生物柴油磁性固体催化剂的制备及评价
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摘要
目前生物柴油产业技术为液体催化工艺,存在设备腐蚀、工艺复杂、环境污染等问题,固体催化技术是解决的有效途径已成为研究的热点,但催化剂回收工艺复杂、不彻底,磁性固体催化剂不仅有固体催化剂的优点,而且具有易回收、反应操作简便等优点,本文对磁性固体催化剂进行了研究,主要内容和结果如下:
1、用共沉淀法制备出比饱和磁化强度为70.11emu/g的磁核,并创新性地将磁核引入本实验室筛选并优化的固体催化剂中,使其中的载体SiO_2兼备负载活性成分与保护磁核的作用,所得催化剂用磁场可简单高效回收。研究确定了催化剂制备工艺为:溶胶中超声分散磁核→凝胶→陈化→抽滤→真空干燥→研磨→预湿→浸渍→真空干燥→煅烧。
2、采用单因素实验和正交实验研究了磁性固体催化剂制备工艺,确定最佳条件为:Si/Fe摩尔比2,陈化温度65℃,陈化时间3h,K/Si摩尔比为1.5,煅烧温度450℃,煅烧时间3h。红外、X-衍射、振动样品磁强计、扫描电镜表征催化剂组成为K_2CO_3/SiO_2-Fe_3O_4,其中SiO_2和K_2CO_3均为无定形结构,比饱和磁化强度为4.18 emu/g,催化剂表面烧结,内部包有磁性载体小颗粒。
3、通过单因素和正交实验确定磁性固体催化剂催化制备生物柴油的最佳反应条件为:催化剂加入量10%,醇油比12,反应温度65℃,反应时间40min,搅拌速度400r/min。在此条件下,第一批次反应的相对转化率为105.48%,第二批次为99.50%,磁性固体催化剂可重复使用。通过煅烧再生,催化剂可进一步延长使用。
At present, liguid catalyst is mainly utilized in biodiesel industry, but there are problems such as equipment corrosion, environment pollution and complex process. Biodiesl solid catalyst is becoming more and more important because it is an effective way to solve these problems. However, solid catalyst is hard to be recycled completely with complex technology. Magnetic solid catalyst not only has advantages of the solid catalyst but also is easy to be recycled and operated. In this dissertation, magnetic solid catalyst was prepared, and the main content and results were as follows:
1. Magnetic core was prepared with co-precipitation method and its Specific Saturation Magnetization reached 70.11 emu/g. This magnetic core was innovativly introduced into the catalyst made in our lab. So the carrier SiO_2 of this catalyst could play two roles: loading active component and protectiong magnetic core. The magnetic solid catalyt could be recycled easily and efficiently. The process to prepare the catalyst was confirmed as follows: dispersing the magnetic core in sol with ultrasonic method→forming gel→aging→filtrating gel in vacuum→drying in vocuum→crushing→prewetting—"-impregnating—* drying in vocuum→calcining.
2. Single factor and orthogonal experiment were applied to research the process to prepare magnetic solid catalyst, and finally the optimal conditions were confirmed as follows: Si/Fe molar ratio 2, aging temperature 65℃, aging time 3h, K/Si molar ratio 1.5, calcining temperature 450℃, calcining time 3h. By characterization with Infrared Ray, X-ray Diffraction, Vibrating Sample Magnetometer, Scanning Electron Micrographs, it was found that the component of the catalyst was K_2CO_3/SiO_2-Fei_3O_4 therein SiO_2 and K_2CO_3 were both amorphous structure, the Specific Saturation Magnetization value of magnetic solid catalyst was 4.18 emu/g and the surface of the catalyst was sintered, but there were small particles of magnetic carrier under the surface.
3. By single factor and orthogonal experiment, the reaction conditions to procduce biodiesel with magnetic solid catalyst were optimized as follows: catalyst dose 10%, molar ratio of methonal to oil 12, reaction temperature 65℃, reaction time 40 min, and stirring speed 400r/min. Under the optimal conditions, the comparative conversion was 105.48% in the first reaction, 99.50% in the second reaction. The magnetic solid catalyst could be reused; moreover it could be regenerated to prolong its application by calcining.
