阅读说明：本技术 一种碱式氯化铅材料的室温固相合成方法 (Room temperature solid phase synthesis method of basic lead chloride material ) 是由 梁宝岩 代振 张旺玺 于 2019-11-26 设计创作，主要内容包括：本发明公开了一种碱式氯化铅材料的室温固相合成方法,包括如下步骤：将三水合乙酸铅、氢氧化钠、氯化铵和添加剂置于玛瑙研钵中,在室温下充分研磨1-2h使其反应完全。其中三水合乙酸铅、氢氧化钠、氯化铵和添加剂的质量比为3.31:(1-1.5):(0.6-1.5):(0-1)。待研磨结束后,将产物用去离子水和无水乙醇反复洗涤过滤,直至过滤后的去离子水的pH值为中性；将所得到的产物置于烘箱中于60-90℃烘干10-12h,得到碱式氯化铅材料。本发明方法工艺简单,成本低廉且可操作性强,能够在较低的温度,较短的保温时间内获得单相纯净的氧化锌晶须材料。(The invention discloses a room temperature solid phase synthesis method of basic lead chloride material, which comprises the following steps: putting lead acetate trihydrate, sodium hydroxide, ammonium chloride and an additive into an agate mortar, and fully grinding for 1-2h at room temperature to ensure that the reaction is complete. Wherein the mass ratio of the lead acetate trihydrate, the sodium hydroxide, the ammonium chloride and the additive is 3.31 (1-1.5) to (0.6-1.5) to (0-1). After grinding is finished, repeatedly washing and filtering the product by using deionized water and absolute ethyl alcohol until the pH value of the filtered deionized water is neutral; and (3) drying the obtained product in an oven at 60-90 ℃ for 10-12h to obtain the basic lead chloride material. The method has the advantages of simple process, low cost and strong operability, and can obtain single-phase pure zinc oxide whisker materials at lower temperature and within shorter heat preservation time.)

1. A room temperature solid phase synthesis method of basic lead chloride material is characterized by comprising the following steps: putting lead acetate trihydrate, sodium hydroxide, ammonium chloride and an additive into a grinding reaction device, fully grinding for 1-2h at room temperature to enable the lead acetate trihydrate, the sodium hydroxide, the ammonium chloride and the additive to react completely, and repeatedly washing and filtering a product by deionized water and absolute ethyl alcohol after grinding is finished until the pH value of the filtered deionized water is neutral; and (4) drying the obtained product in an oven to obtain the basic lead chloride material.

2. The room temperature solid phase synthesis method of a basic lead chloride material according to claim 1, characterized in that: the mass ratio of the lead acetate trihydrate, the sodium hydroxide, the ammonium chloride and the additive is 3.31 (1-1.5) to (0.6-1.5) to (0-1).

3. The room temperature solid phase synthesis method of a basic lead chloride material according to claim 1, characterized in that: the lead acetate trihydrate, the sodium hydroxide, the ammonium chloride and the additive powder are analytically pure and can be directly purchased from common commercial products.

4. The room temperature solid phase synthesis method of a basic lead chloride material according to claim 1, characterized in that: the grinding reaction device is an agate mortar.

5. The room temperature solid phase synthesis method of a basic lead chloride material according to claim 1, characterized in that: the additive is sodium chloride, urea, glucose, sodium dodecyl benzene sulfonate or polyvinylpyrrolidone.

6. The room temperature solid phase synthesis method of a basic lead chloride material according to claim 1, characterized in that: the drying temperature is 60-90 ℃ and the drying time is 10-12 h.

Technical Field

The invention relates to the field of preparation of basic lead chloride, in particular to a room-temperature solid-phase synthesis method of a basic lead chloride material.

