CN111841624A - 一种高效amox整体式催化剂的制备方法 - Google Patents
一种高效amox整体式催化剂的制备方法 Download PDFInfo
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- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 abstract description 4
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- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 16
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- 239000000243 solution Substances 0.000 description 14
- 238000006722 reduction reaction Methods 0.000 description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical group N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 5
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Abstract
本发明涉及一种应用于汽车尾气后处理的AMOX催化剂及其制备方法,通过采用分段涂覆、Ce‑分子筛‑SiO2改性Al2O3、糖分散贵金属、自制高分散Si‑Al复合胶、较高温水浴、调节pH值的方法进行催化剂制备,显著提高了AMOX催化剂的NH3氧化能力和低NOx催化性能,同时具有非常优异的N2选择性,并且自制的Al‑Si复合胶作为粘接剂,可以显著提高了堇青石整体式催化剂的附着力。该制备方法首先将CeO2、SiO2、Al2O3和分子筛按照比例混合,分散砂磨后,通过糖分散贵金属,缓慢滴入贵金属,涂覆后制备底层氧化层。随后通过离子交换,制备Si‑Al复合胶,按比例混合后,涂覆制备上层SCR层。本发明合提供一种最优的Fe‑β分子筛离子交换技术,同时制备出具有较高附着力,具有优异催化剂催化性能的Fe‑SCR堇青石整体式催化剂。本发明提供一种高效AMOX整体式催化剂的制备方法,同时制备出具有非常高效的NH3捕集氧化能力,且可以满足欧六排放法规要求,具有非常优异性能的AMOX催化剂。
Description
技术领域
本发明属于工业催化领域,特别是涉及一种高效AMOX整体式催化剂的制备方法。
背景技术
柴油机SCR尾气后处理,是针对在废气中的一氧化碳(CO)、碳氢化合物(HC)及颗粒(PM)等排放物得到有效控制并达到法规的要求,最后对发动机排出尾气中含量较高的氮氧化物(NOX)再利用专门的车载后处理***进行处理的一种尾气处理策略,其中NOx的净化技术是用到选择性催化还原法。选择性催化还原法(Selective Catalytic Reduction,SCR)的原理是在催化剂作用下,还原剂NH3在200-600℃下有选择的将NO和NO2还原成N2,而几乎不发生NH3与O2的氧化反应。目前常见的SCR催化剂有V-W-Ti、Cu-SCR、Fe-SCR,还原剂为NH3。随着排放法规的日趋严苛,NOx排放值越来越低,且允许NH3泄露值也严格起来。由于国五标准要求SCR催化剂更高的转化效率,同时也就需要更高的尿素喷射量,从而容易造成多余NH3逸出,所以需要在后端加装氨捕集催化剂,即AMOX催化剂。
