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学者姓名：俞秀金
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Abstract ：
本发明公开了一种以多羟基钌络合物为前驱体的钌系氨合成催化剂及其制备方法，它的组成为RuL+M1+M2/AC，M1-(RuL+M1+M2)/AC，(RuL+M1+M2)-M1/AC，(RuL+M1+M2)-M2-M1/AC中的一种；其中RuL为钌与多羟基醚、多羟基醛或多羟基酮反应生成的水溶性的钌络合物；M1为硝酸钡、乙酸钡、硝酸镁、硝酸铵、硝酸铝、硝酸锆中的一种或多种的混合物；M2是碱金属钠、钾、铷、铯、稀土金属的硝酸盐、乙酸盐或氢氧化物中的一种或多种的混合物；AC是载体，即活性炭或石墨化活性炭。该方法以石墨化活性炭为载体，经过钌酸钾制备、前驱体制备、混合溶液制备、催化剂制备、干燥等步骤制得氨合成催化剂。本发明的设备、流程简单，制备周期短，效率高，节能环保，易于实现规模化生产；制备的催化剂性价比高。
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| GB/T 7714 | 倪军 , 陈赓 , 魏可镁 et al. 以多羟基钌络合物为前驱体的钌系氨合成催化剂 : CN201210024788.0[P]. | 2012/2/6 . |
| MLA | 倪军 et al. "以多羟基钌络合物为前驱体的钌系氨合成催化剂" : CN201210024788.0. | 2012/2/6 . |
| APA | 倪军 , 陈赓 , 魏可镁 , 林建新 , 林炳裕 , 王榕 et al. 以多羟基钌络合物为前驱体的钌系氨合成催化剂 : CN201210024788.0. | 2012/2/6 . |
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本发明提供了一种以亚硝酰基硝酸钌为前驱体的氨合成催化剂及其制备方法，该催化剂的组成为(RuL+M1+M2)/AC，RuL-M1-M2/AC，M1-(RuL+M2)/AC，M1-(RuL+M2)-M1/AC中的一种，其中AC为石墨化活性炭；M1为钡、镁、铵的硝酸盐、乙酸盐中的一种或多种混合物；M2为碱金属钠、钾、铷、铯、稀土金属硝酸盐、乙酸盐、氢氧化物中的一种或多种混合物；RuL为亚硝酰基硝酸钌络合物；钌的浸渍量为活性炭重量的2-9%，M1的浸渍量为活性炭重量的4-16%，M2的浸渍量为活性炭重量的10-20%；活性组分Ru与助剂采用等体积多次浸渍法浸渍到载体上。本发明的设备、流程简单，制备周期短，易于实现规模生产；本发明制备的催化剂与已有的氯化钌作前驱体的钌基氨合成催化剂相比，催化剂的制备效率大幅度提高，催化剂的性价比高。
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| GB/T 7714 | 倪军 , 陈赓 , 魏可镁 et al. 以亚硝酰基硝酸钌为前驱体的氨合成催化剂及其制备方法 : CN201210024855.9[P]. | 2012/2/6 . |
| MLA | 倪军 et al. "以亚硝酰基硝酸钌为前驱体的氨合成催化剂及其制备方法" : CN201210024855.9. | 2012/2/6 . |
| APA | 倪军 , 陈赓 , 魏可镁 , 林建新 , 林炳裕 , 王榕 et al. 以亚硝酰基硝酸钌为前驱体的氨合成催化剂及其制备方法 : CN201210024855.9. | 2012/2/6 . |
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Abstract ：
本发明公开了一种氨合成催化剂及其制备方法，它的组成为RuL+M1+M2/AC，M1-(RuL+M1+M2)/AC，(RuL+M1+M2)-M1/AC或(RuL+M1+M2)-M2-M1/AC中的一种；其中RuL为钌与多元醇、多元醛、多元酸反应生成的水溶性的钌络合物；M1为硝酸钡、乙酸钡、硝酸镁、硝酸铵中的一种或多种的组合物；M2是碱金属钠、钾、铷、铯和稀土硝酸盐、乙酸盐或氢氧化物中的一种或多种的组合物；AC是载体，即石墨化活性炭。该方法以石墨化活性炭为载体，经过钌酸钾制备、前驱体制备、混合溶液制备、催化剂制备、干燥这些步骤制得氨合成催化剂。本发明的设备、流程简单，制备周期短，效率高，节能环保，易于实现规模化生产；制备的催化剂性价比高。
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| GB/T 7714 | 魏可镁 , 倪军 , 林建新 et al. 一种氨合成催化剂及其制备方法 : CN201110258118.0[P]. | 2011/9/2 . |
| MLA | 魏可镁 et al. "一种氨合成催化剂及其制备方法" : CN201110258118.0. | 2011/9/2 . |
| APA | 魏可镁 , 倪军 , 林建新 , 林炳裕 , 王榕 , 俞秀金 . 一种氨合成催化剂及其制备方法 : CN201110258118.0. | 2011/9/2 . |
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Tunable carbon nanotubles (CNTs)-coated monoliths as catalyst supports were prepared by catalytic chemical vapor deposition (CCVD) over deposited cobalt on cordierite. The influence of the preparation conditions such as the cobalt nitrate loading on the cordierite monoliths, the flow rate of reaction gases, reaction time and temperature on CNTs yield, thermal properties and structural features of the resulting materials were studied. The CNTs-cordierite was characterized by TEM/HREM, SEM, N-2 physisorption and TGA. The SEM showed that a relatively homogeneous