WO2021072635A1 - Method for preparing rod-shaped ferrous chloride nano-material - Google Patents

Method for preparing rod-shaped ferrous chloride nano-material Download PDF

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WO2021072635A1
WO2021072635A1 PCT/CN2019/111255 CN2019111255W WO2021072635A1 WO 2021072635 A1 WO2021072635 A1 WO 2021072635A1 CN 2019111255 W CN2019111255 W CN 2019111255W WO 2021072635 A1 WO2021072635 A1 WO 2021072635A1
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shaped
rod
deionized water
fecl2
precipitate
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PCT/CN2019/111255
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何洪波
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诸暨易联众创企业管理服务有限公司
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Priority to PCT/CN2019/111255 priority Critical patent/WO2021072635A1/en
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/10—Halides

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  • the invention belongs to the technical field of preparation of inorganic compound new energy materials, and relates to a preparation method of a photocatalytic material rod-shaped FeCl2 nano material.
  • the purpose of the present invention is to use sodium chloride, iron acetate, dimethyl sulfoxide (DMSO) and polyvinylpyrrolidone (PVP) as raw materials to provide a rod-shaped FeCl2 with simple operation, high yield, low cost, and environmental protection.
  • the preparation method of nanomaterials includes the following steps:
  • the first step is to dissolve 50-100mg PVP (MW5800) and 45mg sodium chloride in a mixed solvent of dimethyl sulfoxide/deionized water (30mL, 10/20, V/V) at room temperature to obtain a colorless and transparent Solution
  • the colorless and transparent solution obtained in the first step was stirred at 60°C for 30 minutes, and then 8-12ml of iron acetate aqueous solution (5mg/ml) was slowly added dropwise to it, and stirred at 60°C for 30 minutes;
  • the third step put the solution obtained in the second step into a 45mL polytetrafluoroethylene-lined stainless steel reactor, and hydrothermally react at 130°C in an oven for more than 2-14 hours. After the system is naturally cooled, a precipitate is obtained;
  • the precipitate is separated from the solution using a centrifuge.
  • the precipitate is washed with deionized water to remove excess reactants, and then washed with absolute ethanol. After multiple washings and centrifugation, The precipitate is dried in a vacuum oven at 60° C. to obtain a yellow solid, that is, the rod-shaped FeCl 2 nano material prepared in the present invention.
  • the solutions used are all prepared under conventional conditions, such as those prepared by dissolving substances in an aqueous solution at room temperature.
  • the adopted devices, instruments, equipment, materials, processes, methods, steps, preparation conditions, etc. are all conventionally used in the field or those of ordinary skill in the art are conventionally used in the field. Technology can be easily obtained.
  • the present invention Compared with the existing chemical methods for preparing rod-shaped FeCl2 nanomaterials, the present invention has the following advantages:
  • the first step is to dissolve 54mg PVP (MW5800) and 45mg sodium chloride in a mixed solvent of dimethyl sulfoxide/deionized water (30mL, 10/20, V/V) at room temperature to obtain a colorless and transparent solution.
  • the colorless and transparent solution was stirred at 60°C for 30 minutes, and then 10 mL of a 5mg/mL iron acetate aqueous solution was slowly added dropwise to it, and stirred at 60°C for 30 minutes.
  • the obtained solution was put into a 45mL polytetrafluoroethylene-lined stainless steel reaction kettle, and hydrothermally reacted in an oven at 130°C for 12 hours. After the system was naturally cooled, a precipitate was obtained.
  • the fourth step use a centrifuge to separate the solid precipitate from the solution.
  • the precipitate is first washed with deionized water to remove excess impurities, and then washed with absolute ethanol. After multiple washings and centrifugation, the precipitate Dry in a vacuum oven at 60°C to obtain rod-shaped FeCl2 nanomaterials.
  • the colorless and transparent solution was stirred at 60°C for 30 minutes, and then 10 mL of a 5mg/mL iron acetate aqueous solution was slowly added dropwise to it, and stirred at 60°C for 30 minutes.
  • the obtained solution into a 45mL polytetrafluoroethylene-lined stainless steel reactor, and hydrothermally react in an oven at 130°C for 2 hours, and wait for the system to cool naturally.
