CN115006989A - 一种同时脱除甲硫醇和乙硫醇的方法 - Google Patents
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Abstract
本发明公开一种同时脱除甲硫醇和乙硫醇的方法，该方法以ZSM5分子筛为载体，通过等体积浸渍法，将ZSM5分子筛置于六水合硝酸铈溶液中，六水合硝酸铈与ZSM5分子筛的质量比为20:100~50:100，搅拌混匀后，25~35℃水浴超声，然后干燥焙烧，压片粉碎过筛，制得制得耦合酸碱位点的催化剂；将含有甲硫醇和乙硫醇的混合物通入装有耦合酸碱位点的催化剂的反应器中，空速为5000~14000h‑1，在400~450℃反应，实现甲硫醇和乙硫醇的同时脱除。本发明的方法可在常压下有效分解多种浓度，多种比例，多种空速的甲乙混合硫醇，并可持续分解高空速、低浓度的甲乙混合硫醇150h无失活迹象。
Description
技术领域
本发明涉及一种同时催化分解甲硫醇和乙硫醇的方法，属于催化分解恶臭气体技术领域。
背景技术
石油化工行业中含硫化合物严重制约着液化石油气的高值资源化利用，也是导致我国日益严峻酸雨和雾霾等大气污染的主要原因之一。石油在开采、炼化及运输过程中产生的主要污染物——硫醇，已被列为我国挥发性有机物（VOCs）排放控制的重点污染物，常见的硫醇有甲硫醇（CH3SH）和乙硫醇（C2H5SH）。由于其高毒高腐蚀性及嗅阈值低的特点，中华人民共和国国家标准《恶臭污染物排放标准》（GB-14554-93）中对其排放有着严格的限定要求。因此，研究人员一直致力于探索一种高效和安全的技术来去除有机硫醇。
过去几十年里研究者们一直致力于研究单一体系下催化脱除CH3SH的方法，并且也取得了瞩目的成果。在实际工业环境中，CH3SH一般与C2H5SH共存，然而，目前还没有关于多组分硫醇催化分解的报道。此前对多组分挥发性有机化合物（VOC）的研究已经表明，去除多组分混合污染物和单组分污染物之间存在区别。在催化分解去除单组分VOCs的过程中，污染物的脱除效率只与催化剂有关，而混合污染物中各目标污染物之间的相互作用可以改变单个化合物的去除效率，有的是相互促进，有的是单方向抑制，有的是双向抑制。因此甲硫醇与乙硫醇混合后，二者催化脱除的性能如何变化目前仍有待研究。
发明内容
本发明的目的在于提供一种同时脱除甲硫醇和乙硫醇的方法，该方法以ZSM5分子筛为载体，通过等体积浸渍法，将ZSM5分子筛置于六水合硝酸铈溶液中，六水合硝酸铈与ZSM5分子筛的质量比为20:100~50:100，搅拌混匀后，25~35℃水浴超声10~20min，然后在120℃下干燥6h，500~600℃下焙烧5h，压片粉碎过筛，制得制得耦合酸碱位点的催化剂；将含有甲硫醇和乙硫醇的混合物通入装有耦合酸碱位点的催化剂的反应器中，空速为5000~14000h-1，在400~450℃反应，实现甲硫醇和乙硫醇的同时脱除。
本发明催化剂在各种浓度、各种比例的甲乙混合硫醇体系中均表现出良好的催化性能，可连续分解低浓度高空速的甲乙混合硫醇150h无失活迹象。
与现有技术相比，本发明具有以下有益效果：
（1）填补了目前催化分解混合硫醇的空白。目前还未有混合硫醇催化分解的报道，但实际工业条件下，甲乙硫醇共存，两种硫醇的混合对催化性能的影响，目前还未可知，本发明探究了甲乙硫醇混合后二者的相互作用对分解性能的影响；
（2）所制备的耦合酸碱位点的催化剂对各浓度的混合硫醇均表现出良好的催化活性，反应气浓度最高时仍可在450℃被完全分解；
（3）实际工业条件下，硫醇的浓度较低，为此本发明模拟了工业条件下，所制备的耦合酸碱位点的催化剂催化分解低浓度高空速下的混合硫醇的稳定性，结果表明该催化剂稳定性优异，反应150h仍无失活迹象；
（4）所制备的耦合酸碱位点的催化剂再生性能优异，多次再生后仍可恢复到最初的催化性能。
