CN113603479A - 一种改性钛酸钡泡沫陶瓷材料的制备方法及其所得材料 - Google Patents
一种改性钛酸钡泡沫陶瓷材料的制备方法及其所得材料 Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical class [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000000463 material Substances 0.000 title abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 60
- 239000000843 powder Substances 0.000 claims abstract description 54
- 238000003756 stirring Methods 0.000 claims abstract description 38
- 238000001035 drying Methods 0.000 claims abstract description 27
- 239000000919 ceramic Substances 0.000 claims abstract description 25
- 239000002699 waste material Substances 0.000 claims abstract description 24
- 238000000227 grinding Methods 0.000 claims abstract description 23
- 238000005498 polishing Methods 0.000 claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 238000007873 sieving Methods 0.000 claims abstract description 15
- 238000005245 sintering Methods 0.000 claims abstract description 14
- 239000002893 slag Substances 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 238000000465 moulding Methods 0.000 claims abstract description 12
- 239000011521 glass Substances 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 229910052839 forsterite Inorganic materials 0.000 claims abstract description 8
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000010791 quenching Methods 0.000 claims abstract description 7
- 230000000171 quenching effect Effects 0.000 claims abstract description 7
- 238000000137 annealing Methods 0.000 claims abstract description 6
- 238000000498 ball milling Methods 0.000 claims abstract description 6
- 238000005520 cutting process Methods 0.000 claims abstract description 6
- 238000011049 filling Methods 0.000 claims abstract description 6
- 238000002844 melting Methods 0.000 claims abstract description 6
- 230000008018 melting Effects 0.000 claims abstract description 6
- 238000003825 pressing Methods 0.000 claims abstract description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 39