  • the fourth step is to use a centrifuge to separate the product from the solution.
  • the product is washed with deionized water and then with absolute ethanol. After washing and centrifugation for many times, the precipitate is placed in a vacuum oven at 60°C. After drying, a rod-shaped FeCl2 nano material is obtained.
  • the first step is to dissolve 50mg PVP (MW5800) and 45mg sodium chloride in a mixed solvent of dimethyl sulfoxide/deionized water (30mL, 10/20, V/V) at room temperature to obtain a colorless and transparent solution.
  • the colorless and transparent solution was stirred at 60°C for 30 minutes, and then 8 mL of 5 mg/mL iron acetate aqueous solution was slowly added dropwise to it, and stirred at 60°C for 30 minutes.
  • the obtained solution was put into a 45mL polytetrafluoroethylene-lined stainless steel reactor, and hydrothermally reacted in an oven at 130°C for 10 hours. After the system was naturally cooled, a precipitate was obtained.
  • the fourth step use a centrifuge to separate the solid precipitate from the solution.
  • the precipitate is first washed with deionized water to remove excess impurities, and then washed with absolute ethanol. After multiple washings and centrifugation, the precipitate Dry in a vacuum oven at 60°C to obtain rod-shaped FeCl2 nanomaterials.
  • the overall morphology of the obtained rod-shaped FeCl2 nanomaterial is a rod-shaped nanostructure with uniform size.
  • the rod-shaped FeCl2 nanomaterial is about 2-5 microns long and about 80-120 nanometers thick.
  • the first step is to dissolve 100mg PVP (MW5800) and 45mg sodium chloride in a mixed solvent of dimethyl sulfoxide/deionized water (30mL, 10/20, V/V) at room temperature to obtain a colorless and transparent solution.
  • the colorless and transparent solution was stirred at 60°C for 30 minutes, and then 12 mL of a 5 mg/mL iron acetate aqueous solution was slowly added dropwise to it, and stirred at 60°C for 30 minutes.
  • the obtained solution was put into a 45mL polytetrafluoroethylene-lined stainless steel reaction kettle, and hydrothermally reacted in an oven at 130°C for 12 hours. After the system was naturally cooled, a precipitate was obtained.
  • the fourth step use a centrifuge to separate the solid precipitate from the solution.
  • the precipitate is first washed with deionized water to remove excess impurities, and then washed with absolute ethanol. After multiple washings and centrifugation, the precipitate Dry in a vacuum oven at 60°C to obtain rod-shaped FeCl2 nanomaterials.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Compounds Of Iron (AREA)

Abstract

Disclosed is a method for preparing a rod-shaped FeCl2 nano-material. The present invention belongs to the technical field of the preparation of inorganic compound new energy materials. In the method, a rod-shaped FeCl2 nano-material is prepared using a hydrothermal method, with sodium chloride, iron acetate, dimethyl sulfoxide and polyvinylpyrrolidone as raw materials. The specific method involves dissolving polyvinylpyrrolidone and sodium chloride in a mixed solvent of dimethyl sulfoxide/deionized water at room temperature, and then slowly and dropwise adding an aqueous solution of iron acetate to produce a precursor; subjecting same to a hydrothermal reaction in a reaction kettle at 130°C for 2-14 hours; and after the reaction is completed, subjecting same to centrifugal separation, washing same many times with deionized water and absolute ethanol, and drying same to obtain the rod-shaped FeCl2 nano-material. The method has the advantages of being simple in terms of operation, and having a low raw material price, a high yield, etc.

Description

一种棒状氯化亚铁纳米材料的制备方法Method for preparing rod-shaped ferrous chloride nano material 技术领域Technical field
本发明属于无机化合物新能源材料制备技术领域，涉及一种光催化材料棒状FeCl2纳米材料的制备方法。The invention belongs to the technical field of preparation of inorganic compound new energy materials, and relates to a preparation method of a photocatalytic material rod-shaped FeCl2 nano material.
技术背景technical background
目前规则的卤化铁/Fe纳米结构的制备还比很少，对其规则形貌的制备以及研究其形貌对其性能的影响应该引起关注。At present, the preparation of regular iron halide/Fe nanostructures is still rare. The preparation of regular morphology and the study of the influence of its morphology on its performance should be paid attention to.
