CN106902766B - 一种用于scr系统的固载还原剂及其制备方法 - Google Patents

一种用于scr系统的固载还原剂及其制备方法 Download PDF

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CN106902766B
CN106902766B CN201710085624.1A CN201710085624A CN106902766B CN 106902766 B CN106902766 B CN 106902766B CN 201710085624 A CN201710085624 A CN 201710085624A CN 106902766 B CN106902766 B CN 106902766B
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严军表
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Jiangsu kelansu Environmental Protection Technology Co., Ltd
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Abstract

本发明公开了一种用于SCR系统的固载还原剂及其制备方法，该还原剂包括无机盐60‑95％、无机氧化物1‑20％、粘结剂0.5‑15.0％、分散剂0.2‑10％及添加剂0.1‑10％；制法为将无机盐、无机氧化物、粘结剂及添加剂混合，加水搅拌升温至50～60℃，加入分散剂，制得粘稠物，保温分散1.5～4h，干燥，即可。优点为该固载还原剂的充氨次数高、耐高温及对热、机械的稳定性强，且氨的吸附率高达35～55％，大大提高了SCR系统的使用周期、降低了后期使用过程中的维系成本和使用成本；同时其制法简便，可操作性强，环保无污染。

Description

一种用于SCR系统的固载还原剂及其制备方法
技术领域
本发明属于还原剂领域，尤其涉及一种用于SCR系统的固载还原剂及其制备方法。
背景技术
选择性催化还原技术—SCR是针对柴油车尾气排放中NOx的一项处理工艺，即在催化剂的作用下，喷入还原剂氨或尿素，把尾气中的NOx还原成N2和H2O。催化剂有贵金属和非贵金属两类。该技术也被广泛应用于柴油机尾气后处理，通过优化喷油和燃烧过程，尽量在机内控制微粒PM的产生，而后在机外处理富氧条件下形成氮氧化物，即使用车用尿素(车用尿素在一定温度下分解生成氨)对氮氧化物(NOx)进行选择性催化还原，从而达到既节能、又减排的目的，该项技术是欧洲主流技术路线，欧洲长途载货车和大型客车几乎全部采用该技术。
目前传统用于SCR系统的催化还原剂--车用尿素溶液(AdBlue)是用不含其他任何添加物的高纯尿素和纯水一起配制的溶液，该溶液中尿素含量为32.5％(质量分数)。国内外重型柴油机厂家大多数采用了SCR(选择性催化还原)技术来满足欧IV、欧Ⅴ机动车排放标准的要求。选择SCR技术的的车辆必须添加尿素溶液作为催化还原剂，使车辆达标排放。
AdBlue用于配有SCR(车用选择性催化还原尾气后处理)系统的轿车、卡车、客车和重型非道路使用柴油发动机车辆，是SCR技术中必须要用到的消耗品，与SCR催化剂一起将柴油发动机排放的有害氮氧化物转换成无害的水蒸气和氮。SCR系统的主要组成部分包括催化剂，AdBlue注入装置，AdBlue容器和AdBlue剂量控制器。几乎所有欧洲、美国和亚洲，包括中国的重型汽车制造商也为车辆配备选择性催化还原系统并配以AdBlue工作液，以达到新的氮氧化物排放标准(如欧四、欧五)。AdBlue和SCR技术共同作用下，能优化发动机性能和燃料消耗，减少柴油消耗可高达6％，显著降低成本。AdBlue的平均消耗量是一般柴油消耗量的5％，约为高速公路驾驶每100公里消耗1.5升。AdBlue只可使用于配置SCR系统的引擎组合，因为它既不是燃料，也不是燃料添加剂。AdBlue执行符合ISO22241，DIN70070和CEFIC规章内的标准，以确保SCR系统有效运行。AdBlue对环境没有危害，并分类为最低风险的可运输液体。
目前，由于车用尿素溶液(AdBlue)在使用过程中出现了大量的故障，导致目前符合国四排放法规车辆大面积后处理系统维修，主要由于行驶过程中尾气系统的温度以及尿素溶液喷射系统的问题导致SCR催化系统的结垢堵塞，并且在500-1000公里后就出现大面积的亮红灯—喷嘴结晶引起的喷射问题。目前没有任何办法能够彻底解决现有采用车用尿素溶液产品引起的问题。
发明内容
发明目的：本发明的第一目的是提供一种具有高吸附率、高充氮次数且耐高温的用于SCR系统的固载还原剂；本发明的第二目的是提供该固载还原剂的制备方法。
技术方案：本发明用于SCR系统的固载还原剂，按重量百分比计包括如下原料：无机盐60-95％、无机氧化物1-20％、粘结剂0.5-15.0％、分散剂0.2-10％及添加剂0.1-10％。
优选的，无机盐80-90％、无机氧化物5-10％、高分子粘结剂1-7％、分散剂0.25-5％及添加剂1.0-6.0％。
本发明通过添加无机盐、无机氧化物、粘结剂、分散剂及添加剂，各组分间相容、相辅相成，从而使制备的固载还原剂不仅具有储氨功能，且能够改善固体储氨材料的导热性能及机械强度，使产品成型稳定，防止散裂。优选的，无机盐可包括氯化锶、氯化钙或氯化镁，进一步优选可为氯化钙，氯化钙吸附氨，理论有效氨含量高；无机氧化物可包括氧化铝、膨润土、改性高岭土或硅酸钠；粘结剂可以但不限于聚乙烯醇或PVP k90；分散剂可以但不限于司盘80或乳化剂hypmer B246；添加剂可包括膨胀石墨、分子筛或稀土金属。
在同等体积的有效氨下，本发明的固载还原剂与Adblue相比，首先，其能够在仅140℃时便开始释放氨，因此装备了SSCR系统的车辆开始控制NOx排放的时间要远早于装备SCR系统的车辆，且在冷启动条件下，固载还原剂中氨的激活速度也快于SCR系统，在发动机温度持续低下的情况下，也能够在城市作业的车辆上持续不断地工作，气体不会因为低温环境导致结晶堆积和堵塞，降低了维护成本，避免了低温条件下AdBlue溶液会凝固的问题；其次，由于储存密度大，装载该固载还原剂的储氨罐的更换频率显著低于补充AdBlue溶液的频率，从而大大缩短了维护的时间；此外，由于选择性催化还原系统的使用效率大幅提高，该固载还原剂分解NOx的能力显著增强，且不需要通过尿素水解得到氨气，进而降低了温室气体二氧化碳的排放量。
