CN104383968B - 一种氧化钛-海泡石-活性炭复合载体的制备方法 - Google Patents

一种氧化钛-海泡石-活性炭复合载体的制备方法 Download PDF

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CN104383968B
CN104383968B CN201410732810.6A CN201410732810A CN104383968B CN 104383968 B CN104383968 B CN 104383968B CN 201410732810 A CN201410732810 A CN 201410732810A CN 104383968 B CN104383968 B CN 104383968B
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CN104383968A (zh
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李程伟
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Tang Qun
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FUYANG HONGXIANG TECHNOLOGY SERVICES Co Ltd
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Abstract

本发明公开了一种包含活性炭、海泡石和氧化钛三种组分的复合载体,以PEG-2000作为复合催化剂的扩孔剂,经特定的改性、复合、扩孔工艺,制得具有特殊孔结构和高比表面积的载体材料。

Description

一种氧化钛-海泡石-活性炭复合载体的制备方法
技术领域
本发明涉及一种氧化钛-海泡石-活性炭复合载体的制备方法。
背景技术
负载型催化剂是现有技术中常规的催化剂结构类型,活性炭因其具有高比表面积而被用于催化剂载体材料,通过浸渍等负载方式使催化活性组分担载在活性炭表面上,从而形成负载型催化剂。海泡石由于具有特殊的结构而表现出优异的吸附性、流变性和催化性能等,在很多领域尤其是催化领域日益收到研究者的关注。二氧化钛作为催化剂载体是近年来发展起来的,常用的二氧化钛载体类型如P-25。
现有技术中活性炭、海泡石或二氧化钛大多是单独用作催化剂载体的,目前还没有将三种材料复合在一起,且具有特定孔结构和比表面积的载体的相关报道。
发明内容
本发明的目的在于,提供一种以活性炭、氧化钛和海泡石为主要组分的复合型催化剂载体,通过以下方法得以实现。
一种氧化钛-海泡石-活性炭复合载体的制备方法,包括如下步骤:
取100重量份的麦秸杆,经破碎,超微粉碎机粉碎和超微磨粉机细化后,获得粒度为325-500目的粉末颗粒;
取80重量份的海泡石,经粉碎机粉碎,筛分,将筛分后的粉末颗粒置于马弗炉中,以5℃/min的升温速率,升温至250℃,保温1小时,冷却至室温后,将焙烧后的粉末用HCl溶液充分浸泡2小时,而后过滤,洗涤,获得活化改性海泡石;
取钛酸丁酯50ml,在搅拌状态下向其中加入150ml乙醇,而后加入10mlHNO3和10ml蒸馏水,混合搅拌2小时,获得二氧化钛溶胶,将上述获得的活化改性海泡石加入该溶胶中,充分搅拌1小时,而后将该混合物置于马弗炉中500℃焙烧,获得氧化钛-海泡石;
将前述步骤获得的麦秸秆粉末颗粒和氧化钛-海泡石混合,向该混合物中加入100ml的PEG-2000,充分搅拌1小时,而后将混合物置于马弗炉中,以5℃/min的升温速率加热到700℃炭化,保温2小时,停止加热后,通入氮气保护,缓慢降温至室温,获得氧化钛-海泡石-活性炭复合载体。
所述麦秸秆粉碎后获得的粉末颗粒粒度为500目。
所述缓慢降温至室温的降温速率为5℃/min。
本发明的有益效果
本发明的复合载体中海泡石组分经过酸改性和高温改性两个步骤,使改性后的海泡石具有最大的比表面积。
本发明的复合载体包含活性炭、海泡石和氧化钛三种组分,以PEG-2000作为复合催化剂的扩孔剂,经特定的改性、复合、扩孔工艺,制得具有特殊孔结构和高比表面积的载体材料。
具体实施方式
下面结合实施例对本发明作进一步说明。
实施例1
取100重量份的麦秸杆,经破碎,超微粉碎机粉碎和超微磨粉机细化后,获得粒度为325目的粉末颗粒;
取80重量份的海泡石,经粉碎机粉碎,筛分,将筛分后的粉末颗粒置于马弗炉中,以5℃/min的升温速率,升温至250℃,保温1小时,冷却至室温后,将焙烧后的粉末用HCl溶液充分浸泡2小时,而后过滤,洗涤,获得活化改性海泡石;
取钛酸丁酯50ml,在搅拌状态下向其中加入150ml乙醇,而后加入10mlHNO3和10ml蒸馏水,混合搅拌2小时,获得二氧化钛溶胶,将前述步骤获得的活化改性海泡石加入该溶胶中,充分搅拌1小时,而后将该混合物置于马弗炉中500℃焙烧,获得氧化钛-海泡石;将前述步骤获得的麦秸秆粉末颗粒和氧化钛-海泡石混合,向该混合物中加入100ml的PEG-2000,充分搅拌1小时,而后将混合物置于马弗炉中,以5℃/min的升温速率加热到700℃炭化,保温2小时,停止加热后,通入氮气保护,缓慢降温至室温,获得氧化钛-海泡石-活性炭复合载体。
实施例2
取100重量份的麦秸杆,经破碎,超微粉碎机粉碎和超微磨粉机细化后,获得粒度为500目的粉末颗粒;
取80重量份的海泡石,经粉碎机粉碎,筛分,将筛分后的粉末颗粒置于马弗炉中,以5℃/min的升温速率,升温至250℃,保温1小时,冷却至室温后,将焙烧后的粉末用HCl溶液充分浸泡2小时,而后过滤,洗涤,获得活化改性海泡石;
取钛酸丁酯50ml,在搅拌状态下向其中加入150ml乙醇,而后加入10mlHNO3和10ml蒸馏水,混合搅拌2小时,获得二氧化钛溶胶,将前述步骤获得的活化改性海泡石加入该溶胶中,充分搅拌1小时,而后将该混合物置于马弗炉中500℃焙烧,获得氧化钛-海泡石;将前述步骤获得的麦秸秆粉末颗粒和氧化钛-海泡石混合,向该混合物中加入100ml的PEG-2000,充分搅拌1小时,而后将混合物置于马弗炉中,以5℃/min的升温速率加热到700℃炭化,保温2小时,停止加热后,通入氮气保护,缓慢降温至室温,获得氧化钛-海泡石-活性炭复合载体,

