阅读说明：本技术 铁掺杂的凹凸棒石光电材料的制备方法 (Preparation method of iron-doped attapulgite photoelectric material ) 是由 张立静 杨春雷 杨烨 张玉婷 闾蓉蓉 徐孙悦 于 2019-11-14 设计创作，主要内容包括：本发明涉及纳米复合光电材料的制备技术领域,公开了一种铁掺杂凹凸棒石光电材料的制备方法,将高纯度的纳米凹凸棒石均匀分散到三氯化铁的酸性溶液中,然后将上述混合溶液放在反应釜中,100-180oC水热条件下反应24h-150h,然后将所得到的产品离心、清洗、干燥,得到铁掺杂的凹凸棒石光电材料；其中,所述纳米凹凸棒石与所述六水合三氯化铁的质量比为100：1-5。本发明通过水热法将Fe离子引入到凹凸棒石中,制成的光电材料具有较好的光电响应,成本低,操作简单,对环境污染小。(The invention relates to the technical field of preparation of nano composite photoelectric materials, and discloses a preparation method of an iron-doped attapulgite photoelectric material, which comprises the steps of uniformly dispersing high-purity nano attapulgite into an acidic solution of ferric trichloride, then placing the mixed solution into a reaction kettle, reacting for 24-150 h under the hydrothermal condition of 100-180 ℃, and then centrifuging, cleaning and drying the obtained product to obtain the iron-doped attapulgite photoelectric material; wherein the mass ratio of the nano attapulgite to the ferric trichloride hexahydrate is 100: 1-5. According to the invention, Fe ions are introduced into the attapulgite by a hydrothermal method, and the prepared photoelectric material has the advantages of good photoelectric response, low cost, simplicity in operation and small environmental pollution.)

1. A preparation method of an iron-doped attapulgite photoelectric material is characterized in that nano attapulgite is uniformly dispersed into an acidic solution of ferric trichloride, then the mixed solution is placed in a reaction kettle and reacts for 24-150 h under the hydrothermal condition of 100-;

wherein the mass ratio of the nano attapulgite to the ferric trichloride hexahydrate is 100: 1-5.

2. The method for preparing the iron-doped attapulgite photoelectric material according to claim 1, wherein the acidic solution of ferric chloride is prepared by dispersing ferric chloride into a sulfuric acid solution with pH =2.

3. The method for preparing the iron-doped attapulgite photoelectric material according to claim 1 or 2, wherein the washing method comprises washing with water three times, and then washing with ethanol once.

Technical Field

The invention relates to the technical field of preparation of nano composite photoelectric materials, in particular to a preparation method of an iron-doped attapulgite photoelectric material.

Background

Attapulgite is a rare non-metal mineral resource, and has wide application in agriculture and animal husbandry, building materials, medicine, petroleum, food, etc. Attapulgite is an aqueous magnesium-rich aluminosilicate with a layered chain structure, which is itself an insulator, and silicate semiconductors are rare. There are reports in the literature that theoretical calculation indicates that the attapulgite can be changed into a semiconductor from an insulator by introducing iron ions into the attapulgite (Zhang Ke, research on hydrogen production by decomposing water by natural iron-containing cinnamon black salt through visible light catalysis [ D ], Nanjing university of science and technology, 2014). However, the artificially synthesized iron ion doped attapulgite is easy to hydrolyze and conglomerate, so that iron oxide is only introduced to the surface of the attapulgite or single iron oxide particles are formed, and Fe ions are difficult to enter the inside of the attapulgite.

Disclosure of Invention

The purpose of the invention is as follows: aiming at the problems in the prior art, the invention provides a preparation method of an iron-doped attapulgite photoelectric material, Fe ions are introduced into the attapulgite by a hydrothermal method, and the prepared photoelectric material has good photoelectric response, simple preparation method, low cost and environmental friendliness.

The technical scheme is as follows: the invention also provides a preparation method of the iron-doped attapulgite photoelectric material, which comprises the steps of uniformly dispersing the nano attapulgite into an acidic solution of ferric trichloride, then placing the mixed solution into a reaction kettle, reacting for 24-150 h under the hydrothermal condition of 100-;

wherein the mass ratio of the nano attapulgite to the ferric trichloride hexahydrate is as follows: 100: 1-5; preferably 100: 4.8.

preferably, the acidic solution of ferric trichloride is prepared by dispersing ferric trichloride hexahydrate in a solution of sulfuric acid at pH =2.

Preferably, the washing method is that after three times of washing with water, the washing is carried out once with ethanol.

Has the advantages that: according to the invention, Fe ions are introduced into the attapulgite through a simple hydrothermal method, ferric trichloride hexahydrate is dissolved in a sulfuric acid solution with the pH =2, and the purpose is to prevent ferric ions from hydrolyzing and prevent the formation of massive iron micelles, and then the iron ions and the attapulgite are subjected to ion exchange in a high-temperature and high-pressure state formed in a reaction kettle through the hydrothermal method, so that the Fe ion-doped attapulgite is formed, the attapulgite becomes a semiconductor material with better photoelectric response, and the prepared iron-doped attapulgite photoelectric material has better photoelectric response. The method has the advantages of simple synthesis steps, no pollution, no toxicity, environmental friendliness and convenience for industrialization.

Drawings

FIG. 1 is an XRD (X-ray diffraction) diagram of Attapulgite (ATP) and iron-doped attapulgite subjected to hydrothermal reaction at 150 ℃ for 24h, 72h and 150 h;

FIG. 2 is SEM images of different hydrothermal temperatures and times, wherein (1) the SEM images are composite samples of Fe-attapulgite subjected to hydrothermal reaction at 150 ℃ for 24 hours; (2) is a Fe-attapulgite composite sample which is subjected to hydrothermal reaction at 150 ℃ for 72 h; (3) an SEM image of a composite sample of Fe-attapulgite subjected to hydrothermal reaction at 150 ℃ for 150 h;

FIG. 3 is a graph of the I-V curves at different reaction times at 150 ℃. (1) I-V plot of Attapulgite (ATP); (2) an I-V curve chart of a composite sample of Fe-attapulgite subjected to hydrothermal reaction at 150 ℃ for 72 h;

FIG. 4 is an impedance spectrogram of attapulgite and Fe-doped attapulgite subjected to hydrothermal reactions at 150 ℃ for 24h, 72h and 150h, and the test voltage is 0.33V vs. SCE.

Detailed Description

The present invention will be described in detail with reference to the accompanying drawings.