CN107486237A - 一种甲酰氯茶梗基生物炭吸附催化剂及其制备方法 - Google Patents
一种甲酰氯茶梗基生物炭吸附催化剂及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种甲酰氯茶梗基生物炭吸附催化剂及其制备方法,属于催化剂技术领域。本发明将茶梗粉碎至粒径为40~200目得到茶梗粉;在温度为600~800℃、氮气氛围条件下,将茶梗粉焙烧1~3h得到碳粉;将碳粉加入到硝酸溶液中混合均匀,在温度为70~90℃条件下反应1~3h,过滤、洗涤、干燥即得生物炭;将生物炭与氯化亚砜、二甲基甲酰胺混合均匀,然后在温度为20~30℃、超声条件下浸渍反应1~3h,采用无水四氢呋喃洗涤,真空过滤后即得甲酰氯茶梗基生物炭吸附催化剂。本发明的吸附催化剂有良好的脱硝活性以及较高的汞吸附效果,净化烟气的同时也可以废物再利用,价格低廉,经济可行性高。
Description
技术领域
本发明涉及一种甲酰氯茶梗基生物炭吸附催化剂及其制备方法,属于催化剂技术领域。
背景技术
火电厂燃煤烟气是大气中氮氧化物和气态单质汞的主要排放源,氮氧化物会导致光化学烟雾、酸雨、臭氧空洞、温室效应等一系列环境问题。而单质汞由于其难溶于水、剧毒性、挥发性、生物累积性等特点,引起了世界各国和国际组织的广泛关注。我国新制订的火电厂大气污染物标准中单质汞的排放限制规定为30μg/m3。目前为止,国内外较成熟的联合脱除技术是选择性催化还原技术(selective catalytic reduction)(SCR),在脱除氮氧化物的同时,部分汞单质也会被氧化成离子态汞,进而被湿法脱硫装置吸收。当前较为主流的催化剂是V2O5-WO3/TiO2,其工作范围在300℃-400℃,然而在催化剂的制备过程中,会产生钒基副产物,对环境造成不利影响。除此之外,烟气中含有的SO2、飞灰会对催化剂造成失活。当前可行的方法是在脱硫装置的下游注入一种可以在低温条件下同时脱硝除汞的催化剂。
发明申请CN104148095A公开了一种脱硝脱汞催化剂及其制备方法,它是以TiO2或Al2O3为载体,活性物质为K2TaF7和NiO,并添加了助剂、粘结剂和辅助成分。具有较高的汞吸附和氧化能力,良好的脱硝活性,而且稳定性强,耐磨性高。
发明申请CN103480371A公开了一种脱硝脱汞催化剂及其制备方法,它是将含钌物质、钛基脱硝催化剂与双氧水混合接触,将解除后的混合物干燥或不干燥后进行焙烧,制备出的催化剂相比于单一功能的钛基催化剂脱硝效率明显增高,单质汞的氧化率也很高。
目前催化剂虽然都具有较高的脱硝除汞效率,但是由于原料成本,制作工艺成本的限制,不适合大量用于工业,因此寻求吸附催化能力强,且价格低廉的吸附催化剂非常重要。
发明内容
本发明针对现有技术的不足,提供一种甲酰氯茶梗基生物炭吸附催化剂及其制备方法,选用废弃茶梗作为碳源,既可以废物利用,又节省了成本;本发明将生物炭原料与硝酸溶液反应,会促进诸如羧基等含氧官能团的生成,此时的反应产物继续在二甲基甲酰胺(DMF)存在的条件下与过量的SOCl2反应,进而生成甲酰氯生物炭,甲酰氯生物炭的碳氧双键会促进NO的转化,而碳氯键会促进单质汞的氧化,并且同时存在的NO和Hg0的协同作用和汞单质的吸附作用也会大大增强此吸附催化剂的效果。
一种甲酰氯茶梗基生物炭吸附催化剂的制备方法,具体步骤如下:
(1)将茶梗粉碎至粒径为40~200目得到茶梗粉;
(2)在温度为600~800℃、氮气氛围条件下,将步骤(1)所得茶梗粉焙烧1~3h得到碳粉;
(3)将步骤(2)所得碳粉加入到硝酸溶液中混合均匀,在温度为70~90℃条件下反应1~3h,过滤、洗涤、干燥即得生物炭;
