CN117923893A - 一种钛酸铝陶瓷的制备方法 - Google Patents
一种钛酸铝陶瓷的制备方法 Download PDFInfo
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- 229910000505 Al2TiO5 Inorganic materials 0.000 title claims abstract description 31
- AABBHSMFGKYLKE-SNAWJCMRSA-N propan-2-yl (e)-but-2-enoate Chemical compound C\C=C\C(=O)OC(C)C AABBHSMFGKYLKE-SNAWJCMRSA-N 0.000 title claims abstract description 31
- 239000000919 ceramic Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000003054 catalyst Substances 0.000 claims abstract description 51
- 239000002699 waste material Substances 0.000 claims abstract description 39
- GFNGCDBZVSLSFT-UHFFFAOYSA-N titanium vanadium Chemical compound [Ti].[V] GFNGCDBZVSLSFT-UHFFFAOYSA-N 0.000 claims abstract description 23
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000010531 catalytic reduction reaction Methods 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 238000003825 pressing Methods 0.000 claims abstract description 8
- 238000005245 sintering Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims description 15
- 238000000498 ball milling Methods 0.000 claims description 13
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 8
- 238000001238 wet grinding Methods 0.000 claims description 6
- 239000004408 titanium dioxide Substances 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 4
- 239000002270 dispersing agent Substances 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
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- 238000010298 pulverizing process Methods 0.000 claims 1
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- 239000000463 material Substances 0.000 abstract description 3
- 150000002736 metal compounds Chemical class 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract description 3
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 239000010812 mixed waste Substances 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 238000000643 oven drying Methods 0.000 description 5
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
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- 239000012535 impurity Substances 0.000 description 2
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- 239000007788 liquid Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 229910001930 tungsten oxide Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 101001121408 Homo sapiens L-amino-acid oxidase Proteins 0.000 description 1
- 102100026388 L-amino-acid oxidase Human genes 0.000 description 1