- 239000000243 solution Substances 0.000 claims description 37
- 239000002956 ash Substances 0.000 claims description 33
- 238000006477 desulfuration reaction Methods 0.000 claims description 25
- 230000023556 desulfurization Effects 0.000 claims description 25
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 229960000583 acetic acid Drugs 0.000 claims description 17
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000010881 fly ash Substances 0.000 claims description 16
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 15
- 238000005303 weighing Methods 0.000 claims description 15
- ITHZDDVSAWDQPZ-UHFFFAOYSA-L barium acetate Chemical compound [Ba+2].CC([O-])=O.CC([O-])=O ITHZDDVSAWDQPZ-UHFFFAOYSA-L 0.000 claims description 12
- 239000012362 glacial acetic acid Substances 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 10
- 229910002651 NO3 Inorganic materials 0.000 claims description 8
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 8
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 7
- 239000003546 flue gas Substances 0.000 claims description 7
- 238000005187 foaming Methods 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 5
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 5
- 239000003513 alkali Substances 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
- 229910052593 corundum Inorganic materials 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 239000007863 gel particle Substances 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 235000006408 oxalic acid Nutrition 0.000 claims description 5
- 239000011819 refractory material Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 5
- 230000004907 flux Effects 0.000 claims description 3
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 1
- 229910017604 nitric acid Inorganic materials 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000006260 foam Substances 0.000 description 5
