[go: up one dir, main page]

WO2021072635A1 - Procédé de préparation de nanomatériau de chlorure ferreux en forme de tige - Google Patents

Procédé de préparation de nanomatériau de chlorure ferreux en forme de tige Download PDF

Info

Publication number
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
Authority
WO
WIPO (PCT)
Prior art keywords
shaped
fecl2
rod
deionized water
precipitate
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/CN2019/111255
Other languages
English (en)
Chinese (zh)
Inventor
何洪波
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zhuji Yilian Zhongchuang Enterprise Management Service Co Ltd
Original Assignee
Zhuji Yilian Zhongchuang Enterprise Management Service Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Zhuji Yilian Zhongchuang Enterprise Management Service Co Ltd filed Critical Zhuji Yilian Zhongchuang Enterprise Management Service Co Ltd
Priority to PCT/CN2019/111255 priority Critical patent/WO2021072635A1/fr
Publication of WO2021072635A1 publication Critical patent/WO2021072635A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • 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

Definitions

  • 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.

Landscapes

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

Abstract

L'invention concerne un procédé de préparation d'un nanomatériau FeCl2 en forme de tige. La présente invention concerne le domaine technique de la préparation de nouveaux matériaux énergétiques de composés inorganiques. Dans le procédé, un nanomatériau FeCl2 en forme de tige est préparé à l'aide d'un procédé hydrothermique, avec du chlorure de sodium, de l'acétate de fer, du diméthylsulfoxyde et de la polyvinylpyrrolidone en tant que matières premières. Le procédé spécifique consiste à dissoudre de la polyvinylpyrrolidone et du chlorure de sodium dans un solvant mélangé de diméthylsulfoxyde/eau désionisée à température ambiante, puis ajouter lentement et en goutte à goutte une solution aqueuse d'acétate de fer pour produire un précurseur ; le soumettre à une réaction hydrothermique dans une cuve de réaction à 130°C pendant 2 à 14 heures ; et après que la réaction a été achevée, le soumettre à une séparation centrifuge, le laver de nombreuses fois avec de l'eau désionisée et de l'éthanol absolu, et le sécher pour obtenir le nanomatériau FeCl2 en forme de tige. Le procédé présente les avantages d'être simple en termes de fonctionnement, et de présenter un prix de matière première faible, un rendement élevé, etc.
PCT/CN2019/111255 2019-10-15 2019-10-15 Procédé de préparation de nanomatériau de chlorure ferreux en forme de tige Ceased WO2021072635A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/CN2019/111255 WO2021072635A1 (fr) 2019-10-15 2019-10-15 Procédé de préparation de nanomatériau de chlorure ferreux en forme de tige

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/CN2019/111255 WO2021072635A1 (fr) 2019-10-15 2019-10-15 Procédé de préparation de nanomatériau de chlorure ferreux en forme de tige

Publications (1)

Publication Number Publication Date
WO2021072635A1 true WO2021072635A1 (fr) 2021-04-22

Family

ID=75537401

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2019/111255 Ceased WO2021072635A1 (fr) 2019-10-15 2019-10-15 Procédé de préparation de nanomatériau de chlorure ferreux en forme de tige

Country Status (1)

Country Link
WO (1) WO2021072635A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114388776A (zh) * 2021-12-06 2022-04-22 宜宾光原锂电材料有限公司 镍钴锰三元前驱体洗涤去除杂质钠的方法

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1085190A (zh) * 1993-09-22 1994-04-13 山东蒙阴绵纺织厂染织分厂 氯化亚铁溶液的生产方法和应用
MX2007012200A (es) * 2007-10-02 2009-04-01 Univ Mexico Nacional Autonoma Metodo para sintetizar magnetita en tamaño nanometrico por coprecipitacion en medio basico.
KR20090033524A (ko) * 2007-10-01 2009-04-06 현대자동차주식회사 비자성 나노 알루미나 분말 절연층으로 코팅된 자성분말코어 제조 방법
CN102107910A (zh) * 2011-03-23 2011-06-29 上海理工大学 一种纳米铁酸镁的制备方法
CN103172106A (zh) * 2013-03-22 2013-06-26 北京航空航天大学 棒状AgBr纳米材料的制备方法
CN106587000A (zh) * 2016-12-27 2017-04-26 陕西科技大学 一种NaFePO4纳米棒的制备方法
CN107162064A (zh) * 2017-06-26 2017-09-15 浙江工业大学 一种高温分解法制备氟化亚铁纳米材料的方法
CN107205931A (zh) * 2014-08-01 2017-09-26 安邦国际有限公司 通过共沉淀制备亚微米级别的无定形固体分散体的方法
CN107500364A (zh) * 2017-09-25 2017-12-22 昆明理工大学 一种高纯度FeCl2·4H2O的制备方法
CN107585792A (zh) * 2017-09-28 2018-01-16 唐山市斯瑞尔化工有限公司 二水合氯化亚铁固体的制备方法及二水合氯化亚铁固体

