CN111943652B - 铝镁轻质耐火材料的制备方法 - Google Patents
铝镁轻质耐火材料的制备方法 Download PDFInfo
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- aluminum
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- 239000011819 refractory material Substances 0.000 title claims abstract description 26
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 55
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 49
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 239000011230 binding agent Substances 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 10
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000003825 pressing Methods 0.000 claims abstract description 6
- 238000005245 sintering Methods 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 12
- 239000012629 purifying agent Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 7
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 4
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 claims description 3
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 3
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 claims description 3
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 3
- 239000001099 ammonium carbonate Substances 0.000 claims description 3
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 3
- 239000006229 carbon black Substances 0.000 claims description 3
- -1 polyethylene Polymers 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 2
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 2
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims description 2
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 2
- 238000011049 filling Methods 0.000 abstract description 2
- 229910052749 magnesium Inorganic materials 0.000 abstract description 2
- 239000011777 magnesium Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 10
- 229910004298 SiO 2 Inorganic materials 0.000 description 7
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 6
- 239000001103 potassium chloride Substances 0.000 description 6
- 235000011164 potassium chloride Nutrition 0.000 description 6
- 239000012535 impurity Substances 0.000 description 5
- 239000011780 sodium chloride Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- GANNOFFDYMSBSZ-UHFFFAOYSA-N [AlH3].[Mg] Chemical compound [AlH3].[Mg] GANNOFFDYMSBSZ-UHFFFAOYSA-N 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 239000008247 solid mixture Substances 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000002893 slag Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 159000000000 sodium salts Chemical class 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910018134 Al-Mg Inorganic materials 0.000 description 1
