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1. 发明授权

EP2823888B1 SURFACE MODIFICATION METHOD OF ALUMINUM OXIDE CARRIER 有权
公开(公告)号：EP2823888B1
公开(公告)日：2017-05-10
申请号：EP13758344.9
申请日：2013-03-04
申请人： Sunshine Kaidi New Energy Group Co., Ltd.
发明人： ZHENG, Shenke , SONG, Dechen , ZHAN, Xiaodong
IPC分类号： B01J32/00 , B01J21/04 , B01J35/02 , B01J35/10 , C01F7/02
CPC分类号： B01J21/04 , B01J35/023 , B01J35/1014 , B01J35/1038 , B01J35/1042 , B01J35/1061 , C01F7/021 , C01P2004/61 , C01P2006/12 , C01P2006/14 , C01P2006/16 , C01P2006/90

2. 发明公开

EP2824200A1 PROCESS FOR THE COMPREHENSIVE RECOVERY OF METAL COBALT, RUTHENIUM AND ALUMINUM FROM WASTE CATALYST CO-RU/AL2O3 IN FISCHER-TROPSCH SYNTHESIS 有权
标题翻译： PROCEDURE用于金属钴，钌和铝的从废催化剂CO RU / Al2O3的AT费 - 托工艺完全恢复
公开(公告)号：EP2824200A1
公开(公告)日：2015-01-14
申请号：EP13758445.4
申请日：2013-03-04
申请人： Sunshine Kaidi New Energy Group Co., Ltd.
发明人： LIU, Qianqian , HAN, Yiming , SONG, Dechen , XU, Li , LAI, Bo
IPC分类号： C22B7/00
CPC分类号： C22B23/0446 , C01F7/142 , C01G51/00 , C01G51/04 , C01G55/004 , C01G55/005 , C01P2006/80 , C22B7/00 , C22B7/009 , C22B11/026 , C22B11/04 , C22B11/048 , C22B11/06 , C22B21/003 , C22B21/02 , C22B23/00 , C22B23/026 , Y02P10/214 , Y02P10/218 , Y02P10/224 , Y02P10/234 , Y02P20/129 , Y02P20/142
摘要： Provided is a process for the comprehensive recovery of metal cobalt, ruthenium and aluminum from a waste catalyst Co-Ru/Al 2 O 3 in a Fischer-Tropsch synthesis. First, a waste catalyst is subjected to hydrocarbon removal, and reduction treatment, to effectively separate a cobalt slag in an alkali fusion step, and then the cobalt slag is subjected to the steps of acid leaching, cobalt precipitation with oxalic acid or ammonium oxalate, reduction of cobalt oxalate, dissolution of metal cobalt with nitric acid, etc., to obtain Co(N0 3 ) 2 ·6H 2 O. A ruthenate which is dissolved by steps such as alkali fusion, and leaching with deionized water, is subjected to the steps of reduction with ethanol, dissolution with concentrated hydrochloric acid, distillation under reduced pressure, etc., to obtain a β-RuCl 3 ·xH 2 O product with a high purity. Aluminum hydroxide is prepared from a meta-aluminate solution by CO 2 carbonation, by controlling the parameters such as reaction temperature, flow rate of CO 2 , pH value at the end point of the reaction, etc., and the aluminum hydroxide is calcined to obtain aluminum oxide with a product quality achieving the quality requirements of first-class aluminum oxide in the Chinese national standard. The resulting product has a high yield, wherein cobalt is ≥ 97%, ruthenium is ≥ 95%, and aluminum is ≥ 92%.
摘要翻译：本发明提供用于从废催化剂共同的Ru /的Al 2 O 3在费 - 托合成金属钴，钌和铝的综合回收的方法。首先，将废弃物催化剂进行烃脱除，和还原处理，在超过碱熔步骤有效地分离钴炉渣，然后将钴炉渣进行酸浸出，钴沉淀的步骤用草酸或草酸铵，减少草酸盐的钴，金属钴溶解用硝酸等，以获得的Co（NO 3）2·6H 2 O的钌所有这是由溶解的步骤：如碱熔，并与去离子水沥滤，进行在减压下等，还原用乙醇，溶解，用浓盐酸，蒸馏的步骤，以得到一个²-的RuCl 3·XH 2 O产物具有高纯度。氢氧化铝是由偏铝溶液通过CO 2碳酸化制备，通过控制参数：如反应温度，流量的CO 2的速率，在反应中，等，且氢氧化铝的终点PH值煅烧以获得与产品质量实现一流的氧化铝在中国国家标准的质量要求氧化铝。所得到的产品具有高的产率，worin钴是‰¥97％，钌是‰¥95％，铝是‰¥92％。