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910002113 barium titanate Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000003570 air Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- IQYKECCCHDLEPX-UHFFFAOYSA-N chloro hypochlorite;magnesium Chemical compound [Mg].ClOCl IQYKECCCHDLEPX-UHFFFAOYSA-N 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000007688 edging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- C04B35/46—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 titanium oxides or titanates
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Abstract
本发明公开了一种改性钛酸钡泡沫陶瓷材料的制备方法及其所得材料，制备方法包括如下步骤：S1、制备干凝胶粉体；S2、制备助熔剂粉体：将陶瓷抛磨废料、高炉炉渣、改性脱硫灰、镁橄榄石按照质量比混合，球磨后干燥、过筛后熔制成玻璃液，玻璃液经淬冷、破碎、烘干后，过筛得到助熔剂粉体；S3、预烧结：将得到的干凝胶粉体和助熔剂粉体按配比搅拌混合，预烧后冷却；S4、成型烧结：将粉体冷压成型并装入模具，将模具送入加热炉内加热，加热，退火，冷却、脱模、切割，即得泡沫陶瓷材料。本发明在满足常规使用需求的基础上，能够实现对陶瓷抛磨废料、高炉炉渣、脱硫灰的高效利用，不仅节约资源，降低生产成本，而且保护了环境，变废为宝。
Description
技术领域
本发明涉及泡沫陶瓷材料技术领域，尤其涉及一种改性钛酸钡泡沫陶瓷材料的制备方法及其所得材料。
背景技术
泡沫陶瓷(FoamCeramic，FC)是一种经特殊工艺制作而成的具有三维立体网络骨架结构和贯通气孔的新型多孔陶瓷材料。比较成熟的泡沫陶瓷制备工艺有发泡工艺、添加造孔剂工艺及有机泡沫浸渍法等。其中，有机泡沫浸渍法具有工艺简单、可批量生产等优点。然而，该工艺大部分采用微米或是更大尺寸的陶瓷原料以及无机助剂制备陶瓷浆料，因此常常需要进行长时间的研磨以得到分散均匀、流动性良好的浆料。鉴于泡沫陶瓷所具有的高化学稳定性、高强度、耐高温、抗热震、低密度、高气孔率、大比表面积等诸多优点，因此其广泛应用于制备汽车尾气装置、节能隔热材料、工业污水处理、化学催化剂载体、生物材料等。
在陶瓷砖的生产过程中将产生大量的磨边和抛光废料，由于这些抛磨废料中混有大量以碳化硅、树脂、氯氧镁水泥粘结剂等为主要成分的磨头废料，很难回收利用，因此我国大部分陶瓷企业主要采取填埋方式处理废料，但是这样不仅挤占了土地，同时对水、空气和土壤等环境造成了严重污染。
高炉炉渣是在高炉炼铁过程中，由矿石中的脉石、燃料中的灰分和熔剂中的非挥发组分形成的固体废物，经过水淬处理制成。
钢铁产量的剧增导致矿石和燃料在烧结过程中产生大量SO2，为此研发了多种脱硫技术，其中燃烧后烟气脱硫(FGD)技术较为成功。其中半干法脱硫技术因其操作简单、适应性强、脱硫效率高等优点，在烧结烟气脱硫中得到广泛应用。但半干法脱硫过程中会产生大量的副产物脱硫灰。目前，我国脱硫灰利用率仅为30％，大量的脱硫灰被堆放或抛弃，不仅占用大量土地，浪费资源，而且脱出来的硫又回到地面造成二次污染。
因此，有必要提供一种改性钛酸钡泡沫陶瓷材料的制备方法，解决陶瓷抛磨废料、高炉炉渣、脱硫灰利用率较低的问题。
发明内容
本发明的目的在于克服传统技术中存在的上述问题，提供一种改性钛酸钡泡沫陶瓷材料的制备方法及其所得材料。
为实现上述技术目的，达到上述技术效果，本发明是通过以下技术方案实现：
一种改性钛酸钡泡沫陶瓷材料的制备方法，包括如下步骤：
S1、制备干凝胶粉体：
按配比称取钛酸丁酯、异丙醇、冰醋酸、硝酸澜、醋酸钡，称取钛酸丁酯溶于异丙醇，在室温条件下搅拌均匀，再滴加冰醋酸，滴加完毕后继续搅拌，得到近乎透明的溶液A；称取硝酸澜、醋酸钡溶于36％醋酸溶液，并加入蒸馏水，搅拌使所有固体都均匀溶解形成透明溶液B；将溶液B缓慢滴加到溶液A中，边滴加边搅拌，搅拌均匀后将所得混合溶液在水浴中80-90℃条件下进行加热1-2h，得到透明凝胶；将所得透明凝胶放入干燥箱中110-120℃条件下干燥2-3h，得到干凝胶颗粒，研磨后，得到干凝胶粉体；