本发明制备用于SCR系统的固载还原剂的方法，包括如下步骤按重量百分比将无机盐、无机氧化物、粘结剂及添加剂混合，加水搅拌升温至50～60℃，加入分散剂，制得粘稠物，保温分散1.5～4h，干燥，即可。
进一步说，本发明的固载还原剂的制备方法中，所述的干燥是在120～150℃条件下干燥6～12h。
有益效果：与现有技术相比，本发明的显著优点为：该固载还原剂的充氨次数高、耐高温及对热、机械的稳定性强，且氨的吸附率高达35～55％，尤其适合用于柴油发动机SCR系统中的催化还原剂，大大提高了SCR系统的使用周期、降低了后期使用过程中的维系成本和使用成本，有效提高了SCR系统运行的可靠性和稳定性，且杜绝了使用Adblue产品引起的SCR系统催化剂结垢堵塞、尿素溶液喷嘴的结晶和尿素泵的电气问题；同时，其制法简便，可操作性强，环保无污染。
具体实施方式
下面结合实施例对本发明的技术方案作进一步说明。
实施例1
本发明的固载还原剂原料及配比如表1所示。
表1实施例1的原料及配比
组分 氯化锶 HX分子筛 膨润土 聚乙烯醇 司盘80
加入量/克 900 10 40 30 20
配比/％ 90 1 4 3 2
本实施中采用的原料均可从市场上购买得到。
制备方法：首先将氯化锶、HX分子筛、膨润土及聚乙烯醇加入到不锈钢调合釜中，加入100g蒸馏水，水的加入量能够使各组分混合均匀即可，开始升温搅拌2000转；待温度升至50℃后，加入司盘80，保温30min后观察体系外观，搅拌均匀后得到粘稠物，保温分散4h后，将该粘稠物放置于120℃恒温烘箱内加热干燥12h，待水分完全蒸发后，便制成本发明的固载还原剂。
实施例2
本实施例的固载还原剂原料及配比如表2所示。
表2原料及配比
组分 氯化锶 膨胀石墨 膨润土 PVP K90 HypmerB246
加入量/克 800 40 80 30 50
配比/％ 80 4 8 3 5
制备方法：制备方法：首先将氯化锶、膨胀石墨、膨润土及PVP K90加入到不锈钢调合釜中，加入85g蒸馏水，开始升温搅拌4000转；待温度升至60℃后，加入HypmerB246，开始保温30min后观察体系外观，搅拌均匀后得到粘稠物，保温分散2.5h后，将该粘稠物放置130℃恒温烘箱内加热干燥8h，待水分完全蒸发后，便制成固载还原剂。
实施例3
本实施的固载还原剂原料及配比如表3所示。
表3原料及配比
组分 氯化钙 HX分子筛 改性高岭土 聚乙烯醇 HypmerB246
加入量/克 870 20 60 20 30
配比/％ 87 2 6 2 3
制备方法：首先将氯化钙、HX分子筛、改性高岭土及聚乙烯醇加入到不锈钢调合釜中，加入95g蒸馏水，开始升温搅拌2000转；待温度升至55℃后，加入HypmerB246，开始保温30min后观察体系外观，搅拌均匀后得到粘稠物，保温分散4h后，将该粘稠物放置130℃恒温烘箱内加热干燥10h，待水分完全蒸发后，便制成固载还原剂。
实施例4
本实施例的固载还原剂原料及配比如表4所示。
表4原料及配比
Figure BDA0001227302500000051
制备方法：首先将氯化钙、稀土金属、膨润土及PVP K90加入到不锈钢调合釜中，加入105g蒸馏水，开始升温搅拌5000转；待温度升至50℃后，加入HypmerB246，开始保温30min后观察体系外观，搅拌均匀后得到粘稠物，保温分散2h后，将该粘稠物放置130℃恒温烘箱内加热干燥12h，待水分完全蒸发后，便制成固载还原剂。
实施例5
本实施例的固载还原剂原料及配比如表5所示。
表5原料及配比
组分 氯化锶 稀土金属 膨润土 PVP K90 HypmerB246
加入量/克 750 60 90 50 50
占比/％ 75 6 9 5 5
制备方法：首先将氯化锶、稀土金属、膨润土及PVP K90加入到不锈钢调合釜中，加入90g蒸馏水，开始升温搅拌6000转；待温度升至60℃后，加入HypmerB246，开始保温30min后观察体系外观，搅拌均匀后得到粘稠物，保温分散1.5h后，将该粘稠物放置140℃恒温烘箱内加热干燥8h，待水分完全蒸发后，便制成固载还原剂。
将实施例1-5制得的固载还原剂进行性能检测，获得的技术指标如表6所示。
表6实施例1-5测试结果
Figure BDA0001227302500000052
Figure BDA0001227302500000061
通过表6可知，本发明制备的固载还原剂不仅耐高温及对热、机械的稳定性强，且氨的吸附率高达35～48％，大大提高了SCR系统的使用周期、降低了后期使用过程中的维系成本和使用成本，有效提高了SCR系统运行的可靠性和稳定性，且杜绝了使用Adblue产品引起的SCR系统催化剂结垢堵塞、尿素溶液喷嘴的结晶和尿素泵的电气问题。
实施例6
组分的配比与实施例5相同，不同之处在于无机盐为氯化镁，无机氧化物为氧化铝。制备方法为：首先将氯化镁、稀土金属、氧化铝及PVP K90加入到不锈钢调合釜中，加入90g蒸馏水，开始升温搅拌6000转；待温度升至60℃后，加入HypmerB246，开始保温30min后观察体系外观，搅拌均匀后得到粘稠物，保温分散1.5h后，将该粘稠物放置150℃恒温烘箱内加热干燥6h，待水分完全蒸发后，便制成固载还原剂。
该实施例中的无机氧化物可替换为硅酸钠。
实施例7
基本步骤与实施例5相同，不同之处在于组分的配比，具体如表7所示：
表7原料及配比
组分 氯化锶/％ 稀土金属/％ 膨润土/％ PVP K90/％ HypmerB246/％
1 95 3.3 1 0.5 0.2
2 60 10 10 10 10
3 60 0.1 20 15 4.9
4 90 6.75 5 1 0.25
5 80 1 7 7 5
6 80 6 10 10 2
对比例
基本步骤与实施例6相同，不同之处在于组分配比，如表8所示。
表8原料及配比
组号 氯化锶/％ 稀土金属/％ 膨润土/％ PVP K90/％ HypmerB246/％
1 99 0.08 0.5 0.25 0.17
2 34 12 25 17 12
3 55 12 1 20 12
将本实施例的1-6组及对比例1-3制备的固载还原剂进行性能检测，获得的技术指标如表9所示。
表9实施例7及对比例测试结果
Figure BDA0001227302500000071
通过表9对比可知，在本发明组分配比范围内制备的固载还原剂，氨吸附率大40％左右，且分解温度低，这主要是因为在组分配比范围内制备的固载还原剂具有较好的导热性，孔隙率高，氨的吸附量高。在确保固载还原剂导热性及吸附量后，本发明范围内制备的固载还原剂具有较好的机械性能，确保固载还原剂的安装使用。

