CN110508277A - 一种高分散钯纳米颗粒催化剂及其制备方法和应用 - Google Patents
一种高分散钯纳米颗粒催化剂及其制备方法和应用 Download PDFInfo
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- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims abstract description 153
- 229910052763 palladium Inorganic materials 0.000 title claims abstract description 66
- 239000003054 catalyst Substances 0.000 title claims abstract description 65
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000002270 dispersing agent Substances 0.000 claims abstract description 40
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 38
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims abstract description 30
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims abstract description 28
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 24
- 150000002941 palladium compounds Chemical class 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 10
- 235000019353 potassium silicate Nutrition 0.000 claims description 9
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 8
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 7
- 239000000460 chlorine Substances 0.000 claims description 7
- 229910052801 chlorine Inorganic materials 0.000 claims description 7
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- 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 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 3
- LNAZSHAWQACDHT-XIYTZBAFSA-N (2r,3r,4s,5r,6s)-4,5-dimethoxy-2-(methoxymethyl)-3-[(2s,3r,4s,5r,6r)-3,4,5-trimethoxy-6-(methoxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6r)-4,5,6-trimethoxy-2-(methoxymethyl)oxan-3-yl]oxyoxane Chemical compound CO[C@@H]1[C@@H](OC)[C@H](OC)[C@@H](COC)O[C@H]1O[C@H]1[C@H](OC)[C@@H](OC)[C@H](O[C@H]2[C@@H]([C@@H](OC)[C@H](OC)O[C@@H]2COC)OC)O[C@@H]1COC LNAZSHAWQACDHT-XIYTZBAFSA-N 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 2
- 125000003963 dichloro group Chemical group Cl* 0.000 claims description 2
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- 239000000203 mixture Substances 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- YJVFFLUZDVXJQI-UHFFFAOYSA-L palladium(ii) acetate Chemical compound [Pd+2].CC([O-])=O.CC([O-])=O YJVFFLUZDVXJQI-UHFFFAOYSA-L 0.000 claims description 2
- JKDRQYIYVJVOPF-FDGPNNRMSA-L palladium(ii) acetylacetonate Chemical compound [Pd+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O JKDRQYIYVJVOPF-FDGPNNRMSA-L 0.000 claims description 2
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims description 2