S2、制备助熔剂粉体：
将陶瓷抛磨废料、高炉炉渣、改性脱硫灰、镁橄榄石按照质量比混合，经湿法球磨后干燥，过100目筛后熔制成玻璃液，玻璃液经淬冷、破碎、烘干后，过100目筛得到助熔剂粉体；
S3、预烧结：
将步骤S1得到的干凝胶粉体和步骤S2得到的助熔剂粉体按配比搅拌混合，而后放入马弗炉中在800℃温度下预烧1.5-2h，然后自然冷却到室温；
S4、成型烧结：
将预烧冷却后的粉体冷压成型，并装入发泡耐火材料模具，将模具送入加热炉内加热，加热至1180℃，保温10-30min，然后退火，冷却、脱模、切割，即得泡沫陶瓷材料。
进一步地，如上所述改性钛酸钡泡沫陶瓷材料的制备方法，步骤S1中，钛酸丁酯、异丙醇、冰醋酸、硝酸澜、醋酸钡的摩尔比为2:5-7:2-4:1-2:1-2。
进一步地，如上所述改性钛酸钡泡沫陶瓷材料的制备方法，步骤S2中，将陶瓷抛磨废料、高炉炉渣、改性脱硫灰、镁橄榄石按照质量比20-30：20-30：30-40：5-8混合。
进一步地，如上所述改性钛酸钡泡沫陶瓷材料的制备方法，步骤S2中，陶瓷抛磨废料按质量百分比计，包含60-64％的SiO2、13-16％的Al2O3、3-5％的MgO、1-2％的CaO、1-3％的Na2O、1-2％的K2O、0.5-1％的Fe2O3和余量杂质。
进一步地，如上所述改性钛酸钡泡沫陶瓷材料的制备方法，步骤S2中，改性脱硫灰的制备工艺为：
1)将半干法烧结烟气脱硫灰研磨，过100目筛，得脱硫灰I；
2)将所得的脱硫灰I浸渍于去离子水中，加热至50-60℃，保温2-3h；过滤，滤液为氯化盐溶液，滤渣为脱硫灰II；
3)将所得的脱硫灰II浸渍于草酸溶液中，加热至70-72℃，保温搅拌5-6h，其中采用碱液吸收SO2气体；过滤，取滤渣采用去离子水洗3-4次，于70℃下干燥，即得改性脱硫灰。
进一步地，如上所述改性钛酸钡泡沫陶瓷材料的制备方法，步骤S3中，将步骤S1得到的干凝胶粉体和步骤S2得到的助熔剂粉体按质量比2-4：1搅拌混合。
进一步地，如上所述改性钛酸钡泡沫陶瓷材料的制备方法，步骤S4中，加热炉采用分步加热方式，先以8-10℃/min的速率从室温升到620℃，保温10-15min；然后以6-8℃/min的升温速率升到940℃，保温20-25min；再以2-3℃/min的升温速率升到烧成温度1180℃，保温10-30min。
本发明还提供了一种改性钛酸钡泡沫陶瓷材料，采用上述制备方法制备而成。
本发明的有益效果是：
1、本发明泡沫陶瓷材料的制备方法设计科学合理，在满足常规使用需求的基础上，能够实现对陶瓷抛磨废料、高炉炉渣、脱硫灰的高效利用，不仅节约资源，降低生产成本，而且保护了环境，变废为宝。
2、本发明制备的泡沫陶瓷材料以闭孔结构为主，由于泡沫陶瓷材料中闭口气孔减少了热对流的发生，有效降低了材料的传热效率，从而使泡沫陶瓷具有低热导率的特性，适用于作为保温材料使用。
3、本发明采用水热合成法来制备钛酸钡粉体，能够在较低温度下，直接从溶液中获得晶粒发育完整的粉末，粉体的纯度高、化学成本均匀，粒径小、粒子尺寸分布好。
当然，实施本发明的任一产品并不一定需要同时达到以上的所有优点。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例，都属于本发明保护的范围。
实施例1
一种改性钛酸钡泡沫陶瓷材料的制备方法，包括如下步骤：
S1、制备干凝胶粉体：
按摩尔比为2:6:3:1:1称取钛酸丁酯、异丙醇、冰醋酸、硝酸澜、醋酸钡，称取钛酸丁酯溶于异丙醇，在室温条件下搅拌均匀，再滴加冰醋酸，滴加完毕后继续搅拌，得到近乎透明的溶液A；称取硝酸澜、醋酸钡溶于36％醋酸溶液，并加入蒸馏水，搅拌使所有固体都均匀溶解形成透明溶液B；将溶液B缓慢滴加到溶液A中，边滴加边搅拌，搅拌均匀后将所得混合溶液在水浴中85℃条件下进行加热1.5h，得到透明凝胶；将所得透明凝胶放入干燥箱中115℃条件下干燥2.5h，得到干凝胶颗粒，研磨后，得到干凝胶粉体；
S2、制备助熔剂粉体：
将陶瓷抛磨废料、高炉炉渣、改性脱硫灰、镁橄榄石按照质量比25：25：35：7混合，经湿法球磨后干燥，过100目筛后熔制成玻璃液，玻璃液经淬冷、破碎、烘干后，过100目筛得到助熔剂粉体；
其中，陶瓷抛磨废料按质量百分比计，包含62％的SiO2、15％的Al2O3、4％的MgO、1.8％的CaO、2.3％的Na2O、1.4％的K2O、0.8％的Fe2O3和余量杂质；
其中，改性脱硫灰的制备工艺为：
1)将半干法烧结烟气脱硫灰研磨，过100目筛，得脱硫灰I；
2)将所得的脱硫灰I浸渍于去离子水中，加热至55℃，保温2.5h；过滤，滤液为氯化盐溶液，滤渣为脱硫灰II；