(4)将步骤(3)所得生物炭与氯化亚砜(SOCl2)、二甲基甲酰胺混合均匀,然后在温度为20~30℃、超声条件下浸渍反应1~3h,采用无水四氢呋喃洗涤,真空过滤即得甲酰氯茶梗基生物炭吸附催化剂;
所述步骤(3)中硝酸溶液的浓度为4~8mol/L,碳粉体积与硝酸溶液体积比为1:(1~3);
所述步骤(4)中生物炭与氯化亚砜(SOCl2)、二甲基甲酰胺的固液比g:mL:mL为1:(10~30): (10~30);
本发明的另一目的是,提供所述甲酰氯茶梗基生物炭吸附催化剂的制备方法所制备的甲酰氯茶梗基生物炭吸附催化剂。
本发明的有益效果:
(1)本发明方法采用硝酸处理原料生物炭,会增加表面含氧官能团,减少活性炭的灰分含量,降低活性炭的pH值,更有利于未来浸渍后脱硝反应的进行,从而有利于吸附质分子的扩散,汞单质吸附能力得以提高;
(2)本发明方法采用与有机溶剂反应制备吸附剂,用量少,有效地节约了能源,减少了污染控制的成本,可行性高;
(3)本发明方法采用的载体是茶梗基生物炭,属于废物再利用,经济可行性高;
(4)本发明中制备的改性吸附催化剂适用于燃煤电厂和其他工业废气中的脱硝除汞。
附图说明
图1为实施例1甲酰氯茶梗基生物炭吸附催化剂的扫描电镜图;
图2为实施例1甲酰氯茶梗基生物炭吸附催化剂的红外分析图。
具体实施方式
下面结合具体实施例对本发明作进一步详细说明,但本发明的保护范围并不限于所述内容。
实施例1:一种甲酰氯茶梗基生物炭吸附催化剂的制备方法,具体步骤如下:
(1)将茶梗粉碎至粒径为40目得到茶梗粉;
(2)在温度为600℃、氮气氛围条件下,将步骤(1)所得茶梗粉焙烧1h得到碳粉;
(3)将步骤(2)所得碳粉加入到硝酸溶液中混合均匀,在温度为70℃条件下反应1h,过滤,用去离子水洗涤至中性,在温度为95℃条件下干燥8h即得生物炭,其中硝酸溶液的浓度为4mol/L,碳粉体积与硝酸溶液体积比为1:1;
(4)将步骤(3)所得生物炭与SOCl2、二甲基甲酰胺混合均匀,然后在温度为20℃、超声条件下浸渍反应1h,采用无水四氢呋喃(DMF)洗涤,真空过滤即得甲酰氯茶梗基生物炭吸附催化剂,其中生物炭与SOCl2、二甲基甲酰胺的固液比g:mL:mL为1:10:10;
本实施例制备的甲酰氯茶梗基生物炭吸附催化剂的扫面电镜(SEM)图如图1所示,放大倍数10K倍;从图1可知,制备的成品生物炭具有丰富发达的孔结构,对于活性点位的增多,基团的负载都有很好的促进作用,直接影响着联合脱除反应的进行。
本实施例制备的甲酰氯茶梗基生物炭吸附催化剂的红外分析图如图2所示,首先参考苯甲酰氯的标准图谱可知,苯甲酰氯C=O键的伸缩振动在1730cm-1附近,C-Cl键的伸缩振动在874cm-1附近,但本发明中连接有甲酰氯基团的是碳材料,没有形成环状,不同材料间的结构不同,因此甲酰氯中的C原子的化学键的力常数不同,导致振动频率不同;本实施例的甲酰氯茶梗基生物炭吸附催化剂的红外分析图如图2所示,由图2可知,C=O键的伸缩振动在1632cm-1附近,振动频率降低,而C-Cl键的伸缩振动频率降低到430 cm-1-509 cm-1附近,另外,C-Cl键的透过率较低,可能与该结构的吸收系数、厚度和含量有关。
本实施例制备的甲酰氯茶梗基生物炭吸附催化剂的吸附性能测试:配气总流量800mL/min,NO浓度500ppm,氨气浓度600ppm,氧气含量5%,载气为氮气,混气罐温度200℃,空速96000/h;进行联合脱除实验时,水浴锅温度维持在70℃,汞蒸气载气N2流量控制在100mL/min,入口汞空白浓度为47.8μg/m3,实验温度条件100~300℃;
本实施例制备的甲酰氯茶梗基生物炭吸附催化剂的吸附性能如表1所示,在温度为100℃时,NO转化率为54.8%,Hg0去除率为70.2%;在温度为200℃时,NO转化率为69.3%,Hg0去除率为93.3%;在温度为300℃时,NO转化率为82.1%,Hg0去除率为34.2%。
