CN108031431B - 一种表面改性的复合活性Al2O3-ZnO载体球形颗粒的制备方法 - Google Patents
一种表面改性的复合活性Al2O3-ZnO载体球形颗粒的制备方法 Download PDFInfo
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Abstract
本发明涉及一种表面改性的复合活性Al2O3‑ZnO球形载体颗粒的制备方法,在活性氧化铝的表面用乙氧基修饰,包括以下操作步骤:将纯度大于98.50%的活性γ‑Al2O3或ρ‑Al2O3、纯度大于98.50%的活性ZnO、AgNO3、碳酸氢钠以及羧甲基纤维素按比例混合,在粉末分散机内分散打匀,按照常规方法制成一定规格的球形颗粒,在容器内通入乙醇、二氧化碳和水蒸气熏制3~4小时进行钝化,之后在350℃~450℃烘干,改性及活化,制备成具有表面改性的复合活性载体球形颗粒。本发明制备的复合活性载体具有孔径结构合理、吸附容量高以及结构强度好的特性,是氧化剂优良的载体,可用于室内空气的吸附‑氧化过程。
Description
技术领域
本发明涉及一种表面改性的复合活性Al2O3-ZnO载体球形颗粒的制备方法。
背景技术
活性氧化铝是一种多孔性、高分散性材料,其微孔所表现的吸附性能、表面活性、良好的热稳定性等;氧化铝载体颗粒机械强度好,吸湿性强,吸水后颗粒不裂不胀,满足了化学反应催化剂和催化剂载体的基本要求。
然而,活性氧化铝作为空气净化载体,其吸附容量不如活性炭,又不能与被氧化降解的有机硫化物、有机胺类、不饱和烃等发生化学反应,所以单一的活性氧化铝不适合作为空气净化剂载体使用。
发明内容
本发明所要解决的技术问题是,克服现有技术的缺点,提供一种微孔分布均匀,吸附容量大,性能稳定及抗压强度好的表面改性的活性氧化铝-活性氧化锌球形载体的制备方法。
本发明的技术解决方案是提供一种表面改性的复合活性Al2O3-ZnO载体球形颗粒的制备方法,其步骤如下:
①将活性三氧化二铝球磨至平均粒径0.8~1.0μm,得到氧化铝微粉;将氧化锌球磨至平均粒径1~1.5μm,得到氧化锌微粉;将碳酸氢钠、硝酸银和羧甲基纤维素混合,球磨至平均粒径0.8~1.0μm,得到粘结剂微粉;
②将步骤①所制备的三份微粉混合均匀,其中各个组分的质量比为:氧化铝800~900份,氧化锌50~100份,硝酸银20~40份,碳酸氢钠20~30份,羧甲基纤维素10~15份,经过造粒后筛分出5.0~7.0mm的颗粒,然后经过130~150Mpa压力成型,再放入乙醇、二氧化碳和水蒸气的混合气体中熏蒸3~4小时进行钝化;
③将步骤②中所得到的颗粒进行活化和改性,温度350℃~450℃,升温速率35℃~40℃/h,保温2.5~3.5小时,冷却后得到复合活性颗粒。
作为优化,所述活性氧化铝为活性γ-Al2O3或ρ-Al2O3。
作为优化,所述氧化锌为活性ZnO。
作为优化,所述步骤②中的乙醇、二氧化碳和水蒸气体积比为1:(1~2):(3~4)。
作为优化,所述步骤③中得到的复合活性载体颗粒的含水量不高于3.5%。
此外,本发明还涉及保护利用上述方法制备的表面改性的复合活性Al2O3-ZnO载体球形颗粒。
在活性氧化铝和氧化锌表面形成乙氧基,氧化铝和氧化锌的水化及乙氧基化的反应式如下:
本发明的有益技术效果是:
本发明在活性氧化铝表面,用乙氧基(CH3CH2O-)修饰,可提高氧化铝对苯系物、烯烃类有机污染物的吸附性能。
