CN107649113A - 一种带有氧化石墨烯的催化剂 - Google Patents

一种带有氧化石墨烯的催化剂 Download PDF

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CN107649113A
CN107649113A CN201710991640.7A CN201710991640A CN107649113A CN 107649113 A CN107649113 A CN 107649113A CN 201710991640 A CN201710991640 A CN 201710991640A CN 107649113 A CN107649113 A CN 107649113A
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朱洋
邵蓉
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Nanjing Xuyurui Material Technology Co Ltd
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/0009Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/34Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
    • B01J37/341Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
    • B01J37/343Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
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    • C07DHETEROCYCLIC COMPOUNDS
    • C07D307/00Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
    • C07D307/02Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
    • C07D307/34Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
    • C07D307/38Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with substituted hydrocarbon radicals attached to ring carbon atoms
    • C07D307/40Radicals substituted by oxygen atoms
    • C07D307/46Doubly bound oxygen atoms, or two oxygen atoms singly bound to the same carbon atom
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Abstract

本发明公开了本发明公开了一种带有氧化石墨烯的催化剂,包括如下步骤:(1)通过化学法制得氧化石墨烯,并将氧化石墨均匀加入到乙醇中,利用超声搅拌0.5‑4小时,形成氧化石墨悬浊液,并放置备用;(2)将四氧化三铁研磨0.5‑1小时,并加入到稀硝酸中,并加以搅拌,(3)将步骤(1)得到的氧化石墨悬浊液逐滴加入到步骤(2)所得的四氧化三铁悬浊液中;(4)将步骤(3)所得的溶液静置3‑5小时,并过滤掉上层溶液;(5)然后在真空条件下,将步骤(4)所得到的颗粒进行干燥,得到固体物质;(6)将固体物质研磨0.5‑1小时即可得到所需物质,该催化剂具有较高的催化活性,具有良好的磁性,有利于后期催化剂的分离回收以及重复使用。

Description

一种带有氧化石墨烯的催化剂
技术领域
本发明涉及石墨烯技术领域,具体为一种带有氧化石墨烯的催化剂。
背景技术
石墨烯的复合材料是石墨烯和其衍生物应用领域中的重要研究方向,其在能量储存、液品器件、电子器件、生物材料、传感材料和催化剂载体等领域展现出了优良性能,具有广問的应用前景。目前石墨烯复合材料的研究主要集中在石墨烯聚合物复合材料和石墨烯基无机纳米复合材料上,而随着对石墨烯研究的深入,石墨烯增强体在块体金属基复合材料中的应用也越来越受到人们的重视。石墨烯作为一种新型碳材料,由于其高比表面积、易分散、易于功能化和化学环境稳定性高等特点,在催化体系中得到了广泛的关注。
生物质是替代化石资源生产化学品与液体燃料的有机碳资源的重要来源,具有可再生的优势。研究将生物质转化为液体燃料和化学品的新方法和新技术,对于实现社会的可持续发展、缓解环境压力等具有非常重要的意义。生物质可经热化学转化、生物技术转化以及催化转化等途径制备生物燃料。其中,催化转化方法的应用为低能耗、高效率的生物质转化提供了一条可能的技术路线。
碳水化合物是自然界中储量最为丰富的生物质原料,经酸催化脱水可生成重要的平台化合物——糠醛。糠醛是由木糖,即半纤维素主要成分制备的一种可再生、绿色的化工产品,具有多种用途。
目前对糠醛制备的研究中不再用均相体系中的无机酸如水、有机溶剂以及离子液体,而是用无机盐如卤代盐、金属氧化物以及固体酸等来取代。虽然在糠醛的工业生产中,均相体系更加经济和环保,但是由于糠醛进一步的降解和糠醛自身及与木糖的连续反应产生低聚物而使效率降低。现有技术中糠醛的制作方法存在着腐蚀与污染严重、分离与循环利用困难、反应时间周期长等缺点,因此绿色廉价高效的催化剂和适用于糠醛制备的溶剂体系很有必要。
发明内容
本发明的目的在于提供一种带有氧化石墨烯的催化剂,以解决上述背景技术中提出的问题。
为实现上述目的,本发明提供如下技术方案:本发明公开了一种带有氧化石墨烯的催化剂,其特征在于,包括如下步骤:
(1)通过化学法制得氧化石墨烯,并将氧化石墨均匀加入到乙醇中,利用超声搅拌0.5-4小时,形成氧化石墨悬浊液,并放置备用;
(2)将四氧化三铁研磨0.5-1小时,并按照摩尔质量比为1:9加入到稀硝酸中,并加以搅拌,得到四氧化三铁悬浊液;
(3)将步骤(1)得到的氧化石墨悬浊液在30-50℃的条件下逐滴加入到步骤(2)所得的四氧化三铁悬浊液中,每次滴加间隔2-4秒,并高速搅拌;
(4)将步骤(3)所得的溶液静置3-5小时,并过滤掉上层溶液;
(5)然后在真空条件下,将步骤(4)所得到的颗粒进行干燥,得到固体物质;
(6)将固体物质研磨0.5-1小时即可得到所需物质。
优选的,所述乙醇为无水乙醇。
优选的,所述步骤(3)中的搅拌速度为500-1500r/min。
优选的,所述步骤(1)氧化石墨烯与乙醇的比例为1:2。
优选的,所述氧化石墨烯通过改进的Hummers法制得。
与现有技术相比,本发明的有益效果是:该一种带有氧化石墨烯的催化剂,所需原料易得,制备成本较低, 采用本发明方法合成出的磁性粒子形貌均一,分布均匀,具有较高的催化活性,具有良好的磁性,有利于后期催化剂的分离回收以及重复使用。
具体实施方式
下面将结合本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
本发明提供一种技术方案:本发明公开了一种带有氧化石墨烯的催化剂,其特征在于,包括如下步骤:
(1)通过化学法制得氧化石墨烯,并将氧化石墨均匀加入到乙醇中,利用超声搅拌0.5-4小时,形成氧化石墨悬浊液,并放置备用;
(2)将四氧化三铁研磨0.5-1小时,并按照摩尔质量比为1:9加入到稀硝酸中,并加以搅拌,得到四氧化三铁悬浊液;
(3)将步骤(1)得到的氧化石墨悬浊液在30-50℃的条件下逐滴加入到步骤(2)所得的四氧化三铁悬浊液中,每次滴加间隔2-4秒,并高速搅拌;
(4)将步骤(3)所得的溶液静置3-5小时,并过滤掉上层溶液;
(5)然后在真空条件下,将步骤(4)所得到的颗粒进行干燥,得到固体物质;
(6)将固体物质研磨0.5-1小时即可得到所需物质。
优选的,所述乙醇为无水乙醇。
优选的,所述步骤(3)中的搅拌速度为500-1500r/min。
优选的,所述步骤(1)氧化石墨烯与乙醇的比例为1:2。
优选的,所述氧化石墨烯通过改进的Hummers法制得。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。