目前汽车尾气后处理行业,针对NH3泄露问题,常见两种方案,第一种是在SCR后端添加一块1~2英寸长的AMOX催化剂,这种催化剂不仅易导致NOx排放值得超标,而且还额外增加封装体积。另一种是底层涂覆贵金属涂层,上层涂覆SCR层,这种方案的优点在于可以有效节省空间,但低的NH3捕集效率、存在NOx超标、且涂覆工艺复杂等问题,仍限值其大规模应用。因此,如何保证同时降低NH3的泄露值和NOx的排放,且具有简单的制备工艺,在当下国六马上实施的时期,具有非常重大的战略意义。
本发明的目的是提供一种高效AMOX整体式催化剂的制备方法,同时制备出具有非常高效的NH3捕集氧化能力,且可以满足欧六排放法规要求,具有非常优异性能的AMOX催化剂。
发明内容
本发明针对AMOX催化剂的NH3捕集效率差、存在NOx超标,且涂覆工艺复杂等问题,提供了一种不仅具有提高NH3捕集效率和NOx处理效率,且涂覆工艺简单,且具有很高催化剂附着力的催化剂制备方法。
一种高效AMOX整体式催化剂的制备方法,催化剂分为两层涂覆,具体包括以下步骤:
(1)底层NH3氧化层制备
a,按固体含量为30-45%,分别计算粉体用量,Al2O3粉末占粉体总质量的40-80%,SiO2粉末占粉体总质量的0-50%,CeO2粉末占粉体总质量的10-50%,HBEA分子筛占粉体总质量的5-45%;
b,称取Al2O3粉末40-60g和SiO2粉末0-30g加入去100g离子水中,搅拌20-60min;
c,称取CeO2粉末10-50g和HBEA 5-15g加入步骤b搅拌好的浆液中,继续搅拌20-60min;
d,将步骤c搅拌均匀的浆液加入砂磨机中,砂磨5-60min,磨至颗粒度为5-15μm;
e,取出浆液,调节固含量至25-45%;
f,配制1-5%麦芽糖溶液约5-50g,缓慢滴加Pt溶液,Pt含量0.5-8g/ft3;
g,采用浸渍法涂覆底层氧化层,控制涂覆量30-100g/L;
h,120℃烘干20-120min,400-650℃焙烧20-180min后,得到底层NH3氧化层;
(2)上层SCR还原层制备
a,将Cu源同去离子水混合,并搅拌均匀,水浴加热至20-60℃,待Cu源完全溶解,然后按Cu/分子筛重量比为0.1-0.6加入分子筛,继续升温至70-90℃,均匀搅拌0.5-2h;
b,离子交换完成后,将交换液冷却后,通过抽滤机中进行抽滤,洗涤,待抽出液呈无色后,将滤饼放入100-120℃烘箱干燥;
c,干燥后,以2-8℃/min的速度升温至400-600℃,保温1-3h,随炉冷却待用;
d,将纳米Al2O3粉30-50g在去离子水中充分搅拌,然后缓慢加入浓度为1-5%HNO3溶液,待纳米Al2O3粉胶溶后,水浴升温至40-60℃,保温60min,得到纳米Al2O3胶体;
e,将纳米SiO2粉末30-50g缓慢加入纳米Al2O3胶体中,匀速搅拌,并调节pH值至2.5-4,水浴加热至65-90℃,保温2-5h,陈化1-2d后得到Si-Al复合胶作为粘接剂备用;
f,将分子筛粉碎后,加入去离子水,调节固含量25-45%,搅拌20-60min;
g,向上述分子筛溶液中添加1-8%的Si-Al复合胶,搅拌20-60min,调节粘度至500-2000cp;
h,采用定量涂覆法制备AMOX催化剂,控制涂覆量30-200g/L;
i,110-160℃快速烘干后,升温至300-600℃焙烧1-3h后,得到AMOX催化剂。