实施例2:一种甲酰氯茶梗基生物炭吸附催化剂的制备方法,具体步骤如下:
(1)将茶梗粉碎至粒径为100目得到茶梗粉;
(2)在温度为700℃、氮气氛围条件下,将步骤(1)所得茶梗粉焙烧2h得到碳粉;
(3)将步骤(2)所得碳粉加入到硝酸溶液中混合均匀,在温度为80℃条件下反应2h,过滤,用去离子水洗涤至中性,在温度为100℃条件下干燥9h即得生物炭,其中硝酸溶液的浓度为6mol/L,碳粉体积与硝酸溶液体积比为1:2;
(4)将步骤(3)所得生物炭与SOCl2、二甲基甲酰胺混合均匀,然后在温度为25℃、超声条件下浸渍反应2h,采用无水四氢呋喃(DMF)洗涤,真空过滤即得甲酰氯茶梗基生物炭吸附催化剂,其中生物炭与SOCl2、二甲基甲酰胺的固液比g:mL:mL为1:20:20;
本实施例制备的甲酰氯茶梗基生物炭吸附催化剂的吸附性能测试方法同实施例1;
本实施例制备的甲酰氯茶梗基生物炭吸附催化剂的吸附性能如表1所示,在温度为100℃时,NO转化率为52.1%,Hg0去除率为68.2%;在温度为200℃时,NO转化率为68.8%,Hg0去除率为92.5%;在温度为300℃时,NO转化率为83.0%,Hg0去除率为31.4%。
实施例3:一种甲酰氯茶梗基生物炭吸附催化剂的制备方法,具体步骤如下:
(1)将茶梗粉碎至粒径为200目得到茶梗粉;
(2)在温度为800℃、氮气氛围条件下,将步骤(1)所得茶梗粉焙烧3h得到碳粉;
(3)将步骤(2)所得碳粉加入到硝酸溶液中混合均匀,在温度为90℃条件下反应3h,过滤,用去离子水洗涤至中性,在温度为105℃条件下干燥10h即得生物炭,其中硝酸溶液的浓度为8mol/L,碳粉体积与硝酸溶液体积比为1:3;
(4)将步骤(3)所得生物炭与SOCl2、二甲基甲酰胺混合均匀,然后在温度为30℃、超声条件下浸渍反应3h,采用无水四氢呋喃(DMF)洗涤,真空过滤即得甲酰氯茶梗基生物炭吸附催化剂,其中生物炭与SOCl2、二甲基甲酰胺的固液比g:mL:mL为1:30:30;
本实施例制备的甲酰氯茶梗基生物炭吸附催化剂的吸附性能测试方法同实施例1;
表 1
本实施例制备的甲酰氯茶梗基生物炭吸附催化剂的吸附性能如表1所示,在温度为100℃时,NO转化率为52.6%,Hg0去除率为70.4%;在温度为200℃时,NO转化率为70.5%,Hg0去除率为93.1%;在温度为300℃时,NO转化率为86.9%,Hg0去除率为34.2%。
Claims (4)
1.一种甲酰氯茶梗基生物炭吸附催化剂的制备方法,其特征在于,具体步骤如下:
(1)将茶梗粉碎至粒径为40~200目得到茶梗粉;
(2)在温度为600~800℃、氮气氛围条件下,将步骤(1)所得茶梗粉焙烧1~3h得到碳粉;
(3)将步骤(2)所得碳粉加入到硝酸溶液中混合均匀,在温度为70~90℃条件下反应1~3h,过滤、洗涤、干燥即得生物炭;
(4)将步骤(3)所得生物炭与氯化亚砜、二甲基甲酰胺混合均匀,然后在温度为20~30℃、超声条件下浸渍反应1~3h,采用无水四氢呋喃洗涤,真空过滤即得甲酰氯茶梗基生物炭吸附催化剂。
2.根据权利要求1所述甲酰氯茶梗基生物炭吸附催化剂的制备方法,其特征在于:步骤(3)中硝酸溶液的浓度为4~8mol/L,碳粉体积与硝酸溶液体积比为1:(1~3)。
3.根据权利要求1所述甲酰氯茶梗基生物炭吸附催化剂的制备方法,其特征在于:步骤(4)中生物炭与氯化亚砜、二甲基甲酰胺的固液比g:mL:mL为1:(10~30): (10~30)。
4.权利要求1~3所述甲酰氯茶梗基生物炭吸附催化剂的制备方法所制备的甲酰氯茶梗基生物炭吸附催化剂。
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