- 229910018467 Al—Mg Inorganic materials 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 238000009614 chemical analysis method Methods 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 150000004673 fluoride salts Chemical class 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 238000009875 water degumming Methods 0.000 description 1
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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
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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Abstract
本发明公开了一种铝镁轻质耐火材料的制备方法，旨在解决现有技术中高端轻质耐火材料缺乏的技术问题。本发明铝镁轻质耐火材料的制备方法包括以下步骤：取铝灰纯化；取质量比为2～4:1的纯化铝灰和氧化镁配料；粉磨至粒度为200～325目，得粉料；取造孔剂加入粉料中，粉料和造孔剂的体积比为0.5～1:1；再加入粘结剂得混合物；粘结剂的浓度为所述混合物质量的3～30%；搅拌均匀；压制成坯体，干燥，1200～1650℃温度下烧结，保温即成。本发明采用铝灰制备铝镁质轻质耐火材料可以充分利用铝灰中的铝质和镁质成分、实现铝灰的无害化和资源化，节约自然资源、降低生产成本；实现了填补市场中高端铝镁质轻质耐火材料的缺口的目的。
Description
技术领域
本发明涉及耐火材料制备技术领域，具体涉及一种铝镁轻质耐火材料的制备方法。
背景技术
铝灰是铝工业生产过程中产生的废弃物，主要成分为单质铝、铝的化合物、氧化硅、氧化镁、钠盐、钾盐、氟化盐、氧化钛等，具有毒性及易燃性。电解铝工艺熔体转移、净化、除杂过程熔体表面产生的浮渣，废铝熔炼熔体转移、净化、除杂过程熔体表面产生的浮渣（盐渣和铝灰），熔盐法从铝灰、铝渣中回收金属铝的过程中产生的盐渣和二次铝灰均被列入2019版《国家危险废物名录》。据统计，每生产1吨铝，大概产生15～30kg的铝灰，2019年国内铝产量为3500万吨，产生铝灰约52.5～105万吨，其无害化和资源化是铝工业生产中迫切需要解决的问题。
另一方面，轻质耐火材料的市场需求也在逐年增加，2018年轻质耐火制品54.10万吨，同比增长5.14%；2019年轻质耐火制品58.9万吨，同比增长8.9%；目前低端轻质耐火材料以低端黏土质和铝硅质为主，高端轻质耐火材料以氧化铝空心球砖为主，中、高端的铝镁质轻质耐火材料较为缺乏。
发明内容
本发明要解决的技术问题是提供一种铝镁轻质耐火材料的制备方法，以期在实现铝灰无害化、资源化利用的同时解决现有技术中高端轻质耐火材料缺乏的技术问题。
为解决上述技术问题，本发明采用如下技术方案：
设计一种铝镁轻质耐火材料的制备方法，包括以下步骤：
（1）取铝灰纯化；
（2）取质量比为2～4:1的纯化铝灰和氧化镁配料；粉磨至粒度为200～325目，得粉料；
（3）取造孔剂加入粉料中，所述粉料和造孔剂的体积比为0.5～1:1；再加入粘结剂得混合物；所述粘结剂占所述混合物质量的3～30%；
（4）搅拌均匀后制成坯体，干燥，1200～1650℃温度下烧结，保温，即成。
优选的，在所述步骤（1）中，采用热法纯化铝灰：将质量比为50～100:1的铝灰和纯化剂在800～1650℃温度下保温0.5～5h。
进一步的，所述纯化剂为碳酸铵、氟化铵、硼酸、氟化铝中的至少一种；此类纯化剂可快速彻底去除铝灰中钠盐、钾盐等杂质，同时促使铝灰中的氮化铝快速氧化脱氮，生成无毒无害的氮气，环保无污染。
优选的，在所述步骤（3）中，造孔剂为炭黑、1～3mm聚乙烯球、50～200目锯末中的至少一种。
优选的，在所述步骤（3）中，粘结剂为聚乙烯醇、羟丙基甲基纤维素、纸浆中的至少一种。
优选的，在所述步骤（4）中，坯体采用振动或压制成型。
优选的，在所述步骤（4）中，干燥方式为先于70～90℃下干燥20～25h，再于100～150℃下干燥10～12h。
优选的，在所述步骤（4）中，保温控制为0.5～5h。
在以上制备过程中，可充分利用现有技术手段及设备对所产生的废气进行回收利用，并经处理达标后排放。
与现有技术相比，本发明的主要有益技术效果在于：
1.本发明应用纯化剂能使铝灰中的NaCl和KCl气化与铝灰分离，可快速彻底去除铝灰中钠盐、钾盐等杂质，使得制备出的铝镁质轻质耐火材料杂质含量低；而NaCl和KCl气化冷凝后变成固体回收，回收之后可复配为铝水精炼剂重复利用；同时使铝灰中的氮化铝在高温下快速氧化脱氮，生成无毒无害氮气（4AlN+3O2=2Al2O3+2N2），环保无污染。
