CN106215522B - 在滤料上原位生成纳米花状二氧化锰催化剂的方法 - Google Patents
在滤料上原位生成纳米花状二氧化锰催化剂的方法 Download PDFInfo
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- 239000000706 filtrate Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 27
- 239000003054 catalyst Substances 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000011572 manganese Substances 0.000 title claims abstract description 16
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 58
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000002131 composite material Substances 0.000 claims abstract description 24
- 238000001914 filtration Methods 0.000 claims abstract description 24
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 20
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 17
- 239000004734 Polyphenylene sulfide Substances 0.000 claims description 13
- 229920000069 polyphenylene sulfide Polymers 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000011010 flushing procedure Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 238000001467 acupuncture Methods 0.000 claims description 5
- 239000003463 adsorbent Substances 0.000 claims description 2
- OQVYMXCRDHDTTH-UHFFFAOYSA-N 4-(diethoxyphosphorylmethyl)-2-[4-(diethoxyphosphorylmethyl)pyridin-2-yl]pyridine Chemical compound CCOP(=O)(OCC)CC1=CC=NC(C=2N=CC=C(CP(=O)(OCC)OCC)C=2)=C1 OQVYMXCRDHDTTH-UHFFFAOYSA-N 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 claims 1
- 239000000835 fiber Substances 0.000 abstract description 6
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 2
- 238000009792 diffusion process Methods 0.000 abstract description 2
- 239000007800 oxidant agent Substances 0.000 abstract description 2
- 230000001590 oxidative effect Effects 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 9
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 7
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 description 6
- 230000035699 permeability Effects 0.000 description 6
- 229920006389 polyphenyl polymer Polymers 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 150000003568 thioethers Chemical class 0.000 description 5