在上述步骤中,CeO2可以替换为Ce(NO3)2、Ce(CH3COO)2中的至少一种;在底层Al2O3和SiO2添加中,可以是两种不同的粉体添加,也可以是通过改性后制备的复合粉体,也可以是通过其他元素进行的改性复合粉体或单一粉体;在底层添加的CeO2,可以是单一粉体,也可以是通过改性后制备的复合粉体;在底层添加的贵金属分散剂麦芽糖,可以替换成果糖、葡聚糖、蔗糖、葡萄糖等糖类,也可以是乙二醇、丙醇、聚乙烯醇等醇类,也可以是乙酸乙酯、乙酸丁酯等脂类。
上层SCR涂层离子交换投加比例为Cu/分子筛为0.1-0.6,比例可以是摩尔比也可以换算成质量比,水浴温度为70-85℃;所使用的粘接剂为Al-Si复合胶,Al/Si的质量比为1-9,pH值为2.5-6,水浴温度为60-90℃;对上层SCR层Si-Al复合胶制备安定剂,不仅限于HNO3,也可以是乙酸、盐酸等酸溶液,也可以是通过NH3水等碱溶液调节的碱性Si-Al复合胶;对上层SCR层Si-Al复合胶,也可以是通过分散剂制备的公平衡状态Si-Al复合胶,也可以是通过Si胶和Al胶按一定比例直接复合的混合胶体;Cu盐可以是乙酸铜、硝酸铜等铜盐,也可以纳米Cu离子、纳米Cu颗粒,也可以是Cu氧化物,Cu单质等。
对NH3氧化层原料进行降低粒度的方法,不仅限于砂磨机,也可以是球磨机、水磨机等。
对Al2O3、CeO2、SiO2和去离子水等原料添加不限于步骤(1)中顺序;对Cu源、分子筛、纳米Al2O3及SiO2等原料添加不限于步骤(2)中顺序。
分子筛可以是CHA型,也可以是BEA、MFI、FAU、CFI等分子筛。
在Cu-分子筛离子交换结束后所得分子筛也可以用压滤、离心、喷雾、洗涤等方法。
AMOX整体式催化剂涂覆方法不限于定量涂覆法,也可以是浸渍提拉法,浸渍专机,抽涂专机,吹扫专机等涂覆方法。
在溶胶水浴加热采用程序升温过程,升温速率范围为0.3~10℃/min,水浴温度为70-85℃
本发明解决了Fe-β分子筛离子交换量低,堇青石整体式催化剂附着力差等问题,提供了一种可以提高离子交换量的交换参数,并提供了一种可以有效提高整体式催化剂附着力的方法,所得Fe-SCR堇青石整体式催化剂附着力高,同时可以显著提高催化剂低温催化性能。
附图说明
附图1实施例1所得AMOX催化剂NH3氧化能力对比。
附图2实施例1所得AMOX催化剂NOx生产量对比。
附图3实施例1所得AMOX催化剂N2选择性对比。
具体实施方式
实施例1
(1)底层NH3氧化层制备
a,按固体含量为45%,分别计算粉体用量,Al2O3粉末占60%,SiO2粉末占15%,CeO2粉末占10%,HBEA分子筛占15%;
b,称取Al2O3粉末60g和SiO2粉末15g加入去122g离子水中,搅拌30min;
c,称取CeO2粉末10g和HBEA 15g加入搅拌好的浆液中,继续搅拌30min;
d,将搅拌均匀的浆液加入砂磨机中,砂磨60min,磨至颗粒度为8μm;
e,取出浆液,调节固含量至40%;
f,配制1-5%麦芽糖溶液约5g,缓慢滴加Pt溶液,Pt含量2g/ft3;
g,采用浸渍法涂覆底层氧化层,控制涂覆量50g/L;
h,120℃烘干120min,500℃焙烧60min。
(2)上层SCR还原层制备
a,将Cu(NO3)2同去离子水混合,并搅拌均匀,水浴加热至40℃,待Cu源完全溶解,然后按Cu/分子筛比为0.5加入H-SSZ13,继续升温至80℃,均匀搅拌2h;
b,离子交换完成后,将交换液冷却后,通过抽滤机中进行抽滤,洗涤,待抽出液呈无色后放入120℃烘箱干燥。
c,干燥后,以5℃/min的速度升温至500℃,保温1h,随炉冷却待用。
d,将纳米Al2O3粉30g在去离子水中充分搅拌,然后缓慢加入浓度为1%HNO3溶液,纳米Al2O3粉胶溶后,水浴升温至60℃,保温60min。
e,将纳米SiO2粉末30g缓慢加入纳米Al2O3胶体中,匀速搅拌,并调节pH值至2.5,水浴加热至90℃,保温2h,陈化1d后作为粘接剂备用。