发明内容Summary of the invention
本发明的目的在于利用氯化钠、乙酸铁、二甲基亚砜(DMSO)和聚乙烯吡咯烷酮(PVP)等为原料，提供一种操作简单、产率高、成本低、绿色环保的棒状FeCl2纳米材料的制备方法，其包括如下步骤：The purpose of the present invention is to use sodium chloride, iron acetate, dimethyl sulfoxide (DMSO) and polyvinylpyrrolidone (PVP) as raw materials to provide a rod-shaped FeCl2 with simple operation, high yield, low cost, and environmental protection. The preparation method of nanomaterials includes the following steps:
第一步，室温下将50-100mgPVP(MW5800)和45mg氯化钠溶解在二甲基亚砜/去离子水的混合溶剂中(30mL，10/20,V/V),得到无色透明的溶液；The first step is to dissolve 50-100mg PVP (MW5800) and 45mg sodium chloride in a mixed solvent of dimethyl sulfoxide/deionized water (30mL, 10/20, V/V) at room temperature to obtain a colorless and transparent Solution
第二步，将第一步中得到的无色透明溶液在60℃搅拌30分钟，然后向其中缓慢滴加8-12ml的乙酸铁水溶液(5mg/ml)，保持60°C搅拌30分钟；In the second step, the colorless and transparent solution obtained in the first step was stirred at 60°C for 30 minutes, and then 8-12ml of iron acetate aqueous solution (5mg/ml) was slowly added dropwise to it, and stirred at 60°C for 30 minutes;
第三步，将第二步得到的溶液放入45mL聚四氟乙烯衬里不锈钢反应釜中，在烘箱中130℃水热反应2～14小时以上，待体系自然冷却，得到沉淀；In the third step, put the solution obtained in the second step into a 45mL polytetrafluoroethylene-lined stainless steel reactor, and hydrothermally react at 130°C in an oven for more than 2-14 hours. After the system is naturally cooled, a precipitate is obtained;
第四步，使用离心机将所述沉淀从溶液中分离出来，将所述沉淀先用去离子水洗涤以除去多余的反应物，再用无水乙醇洗涤，经过多次的洗涤、离心后，将沉淀在60℃真空烘箱中干燥，得到黄色固体，即本发明制备的棒状FeCl2纳米材料。In the fourth step, the precipitate is separated from the solution using a centrifuge. The precipitate is washed with deionized water to remove excess reactants, and then washed with absolute ethanol. After multiple washings and centrifugation, The precipitate is dried in a vacuum oven at 60° C. to obtain a yellow solid, that is, the rod-shaped FeCl 2 nano material prepared in the present invention.
在本发明中，如果没有特别地说明，所采用的溶液都是在常规条 件下制备的，比如在室温下将物质溶解在水溶液中制备得到的。In the present invention, unless otherwise specified, the solutions used are all prepared under conventional conditions, such as those prepared by dissolving substances in an aqueous solution at room temperature.
在本发明中，如果没有特别地说明，所采用的装置、仪器、设备、材料、工艺、方法、步骤、制备条件等都是本领域常规采用的或者本领域普通技术人员按照本领域常规采用的技术可以容易地获得的。In the present invention, unless otherwise specified, the adopted devices, instruments, equipment, materials, processes, methods, steps, preparation conditions, etc. are all conventionally used in the field or those of ordinary skill in the art are conventionally used in the field. Technology can be easily obtained.
相比于现有制备棒状FeCl2纳米材料的化学方法，本发明具有如下优点：Compared with the existing chemical methods for preparing rod-shaped FeCl2 nanomaterials, the present invention has the following advantages:
实际上，现有制备FeCl2规则形貌的方法很少，以贵金属Fe单质为原料，不仅价格昂贵，而且很有局限性，所长出来的一维纳米线只能在Fe基底上，产率低而没法广泛使用。而本发明提供的方法是以乙酸铁为原料，价格低廉，操作简单。而且本发明得到的产物是粉末状，产量高，可以广泛使用。In fact, there are few existing methods for preparing FeCl2 with regular morphology. Using precious metal Fe as raw material is not only expensive, but also very limited. The one-dimensional nanowires that can be grown can only be on Fe substrates, and the yield is low. It cannot be widely used. The method provided by the present invention uses ferric acetate as a raw material, has low price and simple operation. Moreover, the product obtained by the present invention is in powder form, has high yield, and can be widely used.
