CN106881145A - 一种酸碱后处理介孔丝光沸石脱硝催化剂的制备方法 - Google Patents
一种酸碱后处理介孔丝光沸石脱硝催化剂的制备方法 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 17
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 title claims abstract description 9
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000002253 acid Substances 0.000 title claims abstract description 8
- 229910052680 mordenite Inorganic materials 0.000 title claims abstract description 6
- 239000000969 carrier Substances 0.000 claims abstract description 7
- 239000013078 crystal Substances 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 239000002808 molecular sieve Substances 0.000 claims description 7
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000009740 moulding (composite fabrication) Methods 0.000 claims description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 4
- 238000002425 crystallisation Methods 0.000 claims description 4
- 230000008025 crystallization Effects 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- 206010013786 Dry skin Diseases 0.000 claims description 2
- 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 claims description 2
- 235000019270 ammonium chloride Nutrition 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 239000003643 water by type Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims 1
- 238000012805 post-processing Methods 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 238000013459 approach Methods 0.000 abstract 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 238000001802 infusion Methods 0.000 abstract 1
- 239000013067 intermediate product Substances 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 abstract 1
- 238000012546 transfer Methods 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/18—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the mordenite type
- B01J29/20—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the mordenite type containing iron group metals, noble metals or copper
- B01J29/24—Iron group metals or copper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/54—Nitrogen compounds
- B01D53/56—Nitrogen oxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
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- B01J35/613—
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/26—Mordenite type
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
- B01D2258/0283—Flue gases
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/10—After treatment, characterised by the effect to be obtained
- B01J2229/18—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/30—After treatment, characterised by the means used
- B01J2229/37—Acid treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/30—After treatment, characterised by the means used
- B01J2229/38—Base treatment
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01P2006/14—Pore volume