f,将分子筛粉碎后,加入去离子水,调节固含量35%,搅拌20min。
g,添加3%的Si-Al复合胶,搅拌60min,调节粘度至1500cp。
h,采用定量涂覆法制备AMOX催化剂,控制涂覆量100g/L;
i,110℃快速烘干后,升温至400℃焙烧3h。
对比案例1
(1)底层NH3氧化层制备
a,按固体含量为35%,分别计算粉体用量,Al2O3粉末占90%,CeO2粉体占10%。
b,称取Al2O3粉末90g和CeO2粉末10g加入去160g离子水中,搅拌30min;
c,将搅拌均匀的浆液加入砂磨机中,砂磨30min,磨至颗粒度为8μm;
d,取出浆液,调节固含量至32%;
e,缓慢滴加Pt溶液,Pt含量2g/ft3,调节pH=5;
f,采用浸渍法涂覆底层氧化层,控制涂覆量50g/L;
g,120℃烘干120min,500℃焙烧60min。
(2)上层SCR还原层制备
a,将Cu(NO3)2同去离子水混合,并搅拌均匀,加入乙醇溶液,水浴加热至40℃,待Cu源完全溶解,均匀搅拌30min;
b,然后按Cu/CHA比为0.5加入H-SSZ13,继续搅拌60min。
c,将浆液通入砂磨机中,砂磨20min,磨至颗粒度为8μm;
d,取出浆液,调节固含量至32%;
e,添加3%的Al胶,搅拌60min,调节粘度至1000cp。
f,采用定量涂覆法制备AMOX催化剂,控制涂覆量100g/L;
g,110℃快速烘干后,升温至400℃焙烧3h。
附图1为对比例方法制备AMOX催化剂和本发明制备的AMOX催化剂NH3氧化能力的对比,可以本发明制备的AMOX催化剂,具有非常优异的NH3氧化能力,比常规催化剂低温起燃温度,高出20℃左右。
附图2为对比例方法制备AMOX催化剂和本发明制备的AMOX催化剂NOx生成能力的对比,可以本发明制备的AMOX催化剂,具有非常低的NOx生成量,满足日趋严格的排放法规要求。
附图3为对比例方法制备AMOX催化剂和本发明制备的AMOX催化剂N2选择性的对比,可以明显看出,本发明制备的催化剂,具有非常优异的N2选择性,副产物N2O生成量最低。
实施例2
(1)底层NH3氧化层制备
a,按固体含量为35%,分别计算粉体用量,Al2O3粉末占70%,SiO2粉末占10%,CeO2粉末占10%,HBEA分子筛占10%;
b,称取Al2O3粉末70g和SiO2粉末10g加入去185g离子水中,搅拌20min;
c,称取CeO2粉末10g和HBEA 10g加入搅拌好的浆液中,继续搅拌20min;
d,将搅拌均匀的浆液加入砂磨机中,砂磨5min,磨至颗粒度为12μm;
e,取出浆液,调节固含量至30%;
f,配制2%麦芽糖约10g,缓慢滴加Pt溶液,Pt含量3g/ft3;
g,采用浸渍法涂覆底层氧化层,控制涂覆量30g/L;
h,120℃烘干80min,450℃焙烧80min。
(2)上层SCR还原层制备
a,将Cu(CH3COO)2同去离子水混合,并搅拌均匀,水浴加热至40℃,待Cu源完全溶解,然后按Cu/CHA比为0.2加入H-SSZ13,继续升温至70℃,均匀搅拌0.5h;
b,离子交换完成后,将交换液冷却后,通过抽滤机中进行抽滤,洗涤,待抽出液呈无色后放入100℃烘箱干燥。
c,干燥后,以8℃/min的速度升温至600℃,保温1h,随炉冷却待用。
d,将纳米Al2O3粉50g在去离子水中充分搅拌,然后缓慢加入浓度为2%HNO3,纳米Al2O3粉胶溶后,水浴升温至40℃,保温60min。
e,将纳米SiO2粉末40g缓慢加入纳米Al2O3胶体中,匀速搅拌,并调节pH值至4,水浴加热至65℃,保温5h,陈化2d后作为粘接剂备用。