附图说明
图1为实施例1甲乙硫醇转化率随反应气空速的变化图；
图2为实施例2甲乙硫醇转化率随CH3SH和C2H5SH配比变化图；
图3为实施例3~6 不同浓度甲乙混合硫醇体系中甲硫醇转化率随温度变化图；
图4为实施例3~6 不同浓度甲乙混合硫醇体系中乙硫醇转化率随温度变化图；
图5为实施例7 低浓度高空速甲乙混合硫醇转化率随时间变化图。
具体实施方式
下面通过实施例对本发明作进一步详细说明，但本发明保护范围不局限于所述内容，实施例中方法如无特殊说明均为常规方法，试剂如无特殊说明均为常规试剂或按常规方法配制的试剂；
实施例1
将六水合硝酸铈0.9261g溶于水中，采用等体积浸渍法，将市售的ZSM5分子筛2g置于六水合硝酸铈溶液中，搅拌5min后，30℃水浴超声15min，继而在120℃烘箱中干燥6h，550℃焙烧5h，压片粉碎过筛，制得40-60目的耦合酸碱位点的催化剂；
取0.2g催化剂装入管式炉反应器中，通入含体积浓度2500ppm CH3SH、C2H5SH2500ppm的混合反应气，反应体系压力为常压，反应温度为450℃，在进料总空速分别为6400、9500、13000 h-1的条件下，进行甲乙混合硫醇分解，结果见图1，结果显示空速为6400h-1时，转化率最高，甲硫醇和乙硫醇的转化率均达100%。
实施例2
将六水合硝酸铈0.9261g溶于水中，采用等体积浸渍法，将市售的ZSM5分子筛2g置于六水合硝酸铈溶液中，搅拌5min后，30℃水浴超声15min，继而在120℃烘箱中干燥6h，550℃焙烧5h，压片粉碎过筛，制得40-60目的耦合酸碱位点的催化剂；
取0.2g催化剂装入管式炉反应器中，分别按CH3SH:C2H5SH体积比=1:2、1:1、2:1的比例通入CH3SH/C2H5SH混合反应气（5000ppm），反应体系压力为常压，反应温度为350℃，在进料总空速为6400h-1的条件下，进行甲乙混合硫醇分解，结果见图2，结果表明CH3SH与C2H5SH间存在相互抑制，增大CH3SH比例则CH3SH转化率增加，C2H5SH转化率降低，增大C2H5SH比例则C2H5SH转化率增高，CH3SH转化率降低。
实施例3
将六水合硝酸铈0.9261g溶于水中，采用等体积浸渍法，将市售的ZSM5分子筛2g置于六水合硝酸铈溶液中，搅拌5min后，30℃水浴超声15min，继而在120℃烘箱中干燥6h，550℃焙烧5h，压片粉碎过筛，制得40-60目的耦合酸碱位点的催化剂；
取0.2g催化剂装入管式炉反应器中，通入含体积浓度2500ppm CH3SH、C2H5SH2500ppm的混合反应气，反应体系压力为常压，反应温度分别为300、350、400、450℃，在进料总空速为6400h-1的条件下，进行甲乙混合硫醇分解，结果见图3、4，结果表明300℃时，CH3SH转化率达33%，C2H5SH转化率达83%；450℃时，CH3SH和C2H5SH可被完全分解。
实施例4
将六水合硝酸铈0.9261g溶于水中，采用等体积浸渍法，将市售的ZSM5分子筛2g置于六水合硝酸铈溶液中，搅拌5min后，30℃水浴超声15min，继而在120℃烘箱中干燥6h，550℃焙烧5h，压片粉碎过筛，制得40-60目的耦合酸碱位点的催化剂；
取0.2g催化剂装入管式炉反应器中，通入含体积浓度1000ppm CH3SH、C2H5SH1000ppm的混合反应气，反应体系压力为常压，反应温度分别为300、350、400、450℃，在进料总空速为6400h-1的条件下，进行甲乙混合硫醇分解，结果见图3、4，结果表明300℃时，CH3SH转化率达47%，C2H5SH转化率达87%；450℃时，CH3SH和C2H5SH可被完全分解。
实施例5