mesoporous layer of CNTs covered on the surface of the cordierite monoliths. Comparing with the bare cordierite, the BET surface area and pore volume of CNTs-cordierite increased significantly. CNTs have penetrated into the cordierite substrate and led to a remarkable mechanical stability of the CNTs-cordierite monoliths against ultrasound maltreatment. The CNTs content, BET surface area, pore volume and thermal properties of CNT-scordierite monoliths all could be changed by the variation of the synthesis conditions. Barium promoted ruthenium catalysts supported on the as-synthesized materials showed much higher activity for ammonia synthesis than their counterparts deposited on bare cordierite monoliths. Furthermore, the catalytic activity linearly increased with the BET surface area of CNTs-cordierite monoliths. The CNT-scordierite monoliths were proved to be promising candidates as catalyst supports and the performance of catalysts supported on as-prepared materials would be easily modified by changing the growth conditions of CNTs.
Keyword ：
ammonia synthesis ammonia synthesis CCVD CCVD CNTs-cordierite monolith CNTs-cordierite monolith support support
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| GB/T 7714 | Gong, Binbin , Wang, Rong , Lin, Bingyu et al. Preparation of carbon nanotubes (CNTs)-cordierite monoliths by catalytic chemical vapor deposition as catalyst supports for ammonia synthesis [J]. | CATALYSIS LETTERS , 2008 , 122 (3-4) : 287-294 . |
| MLA | Gong, Binbin et al. "Preparation of carbon nanotubes (CNTs)-cordierite monoliths by catalytic chemical vapor deposition as catalyst supports for ammonia synthesis" . | CATALYSIS LETTERS 122 . 3-4 (2008) : 287-294 . |
| APA | Gong, Binbin , Wang, Rong , Lin, Bingyu , Me, Feng , Yu, Xiujin , Wei, Kemei . Preparation of carbon nanotubes (CNTs)-cordierite monoliths by catalytic chemical vapor deposition as catalyst supports for ammonia synthesis . | CATALYSIS LETTERS , 2008 , 122 (3-4) , 287-294 . |
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Rare earth gangue, which mainly consists of mixtures of light rare earths such as lanthana, ceria, neodymium oxide and praseodymium oxide, was used as the promoter of fused iron catalysts for ammonia synthesis. The result showed that the activity of the catalyst promoted with rare earth gangue was comparable with those of commercial iron catalysts with high amount of cobalt. The role of rare earths was owed to their advantages for favoring the deep reduction of the main composite in catalyst, i.e., iron oxide. This finding indicated that the use of rare earth gangue could decrease the content of cobalt or even completely replace cobalt, which was used to be regarded as unsubstitutable promoters for high performance ammonia catalyst; therefore, the cost of fused iron catalysts would decrease significantly.