f,将分子筛粉碎后,加入去离子水,调节固含量45%,搅拌60min。
g,添加2%的Si-Al复合胶,搅拌50min,调节粘度至1000cp。
h,采用定量涂覆法制备AMOX催化剂,控制涂覆量30g/L;
i,110℃快速烘干后,升温至300℃焙烧1h。
实施例3
(1)底层NH3氧化层制备
a,按固体含量为38%,分别计算粉体用量,Al2O3粉末占80%,SiO2粉末占5%,CeO2粉末占10%,HBEA分子筛占5%;
b,称取Al2O3粉末80g和SiO2粉末5g加入去150g离子水中,搅拌30min;
c,称取CeO2粉末10g和HBEA 5g加入搅拌好的浆液中,继续搅拌30min;
d,将搅拌均匀的浆液加入砂磨机中,砂磨40min,磨至颗粒度为9μm;
e,取出浆液,调节固含量至38%;
f,配制1-5%果糖约6g,缓慢滴加Pt溶液,Pt含量0.5g/ft3;
g,采用浸渍法涂覆底层氧化层,控制涂覆量30g/L;
h,120℃烘干120min,450℃焙烧180min。
(2)上层SCR还原层制备
a,将纳米Cu离子同去离子水混合,并搅拌均匀,水浴加热至50℃,待Cu源完全分散均匀,然后按Cu/CHA比为0.6加入H-BEA,继续升温至90℃,均匀搅拌1h;
b,离子交换完成后,将交换液冷却后,通过抽滤机中进行抽滤,洗涤,待抽出液呈无色后放入110℃烘箱干燥。
c,干燥后,以5℃/min的速度升温至400℃,保温2h,随炉冷却待用。
d,将纳米Al2O3粉40g在去离子水中充分搅拌,然后缓慢加入浓度为5%HNO3,纳米Al2O3粉胶溶后,水浴升温至50℃,保温60min。
e,将纳米SiO2粉末30g缓慢加入纳米Al2O3胶体中,匀速搅拌,并调节pH值至4,水浴加热至90℃,保温5h,陈化2d后作为粘接剂备用。
f,将分子筛粉碎后,加入去离子水,调节固含量37%,搅拌20min。
g,添加8%的Si-Al复合胶,搅拌20min,调节粘度至500cp。
h,采用定量涂覆法制备AMOX催化剂,控制涂覆量200g/L;
i,160℃快速烘干后,升温至600℃焙烧3h。
实施例4
(1)底层NH3氧化层制备
a,按固体含量为30%,分别计算粉体用量,Al2O3粉末占40%,SiO2粉末占40%,CeO2粉末占10%,HBEA分子筛占10%;
b,称取Al2O3粉末40g和SiO2粉末40g加入去220g离子水中,搅拌60min;
c,称取CeO2粉末10g和HBEA 10g加入搅拌好的浆液中,继续搅拌20min;
d,将搅拌均匀的浆液加入砂磨机中,砂磨60min,磨至颗粒度为5μm;
e,取出浆液,调节固含量至30%;
f,配制5%蔗糖约50g,缓慢滴加Pt溶液,Pt含量8g/ft3;
g,采用浸渍法涂覆底层氧化层,控制涂覆量100g/L;
h,120℃烘干20-120min,400-650℃焙烧20-180min。
(2)上层SCR还原层制备
a,将Cu(NO3)2同去离子水混合,并搅拌均匀,水浴加热至40℃,待Cu源完全溶解,然后按Cu/CHA比为0.6加入H-ZSM-5,继续升温至70℃,均匀搅拌0.5h;
b,离子交换完成后,将交换液冷却后,通过抽滤机中进行抽滤,洗涤,待抽出液呈无色后放入120℃烘箱干燥。
c,干燥后,以2℃/min的速度升温至400℃,保温1h,随炉冷却待用。
d,将纳米Al2O3粉30g在去离子水中充分搅拌,然后缓慢加入浓度为1%HNO3,纳米Al2O3粉胶溶后,水浴升温至40℃,保温60min。
e,将纳米SiO2粉末30-50g缓慢加入纳米Al2O3胶体中,匀速搅拌,并调节PH值至2.5,水浴加热至65℃,保温2h,陈化1d后作为粘接剂备用。
f,将分子筛粉碎后,加入去离子水,调节固含量25%,搅拌50min。