Claims (3)

1.一种氧化钛-海泡石-活性炭复合载体的制备方法,其特征在于包括如下步骤:
a)取100重量份的麦秸杆,经破碎,超微粉碎机粉碎和超微磨粉机细化后,获得粒度为325-500目的粉末颗粒;
b)取80重量份的海泡石,经粉碎机粉碎,筛分,将筛分后的粉末颗粒置于马弗炉中,以5℃/min的升温速率,升温至250℃,保温1小时,冷却至室温后,将焙烧后的粉末用HCl溶液充分浸泡2小时,而后过滤,洗涤,获得活化改性海泡石;
c)取钛酸丁酯50ml,在搅拌状态下向其中加入150ml乙醇,而后加入10mlHNO3和10ml蒸馏水,混合搅拌2小时,获得二氧化钛溶胶,将步骤b)获得的活化改性海泡石加入该溶胶中,充分搅拌1小时,而后将该混合物置于马弗炉中500℃焙烧,获得氧化钛-海泡石;
d)将步骤a)获得的粉末颗粒和步骤c)获得的氧化钛-海泡石混合,向该混合物中加入100ml的PEG-2000,充分搅拌1小时,而后将混合物置于马弗炉中,以5℃/min的升温速率加热到700℃炭化,保温2小时,停止加热后,通入氮气保护,缓慢降温至室温,获得氧化钛-海泡石-活性炭复合载体。
2.如权利要求1所述的制备方法,其特征在于:步骤a)的粉末颗粒粒度为500目。
3.如权利要求1所述的制备方法,其特征在于:步骤d)的降温速率为5℃/min。
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CN1245204A (zh) * 1998-08-18 2000-02-23 中国石油化工集团公司 含铂和钯双金属组分催化剂的制备方法
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CN102234212A (zh) * 2010-04-20 2011-11-09 中国石油化工股份有限公司 合成气直接转化为低碳烯烃的方法

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CN1245204A (zh) * 1998-08-18 2000-02-23 中国石油化工集团公司 含铂和钯双金属组分催化剂的制备方法
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