将六水合硝酸铈0.9261g溶于水中，采用等体积浸渍法，将市售的ZSM5分子筛2g置于六水合硝酸铈溶液中，搅拌5min后，30℃水浴超声15min，继而在120℃烘箱中干燥6h，550℃焙烧5h，压片粉碎过筛，制得40-60目的耦合酸碱位点的催化剂；
取0.2g催化剂装入管式炉反应器中，通入含体积浓度500ppm CH3SH、C2H5SH500ppm的混合反应气，反应体系压力为常压，反应温度分别为300、350、400、450℃，在进料总空速为6400 h-1的条件下，进行甲乙混合硫醇分解，结果见图3、4，结果表明300℃时，CH3SH转化率达52%，C2H5SH转化率达90%；400℃时，CH3SH和C2H5SH可被完全分解。
实施例6
将六水合硝酸铈0.9261g溶于水中，采用等体积浸渍法，将市售的ZSM5分子筛2g置于六水合硝酸铈溶液中，搅拌5min后，30℃水浴超声15min，继而在120℃烘箱中干燥6h，550℃焙烧5h，压片粉碎过筛，制得40-60目的耦合酸碱位点的催化剂；
取0.2g催化剂装入管式炉反应器中，通入含体积浓度250ppm CH3SH、C2H5SH250ppm的混合反应气，反应体系压力为常压，反应温度分别为300、350、400、450℃，在进料总空速为6400 h-1的条件下，进行甲乙混合硫醇分解，结果见图3和图4，结果表明300℃时，CH3SH和C2H5SH即可被完全分解。
实施例7
将六水合硝酸铈0.9261g溶于水中，采用等体积浸渍法，将市售的ZSM5分子筛2g置于六水合硝酸铈溶液中，搅拌5min后，30℃水浴超声15min，继而在120℃烘箱中干燥6h，550℃焙烧5h，压片粉碎过筛，制得40-60目的耦合酸碱位点的催化剂；
取0.2g催化剂装入管式炉反应器中，通入含体积浓度250ppm CH3SH、C2H5SH250ppm的混合反应气，反应体系压力为常压，反应温度为450℃，进料总空速为13000 h-1的条件下，进行甲乙混合硫醇分解，结果见图5，结果表明反应150h后，CH3SH和C2H5SH均无失活迹象，仍可被完全分解。
Claims (1)
1.一种同时脱除甲硫醇和乙硫醇的方法，其特征在于，步骤如下：
（1）以ZSM5分子筛为载体，通过等体积浸渍法，将ZSM5分子筛置于六水合硝酸铈溶液中，六水合硝酸铈与ZSM5分子筛的质量比为20:100~50:100，搅拌混匀后，25~35℃水浴超声10~20min，然后在120℃下干燥6h，500~600℃下焙烧5h，压片粉碎过筛，制得40-60目的耦合酸碱位点的催化剂；
（2）将含有甲硫醇和乙硫醇的混合物通入装有耦合酸碱位点的催化剂的反应器中，空速为5000~14000h-1，在常压、300~450℃下反应，实现甲硫醇和乙硫醇的同时脱除。
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| CN104276921A (zh) * | 2013-07-09 | 2015-01-14 | 中国石油化工股份有限公司 | 芳烃脱硫脱氮的方法 |
| CN105233866A (zh) * | 2015-10-20 | 2016-01-13 | 昆明理工大学 | 一种分解甲硫醇气体的re/hzsm-5催化剂的再生方法 |
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| CN104276921A (zh) * | 2013-07-09 | 2015-01-14 | 中国石油化工股份有限公司 | 芳烃脱硫脱氮的方法 |
| CN105233866A (zh) * | 2015-10-20 | 2016-01-13 | 昆明理工大学 | 一种分解甲硫醇气体的re/hzsm-5催化剂的再生方法 |
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