- 101100012902 Saccharomyces cerevisiae (strain ATCC 204508 / S288c) FIG2 gene Proteins 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
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- 238000006243 chemical reaction Methods 0.000 description 1
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- 230000000694 effects Effects 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明属于固废回收技术领域，具体涉及一种钛酸铝陶瓷的制备方法。本发明提供了一种钛酸铝陶瓷的制备方法，包括以下步骤：将钒钛基废选择性催化还原催化剂和氧化铝混合，依次进行压制和烧结，得到所述钛酸铝陶瓷。本发明提供的制备方法以钒钛基废选择性催化还原（SCR）催化剂为原料，与氧化铝粉末进行压制烧结，使废SCR催化剂与氧化铝同时接受高温和压力，有热能和应力去促进粉末颗粒的结合和材料的致密化，得到的钛酸铝陶瓷纯度较高。区别于现有湿法回收工艺中以金属化合物形式回收废SCR催化剂，本发明提供的方法实现了废SCR催化剂的高附加价值利用，并且过程简单，安全环保。
Description
技术领域
本发明属于固废回收技术领域，具体涉及一种钛酸铝陶瓷的制备方法。
背景技术
钒钛基选择性催化还原（SCR）催化剂主要应用于烟气脱硝处理工艺，此种催化剂在使用过程中，受工作环境的影响会导致其活性组分或微观结构发生变化，进而使其脱硝性能下降，严重时失去活性。根据所用钒钛基SCR催化剂所使用的场所的不同，钒钛基SCR催化剂的组成和含量会有所不同，但是主要物质为二氧化钛，占比达到80%以上，回收再利用价值高。
目前，对于失去活性的废SCR催化剂，回收处理主要是通过酸溶、碱溶、盐溶等方法提取其中的贵金属，或者通过高温熔炼将其中的金属元素还原成金属单质或合金。但是，由于废SCR催化剂的成分复杂，不同类型和不同产地的废SCR催化剂可能具有不同的性质和成分，因此需要采取不同的处理方法和工艺，且回收利用率较低。
发明内容
本发明的目的在于提供一种钛酸铝陶瓷的制备方法，本发明提供的方法能够实现钒钛基废选择性催化还原催化剂的高效资源化利用，制备出纯度较高的钛酸铝陶瓷。
为了实现上述目的，本发明提供如下技术方案：
本发明提供了一种钛酸铝陶瓷的制备方法，包括以下步骤：
将钒钛基废选择性催化还原催化剂和氧化铝混合，依次进行压制和烧结，得到所述钛酸铝陶瓷。
优选地，所述钒钛基废选择性催化还原催化剂中二氧化钛的质量百分含量为70~100%。
优选地，所述钒钛基废选择性催化还原催化剂和氧化铝的质量比为9：10~15。
优选地，所述混合为球磨；所述球磨的转速为200~600r/min，时间为4~16h。
优选地，所述球磨为湿磨；所述湿磨的分散剂为酒精。
优选地，所述压制的压力为8~12MPa，保压时间为1~3min。
优选地，所述烧结温度为1300~1600℃，保温时间为2~6h。
优选地，所述混合前还包括将所述钒钛基废选择性催化还原催化剂依次进行清洗、干燥、粉碎和过筛。
优选地，所述清洗为超声清洗；所述超声清洗的时间为8~16h；
所述干燥为烘干；所述烘干的温度为60~120℃，时间为12~36h。
优选地，所述过筛的筛网目数为200~600目。
本发明提供了一种钛酸铝陶瓷的制备方法，包括以下步骤：将钒钛基废选择性催化还原催化剂和氧化铝混合，依次进行压制和烧结，得到所述钛酸铝陶瓷。本发明提供的制备方法以钒钛基废选择性催化还原（SCR）催化剂为原料，与氧化铝粉末进行压制烧结，使废SCR催化剂与氧化铝同时接受高温和压力，用热能和应力去促进粉末颗粒的结合和材料的致密化，得到的钛酸铝陶瓷纯度较高。区别于现有湿法回收工艺中以金属化合物形式回收废SCR催化剂，本发明提供的方法实现了废SCR催化剂的高附加价值利用和固体废物的无害化和资源化，并且过程简单，在回收利用的过程中，无污染性废液或者气体产生，安全环保。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动性的前提下，还可以根据这些附图获得其他的附图。
图1为实施例1所得钛酸铝陶瓷的X射线衍射图谱（上）和钛酸铝标准XRD图谱（下）对照图；
图2为实施例2所得钛酸铝陶瓷的X射线衍射图谱（上）和钛酸铝标准XRD图谱（下）对照图。
具体实施方式
本发明提供了一种钛酸铝陶瓷的制备方法，包括以下步骤：
将钒钛基废选择性催化还原催化剂和氧化铝混合，依次进行压制和烧结，得到所述钛酸铝陶瓷。
在本发明中，若无特殊说明，所有原料组分均为本领域技术人员熟知的市售产品。
在本发明中，所述钒钛基废选择性催化还原催化剂中二氧化钛的质量百分含量优选为70~100%，更优选为80~90%，最优选为86.29%；氧化钨的质量百分含量优选为0~10%，更优选为2~8%，最优选为5.24%；氧化钙的质量百分含量优选为0~3%，更优选为1~2%，最优选为1.40%；氧化硅的质量百分含量优选为0~10%，更优选为2~8%，最优选为4.34%；五氧化二钒的质量百分含量优选为0~5%，更优选为0.5~3%，最优选为0.69%。
在本发明中，所述混合前还包括将所述钒钛基废选择性催化还原催化剂依次进行清洗、干燥、粉碎和过筛。
在本发明中，所述清洗优选为超声清洗；所述超声清洗的时间优选为8~16h，更优选为10~14h；所述超声清洗优选在超声波清洗仪中进行；所述清洗的作用为除灰，去除废SCR催化剂中大量尘土。
在本发明中，所述干燥优选为烘干；所述烘干的温度优选为60~120℃，更优选为80~100℃；时间优选为12~36h，更优选为18~30h。
在本发明中，所述过筛的筛网目数优选为200~600目，更优选为300~500目。