2.本发明采用铝灰制备铝镁质轻质耐火材料可以充分利用铝灰中的铝质和镁质成分、实现铝灰的无害化和资源化利用，节约了自然资源、降低了生产成本；制备得到的铝镁质轻质耐火材料铝镁含量在93%以上、纯度高、耐火度高，应用广泛，实现了填补市场中高端铝镁质轻质耐火材料的缺口的目的。
具体实施方式
下面结合实施例来说明本发明的具体实施方式，但以下实施例只是用来详细说明本发明，并不以任何方式限制本发明的范围。
在以下实施例中所涉及的原料如无特别说明，均为市售常规原料；所涉及的试验或检测方法，如无特别说明，均为常规方法。
实施例1 铝镁轻质耐火材料的制备方法：
先将铝灰（含Al 5%、Al2O3 58%、AlN 17%、NaCl+KCl 6.7%、SiO2 1.8%、MgO 4%，其余为F2O3、TiO2、CaO及氟化物）和纯化剂氟化氨按照100:1的重量比混合均匀，在1200℃下保温2h，得到纯化铝灰（纯化后铝灰中Al2O3 88.2%、Na2O+K2O 0.6%、SiO2 2.4%、MgO 4.7%）。
再将纯化铝灰和氧化镁（纯度为98.7%）按照重量比4:1的比例混合，粉磨至200目，再和炭黑按照1:1的体积比混合均匀得固体混合物，外加固体混合物重量3%的聚乙烯醇粘结剂（由聚乙烯醇和水按1:300的质量比组成）搅拌均匀。
在80MPa压力下压制成40mm×40mm×40mm的坯体；于80℃下烘干24h、120℃烘干12h，在1300℃烧结，保温5h，得到铝镁质轻质耐火材料。
实施例2 铝镁轻质耐火材料的制备方法：
先将铝灰（含Al 10%、Al2O3 55%、AlN 18%、NaCl+KCl 8%、SiO2 1.5%、MgO 5.2%，其余为F2O3、TiO2和CaO）和纯化剂（为重量比1:1的碳酸铵和氯化铵混合物）按照重量比50:1的比例混合均匀，在1100℃保温1h，得到纯化铝灰（纯化后铝灰中Al2O3 89.7%、Na2O+K2O0.3%、SiO2 1.7%、MgO 5.6%）。
再将纯化铝灰和氧化镁（纯度为98.7%）按照重量比7:3的比例混合，球磨至200目，再和1mm聚乙烯球按照体积比3:2的比例混合得固体混合物，外加固体混合物重量的15%的纸浆溶液（浓度为20%）。
所得混合物料充分搅拌均匀，振动成型为40mm×40mm×40mm的坯体，80℃烘干24h、120℃烘干12h，在1380℃烧结，保温1h，得到铝镁质轻质耐火材料。
实施例3 铝镁轻质耐火材料的制备方法：
以锯末为造孔剂，用铝灰和氧化镁压制成型制备铝镁质轻质耐火材料，原铝灰中，氧化镁为；
先将铝灰（含Al 10%、Al2O3 55%、AlN 18%、NaCl+KCl 12%、SiO2 0.7%、MgO 1.5%，其余为F2O3、TiO2和CaO）和纯化剂氟化铝按照重量比50:1的比例混合均匀，在1300℃保温3h，得到纯化铝灰（含Al2O3 92.6%、Na2O+K2O 0.6%、SiO2 1.7%、MgO 2.4%）。
再将纯化铝灰和氧化镁（纯度98.7%）按照重量比3:1的比例混合，球磨至200目，再和150目锯末按照体积比2:3的比例混合均匀得固体混合物，外加固体混合物重量3%聚乙烯醇粘结剂溶液（由聚乙烯醇和水按1:300的质量比组成）搅拌均匀。
在80MPa压力下压制成40mm×40mm×40mm的坯体，80℃烘干24h、120℃烘干12h，在1450℃烧结，保温1h，得到铝镁质轻质耐火材料。
试验例：
取实施例1～3所制备的铝镁质轻质耐火材料，检测其Al2O3、MgO、SiO2、Na2O+K2O的含量，抗压强度和气孔率。
检测标准为GB/T5069《镁铝系耐火材料化学分析方法》、GB/T2998《定形隔热耐火制品体积密度和真气孔率试验方法》、GB/T5072《耐火材料常温耐压强度试验方法》。
各例检测结果如表1所示。
表1 制品性能指标
由表1可知，所得到的铝镁质轻质耐火材料铝镁含量在93%以上、纯度高、耐火度高。
上面结合实施例对本发明作了详细的说明；但是，所属技术领域的技术人员能够理解，在不脱离本发明构思的前提下，还可以对上述实施例中的各个具体参数进行变更，或者是对相关材料及步骤进行等的同替代，从而形成多个具体的实施例，均为本发明的常见变化范围，在此不再一一详述。
Claims (6)
1.一种铝镁轻质耐火材料的制备方法，其特征在于，包括以下步骤：
（1）采用热法纯化铝灰：将质量比为50～100:1的铝灰和纯化剂在800～1650℃温度下保温0.5～5h，所述纯化剂为碳酸铵、氟化铵、硼酸、氟化铝中的至少一种；
（2）以2～4:1的质量比将纯化铝灰和氧化镁混合粉磨至粒度为200～325目，得粉料；
（3）按粉料：造孔剂=0.5～1:1的体积比向上步所得粉料中加入造孔剂，再向其中加入粘结剂得混合物，且使粘结剂占混合物质量的3～30%；
（4）将步骤（3）所得物料搅拌均匀后制成坯体，干燥后于1200～1650℃温度下烧结并保温，即成。
2.根据权利要求1所述的铝镁轻质耐火材料的制备方法，其特征在于，在所述步骤（3）中，造孔剂为炭黑、1～3mm聚乙烯球、50～200目锯末中的至少一种。
3.根据权利要求1所述的铝镁轻质耐火材料的制备方法，其特征在于，在所述步骤（3）中，粘结剂为聚乙烯醇、羟丙基甲基纤维素、纸浆中的至少一种。
4.根据权利要求1所述的铝镁轻质耐火材料的制备方法，其特征在于，在所述步骤（4）中，坯体采用振动或压制成型。
5.根据权利要求1所述的铝镁轻质耐火材料的制备方法，其特征在于，在所述步骤（4）中，干燥方式为：先于70～90℃下干燥20～25h，再于100～150℃下干燥10～12h。
6.根据权利要求1所述的铝镁轻质耐火材料的制备方法，其特征在于，在所述步骤（4）中，保温时间为0.5～5h。
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