3. 发明授权

EP2824200B1 PROCESS FOR THE COMPREHENSIVE RECOVERY OF METAL COBALT, RUTHENIUM AND ALUMINUM FROM WASTE CATALYST CO-RU/AL2O3 IN FISCHER-TROPSCH SYNTHESIS 有权
标题翻译： Fischer-TrOPSCH合成法从废催化剂CO-RU / AL2O3中综合回收金属钴，钌和铝的方法
公开(公告)号：EP2824200B1
公开(公告)日：2018-05-16
申请号：EP13758445.4
申请日：2013-03-04
申请人： Sunshine Kaidi New Energy Group Co., Ltd.
发明人： LIU, Qianqian , HAN, Yiming , SONG, Dechen , XU, Li , LAI, Bo
IPC分类号： C22B7/00
CPC分类号： C22B23/0446 , C01F7/142 , C01G51/00 , C01G51/04 , C01G55/004 , C01G55/005 , C01P2006/80 , C22B7/00 , C22B7/009 , C22B11/026 , C22B11/04 , C22B11/048 , C22B11/06 , C22B21/003 , C22B21/02 , C22B23/00 , C22B23/026 , Y02P10/214 , Y02P10/218 , Y02P10/224 , Y02P10/234 , Y02P20/129 , Y02P20/142
摘要： Provided is a process for the comprehensive recovery of metal cobalt, ruthenium and aluminum from a waste catalyst Co-Ru/Al 2 O 3 in a Fischer-Tropsch synthesis. First, a waste catalyst is subjected to hydrocarbon removal, and reduction treatment, to effectively separate a cobalt slag in an alkali fusion step, and then the cobalt slag is subjected to the steps of acid leaching, cobalt precipitation with oxalic acid or ammonium oxalate, reduction of cobalt oxalate, dissolution of metal cobalt with nitric acid, etc., to obtain Co(N0 3 ) 2 ·6H 2 O. A ruthenate which is dissolved by steps such as alkali fusion, and leaching with deionized water, is subjected to the steps of reduction with ethanol, dissolution with concentrated hydrochloric acid, distillation under reduced pressure, etc., to obtain a ²-RuCl 3 ·xH 2 O product with a high purity. Aluminum hydroxide is prepared from a meta-aluminate solution by CO 2 carbonation, by controlling the parameters such as reaction temperature, flow rate of CO 2 , pH value at the end point of the reaction, etc., and the aluminum hydroxide is calcined to obtain aluminum oxide with a product quality achieving the quality requirements of first-class aluminum oxide in the Chinese national standard. The resulting product has a high yield, wherein cobalt is ‰¥ 97%, ruthenium is ‰¥ 95%, and aluminum is ‰¥ 92%.