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 4
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 4
- 239000000428 dust Substances 0.000 description 4
- 239000003546 flue gas Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000004506 ultrasonic cleaning Methods 0.000 description 4
- 229960003638 dopamine Drugs 0.000 description 3
- 229920001690 polydopamine Polymers 0.000 description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- RZYKUPXRYIOEME-UHFFFAOYSA-N CCCCCCCCCCCC[S] Chemical compound CCCCCCCCCCCC[S] RZYKUPXRYIOEME-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
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- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
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- 238000011173 large scale experimental method Methods 0.000 description 1
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- 231100000719 pollutant Toxicity 0.000 description 1
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- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
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Abstract
本发明公开了一种在滤料上原位生成纳米花状二氧化锰催化剂的方法，将滤料浸入含有十二烷基硫酸钠和硝酸的溶液中，首先利用十二烷基硫酸钠对滤料的表面进行改性，使其表面缠绕一层荷电层，它能够紧密地吸附酸性溶液中的H+；然后加入高锰酸钾作为氧化剂，使高锰酸钾与滤料表面的H+反应，在滤料表面原位生成纳米花状二氧化锰，从而制得具有脱硝功能的复合滤料。由于滤料纤维表面均匀地包覆了一层纳米花状二氧化锰，而该形貌的二氧化锰与普通的二氧化锰相比，具有更大的比表面积和更高的孔容，且更有利于反应气体的扩散，这就使得催化过滤滤料低温活性十分优异，160℃可达到97%以上的转化率。
Description
技术领域
本发明属于功能滤料技术领域，尤其涉及一种在滤料上原位生成纳米花状二氧化锰催化剂的方法。
背景技术
我国正处于经济高速发展阶段，能源需求量很大，尤其是对电力的需求更是有增无减。而我国以煤炭为主题的能源结构，决定了我国电力以火力发电为主，电厂大部分为燃煤电厂。燃煤电厂除了保障经济快速发展以外，会长生大量的污染物，如粉尘、二氧化硫及NOx有毒气体等。目前，工业上主要采用滤袋除尘器控制燃煤电站锅炉产生的大量粉尘和微量颗粒物，其核心是滤料。其中，聚苯硫醚滤料（PPS滤料）因其具有稳定的化学结构、耐酸碱腐蚀性、耐水解性及尺寸稳定性等优点，成为燃煤电厂滤袋上的首选材料。
但是，滤袋除尘器对工业尾气中的氮氧化物的排放，还没有有效的控制方法。因此，研究一种能够同时具备除尘和脱硝功能的复合功能滤料，已经成为众多研究人员关注的热点。公开号为CN 103949115 A的中国专利申请公开了一种在滤料上原位生成脱硝催化剂的方法，首先利用多巴胺的氧化自聚合反应在滤料表面均匀包覆一层聚多巴胺，然后利用聚多巴胺层与二价锰离子的螯合作用，以高锰酸钾作为氧化剂，在聚多巴胺包覆的滤料纤维表面原位生成脱硝催化剂，从而制得具有脱硝功能的复合滤料。然而其缺点在于利用多巴胺对滤料表面进行改性，均匀包覆的聚多巴胺层会影响滤料的透气性，从而影响其除尘功能；并且制备过程复杂。