具体实施方式Detailed ways
下面结合实施例来具体地说明棒状FeCl2纳米材料的制备方法，但应当理解，这些实施例仅仅用于阐述本发明，而并不以任何方式限制本发明的保护范围。The following examples are used to specifically describe the preparation method of the rod-shaped FeCl2 nanomaterials, but it should be understood that these examples are only used to illustrate the present invention, and do not limit the protection scope of the present invention in any way.
实施例1：Example 1:
采用本发明提供的方法制备棒状FeCl2纳米材料，具体步骤如下：Using the method provided by the present invention to prepare rod-shaped FeCl2 nanomaterials, the specific steps are as follows:
第一步，室温下将54mgPVP(MW5800)和45mg氯化钠溶解在二甲基亚砜/去离子水的混合溶剂中(30mL，10/20,V/V),得到无色透明的溶液，The first step is to dissolve 54mg PVP (MW5800) and 45mg sodium chloride in a mixed solvent of dimethyl sulfoxide/deionized water (30mL, 10/20, V/V) at room temperature to obtain a colorless and transparent solution.
第二步，将此无色透明溶液在60℃搅拌30分钟，然后向其中缓慢滴加5mg/mL的乙酸铁水溶液10mL，保持60℃搅拌30分钟，In the second step, the colorless and transparent solution was stirred at 60°C for 30 minutes, and then 10 mL of a 5mg/mL iron acetate aqueous solution was slowly added dropwise to it, and stirred at 60°C for 30 minutes.
第三步，将得到的溶液放入45mL聚四氟乙烯衬里不锈钢反应釜中，在烘箱中130℃水热反应12小时，待体系自然冷却，得到沉淀。In the third step, the obtained solution was put into a 45mL polytetrafluoroethylene-lined stainless steel reaction kettle, and hydrothermally reacted in an oven at 130°C for 12 hours. After the system was naturally cooled, a precipitate was obtained.
第四步，使用离心机将固体沉淀从溶液中分离出来，将所述沉淀 先用去离子水洗涤以除去多余的杂质，再用无水乙醇洗涤，经过多次的洗涤、离心后，将沉淀在60℃真空烘箱中干燥，得到棒状FeCl2纳米材料。In the fourth step, use a centrifuge to separate the solid precipitate from the solution. The precipitate is first washed with deionized water to remove excess impurities, and then washed with absolute ethanol. After multiple washings and centrifugation, the precipitate Dry in a vacuum oven at 60°C to obtain rod-shaped FeCl2 nanomaterials.
实施例2：Example 2:
第一步，室温下将54mgPVP(MW5800)和45mg氯化钠溶解在二甲基亚砜/去离子水的混合溶剂中(30mL，10/20,V/V),得到无色透明的溶液，In the first step, 54mg PVP (MW5800) and 45mg sodium chloride are dissolved in a mixed solvent of dimethyl sulfoxide/deionized water (30mL, 10/20, V/V) at room temperature to obtain a colorless and transparent solution.
第二步，将此无色透明溶液在60℃搅拌30分钟，然后向其中缓慢滴加5mg/mL的乙酸铁水溶液10mL，保持60℃搅拌30分钟，In the second step, the colorless and transparent solution was stirred at 60°C for 30 minutes, and then 10 mL of a 5mg/mL iron acetate aqueous solution was slowly added dropwise to it, and stirred at 60°C for 30 minutes.
第三步，将得到的溶液放入45mL聚四氟乙烯衬里不锈钢反应釜中，在烘箱中130℃水热反应2小时，待体系自然冷却。In the third step, put the obtained solution into a 45mL polytetrafluoroethylene-lined stainless steel reactor, and hydrothermally react in an oven at 130°C for 2 hours, and wait for the system to cool naturally.