- 229940048086 sodium pyrophosphate Drugs 0.000 claims description 2
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 2
- KGYLMXMMQNTWEM-UHFFFAOYSA-J tetrachloropalladium Chemical compound Cl[Pd](Cl)(Cl)Cl KGYLMXMMQNTWEM-UHFFFAOYSA-J 0.000 claims description 2
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims description 2
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 1
- 239000011574 phosphorus Substances 0.000 claims 1
- 229910052698 phosphorus Inorganic materials 0.000 claims 1
- 239000001488 sodium phosphate Substances 0.000 claims 1
- 229960003339 sodium phosphate Drugs 0.000 claims 1
- 235000011008 sodium phosphates Nutrition 0.000 claims 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 abstract description 19
- 239000005977 Ethylene Substances 0.000 abstract description 19
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
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- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 4
- 150000001345 alkine derivatives Chemical class 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000012495 reaction gas Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- -1 polyethylene Polymers 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910002666 PdCl2 Inorganic materials 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000003708 ampul Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
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- 238000007654 immersion Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
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- 239000002245 particle Substances 0.000 description 1
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- 230000009257 reactivity Effects 0.000 description 1
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
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Abstract
本发明提供了一种高分散钯纳米颗粒催化剂及其制备方法与应用,所述催化剂由氧化铝载体、钯化合物、分散剂组成;本发明的氧化铝负载高分散钯纳米颗粒催化剂应用于乙炔选择性加氢反应,具有高的催化活性、高的乙烯选择性、较优的稳定性和低制备成本等优点。
Description
(一)技术领域
本发明涉及一种高分散钯纳米颗粒催化剂及其制备方法,以及在乙炔选择性加氢反应中的应用。
(二)背景技术
乙烯是世界范围内最重要的石油化工产品之一,在工业上主要是通过石脑油的裂解制得。但是通过这种方法值得的乙烯中往往含有大约0.3%~3%摩尔分数的乙炔,最高甚至可达0.9%;这些微量的乙炔会严重的影响工艺设备并毒害生产聚乙烯的Ziegler-Natta催化剂,降低催化剂的活性和使用寿命,同时也会影响聚乙烯的产品质量。为了解决这个问题,工业上常用选择性加氢法来减少原料气中乙炔的含量,这种方法不仅仅可以降低乙炔物料的浓度,而且乙炔会在反应中生成乙烯。然而工业上传统的钯基催化剂虽然在反应中有着较优的反应活性,但是却存在着乙烯选择性低的问题。大部分乙炔会转化生成乙烷和绿油,造成原料气的浪费;因此需要对传统的钯基催化剂进行改性,防止乙烯加氢生成乙烷反应的发生,从而进一步提高乙烯的选择性。
当今乙炔选择性加氢反应的另一热门是建立单原子体系、获得更高的分散度以及调控活性中心的形貌和大小。分散程度更高的钯基催化剂能够使乙烯在钯活性位点上的吸附方式从结合能力较强的e键转变为相对较弱的π键,有利于乙烯从催化剂表面脱附从而抑制了乙烯的过度加氢。另一方面,Pd的几何结构对乙炔选择加氢体系也有很大的影响,拥有更好Pd几何结构的钯基催化剂会表现出更好的乙炔转化率和乙烯选择性。