而如果将脱硝催化剂直接附着在滤料纤维上，则存在催化剂负载不均匀，透气性差，低温活性较差，且催化剂与滤料纤维间的结合力很弱等缺点。因此，研究一种能够均匀且牢固地负载脱硝催化剂，并具有优异低温活性的复合滤料具有非常重要的意义。
发明内容
本发明的目的在于针对现有技术的不足，提供了一种在滤料上原位生成纳米花状二氧化锰催化剂的方法。本发明所得的滤料低温活性十分优异，160℃可达到97%以上的转化率，且该复合滤料的结合强度、透气性能及催化稳定性能均十分优异。
为实现上述发明目的，本发明采用如下技术方案：
一种在滤料上原位生成纳米花状二氧化锰催化剂的方法：将滤料浸入含有十二烷基硫酸钠和硝酸的溶液中，首先利用十二烷基硫酸钠对滤料的表面进行改性，使其表面缠绕一层荷电层，充分吸附溶液中的H+；然后往溶液中加入高锰酸钾，使高锰酸钾与滤料表面的H+反应，在滤料表面原位生成纳米花状二氧化锰，从而制得具有脱硝功能的复合滤料。
所述的含有十二烷基硫酸钠和硝酸的溶液，十二烷基硫酸钠的浓度为0.1–2g/L，硝酸的浓度为0.01~0.2M。
所述的滤料为聚苯硫醚针刺毡滤料。
所述的在滤料上原位生成纳米花状二氧化锰催化剂的方法，具体制备步骤为：
1）将滤料浸入含有十二烷基硫酸钠和硝酸的溶液中，超声分散1h，使十二烷基硫酸钠充分吸附在滤料表面；
2）将步骤1）的反应体系升温至60~80℃后，加入高锰酸钾，继续搅拌反应0.5–2 h，使高锰酸钾与滤料表面的H+反应原位生成纳米花状二氧化锰；
3）将步骤2）获得的滤料用去离子水和乙醇冲洗干净，放入110℃真空干燥箱中干燥6 h，得到具有脱硝功能的复合滤料。
步骤2）中反应体系中高锰酸钾的浓度为0.01~0.2M。
滤料上原位生成纳米花状二氧化锰催化剂，是由以下化学方程式制得：
4MnO4 –＋4H+ → 4MnO2＋3O2＋2H2O。
一种如上述方法制得的脱硝功能复合滤料可用于同时脱除PM2.5和NOx，并且具有优异的脱硝率，160℃可达到97%以上的转化率。
与现有技术相比，本发明的有益效果在于：
1、本发明利用十二烷基硫酸钠对滤料表面进行改性，并未对滤料表面造成影响，也不会影响其透气性（见图1）；由于滤料纤维表面均匀地包覆了一层纳米花状二氧化锰，而该形貌的二氧化锰与普通的二氧化锰相比，具有更大的比表面积和更高的孔容，且更有利于反应气体的扩散，这就使得催化过滤滤料低温活性十分优异，160℃可达到97%以上的转化率，且该复合滤料的结合强度、透气性能及催化稳定性能均十分优异；
2、本发明的制备方法简单，对环境友好；实验所用试剂廉价易得，且实验过程容易操作，反应过程只需2~3h，因此适合大规模实验生产。
附图说明
图1原始聚苯硫醚针刺毡滤料（A，B）与脱硝功能聚苯硫醚复合滤料（C，D）的SEM图；
图2原始聚苯硫醚针刺毡滤料（A）与脱硝功能聚苯硫醚复合滤料（B，C）的TEM图，及脱硝功能聚苯硫醚复合滤料的EDX图（D）；
图3脱硝功能聚苯硫醚复合滤料纤维表面元素成分分析；
图4脱硝功能聚苯硫醚复合滤料在160℃时的NO转化率图；
图5脱硝功能聚苯硫醚复合滤料的结合强度；
图6原始聚苯硫醚针刺毡滤料和脱硝功能聚苯硫醚复合滤料的透气性能。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅用以解释本发明，并不用于限定本发明。下面结合附图及具体实施例对本发明的应用原理作进一步描述。
实施例1
一种在滤料上原位生成纳米花状二氧化锰催化剂的方法，包括以下步骤：
a） 将0.042g十二烷基硫酸钠固体颗粒和微量浓硝酸加入到去离子水中搅拌溶解，配置成浓度为0.84g/L的十二烷基硫酸钠溶液，控制硝酸浓度为0.05M；
b）将直径为3.8cm的圆形聚苯硫醚滤料浸入步骤a）的悬浮溶液中，在超声波清洗器进行超声分散1h，使十二烷基硫酸钠充分吸附在滤料表面；
c）将反应体系升温至70℃，滴加高锰酸钾溶液，高锰酸钾浓度为0.05M，继续搅拌反应1.5 h，使高锰酸钾与滤料表面的H+反应原位生成纳米花状二氧化锰；
d）将步骤c）获得的滤料用去离子水和乙醇冲洗干净，放入110℃真空干燥箱中干燥6 h，得到具有脱硝功能的复合滤料。
该复合滤料的脱硝性能在自制管式SCR反应器中进行评价。测试条件：[NO]=[NH3]= 400 ppm，[O2]= 5%，N2 为平衡气，气体流速为700mL• min-1，温度设置为160℃，用英国KM940烟气分析仪测得脱硝效率为97%。
实施例2
一种在滤料上原位生成纳米花状二氧化锰催化剂的方法，包括以下步骤：
a） 将0.024g十二烷基硫酸钠固体颗粒和微量浓硝酸加入到去离子水中搅拌溶解，配置成浓度为0.48g/L的十二烷基硫酸钠溶液，控制硝酸浓度为0.1M；