4. 发明公开

EP2823900A1 METHOD FOR PREPARING SOLID NITROSYL RUTHENIUM NITRATE BY USING WASTE CATALYST CONTAINING RUTHENIUM 有权
标题翻译： VERFAHREN ZUR HERSTELLUNG VON FESTEM NITROSYL-RUTHENIUM-NITRAT MITTELS EINES RENHENIUMHALTIGEN ABFALLKATALYSATORS
公开(公告)号：EP2823900A1
公开(公告)日：2015-01-14
申请号：EP13758228.4
申请日：2013-03-04
申请人： Sunshine Kaidi New Energy Group Co., Ltd.
发明人： XU, Li , LAI, Bo , SONG, Dechen , LIU, Qianqian , HAN, Yiming
IPC分类号： B09B3/00 , C01G55/00
CPC分类号： C22B11/048 , C01G55/00 , C01P2006/80 , C22B1/005 , C22B7/009 , Y02P10/214 , Y02P10/234
摘要： Disclosed is a method for preparing solid nitrosyl ruthenium nitrate by using a waste catalyst containing ruthenium. Steps of the method are: drying and calcining a waste catalyst containing ruthenium to acquire a black solid containing ruthenium, grinding the black solid containing ruthenium into powder, feeding hydrogen for reduction to form metal ruthenium, oxidizing metal ruthenium by using mixed gas of ozone and air to produce a ruthenium tetra oxide gas, collecting the gas, feeding the gas in a nitric acid solution, adding solid sodium nitrite to prepare a solution containing nitrosyl ruthenium nitrate, and finally using diethyl ether for extraction, and evaporating diethyl ether to acquire a nitrosyl ruthenium nitrate solid. The method can effectively reclaim noble metal ruthenium in various load-type waste catalysts containing ruthenium, so as to achieve effective recycling of ruthenium resources, and has simple operation steps and does not involve the introduction of ruthenium intermediates, which ensures a high product yield. The acquired solid nitrosyl ruthenium nitrate is free of halogen, has high purity, and is capable of being directly applied to the preparation of catalysts.
摘要翻译：公开了通过使用含有钌的废催化剂制备固体亚硝酰钌硝酸盐的方法。该方法的步骤是：干燥和煅烧含钌的废催化剂以获得含有钌的黑色固体，将含有钌的黑色固体粉碎成粉末，将氢气还原以形成金属钌，通过使用臭氧的混合气体氧化金属钌空气中生成四氧化钌四氧化物气体，收集气体，在硝酸溶液中加入气体，加入固体亚硝酸钠，制备含有硝酰基硝酸钌的溶液，最后用乙醚萃取，蒸发乙醚，得到亚硝酰硝酸钌固体。该方法可以有效地回收含有钌的各种载荷型废催化剂中的贵金属钌，从而实现钌资源的有效再循环，操作步骤简单，不需要引入钌中间体，确保了高的产率。获得的固体亚硝酰硝酸钌不含卤素，具有高纯度，并且能够直接用于催化剂的制备。

5. 发明公开

EP2823888A1 SURFACE MODIFICATION METHOD OF ALUMINUM OXIDE CARRIER 有权
标题翻译：氧化铝载体的表面改性方法
公开(公告)号：EP2823888A1
公开(公告)日：2015-01-14
申请号：EP13758344.9
申请日：2013-03-04
申请人： Sunshine Kaidi New Energy Group Co., Ltd.
发明人： ZHENG, Shenke , SONG, Dechen , ZHAN, Xiaodong
IPC分类号： B01J32/00
CPC分类号： B01J21/04 , B01J35/023 , B01J35/1014 , B01J35/1038 , B01J35/1042 , B01J35/1061 , C01F7/021 , C01P2004/61 , C01P2006/12 , C01P2006/14 , C01P2006/16 , C01P2006/90
摘要： Disclosed is a surface modification method of an aluminum oxide carrier. The method sequentially comprises the following steps: 1) dissolving soluble kazoe into deionized water and preparing it into a kazoe aqueous solution; 2) soaking an aluminum oxide carrier into the kazoe aqueous solution and performing vacuum drying; 3) placing the dried aluminum oxide carrier into a reaction vessel, adding silicon tetrachloride, adding a Grignard reagent drop wise, sealing the reaction vessel, heating, and reacting at constant temperature for 3 to 18 hours, wherein the volume ratio of the added silicon tetrachloride to the aluminum oxide carrier is controlled to be (0.5 - 5) to 1 and the heating temperature of the reaction vessel is controlled to be 160°C to 350°C; and 4) cooling the reaction vessel, filtering the aluminum oxide carrier, washing and performing vacuum drying again to obtain the surface modified aluminum oxide carrier. Practice shows that by adopting the method, a compact silicon nitride layer can be synthesized on the surface of the aluminum oxide carrier under mild reaction conditions and the performance of the aluminum oxide carrier can be improved in multiple aspects.
摘要翻译：公开了一种氧化铝载体的表面改性方法。该方法依次包括以下步骤：1）将可溶性卡兹洛克溶解于去离子水中，并制备成卡唑水溶液; 2）将氧化铝载体浸入kazoe水溶液中并进行真空干燥; 3）将干燥后的氧化铝载体放入反应釜中，加入四氯化硅，滴加格氏试剂，密封反应釜，加热，恒温反应3-18小时，其中加入的硅的体积比控制四氯化铝与氧化铝载体的摩尔比为（0.5-5）至1，并将反应容器的加热温度控制在160℃至350℃; 和4）冷却反应容器，过滤氧化铝载体，洗涤并再次真空干燥以获得表面改性的氧化铝载体。实践证明，采用该方法，可以在温和的反应条件下，在氧化铝载体表面合成致密的氮化硅层，从多方面提高氧化铝载体的性能。