第四步，使用离心机将产物从溶液中分离出来，将所述产物先用去离子水洗涤，再用无水乙醇洗涤，经过多次的洗涤、离心后，将沉淀在60℃真空烘箱中干燥，得到棒状FeCl2纳米材料。The fourth step is to use a centrifuge to separate the product from the solution. The product is washed with deionized water and then with absolute ethanol. After washing and centrifugation for many times, the precipitate is placed in a vacuum oven at 60°C. After drying, a rod-shaped FeCl2 nano material is obtained.
实施例3：Example 3:
采用本发明提供的方法制备棒状FeCl2纳米材料，具体步骤如下：Using the method provided by the present invention to prepare rod-shaped FeCl2 nanomaterials, the specific steps are as follows:
第一步，室温下将50mgPVP(MW5800)和45mg氯化钠溶解在二甲基亚砜/去离子水的混合溶剂中(30mL，10/20,V/V),得到无色透明的溶液，The first step is to dissolve 50mg PVP (MW5800) and 45mg sodium chloride in a mixed solvent of dimethyl sulfoxide/deionized water (30mL, 10/20, V/V) at room temperature to obtain a colorless and transparent solution.
第二步，将此无色透明溶液在60℃搅拌30分钟，然后向其中缓慢滴加5mg/mL的乙酸铁水溶液8mL，保持60℃搅拌30分钟，In the second step, the colorless and transparent solution was stirred at 60°C for 30 minutes, and then 8 mL of 5 mg/mL iron acetate aqueous solution was slowly added dropwise to it, and stirred at 60°C for 30 minutes.
第三步，将得到的溶液放入45mL聚四氟乙烯衬里不锈钢反应釜中，在烘箱中130℃水热反应10小时，待体系自然冷却，得到沉淀。In the third step, the obtained solution was put into a 45mL polytetrafluoroethylene-lined stainless steel reactor, and hydrothermally reacted in an oven at 130°C for 10 hours. After the system was naturally cooled, a precipitate was obtained.
第四步，使用离心机将固体沉淀从溶液中分离出来，将所述沉淀先用去离子水洗涤以除去多余的杂质，再用无水乙醇洗涤，经过多次 的洗涤、离心后，将沉淀在60℃真空烘箱中干燥，得到棒状FeCl2纳米材料。In the fourth step, use a centrifuge to separate the solid precipitate from the solution. The precipitate is first washed with deionized water to remove excess impurities, and then washed with absolute ethanol. After multiple washings and centrifugation, the precipitate Dry in a vacuum oven at 60°C to obtain rod-shaped FeCl2 nanomaterials.
所得到的产物棒状FeCl2纳米材料整体形貌为大小均匀的棒状纳米结构。棒状FeCl2纳米材料长约2-5微米，粗约80-120纳米。The overall morphology of the obtained rod-shaped FeCl2 nanomaterial is a rod-shaped nanostructure with uniform size. The rod-shaped FeCl2 nanomaterial is about 2-5 microns long and about 80-120 nanometers thick.
实施例4：Example 4:
采用本发明提供的方法制备棒状FeCl2纳米材料，具体步骤如下：Using the method provided by the present invention to prepare rod-shaped FeCl2 nanomaterials, the specific steps are as follows:
第一步，室温下将100mgPVP(MW5800)和45mg氯化钠溶解在二甲基亚砜/去离子水的混合溶剂中(30mL，10/20,V/V),得到无色透明的溶液，The first step is to dissolve 100mg PVP (MW5800) and 45mg sodium chloride in a mixed solvent of dimethyl sulfoxide/deionized water (30mL, 10/20, V/V) at room temperature to obtain a colorless and transparent solution.
第二步，将此无色透明溶液在60℃搅拌30分钟，然后向其中缓慢滴加5mg/mL的乙酸铁水溶液12mL，保持60℃搅拌30分钟，In the second step, the colorless and transparent solution was stirred at 60°C for 30 minutes, and then 12 mL of a 5 mg/mL iron acetate aqueous solution was slowly added dropwise to it, and stirred at 60°C for 30 minutes.