b）将直径为3.8cm的圆形聚苯硫醚滤料浸入步骤a）的悬浮溶液中，在超声波清洗器进行超声分散1h，使十二烷基硫酸钠充分吸附在滤料表面；
c）将反应体系升温至80℃，滴加高锰酸钾溶液，高锰酸钾浓度为0.1M，继续搅拌反应2h，使高锰酸钾与滤料表面的H+反应原位生成纳米花状二氧化锰；
d）将步骤c）获得的滤料用去离子水和乙醇冲洗干净，放入110℃真空干燥箱中干燥6 h，得到具有脱硝功能的复合滤料。
该复合滤料的脱硝性能在自制管式SCR反应器中进行评价。测试条件：[NO]=[NH3]= 400 ppm, [O2]= 5%，N2 为平衡气，气体流速为700mL• min-1，温度设置为160℃，用英国KM940烟气分析仪测得脱硝效率为100%。
实施例3
一种在滤料上原位生成纳米花状二氧化锰催化剂的方法，包括以下步骤：
a）将0.042g十二烷基硫酸钠固体颗粒和微量浓硝酸加入到去离子水中搅拌溶解，配置成浓度为0.84g/L的十二烷基硫酸钠溶液，控制硝酸浓度为0.02M；
b）将直径为3.8cm的圆形聚苯硫醚滤料浸入步骤a）的悬浮溶液中，在超声波清洗器进行超声分散1h，使十二烷基硫酸钠充分吸附在滤料表面；
c）将反应体系升温至65℃，滴加高锰酸钾溶液，高锰酸钾浓度为0.02M，继续搅拌反应1.5h，使高锰酸钾与滤料表面的H+反应原位生成纳米花状二氧化锰；
d）将步骤c）获得的滤料用去离子水和乙醇冲洗干净，放入110℃真空干燥箱中干燥6 h，得到具有脱硝功能的复合滤料。
该复合滤料的脱硝性能在自制管式SCR反应器中进行评价。测试条件：[NO]=[NH3]= 400 ppm，[O2]= 5%，N2 为平衡气，气体流速为700mL• min-1，温度设置为160℃，用英国KM940烟气分析仪测得脱硝效率为95%。
实施例4
一种在滤料上原位生成纳米花状二氧化锰催化剂的方法，包括以下步骤：
a）将0.042g十二烷基硫酸钠固体颗粒和微量浓硝酸加入到去离子水中搅拌溶解，配置成浓度为0.84g/L的十二烷基硫酸钠溶液，控制硝酸浓度为0.05M；
b）将直径为3.8cm的圆形聚苯硫醚滤料浸入步骤a）的悬浮溶液中，在超声波清洗器进行超声分散1h，使十二烷基硫酸钠充分吸附在滤料表面；
c）将反应体系升温至65℃，滴加高锰酸钾溶液，高锰酸钾浓度为0.05M，继续搅拌反应2.5h，使高锰酸钾与滤料表面的H+反应原位生成纳米花状二氧化锰；
d）将步骤c）获得的滤料用去离子水和乙醇冲洗干净，放入110℃真空干燥箱中干燥6 h，得到具有脱硝功能的复合滤料。
该复合滤料的脱硝性能在自制管式SCR反应器中进行评价。测试条件：[NO]=[NH3]= 400 ppm，[O2]= 5%，N2 为平衡气，气体流速为700mL• min-1，温度设置为160℃，用英国KM940烟气分析仪测得脱硝效率为96%。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。
Claims (5)
1.一种在滤料上原位生成纳米花状二氧化锰催化剂的方法，其特征在于：将滤料浸入含有十二烷基硫酸钠和硝酸的溶液中，首先利用十二烷基硫酸钠对滤料的表面进行改性，使其表面缠绕一层荷电层，充分吸附溶液中的H+；然后往溶液中加入高锰酸钾，使高锰酸钾与滤料表面的H+反应，在滤料表面原位生成纳米花状二氧化锰，从而制得具有脱硝功能的复合滤料；具体制备步骤为：
1）将滤料浸入含有十二烷基硫酸钠和硝酸的溶液中，超声分散1h，使十二烷基硫酸钠充分吸附在滤料表面；
2）将步骤1）的反应体系升温至60~80℃后，加入高锰酸钾，继续搅拌反应0.5–2 h，使高锰酸钾与滤料表面的H+反应原位生成纳米花状二氧化锰；
3） 将步骤2）获得的滤料用去离子水和乙醇冲洗干净，放入110℃真空干燥箱中干燥6h，得到具有脱硝功能的复合滤料。
2.根据权利要求1所述的在滤料上原位生成纳米花状二氧化锰催化剂的方法，其特征在于：所述的含有十二烷基硫酸钠和硝酸的溶液，十二烷基硫酸钠的浓度为0.1–2g/L，硝酸的浓度为0.01~0.2M。
3.根据权利要求1所述的在滤料上原位生成纳米花状二氧化锰催化剂的方法，其特征在于：所述的滤料为聚苯硫醚针刺毡滤料。
4.根据权利要求1所述的在滤料上原位生成纳米花状二氧化锰催化剂的方法，其特征在于：步骤2）中反应体系中高锰酸钾的浓度为0.01~0.2M。
5.根据权利要求1-4任一项所述的方法制得的滤料，其特征在于：可用于同时脱除PM2.5和NOx。
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| WO2018045672A1 (zh) | 2018-03-15 |
| US20200179906A1 (en) | 2020-06-11 |
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