6. 发明授权

EP2823900B1 METHOD FOR PREPARING SOLID NITROSYL RUTHENIUM NITRATE BY USING WASTE CATALYST CONTAINING RUTHENIUM 有权
标题翻译：使用含钌废弃催化剂制备固体硝酸铯硝酸钌的方法
公开(公告)号：EP2823900B1
公开(公告)日：2017-05-17
申请号：EP13758228.4
申请日：2013-03-04
申请人： Sunshine Kaidi New Energy Group Co., Ltd.
发明人： XU, Li , LAI, Bo , SONG, Dechen , LIU, Qianqian , HAN, Yiming
IPC分类号： C01G55/00 , B09B3/00 , C22B1/00 , C22B7/00
CPC分类号： C22B11/048 , C01G55/00 , C01P2006/80 , C22B1/005 , C22B7/009 , Y02P10/214 , Y02P10/234

7. 发明公开

EP2843031A1 GAS-STEAM EFFICIENT COGENERATION PROCESS AND SYSTEM BASED ON BIOMASS GASIFICATION AND METHANATION 审中-公开
标题翻译：燃烧气体吸入器 - 燃烧器 - 宇宙飞行器
公开(公告)号：EP2843031A1
公开(公告)日：2015-03-04
申请号：EP13781061.0
申请日：2013-04-16
申请人： Sunshine Kaidi New Energy Group Co., Ltd.
发明人： YANG, Weiguang , GONG, Yan , ZHAN, Xiaodong , SONG, Dechen
IPC分类号： C10L3/08 , C10L3/10 , F22B1/18
CPC分类号： C10L3/08 , C10J3/82 , C10J3/86 , C10J2300/0916 , C10J2300/1662 , C10J2300/1687 , C10L2200/0469 , C10L2290/04 , C10L2290/06 , C10L2290/10 , C10L2290/42 , F22B1/18 , F22B27/14 , F22G1/02 , Y02E20/16 , Y02E20/18 , Y02E50/32
摘要： The present invention provides a gas-steam efficient cogeneration process and system based on biomass gasification and methanation, comprising a biomass gasification unit, a transformation unit, a purification unit, a methanation unit, and a methane concentration unit. The gasification unit utilizes a locally-external constant high-temperature heat source airflow bed which can remarkably improve effective gas compositions of CO and H2 and improve biomass gasification efficiency. The gasification unit can greatly reduce the quantity of tar produced at a high temperature, improves the carbon conversion rate, and removes investment on a tar removing device. In the process of methanation, the conversion efficiency of CO reaches 100%, and the conversion efficiency of H2 reaches 99%. Also, a large amount of by-product intermediate pressure superheated steam is produced, and power consumption of a circulation compressor in the traditional methanation reaction is reduced. The present invention has the advantages that biomass energy can be converted into clean, high-calorific-value, and convenient-for-use natural gas, and a large amount of heat released in the biomass gasification and methanation reaction can be efficiently recycled through a mode of producing high-quality superheated steam.
摘要翻译：本发明提供一种基于生物质气化和甲烷化的气体蒸汽高效热电联产方法和系统，其包括生物质气化单元，转化单元，纯化单元，甲烷化单元和甲烷浓缩单元。气化单元采用局部外部恒定的高温热源气流床，可显着提高CO和H2的有效气体组成，提高生物质气化效率。气化装置能大大减少在高温下产生的焦油量，提高碳转化率，消除焦油去除装置的投入。在甲烷化过程中，CO的转化效率达到100％，H2的转化效率达到99％。此外，产生大量的副产物中压过热蒸汽，并且减少了传统甲烷化反应中的循环压缩机的功率消耗。本发明具有将生物质能转化为清洁，高热值，方便使用的天然气的优点，生物质气化和甲烷化反应中释放的大量热量可以通过生产高品质过热蒸汽的方式。

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