3)将所得的脱硫灰II浸渍于草酸溶液中，加热至71℃，保温搅拌5.5h，其中采用碱液吸收SO2气体；过滤，取滤渣采用去离子水洗3次，于70℃下干燥，即得改性脱硫灰。
S3、预烧结：
将步骤S1得到的干凝胶粉体和步骤S2得到的助熔剂粉体质量比3：1搅拌混合，而后放入马弗炉中在800℃温度下预烧1.8h，然后自然冷却到室温；
S4、成型烧结：
将预烧冷却后的粉体冷压成型，并装入发泡耐火材料模具，将模具送入加热炉内加热，加热炉采用分步加热方式，先以9℃/min的速率从室温升到620℃，保温12min；然后以7℃/min的升温速率升到940℃，保温23min；再以2℃/min的升温速率升到烧成温度1180℃，保温25min；然后退火，冷却、脱模、切割，即得泡沫陶瓷材料。
经测试该泡沫陶瓷材料的抗压强度为0.35MPa，室温电阻率为1.923。
实施例2
一种改性钛酸钡泡沫陶瓷材料的制备方法，包括如下步骤：
S1、制备干凝胶粉体：
按摩尔比为2:5:4:2:2称取钛酸丁酯、异丙醇、冰醋酸、硝酸澜、醋酸钡，称取钛酸丁酯溶于异丙醇，在室温条件下搅拌均匀，再滴加冰醋酸，滴加完毕后继续搅拌，得到近乎透明的溶液A；称取硝酸澜、醋酸钡溶于36％醋酸溶液，并加入蒸馏水，搅拌使所有固体都均匀溶解形成透明溶液B；将溶液B缓慢滴加到溶液A中，边滴加边搅拌，搅拌均匀后将所得混合溶液在水浴中85℃条件下进行加热1.5h，得到透明凝胶；将所得透明凝胶放入干燥箱中115℃条件下干燥2.5h，得到干凝胶颗粒，研磨后，得到干凝胶粉体；
S2、制备助熔剂粉体：
将陶瓷抛磨废料、高炉炉渣、改性脱硫灰、镁橄榄石按照质量比20：30：30：8混合，经湿法球磨后干燥，过100目筛后熔制成玻璃液，玻璃液经淬冷、破碎、烘干后，过100目筛得到助熔剂粉体；
其中，陶瓷抛磨废料按质量百分比计，包含62％的SiO2、15％的Al2O3、4％的MgO、1.8％的CaO、2.3％的Na2O、1.4％的K2O、0.8％的Fe2O3和余量杂质；
其中，改性脱硫灰的制备工艺为：
1)将半干法烧结烟气脱硫灰研磨，过100目筛，得脱硫灰I；
2)将所得的脱硫灰I浸渍于去离子水中，加热至55℃，保温2.5h；过滤，滤液为氯化盐溶液，滤渣为脱硫灰II；
3)将所得的脱硫灰II浸渍于草酸溶液中，加热至71℃，保温搅拌5.5h，其中采用碱液吸收SO2气体；过滤，取滤渣采用去离子水洗3次，于70℃下干燥，即得改性脱硫灰。
S3、预烧结：
将步骤S1得到的干凝胶粉体和步骤S2得到的助熔剂粉体质量比2：1搅拌混合，而后放入马弗炉中在800℃温度下预烧1.8h，然后自然冷却到室温；
S4、成型烧结：
将预烧冷却后的粉体冷压成型，并装入发泡耐火材料模具，将模具送入加热炉内加热，加热炉采用分步加热方式，先以8℃/min的速率从室温升到620℃，保温15min；然后以6℃/min的升温速率升到940℃，保温25min；再以3℃/min的升温速率升到烧成温度1180℃，保温10min；然后退火，冷却、脱模、切割，即得泡沫陶瓷材料。
经测试该泡沫陶瓷材料的抗压强度为0.28MPa，室温电阻率为1.875。
实施例3
一种改性钛酸钡泡沫陶瓷材料的制备方法，包括如下步骤：
S1、制备干凝胶粉体：
按摩尔比为2:5-7:2-4:1-2:1-2称取钛酸丁酯、异丙醇、冰醋酸、硝酸澜、醋酸钡，称取钛酸丁酯溶于异丙醇，在室温条件下搅拌均匀，再滴加冰醋酸，滴加完毕后继续搅拌，得到近乎透明的溶液A；称取硝酸澜、醋酸钡溶于36％醋酸溶液，并加入蒸馏水，搅拌使所有固体都均匀溶解形成透明溶液B；将溶液B缓慢滴加到溶液A中，边滴加边搅拌，搅拌均匀后将所得混合溶液在水浴中85℃条件下进行加热1.5h，得到透明凝胶；将所得透明凝胶放入干燥箱中115℃条件下干燥2.5h，得到干凝胶颗粒，研磨后，得到干凝胶粉体；
S2、制备助熔剂粉体：
将陶瓷抛磨废料、高炉炉渣、改性脱硫灰、镁橄榄石按照质量比30：20：40：5混合，经湿法球磨后干燥，过100目筛后熔制成玻璃液，玻璃液经淬冷、破碎、烘干后，过100目筛得到助熔剂粉体；
其中，陶瓷抛磨废料按质量百分比计，包含62％的SiO2、15％的Al2O3、4％的MgO、1.8％的CaO、2.3％的Na2O、1.4％的K2O、0.8％的Fe2O3和余量杂质；
其中，改性脱硫灰的制备工艺为：
1)将半干法烧结烟气脱硫灰研磨，过100目筛，得脱硫灰I；
2)将所得的脱硫灰I浸渍于去离子水中，加热至55℃，保温2.5h；过滤，滤液为氯化盐溶液，滤渣为脱硫灰II；
3)将所得的脱硫灰II浸渍于草酸溶液中，加热至71℃，保温搅拌5.5h，其中采用碱液吸收SO2气体；过滤，取滤渣采用去离子水洗3次，于70℃下干燥，即得改性脱硫灰。