Claims (5)

1.本发明公开了一种带有氧化石墨烯的催化剂,其特征在于,包括如下步骤:
(1)通过化学法制得氧化石墨烯,并将氧化石墨均匀加入到乙醇中,利用超声搅拌0.5-4小时,形成氧化石墨悬浊液,并放置备用;
(2)将四氧化三铁研磨0.5-1小时,并按照摩尔质量比为1:9加入到稀硝酸中,并加以搅拌,得到四氧化三铁悬浊液;
(3)将步骤(1)得到的氧化石墨悬浊液在30-50℃的条件下逐滴加入到步骤(2)所得的四氧化三铁悬浊液中,每次滴加间隔2-4秒,并高速搅拌;
(4)将步骤(3)所得的溶液静置3-5小时,并过滤掉上层溶液;
(5)然后在真空条件下,将步骤(4)所得到的颗粒进行干燥,得到固体物质;
(6)将固体物质研磨0.5-1小时即可得到所需物质。
2.根据权利要求1所述的一种带有氧化石墨烯的催化剂,其特征在于:所述乙醇为无水乙醇。
3.根据权利要求1所述的一种带有氧化石墨烯的催化剂,其特征在于:所述步骤(3)中的搅拌速度为500-1500r/min。
4.根据权利要求1所述的一种带有氧化石墨烯的催化剂,其特征在于:所述步骤(1)氧化石墨烯与乙醇的比例为1:2。
5.根据权利要求1所述的一种带有氧化石墨烯的催化剂,其特征在于:所述氧化石墨烯通过改进的Hummers法制得。
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CN109111361A (zh) * 2018-10-08 2019-01-01 扬州工业职业技术学院 一种一步法高效制备十二烷基二酸单叔丁酯的方法
CN109134257A (zh) * 2018-10-08 2019-01-04 扬州工业职业技术学院 一种两步法制备高纯度十二烷基二酸单叔丁酯的方法
CN109248687A (zh) * 2018-10-08 2019-01-22 扬州工业职业技术学院 一种新型石墨烯/四氧化三铁复合纳米材料及其在催化制备十二烷基二酸单叔丁酯中的应用
CN111777063A (zh) * 2020-07-09 2020-10-16 西安交通大学 一种纳米材料的制备方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109111361A (zh) * 2018-10-08 2019-01-01 扬州工业职业技术学院 一种一步法高效制备十二烷基二酸单叔丁酯的方法
CN109134257A (zh) * 2018-10-08 2019-01-04 扬州工业职业技术学院 一种两步法制备高纯度十二烷基二酸单叔丁酯的方法
CN109248687A (zh) * 2018-10-08 2019-01-22 扬州工业职业技术学院 一种新型石墨烯/四氧化三铁复合纳米材料及其在催化制备十二烷基二酸单叔丁酯中的应用
CN111777063A (zh) * 2020-07-09 2020-10-16 西安交通大学 一种纳米材料的制备方法

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