1、用共沉淀法制备出比饱和磁化强度为70.11emu/g的磁核,并创新性地将磁核引入本实验室筛选并优化的固体催化剂中,使其中的载体SiO_2兼备负载活性成分与保护磁核的作用,所得催化剂用磁场可简单高效回收。研究确定了催化剂制备工艺为:溶胶中超声分散磁核→凝胶→陈化→抽滤→真空干燥→研磨→预湿→浸渍→真空干燥→煅烧。
2、采用单因素实验和正交实验研究了磁性固体催化剂制备工艺,确定最佳条件为:Si/Fe摩尔比2,陈化温度65℃,陈化时间3h,K/Si摩尔比为1.5,煅烧温度450℃,煅烧时间3h。红外、X-衍射、振动样品磁强计、扫描电镜表征催化剂组成为K_2CO_3/SiO_2-Fe_3O_4,其中SiO_2和K_2CO_3均为无定形结构,比饱和磁化强度为4.18 emu/g,催化剂表面烧结,内部包有磁性载体小颗粒。
3、通过单因素和正交实验确定磁性固体催化剂催化制备生物柴油的最佳反应条件为:催化剂加入量10%,醇油比12,反应温度65℃,反应时间40min,搅拌速度400r/min。在此条件下,第一批次反应的相对转化率为105.48%,第二批次为99.50%,磁性固体催化剂可重复使用。通过煅烧再生,催化剂可进一步延长使用。
At present, liguid catalyst is mainly utilized in biodiesel industry, but there are problems such as equipment corrosion, environment pollution and complex process. Biodiesl solid catalyst is becoming more and more important because it is an effective way to solve these problems. However, solid catalyst is hard to be recycled completely with complex technology. Magnetic solid catalyst not only has advantages of the solid catalyst but also is easy to be recycled and operated. In this dissertation, magnetic solid catalyst was prepared, and the main content and results were as follows:
1. Magnetic core was prepared with co-precipitation method and its Specific Saturation Magnetization reached 70.11 emu/g. This magnetic core was innovativly introduced into the catalyst made in our lab. So the carrier SiO_2 of this catalyst could play two roles: loading active component and protectiong magnetic core. The magnetic solid catalyt could be recycled easily and efficiently. The process to prepare the catalyst was confirmed as follows: dispersing the magnetic core in sol with ultrasonic method→forming gel→aging→filtrating gel in vacuum→drying in vocuum→crushing→prewetting—"-impregnating—* drying in vocuum→calcining.
2. Single factor and orthogonal experiment were applied to research the process to prepare magnetic solid catalyst, and finally the optimal conditions were confirmed as follows: Si/Fe molar ratio 2, aging temperature 65℃, aging time 3h, K/Si molar ratio 1.5, calcining temperature 450℃, calcining time 3h. By characterization with Infrared Ray, X-ray Diffraction, Vibrating Sample Magnetometer, Scanning Electron Micrographs, it was found that the component of the catalyst was K_2CO_3/SiO_2-Fei_3O_4 therein SiO_2 and K_2CO_3 were both amorphous structure, the Specific Saturation Magnetization value of magnetic solid catalyst was 4.18 emu/g and the surface of the catalyst was sintered, but there were small particles of magnetic carrier under the surface.
3. By single factor and orthogonal experiment, the reaction conditions to procduce biodiesel with magnetic solid catalyst were optimized as follows: catalyst dose 10%, molar ratio of methonal to oil 12, reaction temperature 65℃, reaction time 40 min, and stirring speed 400r/min. Under the optimal conditions, the comparative conversion was 105.48% in the first reaction, 99.50% in the second reaction. The magnetic solid catalyst could be reused; moreover it could be regenerated to prolong its application by calcining.
引文
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