S3、预烧结：
将步骤S1得到的干凝胶粉体和步骤S2得到的助熔剂粉体质量比4：1搅拌混合，而后放入马弗炉中在800℃温度下预烧1.8h，然后自然冷却到室温；
S4、成型烧结：
将预烧冷却后的粉体冷压成型，并装入发泡耐火材料模具，将模具送入加热炉内加热，加热炉采用分步加热方式，先以10℃/min的速率从室温升到620℃，保温10min；然后以8℃/min的升温速率升到940℃，保温20min；再以2℃/min的升温速率升到烧成温度1180℃，保温30min；然后退火，冷却、脱模、切割，即得泡沫陶瓷材料。
经测试该泡沫陶瓷材料的抗压强度为0.26MPa，室温电阻率为1.992。
本发明实施例1-3提供的泡沫陶瓷材料在满足常规使用需求的基础上，能够实现对陶瓷抛磨废料、高炉炉渣、脱硫灰的高效利用，环保效果较好。
以上公开的本发明优选实施例只是用于帮助阐述本发明。优选实施例并没有详尽叙述所有的细节，也不限制该发明仅为具体实施方式。显然，根据本说明书的内容，可作很多的修改和变化。本说明书选取并具体描述这些实施例，是为了更好地解释本发明的原理和实际应用，从而使所属技术领域技术人员能很好地理解和利用本发明。本发明仅受权利要求书及其全部范围和等效物的限制。
Claims (8)
1.一种改性钛酸钡泡沫陶瓷材料的制备方法，其特征在于，包括如下步骤：
S1、制备干凝胶粉体：
按配比称取钛酸丁酯、异丙醇、冰醋酸、硝酸澜、醋酸钡，称取钛酸丁酯溶于异丙醇，在室温条件下搅拌均匀，再滴加冰醋酸，滴加完毕后继续搅拌，得到近乎透明的溶液A；称取硝酸澜、醋酸钡溶于36％醋酸溶液，并加入蒸馏水，搅拌使所有固体都均匀溶解形成透明溶液B；将溶液B缓慢滴加到溶液A中，边滴加边搅拌，搅拌均匀后将所得混合溶液在水浴中80-90℃条件下进行加热1-2h，得到透明凝胶；将所得透明凝胶放入干燥箱中110-120℃条件下干燥2-3h，得到干凝胶颗粒，研磨后，得到干凝胶粉体；
S2、制备助熔剂粉体：
将陶瓷抛磨废料、高炉炉渣、改性脱硫灰、镁橄榄石按照质量比混合，经湿法球磨后干燥，过100目筛后熔制成玻璃液，玻璃液经淬冷、破碎、烘干后，过100目筛得到助熔剂粉体；
S3、预烧结：
将步骤S1得到的干凝胶粉体和步骤S2得到的助熔剂粉体按配比搅拌混合，而后放入马弗炉中在800℃温度下预烧1.5-2h，然后自然冷却到室温；
S4、成型烧结：
将预烧冷却后的粉体冷压成型，并装入发泡耐火材料模具，将模具送入加热炉内加热，加热至1180℃，保温10-30min，然后退火，冷却、脱模、切割，即得泡沫陶瓷材料。
2.根据权利要求1所述的一种改性钛酸钡泡沫陶瓷材料的制备方法，其特征在于：步骤S1中，钛酸丁酯、异丙醇、冰醋酸、硝酸澜、醋酸钡的摩尔比为2:5-7:2-4:1-2:1-2。
3.根据权利要求1所述的一种改性钛酸钡泡沫陶瓷材料的制备方法，其特征在于：步骤S2中，将陶瓷抛磨废料、高炉炉渣、改性脱硫灰、镁橄榄石按照质量比20-30：20-30：30-40：5-8混合。
4.根据权利要求1所述的一种改性钛酸钡泡沫陶瓷材料的制备方法，其特征在于：步骤S2中，陶瓷抛磨废料按质量百分比计，包含60-64％的SiO2、13-16％的Al2O3、3-5％的MgO、1-2％的CaO、1-3％的Na2O、1-2％的K2O、0.5-1％的Fe2O3和余量杂质。
5.根据权利要求1所述的一种改性钛酸钡泡沫陶瓷材料的制备方法，其特征在于：步骤S2中，改性脱硫灰的制备流程为：
1)将半干法烧结烟气脱硫灰研磨，过100目筛，得脱硫灰I；
2)将所得的脱硫灰I浸渍于去离子水中，加热至50-60℃，保温2-3h；过滤，滤液为氯化盐溶液，滤渣为脱硫灰II；
3)将所得的脱硫灰II浸渍于草酸溶液中，加热至70-72℃，保温搅拌5-6h，其中采用碱液吸收SO2气体；过滤，取滤渣采用去离子水洗3-4次，于70℃下干燥，即得改性脱硫灰。
6.根据权利要求1所述的一种改性钛酸钡泡沫陶瓷材料的制备方法，其特征在于：步骤S3中，将步骤S1得到的干凝胶粉体和步骤S2得到的助熔剂粉体按质量比2-4：1搅拌混合。
7.根据权利要求1所述的一种改性钛酸钡泡沫陶瓷材料的制备方法，其特征在于：步骤S4中，加热炉采用分步加热方式，先以8-10℃/min的速率从室温升到620℃，保温10-15min；然后以6-8℃/min的升温速率升到940℃，保温20-25min；再以2-3℃/min的升温速率升到烧成温度1180℃，保温10-30min。
8.如权利要求1-7任一项所述的制备方法制备的改性钛酸钡泡沫陶瓷材料。
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