新型侧壁材料。
2.根据权利要求1所述的铝电解槽新型侧壁材料的制备方法，其特征在于：步骤(2)中，所述除钠剂为石灰水；或者，所述除钠剂为生石灰与水按4：(8-15)重量比例混合而成；破碎后的物料与除钠剂的重量比例为(6-13)：100。
3.根据权利要求1所述的铝电解槽新型侧壁材料的制备方法，其特征在于：步骤(2)中，经压滤处理后所得固体物料在200～300℃温度区间内烘0.5～1h得到干料。
4.根据权利要求1所述的铝电解槽新型侧壁材料的制备方法，其特征在于：步骤(3)中，所述原材料按重量份数计包括如下组分：
干料 35～40份；
黏结剂 7～8份；
碳粉 1～3份。
5.根据权利要求4所述的铝电解槽新型侧壁材料的制备方法，其特征在于：步骤(3)中，所述黏结剂为磷酸二氢铝、铝溶胶和硅溶胶中的一种或几种。
6.根据权利要求1所述的铝电解槽新型侧壁材料的制备方法，其特征在于：步骤(3)中，所述焙烧的温度为1200～1300℃，焙烧时间2～3小时。
7.根据权利要求4所述的铝电解槽新型侧壁材料的制备方法，其特征在于：步骤(3)中，所述侧壁材料的制备原材料中还含有其它添加剂1-2重量份，所述其它添加剂为氧化铝粉、锆英粉和氧化硼粉中的一种或几种。
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