Claims (4)

1.一种用于SCR系统的固载还原剂，其特征在于按重量百分比计包括如下原料：无机盐60-95%、无机氧化物1-20%、粘结剂0.5-15.0%、分散剂0.2-10%及添加剂0.1-10%；所述无机盐为氯化锶、氯化钙或氯化镁，无机氧化物为氧化铝、膨润土或硅酸钠，粘结剂为聚乙烯醇或PVP k90，分散剂为司盘80或乳化剂hypmer B246，添加剂为膨胀石墨、分子筛或稀土金属；
该固载还原剂的制备方法包括如下步骤：按重量百分比将无机盐、无机氧化物、粘结剂及添加剂混合，加水搅拌升温至50~60℃，加入分散剂，制得粘稠物，保温分散1.5~4h，干燥，即可。
2.根据权利要求1所述的用于SCR系统的固载还原剂，其特征在于：所述无机盐80-90%、无机氧化物5-10%、粘结剂1-7%、分散剂0.25-5%及添加剂1.0-6.0%。
3.根据权利要求1所述的用于SCR系统的固载还原剂，其特征在于：所述无机盐为氯化钙。
4.根据权利要求1所述的用于SCR系统的固载还原剂，其特征在于：所述干燥是在120~150℃条件下干燥6~12h。
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