Abstract
一种酸碱后处理介孔丝光沸石脱硝催化剂的制备方法，主要涉及针对MOR的酸碱后处理方法。本发明使用晶种水热合成MOR载体，通过一定浓度的酸碱处理以达到牺牲一部分微孔从而产生一部分介孔，得到含有介孔的MOR(MOR‑M)。通过交换浸渍法将一定量的Cu(NO3)2负载到MOR载体上，经在一定温度下干燥、焙烧，制成Cu‑MOR。本发明制备的催化剂由于打破了传统MOR孔道单一的现状，加速了中间产物（盐类）在低温下孔道中的传质，从而改善了催化剂在低温下的催化性能。
Description
技术领域
本发明属于环境催化技术领域，涉及一种简单酸碱处理得到多级孔Cu-MOR脱硝催化剂的制备方法。
背景技术
NOx导致光化学烟雾、酸雨、臭氧层的破坏等问题。而其来源基本上是人类的生产、生活的不洁废气的排放。如化石燃料的燃烧过程。而这一过程主要是柴油机的尾气的排放过程。控制柴油机尾气中NOx的排放量已成为国内外尾气催化净化领域得最突出难点之一。氨选择性催化还原（NH3-SCR）去除NOx (脱硝)技术因其高效率、经济性等优点已成为目前适用于移动源主要的脱硝技术。
发明内容
本发明的目的是提供一种酸碱后处理介孔丝光沸石（Cu-MOR-M）催化剂的制备方法。通过后处理的方式以牺牲部分微孔为代价来得到介孔Cu-MOR-M，将其运用到氨选择性催化还原（NH3-SCR）去除NOx，具有制备方法简单，提高了低温NOx的选择性催化还原活性。
本发明所述的一种酸碱后处理介孔丝光沸石催化剂的制备方法，其特征在于包括以下步骤。
分别取18.0g-22.0g质量分数30%SiO2水溶液、24g-28g水、1.5g-1.9g偏铝酸钠、1.1g-1.4g硼酸、0.03gMOR晶种、1.09g氢氧化钠混溶，在室温下搅拌三小时，然后转入反应釜中在180℃晶化90h-100h，所得晶化物过滤、洗涤、干燥、550℃焙烧6h，所得产品即为Na-MOR分子筛。取10g-15 g的氯化铵、4 g Na-MOR、200 ml去离子水在烧杯里混合，待氯化铵完全溶解转入至烧瓶，在80℃搅拌24 h，随后过滤、洗涤、干燥、550℃焙烧6h，所得产品即为H-MOR分子筛。用6M/L的HNO3以1g载体对应42ml的量在80℃处理1小时，过滤、洗涤至pH=7然后80℃干燥12h。用0.1M/L的TMAOH在65℃分别处理20min-60min，过滤、洗涤至pH=7然后80℃干燥12h。得到MOR-M。取0.038gCu(NO3)2前驱体和5ml去离子水配成溶液，加入H-MOR分子筛在室温下搅拌20h-26h，80℃-90℃水浴蒸干，80℃干燥12h，在空气氛中550℃焙烧6h得到Cu-MOR催化剂。
本发明催化剂的优点：（1）催化剂制备方法简单易于操作。（2）采用晶种法合成MOR克服了模板剂的高昂的价格的缺点。（3）通过简单的后处理就可以得到多级孔MOR。
附图说明
图1为本发明制备1%Cu-MOR催化剂的X射线衍射谱图。
图2为本发明制备1%Cu-MOR催化剂的氮气吸脱附谱图。
图3为本发明制备1%Cu-MOR催化剂的孔容孔径分布谱图。
图4为本发明制备1%Cu-MOR催化剂的氮氧化物的选择性催化还原活性测试。
具体实施方式
为更清楚的说明本发明，列举以下实施例，但其对本发明的范围无任何限制。
多级孔MOR载体的制备。
用6M/L的HNO3以1g载体对应42ml的量在80℃处理1小时，过滤、洗涤至PH=7然后80℃干燥12h。用0.1M/L的TMAOH在65℃处理20min、40min，过滤、洗涤至PH=7然后80℃干燥12h。得到MOR-x（x=20、40、60）。
实施例1。
将0.038gCu(NO3)2和5ml去离子水配成溶液，加入H-MOR分子筛在室温下搅拌24h，80℃水浴蒸干，80℃干燥12h，在空气氛中550℃焙烧6h得到Cu-MOR催化剂。
实施例2。
将0.038gCu(NO3)2和5ml去离子水配成溶液，加入H-MOR-20分子筛在室温下搅拌24h，80℃水浴蒸干，80℃干燥12h，在空气氛中550℃焙烧6h得到Cu-MOR-20催化剂。
实施例3。
将0.038gCu(NO3)2和5ml去离子水配成溶液，加入H-MOR-40分子筛在室温下搅拌24h，80℃水浴蒸干，80℃干燥12h，在空气氛中550℃焙烧6h得到Cu-MOR-40催化剂。
表1为本发明制备1%Cu-MOR催化剂载体的氮气吸脱附信息。
表2为本发明制备1%Cu-MOR催化剂的元素分析结果。
Claims (1)
1.一种酸碱后处理介孔丝光沸石脱硝催化剂的制备方法，其特征在于包括以下步骤：
分别取18.0g-22.0g质量分数30%SiO2水溶液、24g-28g水、1.5g-1.9g偏铝酸钠、1.1g-1.4g硼酸、0.03gMOR晶种、1.09g氢氧化钠混溶，在室温下搅拌三小时，然后转入反应釜中在180℃晶化90h-100h，所得晶化物过滤、洗涤、干燥、550℃焙烧6h，所得产品即为Na-MOR分子筛；取10g-15 g的氯化铵、4 g Na-MOR、200 ml去离子水在烧杯里混合，待氯化铵完全溶解转入至烧瓶，在80℃搅拌24 h，随后过滤、洗涤、干燥、550℃焙烧6h，所得产品即为H-MOR分子筛；用6M/L的HNO3以1g载体对应42ml的量在80℃处理1小时，过滤、洗涤至pH=7然后80℃干燥12h；用0.1M/L的TMAOH在65℃分别处理20min-60min，过滤、洗涤至pH=7然后80℃干燥12h；得到MOR-M；取0.038gCu(NO3)2前驱体和5ml去离子水配成溶液，加入H-MOR分子筛在室温下搅拌20h-26h，80℃-90℃水浴蒸干，80℃干燥12h，在空气氛中550℃焙烧6h。
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| CN111589466A (zh) * | 2020-06-02 | 2020-08-28 | 陕西延长石油（集团）有限责任公司 | 一种铜丝光沸石催化剂的合成及应用 |
| CN115069285A (zh) * | 2022-06-14 | 2022-09-20 | 太原理工大学 | 一种甲烷直接制甲醇的光热催化剂及其制备方法和应用 |
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| CN115069285A (zh) * | 2022-06-14 | 2022-09-20 | 太原理工大学 | 一种甲烷直接制甲醇的光热催化剂及其制备方法和应用 |
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