g,添加1%的Si-Al复合胶,搅拌60min,调节粘度至2000cp。
h,采用定量涂覆法制备AMOX催化剂,控制涂覆量90g/L;
i,150℃快速烘干后,升温至600℃焙烧1h。
实施例5
(1)底层NH3氧化层制备
a,按固体含量为45%,分别计算粉体用量,Al2O3粉末占40%,SiO2粉末占40%,CeO2粉末占10%,HBEA分子筛占10%;
b,称取Al2O3粉末40g和SiO2粉末40g加入去100g离子水中,搅拌30min;
c,称取CeO2粉末10g和HBEA 10g加入搅拌好的浆液中,继续搅拌30min;
d,将搅拌均匀的浆液加入砂磨机中,砂磨50min,磨至颗粒度为6μm;
e,取出浆液,调节固含量至37%;
f,配制5%葡聚糖约10g,缓慢滴加Pt溶液,Pt含量5g/ft3;
g,采用浸渍法涂覆底层氧化层,控制涂覆量80g/L;
h,120℃烘干100min,450℃焙烧150min。
(2)上层SCR还原层制备
a,将纳米Cu源同去离子水混合,并搅拌均匀,水浴加热至40℃,待Cu源完全溶解,然后按Cu/SAPO34比为0.3加入H-SAPO34,继续升温至80℃,均匀搅拌1h;
b,离子交换完成后,将交换液冷却后,通过抽滤机中进行抽滤,洗涤,待抽出液呈无色后放入100℃烘箱干燥。
c,干燥后,以6℃/min的速度升温至500℃,保温2h,随炉冷却待用。
d,将纳米Al2O3粉35g在去离子水中充分搅拌,然后缓慢加入浓度为2%HAC,纳米Al2O3粉胶溶后,水浴升温至50℃,保温60min。
e,将纳米SiO2粉末30g缓慢加入纳米Al2O3胶体中,匀速搅拌,并调节pH值至3.5,水浴加热至65℃,保温3h,陈化2d后作为粘接剂备用。
f,将分子筛粉碎后,加入去离子水,调节固含量30%,搅拌30min。
g,添加2%的Si-Al复合胶,搅拌30min,调节粘度至600cp。
h,采用定量涂覆法制备AMOX催化剂,控制涂覆量150g/L。
本发明不限于上述实施例,凡依据本发明的技术实质对上述实施例作的任何简单、等同变化或修饰,均属于本发明技术范围内。
Claims (9)
1.一种高效AMOX整体式催化剂的制备方法,其特征在于,催化剂分为两层涂覆,具体包括以下步骤:
(1)底层NH3氧化层制备
a,按固体含量为30-45%,分别计算粉体用量,Al2O3粉末占粉体总质量的40-80%,SiO2粉末占粉体总质量的0-50%,CeO2粉末占粉体总质量的10-50%,HBEA分子筛占粉体总质量的5-45%;
b,称取Al2O3粉末40-60g和SiO2粉末0-30g加入去100g离子水中,搅拌20-60min;
c,称取CeO2粉末10-50g和HBEA 5-15g加入步骤b搅拌好的浆液中,继续搅拌20-60min;
d,将步骤c搅拌均匀的浆液加入砂磨机中,砂磨5-60min,磨至颗粒度为5-15μm;
e,取出浆液,调节固含量至25-45%;
f,配制1-5%麦芽糖溶液约5-50g,缓慢滴加Pt溶液,Pt含量0.5-8g/ft3;
g,采用浸渍法涂覆底层氧化层,控制涂覆量30-100g/L;
h,120℃烘干20-120min,400-650℃焙烧20-180min后,得到底层NH3氧化层;
(2)上层SCR还原层制备
a,将Cu源同去离子水混合,并搅拌均匀,水浴加热至20-60℃,待Cu源完全溶解,然后按Cu/分子筛重量比为0.1-0.6加入分子筛,继续升温至70-90℃,均匀搅拌0.5-2h;
b,离子交换完成后,将交换液冷却后,通过抽滤机中进行抽滤,洗涤,待抽出液呈无色后,将滤饼放入100-120℃烘箱干燥;