基于以上背景,本发明提出了一种氧化铝负载的高分散钯纳米颗粒催化剂,以提高钯基催化剂在乙炔选择性加氢的选择性。
(三)发明内容
本发明的目的在于提供一种高分散钯纳米颗粒催化剂及其制备与应用。本发明制备方法工艺简单,制得的催化剂能极大程度上提高乙炔选择性加氢反应中的乙烯选择性。
本发明的技术方案如下:
一种高分散钯纳米颗粒催化剂,由氧化铝载体、钯化合物、分散剂组成;
所述氧化铝载体的比表面积为60-380m2/g;
所述钯化合物为氯钯酸、硝酸钯、醋酸钯、乙酰丙酮钯、二氯二氨钯、四氯钯酸铵、氯钯酸钠或硝酸四氨合钯,优选氯钯酸;
所述分散剂为有机分散剂或无机分散剂,具体例如:水玻璃、甲基戊醇、十二烷基硫酸钠、甲基纤维素、三聚磷酸钠、六偏磷酸钠或焦磷酸钠,优选水玻璃或甲基戊醇,最优选水玻璃,分散剂的目的主要是极大程度上的增大钯纳米颗粒在载体中的分散度;
所述催化剂中,基于载体的质量,钯化合物以钯计的负载量为0.01-0.5wt%(优选0.01-0.1wt%,更优选0.01-0.03wt%),分散剂的负载量为5-40wt%(优选10-30wt%,更优选30wt%)。
一种高分散钯纳米颗粒催化剂的制备方法,所述制备方法包括以下步骤:
(1)将钯化合物溶解于溶剂中,制得钯浸渍液;
所述钯浸渍液中,钯化合物以钯计的浓度为0.001-0.01g/mL;
所述溶剂根据钯化合物的种类而定,可以是水、盐酸、乙醇、丙酮等,本发明对此没有特殊要求;
(2)将分散剂溶解在溶剂中,得到分散剂溶液;
所述分散剂溶液中,分散剂的浓度为0.001-0.1g/mL;
所述溶剂根据分散剂的种类而定,可以是水、盐酸、乙醇、丙酮或DMF等,本发明对此没有特殊要求;
(3)将所得分散剂溶液与钯浸渍液混合,在60~80℃下搅拌9-12h,之后放入微波反应器中,在110-130℃下微波并超声2-4h,得到高分散的钯溶液;
(4)将氧化铝载体浸没于高分散的钯溶液中,分散均匀,室温(20-30℃)下浸渍9-12h,之后于110-130℃下干燥9-12h,即得所述高分散钯纳米颗粒催化剂;
本发明中,步骤(4)氧化铝浸渍钯液9-12h后,可将体系置于微波反应器中,在100-130℃下微波20-80min,可进一步促进金属组分的分散,然后再将样品放入110-130℃烘箱中干燥9-12h后得到最终的催化剂。
本发明所述催化剂的制备方法中,钯化合物和分散剂可认为是全部负载,本领域技术人员可以根据需要的负载量选择钯化合物、分散剂的加入量。
本发明所述高分散钯纳米颗粒催化剂可应用于乙炔加氢反应中。具体的,所述应用的方法为:
在乙炔加氢反应前,需要先用氢气对所述催化剂进行还原,还原温度为130-230℃、时间为1-3h;再将还原后的催化剂用于乙炔加氢反应,反应条件为:温度60-180℃(优选70-120℃)、压力0.1-1MPa(优选0.1-0.3MPa,更优选常压)、空速1000-10000h-1(优选4000-8000h-1);
所述乙炔加氢反应中,反应初始的气体组成为(体积分数):0.33%C2H2、0.66%H2、33.3%C2H4、余量的N2。
与现有技术相比,本发明的有益效果在于:
(1)本发明的氧化铝负载高分散钯纳米颗粒催化剂,利用分散剂和一些简单操作,得到高分散的钯纳米颗粒,并制备出了一种高分散钯纳米颗粒催化剂。这种高分散的催化剂表现了高分散的钯纳米颗粒和更小的钯纳米粒子,使得该催化剂在乙炔选择性加氢反应中表现出了较高的活性和乙烯选择性;而且通过加入分散剂使得这种高分散的钯颗粒在反应中表现出了较优的稳定性;最后,高分散的钯催化剂在反应中也体现出了更好的原子利用率和降低了催化剂的制备成本。
(2)本发明的氧化铝负载高分散钯纳米颗粒催化剂的制备方法,工艺简单。
(3)本发明的氧化铝负载高分散钯纳米颗粒催化剂的制备方法引入微波处理步骤,可以进一步促进钯纳米颗粒的分散,从而获得均一稳定的催化剂和进一步提高反应中乙烯选择性。
(4)本发明的氧化铝负载高分散钯纳米颗粒催化剂应用于乙炔选择性加氢反应,具有高的催化活性、高的乙烯选择性、较优的稳定性和低制备成本等优点。
(四)具体实施方式
下面通过具体实施例对本发明作进一步的说明,但本发明的保护范围并不仅限于此。
实施例1-5
称取一定量的PdCl2溶解于浓盐酸中,转移至容量瓶中,加入一定量的去离子水到相应刻度,制得钯的质量浓度为0.001g/mL的氯钯酸溶液。称取一定量的分散剂溶解于盐酸或者DMF中,完全溶解后,转移至容量瓶中,加入一定量的去离子水到容量瓶刻度线处,制得0.03g/ml的分散剂溶液。按照表1所列的负载量及其配比,将计量的氯钯酸溶液和分散剂混合,在磁力搅拌充分后,移取一定量的混合溶液于表面皿中并加入一定量的去离子水,搅拌均匀后,均匀地将氧化铝载体(比表面积为360m2/g)倒入浸渍液中,超声使其分散均匀。将润湿的氧化铝在室温浸渍12h,并在110℃下干燥12h,即制得性能较优的氧化铝负载高分散钯纳米颗粒催化剂。
实施例4中氧化铝载体在负载Pd前后织构性质比较见表1:
表1负载Pd前后载体织构性质比较
实施例6
参照实施例5的操作,区别仅在于载体换成比表面积为60m2/g的氧化铝,制得性能较优的氧化铝负载高分散钯纳米颗粒催化剂。
实施例7
参照实施例5的操作,区别仅在于载体换成比表面积为380m2/g的氧化铝,制得性能较优的氧化铝负载高分散钯纳米颗粒催化剂。
实施例8
将实施例2制备的氧化铝负载高分散钯纳米颗粒催化剂在微波反应器中于100℃反应80min,得到成品催化剂,其具有更高的分散度。
实施例9
将实施例5制备的氧化铝负载高分散钯纳米颗粒催化剂在微波反应器中于120℃反应70min,得到成品催化剂。
制得的催化剂按照下面方法进行乙炔选择性加氢反应催化剂活性评价:
将0.3g催化剂置于小型石英管反应器中,将石英管放置于可控温的加热套中,在乙炔选择性加氢反应前,催化剂在纯H2气氛下180℃还原1h,还原气流速为10mL/min;还原结束后,按表2所示温度下进行反应。反应气体组成为(体积分数):0.33%乙炔,0.66%氢气,33.3%乙烯,余量氮气,反应气的流速为50mL/min,反应压力为常压。反应气出口接气相色谱在线检测,催化剂的评价结果见下表2所示。
表2高分散钯纳米颗粒催化剂的乙炔选择性加氢反应评价结果
实施例 | 负载量/wt% | 分散剂负载量/wt% | 分散剂种类 | 反应温度/℃ | 乙炔转化率/% | 乙烯选择性/% |
实施例1 | Pd=0.1 | 10 | 水玻璃 | 70 | ≥99.5 | 81.3 |
实施例2 | Pd=0.1 | 5 | 水玻璃 | 70 | 98.7 | 78.6 |
实施例3 | Pd=0.3 | 5 | 甲基戊醇 | 70 | ≥99.5 | 86.6 |
实施例4 | Pd=0.1 | 5 | 甲基戊醇 | 70 | ≥99.5 | 82.9 |
实施例5 | Pd=0.1 | 10 | 甲基戊醇 | 70 | ≥99.5 | 83.4 |
实施例6 | Pd=0.1 | 10 | 甲基戊醇 | 70 | ≥99.0 | 84.2 |
实施例7 | Pd=0.1 | 10 | 甲基戊醇 | 70 | ≥99.5 | 85.9 |
实施例8 | Pd=0.1 | 5 | 水玻璃 | 70 | ≥99.5 | 75.8 |
实施例9 | Pd=0.1 | 10 | 甲基戊醇 | 70 | ≥99.5 | 78.5 |
实施例10-15
参照实施例1-5的催化剂的制备方法,分散剂种类、负载量和配比见表3,制备氧化铝负载高分散钯纳米颗粒催化剂。
催化剂活性和选择性的评价方法同上,仅改变反应温度,催化剂的评价结果见下表3所示。
表3高分散钯纳米颗粒催化剂的乙炔选择性加氢反应评价结果
实施例 | 负载量/wt% | 分散剂种类 | 反应温度/℃ | 乙炔转化率/% | 乙烯选择性/% |
实施例10 | Pd=0.1,分散剂=10 | 水玻璃 | 80 | ≥99.8 | 86.1 |
实施例11 | Pd=0.1,分散剂=10 | 水玻璃 | 90 | ≥99.9 | 80.8 |
实施例12 | Pd=0.1,分散剂=10 | 甲基戊醇 | 60 | 95.5 | 82.6 |
实施例13 | Pd=0.1,分散剂=10 | 甲基戊醇 | 70 | ≥99.5 | 81.3 |
实施例14 | Pd=0.1,分散剂=10 | 甲基戊醇 | 80 | ≥99.9 | 80.7 |
实施例15 | Pd=0.1,分散剂=10 | 甲基戊醇 | 90 | ≥99.9 | 78.8 |
对比例16-19
参照实施例1-5,不加入任何分散剂,制备出纯的钯-氧化铝催化剂,催化剂活性和选择性的评价方法同上,仅改变反应温度,催化剂的评价结果见下表4所示。
表4纯钯-氧化铝催化剂的乙炔选择性加氢反应评价结果
对比例 | Pd负载量/wt% | 分散剂种类 | 反应温度/℃ | 乙炔转化率/% | 乙烯选择性/% |
对比例16 | 0.1 | / | 60 | 78.3 | 58.7 |
对比例17 | 0.1 | / | 70 | 89.7 | 46.1 |
对比例18 | 0.1 | / | 80 | ≥99.5 | 5.6 |
对比例19 | 0.1 | / | 90 | ≥99.9 | -20.4 |
Claims (7)
1.一种高分散钯纳米颗粒催化剂,其特征在于,由氧化铝载体、钯化合物、分散剂组成;
所述钯化合物为氯钯酸、硝酸钯、醋酸钯、乙酰丙酮钯、二氯二氨钯、四氯钯酸铵、氯钯酸钠或硝酸四氨合钯;
所述分散剂为:水玻璃、甲基戊醇、十二烷基硫酸钠、甲基纤维素、三聚磷酸钠、六偏磷酸钠或焦磷酸钠;
所述催化剂中,基于载体的质量,钯化合物以钯计的负载量为0.01-0.5wt%,分散剂的负载量为5-40wt%。
2.如权利要求1所述高分散钯纳米颗粒催化剂的制备方法,其特征在于,所述制备方法包括以下步骤:
(1)将钯化合物溶解于溶剂中,制得钯浸渍液;
(2)将分散剂溶解在溶剂中,得到分散剂溶液;
(3)将所得分散剂溶液与钯浸渍液混合,在60~80℃下搅拌9-12h,之后放入微波反应器中,在110-130℃下微波并超声2-4h,得到高分散的钯溶液;
(4)将氧化铝载体浸没于高分散的钯溶液中,分散均匀,室温下浸渍9-12h,之后于110-130℃下干燥9-12h,即得所述高分散钯纳米颗粒催化剂。
3.如权利要求2所述的制备方法,其特征在于,步骤(1)中,所述钯浸渍液中,钯化合物以钯计的浓度为0.001-0.01g/mL。
4.如权利要求2所述的制备方法,其特征在于,步骤(2)中,所述分散剂溶液中,分散剂的浓度为0.001-0.1g/mL。
5.如权利要求2所述的制备方法,其特征在于,步骤(4)氧化铝浸渍钯液9-12h后,将体系置于微波反应器中,在100-130℃下微波20-80min,然后再将样品放入110-130℃烘箱中干燥9-12h后得到最终的催化剂。
6.如权利要求1所述高分散钯纳米颗粒催化剂在乙炔加氢反应中的应用。
7.如权利要求6所述的应用,其特征在于,所述应用的方法为:
在乙炔加氢反应前,先用氢气对所述催化剂进行还原,还原温度为130-230℃、时间为1-3h;再将还原后的催化剂用于乙炔加氢反应,反应条件为:温度60-180℃、压力0.1-1MPa、空速1000-10000h-1;
所述乙炔加氢反应中,反应初始的气体组成为:0.33%C2H2、0.66%H2、33.3%C2H4、余量的N2。
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