第三步，将得到的溶液放入45mL聚四氟乙烯衬里不锈钢反应釜中，在烘箱中130℃水热反应12小时，待体系自然冷却，得到沉淀。In the third step, the obtained solution was put into a 45mL polytetrafluoroethylene-lined stainless steel reaction kettle, and hydrothermally reacted in an oven at 130°C for 12 hours. After the system was naturally cooled, a precipitate was obtained.
第四步，使用离心机将固体沉淀从溶液中分离出来，将所述沉淀先用去离子水洗涤以除去多余的杂质，再用无水乙醇洗涤，经过多次的洗涤、离心后，将沉淀在60℃真空烘箱中干燥，得到棒状FeCl2纳米材料。In the fourth step, use a centrifuge to separate the solid precipitate from the solution. The precipitate is first washed with deionized water to remove excess impurities, and then washed with absolute ethanol. After multiple washings and centrifugation, the precipitate Dry in a vacuum oven at 60°C to obtain rod-shaped FeCl2 nanomaterials.

Claims (4)

  1. 棒状FeCl2纳米材料的制备方法，其特征在于包括如下步骤：The method for preparing rod-shaped FeCl2 nanomaterials is characterized by including the following steps:
    第一步，室温下将50～100mg聚乙烯吡咯烷酮和45mg氯化钠溶解在二甲基亚砜和去离子水的混合溶剂中，得到无色透明的溶液；所述的混合溶剂为30mL，二甲基亚砜和去离子水的体积比为10：20；In the first step, 50-100 mg of polyvinylpyrrolidone and 45 mg of sodium chloride are dissolved in a mixed solvent of dimethyl sulfoxide and deionized water at room temperature to obtain a colorless and transparent solution; the mixed solvent is 30 mL, two The volume ratio of methyl sulfoxide and deionized water is 10:20;
    第二步，将第一步中得到的无色透明溶液在60℃搅拌30分钟，然后向其中缓慢滴加8～12mL的乙酸铁水溶液，保持60℃搅拌30分钟；所述的乙酸铁水溶液的浓度为5mg/mL；In the second step, the colorless and transparent solution obtained in the first step was stirred at 60°C for 30 minutes, and then 8-12 mL of iron acetate aqueous solution was slowly added dropwise thereto, and stirred at 60°C for 30 minutes; The concentration is 5mg/mL;
    第三步，将第二步得到的溶液放入45mL聚四氟乙烯衬里不锈钢反应釜中，在烘箱中130℃水热反应2～14小时，自然冷却，得到沉淀；In the third step, put the solution obtained in the second step into a 45mL polytetrafluoroethylene-lined stainless steel reaction kettle, hydrothermally react in an oven at 130°C for 2-14 hours, and cool naturally to obtain a precipitate;
    第四步，使用离心机将所述沉淀从溶液中分离出来，经过多次的洗涤、离心后，将沉淀在60℃真空烘箱中干燥。In the fourth step, a centrifuge is used to separate the precipitate from the solution, and after multiple washing and centrifugation, the precipitate is dried in a vacuum oven at 60°C.
  2. 根据权利要求1所述的棒状FeCl2纳米材料的制备方法，其特征在于：第四步中所述的洗涤，包括去离子水洗涤和无水乙醇洗涤。The method for preparing rod-shaped FeCl2 nanomaterials according to claim 1, wherein the washing in the fourth step includes washing with deionized water and washing with absolute ethanol.
  3. 根据权利要求1所述的棒状FeCl2纳米材料的制备方法，其特征在于：所述的制备方法中，第一步选取聚乙烯吡咯烷酮54mg；第二步中滴加乙酸铁水溶液10mL；第三步中水热反应时间为10～12小时。The method for preparing rod-shaped FeCl2 nanomaterials according to claim 1, characterized in that: in the preparation method, 54 mg of polyvinylpyrrolidone is selected in the first step; in the second step, 10 mL of iron acetate aqueous solution is added dropwise; in the third step The hydrothermal reaction time is 10-12 hours.
  4. 根据权利要求1所述的棒状FeCl2纳米材料的制备方法，其特征在于：所述的聚乙烯吡咯烷酮为MW5800。The method for preparing rod-shaped FeCl2 nanomaterials according to claim 1, wherein the polyvinylpyrrolidone is MW5800.
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