c,干燥后,以2-8℃/min的速度升温至400-600℃,保温1-3h,随炉冷却待用;
d,将纳米Al2O3粉30-50g在去离子水中充分搅拌,然后缓慢加入浓度为1-5%HNO3溶液,待纳米Al2O3粉胶溶后,水浴升温至40-60℃,保温60min,得到纳米Al2O3胶体;
e,将纳米SiO2粉末30-50g缓慢加入纳米Al2O3胶体中,匀速搅拌,并调节pH值至2.5-4,水浴加热至65-90℃,保温2-5h,陈化1-2d后得到Si-Al复合胶作为粘接剂备用;
f,将分子筛粉碎后,加入去离子水,调节固含量25-45%,搅拌20-60min;
g,向上述分子筛溶液中添加1-8%的Si-Al复合胶,搅拌20-60min,调节粘度至500-2000cp;
h,采用定量涂覆法制备AMOX催化剂,控制涂覆量30-200g/L;
i,110-160℃快速烘干后,升温至300-600℃焙烧1-3h后,得到AMOX催化剂。
2.根据权利要求1所述的一种高效AMOX整体式催化剂的制备方法,其特征在于CeO2可以替换为Ce(NO3)2、Ce(CH3COO)2中的至少一种;在底层Al2O3和SiO2添加中,可以是两种不同的粉体添加,也可以是通过改性后制备的复合粉体,也可以是通过其他元素进行的改性复合粉体或单一粉体;在底层添加的CeO2,可以是单一粉体,也可以是通过改性后制备的复合粉体;在底层添加的贵金属分散剂麦芽糖,可以替换成果糖、葡聚糖、蔗糖、葡萄糖等糖类,也可以是乙二醇、丙醇、聚乙烯醇等醇类,也可以是乙酸乙酯、乙酸丁酯等脂类。
3.根据权利要求1所述的一种高效AMOX整体式催化剂的制备方法,其特征在于上层SCR涂层离子交换投加比例为Cu/分子筛为0.1-0.6,比例可以是摩尔比也可以换算成质量比,水浴温度为70-85℃;所使用的粘接剂为Al-Si复合胶,Al/Si的质量比为1-9,pH值为2.5-6,水浴温度为60-90℃;对上层SCR层Si-Al复合胶制备安定剂,不仅限于HNO3,也可以是乙酸、盐酸等酸溶液,也可以是通过NH3水等碱溶液调节的碱性Si-Al复合胶;对上层SCR层Si-Al复合胶,也可以是通过分散剂制备的公平衡状态Si-Al复合胶,也可以是通过Si胶和Al胶按一定比例直接复合的混合胶体;Cu盐可以是乙酸铜、硝酸铜等铜盐,也可以纳米Cu离子、纳米Cu颗粒,也可以是Cu氧化物,Cu单质等。
4.根据权利要求1所述的一种高效AMOX整体式催化剂的制备方法,其特征在于对NH3氧化层原料进行降低粒度的方法,不仅限于砂磨机,也可以是球磨机、水磨机等。
5.根据权利要求1所述的一种高效AMOX整体式催化剂的制备方法,其特征在于对Al2O3、CeO2、SiO2和去离子水等原料添加不限于步骤(1)中顺序;对Cu源、分子筛、纳米Al2O3及SiO2等原料添加不限于步骤(2)中顺序。
6.根据权利要求1所述的一种高效AMOX整体式催化剂的制备方法,其特征在于,分子筛可以是CHA型,也可以是BEA、MFI、FAU、CFI等分子筛。
7.根据权利要求1所述的一种高效AMOX整体式催化剂的制备方法,其特征在于在Cu-分子筛离子交换结束后所得分子筛也可以用压滤、离心、喷雾、洗涤等方法。
8.根据权利要求1所述的一种高效AMOX整体式催化剂的制备方法,其特征在于AMOX整体式催化剂涂覆方法不限于定量涂覆法,也可以是浸渍提拉法,浸渍专机,抽涂专机,吹扫专机等涂覆方法。
9.根据权利要求1所述的一种高效AMOX整体式催化剂的制备方法,其特征在于在溶胶水浴加热采用程序升温过程,升温速率范围为0.3~10℃/min,水浴温度为70-85℃。
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