在本发明中，所述钒钛基废选择性催化还原催化剂和氧化铝的质量比优选为9：10~15，更优选为9：10~13，最优选为9：10~11。
在本发明中，所述混合为球磨；所述球磨的转速优选为200~600r/min，更优选为300~500r/min；时间优选为4~16h，更优选为8~12h；所述球磨优选为湿磨；所述湿磨的分散剂优选为酒精；本发明对所述酒精的用量没有任何特殊的限定，采用本领域技术人员熟知的球磨分散剂的用量浸没球磨原料即可。
在本发明中，所述球磨后还优选包括烘干；所述烘干的温度优选为60~120℃，更优选为80~100℃；时间优选为12~36h，更优选为18~30h。
在本发明中，所述压制的压力优选为8~12MPa，更优选为9~11MPa；保压时间优选为1~3min，更优选为2~3min。
在本发明中，所述烧结温度优选为1300~1600℃，更优选为1400~1500℃；保温时间优选为2~6h，更优选为3~5h。
本发明提供的制备方法以钒钛基废选择性催化还原（SCR）催化剂为原料，与氧化铝粉末进行压制烧结，使废SCR催化剂与氧化铝同时接受高温和压力，有热能和应力去促进粉末颗粒的结合和材料的致密化，得到的钛酸铝陶瓷纯度较高。区别于现有湿法回收工艺中以金属化合物形式回收废SCR催化剂，本发明提供的方法实现了废SCR催化剂的高附加价值利用和固体废物的无害化和资源化，并且过程简单，在回收利用的过程中，无污染性废液或者气体产生，安全环保。本发明所述制备方法中的主要化学反应式为式1：
TiO2+Al2O3=Al2TiO5（式1）。
为了进一步说明本发明，下面结合附图和实施例对本发明提供的钛酸铝陶瓷的制备方法进行详细地描述，但不能将它们理解为对本发明保护范围的限定。
实施例1
将块状钒钛基废SCR催化剂置于蒸馏水中，置于超声波清洗仪超声清洗12h。将废SCR催化剂取出，在80℃烘干箱中烘24h，然后将废SCR催化剂粉碎，过400目筛，得到粉碎废SCR催化剂。所述钒钛基废选择性催化还原催化剂中二氧化钛的质量百分含量为86.29%，氧化钨的质量百分含量为5.24%，氧化钙的质量百分含量为1.40%，氧化硅的质量百分含量为4.34%，五氧化二钒的质量百分含量为0.69%。
称取9.25g废SCR催化剂与10.2g氧化铝，放入球磨罐中，加入酒精，使酒精刚好淹没粉末，进行机械球磨，转速为300r/min，时间为12h，将混合均匀的废SCR催化剂与氧化铝放入蒸发皿中，在80℃烘干箱中烘24h，最后将干燥的，混合均与的废SCR催化剂与氧化铝取出，进行压片。
称取1g混合均匀的废SCR催化剂与氧化铝放入直径为8mm的圆形模具中进行压片，压力为10MPa，时间为2.5min。
将压好的片放入坩埚中，将坩埚放入高温炉中，升温到1500℃，并在1500℃温度下保温4h，保温结束后，随炉冷却到室温，将烧结后的片取出，得到钛酸铝陶瓷。
本实施例所得钛酸铝陶瓷的X射线衍射图谱（上）和钛酸铝标准XRD图谱（下）如图1所示，从图1可以看出，所得钛酸铝陶瓷主相为钛酸铝，其他杂质相含量低，产物纯度较高。
实施例2
将块状钒钛基废SCR催化剂置于蒸馏水中，置于超声波清洗仪超声清洗12h。将废SCR催化剂取出，在80℃烘干箱中烘24h，然后将废SCR催化剂粉碎，过400目筛，得到粉碎废SCR催化剂。
称取9.25g废SCR催化剂与11.22g氧化铝，放入球磨罐中，加入酒精，使酒精刚好淹没粉末，进行机械球磨，转速为300r/min，时间为12h，将混合均匀的废SCR催化剂与氧化铝放入蒸发皿中，在80℃烘干箱中烘24h，最后将干燥的，混合均与的废SCR催化剂与氧化铝取出，进行压片。
称取1g混合均匀的废SCR催化剂与氧化铝放入直径为8mm的圆形模具中进行压片，压力为10MPa，时间为2.5min。
将压好的片放入坩埚中，将坩埚放入高温炉中，升温到1500℃，并在1500℃温度下保温4h，保温结束后，随炉冷却到室温，将烧结后的片取出，得到钛酸铝陶瓷。
本实施例所得钛酸铝陶瓷的X射线衍射图谱（上）和钛酸铝标准XRD图谱（下）如图2所示，从XRD图中可以看出，所得钛酸铝陶瓷主相为钛酸铝，其他杂质相含量低，产物纯度较高。
尽管上述实施例对本发明做出了详尽的描述，但它仅仅是本发明一部分实施例，而不是全部实施例，还可以根据本实施例在不经创造性前提下获得其他实施例，这些实施例都属于本发明保护范围。
Claims (10)
1.一种钛酸铝陶瓷的制备方法，其特征在于，包括以下步骤：
将钒钛基废选择性催化还原催化剂和氧化铝混合，依次进行压制和烧结，得到所述钛酸铝陶瓷。
2.根据权利要求1所述的制备方法，其特征在于，所述钒钛基废选择性催化还原催化剂中二氧化钛的质量百分含量为70~100%。
3.根据权利要求1或2所述的制备方法，其特征在于，所述钒钛基废选择性催化还原催化剂和氧化铝的质量比为9：10~15。
4.根据权利要求1所述的制备方法，其特征在于，所述混合为球磨；所述球磨的转速为200~600r/min，时间为4~16h。
5.根据权利要求4所述的制备方法，其特征在于，所述球磨为湿磨；所述湿磨的分散剂为酒精。
6.根据权利要求1所述的制备方法，其特征在于，所述压制的压力为8~12MPa，保压时间为1~3min。
7.根据权利要求1所述的制备方法，其特征在于，所述烧结温度为1300~1600℃，保温时间为2~6h。
8.根据权利要求1或4所述的制备方法，其特征在于，所述混合前还包括将所述钒钛基废选择性催化还原催化剂依次进行清洗、干燥、粉碎和过筛。
9.根据权利要求8所述的制备方法，其特征在于，所述清洗为超声清洗；所述超声清洗的时间为8~16h；
所述干燥为烘干；所述烘干的温度为60~120℃，时间为12~36h。
10.根据权利要求8所述的制备方法，其特征在于，所述过筛的筛网目数为200~600目。
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