纳米氧化锌(ZnO)粒径介于1~100nm之间,是一种高端的高功能精细无机产品,表现出许多特殊的性质,如非迁移性、荧光性、压电性、吸收和散射紫外线能力等。纳米氧化锌目前还可用来制造远红外线反射纤维的材料,俗称远红外陶瓷粉。氧化锌是一种半导体催化剂的电子结构,在光照射下,当一个具有一定能量的光子或者具有超过这个半导体带隙能量 Eg的光子射入半导体时,一个电子从价带VB激发到导带CB,而留下了一个空穴。激发态的导带电子和价带空穴能够重新结合消除输入的能量和热,电子在材料的表面态被捕捉,价态电子跃迁到导带,价带的空穴把周围环境中的羟基电子抢夺过来使羟基变成自由基,作为强氧化剂而完成对有机物(或含氯)的降解,将病菌和病毒杀死,尤其适合吸附硫化物、胺类。另外,氧化锌可与氨形成稳定的络离子(Zn[NH3]4 +),与硫化氢形成硫化锌(ZnS),能够完全净化空气中的氨和硫化氢,净化效果突出。
NH3.H2O+ZnO—→Zn[NH3]4.OH
ZnO+H2S—→ZnS
ZnO+SO2+H2O—→ZnSO3
银离子的催化作用,可使污染物在氧化锌表面发生光解;硫类和胺类化合物被氧化后,可与氧化锌(ZnO)反应,形成稳定的复合产物。
本发明将活性氧化铝、活性氧化锌和银离子(粒子)结合起来,解决活性氧化铝的单一吸附性能,提高氧化铝载体材料的承载范围,扩大其用途,尤其适用于承载氧化型空气净化剂。
将各个功能的组分通过合理的粒径比混合造粒,采用乙醇、二氧化碳和水蒸气混合气体进行活化前处理,在氧化铝或氧化锌微孔表面修饰有乙氧基,提高了对苯系物、不饱和烃类、烷烃类等VOCs的吸附性能和效能,硝酸银、羧甲基纤维素在氧化铝-氧化锌焙烧过程中的成孔作用,保证了该材料的微孔形态构造,使复合活性功能载体材料颗粒的抗压强度增大,提高了活性氧化铝载体的吸附性能和容量,能够促进了复合吸附、催化和氧化的净化功能。
本发明制备的复合活性载体具有孔径结构合理、吸附容量高以及结构强度好的特性,是氧化剂优良的载体,可用于室内空气的吸附-氧化过程。
附图说明
图1为实施例1复合活性载体颗粒的电镜图;
图2为实施例2复合活性载体颗粒的电镜图;
图3为实施例3复合活性载体颗粒的电镜图。
具体实施方式
下述非限定性实施例可以使本领域的普通技术人员更全面地理解本发明,但不以任何方式限制本发明。另外,下述实施例中,如无特殊说明,所使用的实验方法均为常规方法,所用材料、试剂等均可从生物或化学试剂公司购买。
活性氧化铝为活性γ-Al2O3或ρ-Al2O3,符合GB/T 6166-1985标准,纯度大于98.50%;氧化锌为活性ZnO,符合GB/T 19589-2004标准,纯度大于98.50%;硝酸银为化学纯(CP),符合GB/T 670-2007标准。
实施例1
①将符合标准的活性三氧化二铝球磨至平均粒径0.8~1.0μm,得到氧化铝微粉;将符合标准的氧化锌球磨至平均粒径1~1.5μm,得到氧化锌微粉;将碳酸氢钠、硝酸银和羧甲基纤维素混合,球磨至平均粒径0.8~1.0μm,得到粘结剂微粉;
②将步骤①所制备的三份微粉在粉末分散机内混合均匀进行喷雾或挤压造粒,造粒后筛分出5.0~7.0mm的颗粒,然后在压力釜中经过130~150Mpa压力成型,再放入乙醇、二氧化碳和水蒸气的混合气体中熏蒸3~4小时进行钝化;
③将步骤②中所得的颗粒在隧道窑中进行活化和改性,温度350℃~450℃,升温速率 35℃~40℃/h,保温2.5~3.5小时,冷却后得到复合活性颗粒。
步骤②中的各个组分的质量为:氧化铝850g,氧化锌100g,硝酸银20g,碳酸氢钠20g,羧甲基纤维素10g。
步骤②中的混合钝化气体中乙醇、二氧化碳和水蒸气的体积比为:1:1:3。
步骤③中得到的复合活性载体颗粒的含水量不高于3.5%。
测得本次实例中复合活性载体球的比表面积为290m2/g,孔容为0.39ml/g,抗压强度>60N/ 颗。
实施例2