Keyword ：
ammonia synthesis ammonia synthesis fused iron catalyst fused iron catalyst promoter promoter rare earth gangue rare earth gangue
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| GB/T 7714 | Yu Xiujin , Lin Bingyu , Lin Jianxin et al. A novel fused iron catalyst for ammonia synthesis promoted with rare earth gangue [J]. | JOURNAL OF RARE EARTHS , 2008 , 26 (5) : 711-716 . |
| MLA | Yu Xiujin et al. "A novel fused iron catalyst for ammonia synthesis promoted with rare earth gangue" . | JOURNAL OF RARE EARTHS 26 . 5 (2008) : 711-716 . |
| APA | Yu Xiujin , Lin Bingyu , Lin Jianxin , Wang Rong , Wei Kemei . A novel fused iron catalyst for ammonia synthesis promoted with rare earth gangue . | JOURNAL OF RARE EARTHS , 2008 , 26 (5) , 711-716 . |
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A series of alumina supported ruthenium catalysts, which prepared by hydrogen treatment or hydrazine reduction, were characterized by N(2) adsorption, X-ray diffraction (XRD), X-ray fluorescence (XRF), CO chemisorption, and Temperature-programmed desorption of hydrogen (H(2)-TPD). In contrast to the samples with conventional hydrogen reduction, there was almost no residual chlorine in the samples using RuCl(3) as precursor with hydrazine treatment. Furthermore, the dissolved aluminum could be removed much more easily in basic solution, which led to the higher BET surface and pore volume of hydrazine-reduction catalysts. Therefore, the active phase (Ru metal) would not be contaminated. Three main peaks, which occurred at about 150, 375, and 650 degrees C, respectively, were observed in the H(2)-TPD profiles of Ru/Al(2)O(3) catalysts with a high amount of residual chlorine. A new peak of desorption hydrogen centering at 240 degrees C, which was completely suppressed by the high amount of residual chlorine, might appear in the profiles of the samples with the washing procedure following hydrogen reduction or hydrazine treatment. The peaks with the desorption temperature lower than 500 degrees C were relative with dissociatively adsorbed hydrogen and spillover hydrogen simultaneity, and the peak at above 500 degrees C was caused by spillover hydrogen and would be stabilized by hydroxyl groups on alumina surface.
Keyword ：
chlorine chlorine H(2)-TPD H(2)-TPD hydrazine reduction hydrazine reduction Ru/Al(2)O(3) Ru/Al(2)O(3)
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| GB/T 7714 | Lin, Bingyu , Wang, Rong , Yu, Xiujin et al. Physicochemical characterization and H(2)-TPD study of alumina supported ruthenium catalysts [J]. | CATALYSIS LETTERS , 2008 , 124 (3-4) : 178-184 . |
| MLA | Lin, Bingyu et al. "Physicochemical characterization and H(2)-TPD study of alumina supported ruthenium catalysts" . | CATALYSIS LETTERS 124 . 3-4 (2008) : 178-184 . |
| APA | Lin, Bingyu , Wang, Rong , Yu, Xiujin , Lin, Jianxin , Xie, Feng , Wei, Kemei . Physicochemical characterization and H(2)-TPD study of alumina supported ruthenium catalysts . | CATALYSIS LETTERS , 2008 , 124 (3-4) , 178-184 . |
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Nitric acid treatment of CNTs-cordierite monolith changes the amount of Mg, Si, Al and oxygen-containing functional groups, thereby influencing on the surface area and pore size distribution of composite materials. Appropriate treatment of CNTs-cordierite with nitric acid increases the surface area and the amount of micropores slightly, but improves the activities for ammonia synthesis noticeable, which might be a consequent of the variation of the amount of Mg, Si, Al and oxygen-containing functional groups. The ammonia synthesis activity of Ba-Ru/CNTs-cordierite increase by more than 30% if the support material is treated at 30 degrees C for 4 h with nitric acid.
Keyword ：
ammonia synthesis ammonia synthesis CNTs-cordierite CNTs-cordierite nitric acid treatment nitric acid treatment Ru Ru
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| GB/T 7714 | Yu, Xiujin , Lin, Bingyu , Gong, Binbin et al. Effect of nitric acid treatment on carbon nanotubes (CNTs)-cordierite monoliths supported ruthenium catalysts for ammonia synthesis [J]. | CATALYSIS LETTERS , 2008 , 124 (3-4) : 168-173 . |
| MLA | Yu, Xiujin et al. "Effect of nitric acid treatment on carbon nanotubes (CNTs)-cordierite monoliths supported ruthenium catalysts for ammonia synthesis" . | CATALYSIS LETTERS 124 . 3-4 (2008) : 168-173 . |
| APA | Yu, Xiujin , Lin, Bingyu , Gong, Binbin , Lin, Jianxin , Wang, Rong , Wei, Kemei . Effect of nitric acid treatment on carbon nanotubes (CNTs)-cordierite monoliths supported ruthenium catalysts for ammonia synthesis . | CATALYSIS LETTERS , 2008 , 124 (3-4) , 168-173 . |
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采用分光光度法测定活性炭负载钌系氨合成催化剂中的钌含量.在强酸和乙醇体系中,Ru(Ⅲ)与硫脲生成蓝色物,于最大吸收波长λ= 620 nm处测定催化剂中的钌含量.测试结果表明,该方法操作简单、干扰小,相对标准偏差为1%～3%,加标回收率在97.5%～102.0%之间,适用于活性炭负载钌系氨合成催化剂中钌含量的准确测定.