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1085190A (zh) * 1993-09-22 1994-04-13 山东蒙阴绵纺织厂染织分厂 氯化亚铁溶液的生产方法和应用
KR20090033524A (ko) * 2007-10-01 2009-04-06 현대자동차주식회사 비자성 나노 알루미나 분말 절연층으로 코팅된 자성분말코어 제조 방법
MX2007012200A (es) * 2007-10-02 2009-04-01 Univ Mexico Nacional Autonoma Metodo para sintetizar magnetita en tamaño nanometrico por coprecipitacion en medio basico.
CN102107910A (zh) * 2011-03-23 2011-06-29 上海理工大学 一种纳米铁酸镁的制备方法
CN103172106A (zh) * 2013-03-22 2013-06-26 北京航空航天大学 棒状AgBr纳米材料的制备方法
CN107205931A (zh) * 2014-08-01 2017-09-26 安邦国际有限公司 通过共沉淀制备亚微米级别的无定形固体分散体的方法
CN106587000A (zh) * 2016-12-27 2017-04-26 陕西科技大学 一种NaFePO4纳米棒的制备方法
CN107162064A (zh) * 2017-06-26 2017-09-15 浙江工业大学 一种高温分解法制备氟化亚铁纳米材料的方法
CN107500364A (zh) * 2017-09-25 2017-12-22 昆明理工大学 一种高纯度FeCl2·4H2O的制备方法
CN107585792A (zh) * 2017-09-28 2018-01-16 唐山市斯瑞尔化工有限公司 二水合氯化亚铁固体的制备方法及二水合氯化亚铁固体

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114388776A (zh) * 2021-12-06 2022-04-22 宜宾光原锂电材料有限公司 镍钴锰三元前驱体洗涤去除杂质钠的方法

Similar Documents

Publication Publication Date Title
Sarkar et al. Amino acid functionalized blue and phosphorous-doped green fluorescent carbon dots as bioimaging probe
CN103100725B (zh) 一种银/碳量子点复合纳米材料的制备方法
Miao et al. Papain-templated Cu nanoclusters: assaying and exhibiting dramatic antibacterial activity cooperating with H 2 O 2
CN102133646B (zh) 一种分散纳米铁颗粒的制备方法
CN103352254B (zh) 一种八面体铂铜合金纳米晶的制备方法及其制备的八面体铂铜合金纳米晶
CN104817111B (zh) 一种硫化铋纳米球的室温水相制备方法
US20200231458A1 (en) Method for preparing hollow octahedral cuprous oxide
CN103691471B (zh) 氮掺杂石墨烯材料的制备方法
CN103990814B (zh) 一种金纳米颗粒的制备方法
CN105664936A (zh) 一种以多巴胺为碳源制备核壳结构纳米复合材料的方法
CN104190459B (zh) 一种氮掺杂石墨烯包覆FeCo纳米晶的制备方法及其制得的产物的应用
Wei et al. An “on–off–on” selective fluorescent probe based on nitrogen and sulfur co-doped carbon dots for detecting Cu 2+ and GSH in living cells
CN102659188A (zh) 一种具有多级结构的磁性三氧化二铁微米花材料及其制备方法
CN103769601B (zh) 三角片状纳米银颗粒的制备方法
CN103523772B (zh) 煅烧合成石墨烯碳量子点的方法
Nguyen et al. Decarboxylative fluorination of aliphatic carboxylic acids under heterogeneous delafossite AgFeO2 nanoparticle catalysis: The utilization of bimetallic cooperativity
Zeng et al. gC 3 N 5-dots as fluorescence probes prepared by an alkali-assisted hydrothermal method for cell imaging
CN105461920A (zh) 一锅法合成海胆状金纳米粒子和球状聚苯胺的方法及应用
CN106047348A (zh) 一种β‑NaYF4:Yb/Tm@CdS核壳纳米结构的制备方法
WO2021072635A1 (fr) Procédé de préparation de nanomatériau de chlorure ferreux en forme de tige
CN102653396A (zh) 具有高分散性的金属纳米点规则修饰的石墨烯片复合材料及原位制备方法
CN108362669B (zh) 用于检测Al3+的有机荧光聚多巴胺纳米粒子溶液及其制备方法
CN107375324B (zh) 一种氧化石墨烯纳米银的合成方法
CN106115795B (zh) 一种功能化碳包覆磁性纳米粒子的制备方法
CN105290414A (zh) 一种合成纳米铜颗粒的方法

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 19949357

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 19949357

Country of ref document: EP

Kind code of ref document: A1