①将符合标准的活性三氧化二铝球磨至平均粒径0.8~1.0μm,得到氧化铝微粉;将符合标准的氧化锌球磨至平均粒径1~1.5μm,得到氧化锌微粉;将碳酸氢钠、硝酸银和羧甲基纤维素混合,球磨至平均粒径0.8~1.0μm,得到粘结剂微粉;
②将步骤1所制备的三份微粉在粉末分散机内混合均匀进行喷雾或挤压造粒,造粒后筛分出5.0~7.0mm的颗粒,然后在压力釜中经过130~150Mpa压力成型,再放入乙醇、二氧化碳和水蒸气中熏蒸3~4小时进行钝化;
③将步骤②中的颗粒在隧道窑中进行活化和改性,温度350℃~450℃,升温速率35℃~40℃/h,保温2.5~3.5小时,冷却后得到复合活性颗粒。
步骤②中的各个组分的质量为:氧化铝900g,氧化锌50g,硝酸银10g,碳酸氢钠25g,羧甲基纤维素15g。
步骤②中的混合钝化气体中乙醇、二氧化碳和水蒸气的体积比为:1:1.5:3.5。
步骤③中得到的复合活性载体颗粒的含水量不高于3.5%。
测得本次实例中复合活性载体球的比表面积为300m2/g,孔容为0.39ml/g,抗压强度>60N/ 颗。
实施例3
①将符合标准的活性三氧化二铝球磨至平均粒径0.8~1.0μm,得到氧化铝微粉;将符合标准的氧化锌球磨至平均粒径1~1.5μm,得到氧化锌微粉;将碳酸氢钠、硝酸银和羧甲基纤维素混合,球磨至平均粒径0.8~1.0μm,得到粘结剂微粉;
②将步骤①所制备的三份微粉在粉末分散机内混合均匀进行喷雾或挤压造粒,造粒后筛分出5.0~7.0mm的颗粒,然后在压力釜中经过130~150Mpa压力成型,再放入乙醇、二氧化碳和水蒸气中熏蒸3~4小时进行钝化;
③将步骤②中的颗粒在隧道窑中进行活化和改性,活化温度350℃~450℃,升温速率 35℃~40℃/h,保温2.5~3.5小时,冷却后得到复合活性颗粒。
步骤②中的各个组分的质量为:氧化铝800g,氧化锌150g,硝酸银10g,碳酸氢钠20g,羧甲基纤维素20g。
步骤②中的混合钝化气体中乙醇、二氧化碳和水蒸气的体积比为:1:2:4。
步骤③中得到的复合活性载体颗粒的含水量不高于3.5%。
测得本次实例中复合活性载体球的比表面积为280m2/g,孔容为0.38ml/g,抗压强度>60N/ 颗。
Claims (3)
1.一种表面改性的复合活性Al2O3-ZnO载体球形颗粒的制备方法,其特征在于,包括如下步骤:
①将活性三氧化二铝球磨至平均粒径0.8~1.0μm,得到氧化铝微粉;将氧化锌球磨至平均粒径1~1.5μm,得到氧化锌微粉;将碳酸氢钠、硝酸银和羧甲基纤维素混合,球磨至平均粒径0.8~1.0μm,得到粘结剂微粉;
②将步骤①所制备的三份微粉混合均匀,其中各个组分的质量比为:氧化铝800~900份,氧化锌50~100份,硝酸银20~40份,碳酸氢钠20~30份,羧甲基纤维素10~15份,经过造粒后筛分出5.0~7.0mm的颗粒,然后经过130~150Mpa压力成型,再放入乙醇、二氧化碳和水蒸气的混合气体中熏蒸3~4小时进行钝化;
③将步骤②中所得到的颗粒进行活化和改性,温度350℃~450℃,升温速率35℃~40℃/h,保温2.5~3.5小时,冷却后得到复合活性颗粒;
所述氧化锌为活性ZnO;
所述步骤②中的乙醇、二氧化碳和水蒸气体积比为1:1~2:3~4;
所述步骤③中得到的复合活性载体颗粒的含水量不高于3.5%。
2.根据权利要求1所述的表面改性的复合活性Al2O3-ZnO载体球形颗粒的制备方法,其特征在于,所述活性氧化铝为活性γ-Al2O3或ρ-Al2O3。
3.如权利要求1-2任意一项所述的方法制备的表面改性的复合活性Al2O3-ZnO载体球形颗粒。
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