Keyword ：
分光光度法 分光光度法 氨合成催化剂 氨合成催化剂 硫脲 硫脲 钌 钌
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| GB/T 7714 | 谢峰 , 俞秀金 , 王榕 et al. 活性炭负载钌系氨合成催化剂中钌含量的分析 [J]. | 分析测试技术与仪器 , 2008 , 14 (1) : 42-45 . |
| MLA | 谢峰 et al. "活性炭负载钌系氨合成催化剂中钌含量的分析" . | 分析测试技术与仪器 14 . 1 (2008) : 42-45 . |
| APA | 谢峰 , 俞秀金 , 王榕 , 林建新 . 活性炭负载钌系氨合成催化剂中钌含量的分析 . | 分析测试技术与仪器 , 2008 , 14 (1) , 42-45 . |
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研究了浸渍条件和还原剂种类对蒽醌氢化制备过氧化氢Pd-BaO/δ,θ-Al2O3催化剂性能的影响.结果表明,当浸渍液温度60℃=和pH=3.5时,催化剂上钯金属的分散度较高,钯粒子较小,催化剂活性较高.使用不同还原剂也会影响催化剂的Pd分散度和粒子大小,其中,以水合肼和H2还原得到的催化剂有较高的活性比表面积、分散度和较小的粒子尺寸,而经硼氢化钾还原的催化剂的分散度偏低.水合肼还原得到的催化剂的活性较高,H2还原的催化荆活性次之,以硼氢化钾还原的催化剂活性最差.
Keyword ：
催化剂制备条件 催化剂制备条件 催化化学 催化化学 蒽醌氢化 蒽醌氢化 过氧化氢 过氧化氢 钯催化剂 钯催化剂
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| GB/T 7714 | 俞秀金 , 杜书伟 , 林炳裕 et al. 制备条件对Pd-BaO/δ,θ-Al2O3催化蒽醌氢化制备过氧化氢性能的影响 [J]. | 工业催化 , 2008 , 16 (7) : 43-46 . |
| MLA | 俞秀金 et al. "制备条件对Pd-BaO/δ,θ-Al2O3催化蒽醌氢化制备过氧化氢性能的影响" . | 工业催化 16 . 7 (2008) : 43-46 . |
| APA | 俞秀金 , 杜书伟 , 林炳裕 , 林建新 , 王榕 . 制备条件对Pd-BaO/δ,θ-Al2O3催化蒽醌氢化制备过氧化氢性能的影响 . | 工业催化 , 2008 , 16 (7) , 43-46 . |
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以蔗糖为碳源,正硅酸乙酯(TEOS)为硅源,草酸为凝胶剂采用溶胶凝胶法制备出前躯体,高温碳热还原合成C/SiC复合物,其比表面积为333 m2/g,孔半径集中在7.9 nm;总孔体积在0.52 cm3/g;以其为载体,钉为活性金属组分,钡和钾为助剂制备催化剂,将其应用于氨合成反应,考察其催化活性.当催化剂中Ru,Ba和K质量分数分别为3.28%,3.28%和11.48%时,在10.0 MPa,空速为10 000 h-1,435℃条件下,出口氨浓度达15.20%(体积分数).
Keyword ：
复合物 复合物 氨合成 氨合成 碳化硅 碳化硅 载体 载体
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| GB/T 7714 | 俞秀金 , 郑瑛 , 郑勇 et al. C/SiC复合材料的合成及在氨合成反应中的应用 [J]. | 分子催化 , 2008 , 22 (5) : 424-428 . |
| MLA | 俞秀金 et al. "C/SiC复合材料的合成及在氨合成反应中的应用" . | 分子催化 22 . 5 (2008) : 424-428 . |
| APA | 俞秀金 , 郑瑛 , 郑勇 , 王榕 , 魏可镁 . C/SiC复合材料的合成及在氨合成反应中的应用 . | 分子催化 , 2008 , 22 (5) , 424-428 . |
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