Background

The study of halides and their related compounds has important fundamental value. In recent years, the lead halide pb (oh) X (X = Cl, Br, I) has attracted attention due to its unique structural and spectral characteristics of specificity. The high-quality Pb (OH) Cl nanowire is successfully prepared in octadecene by taking acetylacetone lead and lead chloride as raw materials and then selecting oleic acid and oleylamine mixed surfactant. In the patent "CN 108807986A", lead chloride is added into deionized water to react with triethylamine liquid phase to obtain Pb (OH) Cl. In addition, there are reports of the preparation of Pb (OH) Cl by solvothermal and reverse micelle methods. Although Pb (OH) Cl can be prepared by the work, the adopted chemical raw materials are mostly inflammable and explosive chemical raw materials such as oleylamine, triethylamine and the like, and in addition, the process is complicated, the cost is high, and the large-scale production cannot be realized.

Disclosure of Invention

Aiming at the problems in the prior art, the invention provides a room-temperature solid-phase synthesis method of a basic lead chloride material. And the granularity and the appearance of the product are regulated and controlled by adding various additives.

The technical scheme adopted by the invention for solving the technical problems is as follows:

a room temperature solid phase synthesis method of basic lead chloride material comprises the following steps: putting lead acetate trihydrate, sodium hydroxide, ammonium chloride and an additive into a grinding reaction device, fully grinding for 1-2h at room temperature to enable the lead acetate trihydrate, the sodium hydroxide, the ammonium chloride and the additive to react completely, and repeatedly washing and filtering a product by deionized water and absolute ethyl alcohol after grinding is finished until the pH value of the filtered deionized water is neutral; and (4) drying the obtained product in an oven to obtain the basic lead chloride material.

Further, the mass ratio of the lead acetate trihydrate, the sodium hydroxide, the ammonium chloride and the additive is 3.31 (1-1.5): (0.6-1.5): (0-1).

Furthermore, the lead acetate trihydrate, sodium hydroxide, ammonium chloride and additive powder are analytically pure and can be directly purchased from common commercial products.

Furthermore, the grinding reaction device is an agate mortar.

Further, the additive is sodium chloride, urea, glucose, sodium dodecyl benzene sulfonate or polyvinylpyrrolidone.

Further, the drying temperature is 60-90 ℃ and the time is 10-12 h.

The solid phase synthesis method adopting the technical scheme has the working principle that: the raw materials are ground to react to generate Pb (OH) Cl material, and NaNO in the product₃And NH₄NO₃Can be removed by washing with water.

Pb(NO₃)₂+NaOH+NH₄Cl=Pb(OH)Cl+NaNO₃+NH₄NO₃

The invention has the beneficial effects that: the raw materials are ground in a solid phase, and different additives are added to quickly react and synthesize the submicron or nanometer basic lead chloride with various appearances. The preparation technology has simple process, is easy for batch production, and promotes the large-scale application of the basic lead chloride.

Drawings

FIG. 1 is a typical X-ray diffraction pattern of the basic lead chloride powder prepared in examples 1-4. It can be seen from the figure that the present invention results in a single phase lead oxychloride material without other impurities.

Fig. 2 is a scanning electron micrograph of the basic lead chloride powder prepared in example 1, and it can be seen from the micrograph that the additive has a large influence on the particle size and morphology of the basic lead chloride powder.

Fig. 3 is a scanning electron micrograph of the basic lead chloride powder prepared in example 2, and it can be seen from the micrograph that the additive has a large influence on the particle size and morphology of the basic lead chloride powder.

Fig. 4 is a scanning electron micrograph of the basic lead chloride powder prepared in example 3, and it can be seen from the micrograph that the additive has a large influence on the particle size and morphology of the basic lead chloride powder.

Fig. 5 is a scanning electron micrograph of the basic lead chloride powder obtained in example 4, from which it can be seen that the additive has a large influence on the particle size and morphology of the basic lead chloride powder.

Detailed Description

The present invention will be further described with reference to the following examples. It is to be understood that the following examples are illustrative only and are not intended to limit the scope of the invention, which is to be given numerous insubstantial modifications and adaptations by those skilled in the art based on the teachings set forth above.