阅读说明：本技术 一种制备磷酸镧三维纳米粒子的方法 (Method for preparing lanthanum phosphate three-dimensional nanoparticles ) 是由 徐玉娜 钟学明 姜凯 谢兢翔 刘松龙 于 2020-06-18 设计创作，主要内容包括：本发明一种制备磷酸镧三维纳米粒子的方法,以氧化镧和磷酸二氢钠为反应原料,乙酸为反应促进剂,制备磷酸镧三维纳米粒子。在水热反应中,实现目标反应；反应过程历经170℃保温水热处理、105℃干燥和800℃,煅烧,最后获得磷酸镧三维纳米粒子。磷酸镧三维纳米粒子产品纯度为99.1%～99.8%,产率为97%～99%,平均粒径为40 nm～60 nm。本发明制备的磷酸镧具有纯度高、产率高、粒径细、分散性能好等特点,制备方法绿色环保。(The invention relates to a method for preparing lanthanum phosphate three-dimensional nanoparticles, which takes lanthanum oxide and sodium dihydrogen phosphate as reaction raw materials and acetic acid as a reaction promoter to prepare the lanthanum phosphate three-dimensional nanoparticles. In the hydrothermal reaction, the target reaction is realized; the reaction process is carried out by heat preservation hydrothermal treatment at 170 ℃, drying at 105 ℃ and calcining at 800 ℃ to finally obtain the lanthanum phosphate three-dimensional nano particles. The purity of the lanthanum phosphate three-dimensional nano particle product is 99.1-99.8%, the yield is 97-99%, and the average particle size is 40-60 nm. The lanthanum phosphate prepared by the method has the characteristics of high purity, high yield, fine particle size, good dispersion performance and the like, and the preparation method is green and environment-friendly.)

1. A method for preparing lanthanum phosphate three-dimensional nanoparticles is characterized by comprising the following steps: the method takes lanthanum oxide and sodium dihydrogen phosphate as reaction raw materials and acetic acid as a reaction promoter to prepare the lanthanum phosphate three-dimensional nano-particles; the method specifically comprises the following steps:

controlling the volume sum of acetic acid and deionized water to be 70.00L in a 100L hydrothermal reaction kettle, sequentially adding 2.140mol of lanthanum oxide, 8.340 mol of sodium dihydrogen phosphate, 2.80-3.20L of acetic acid and 67.20-66.80L of deionized water, and uniformly mixing; heating to 110-120 ℃, reacting for 12-14 h at constant temperature, heating to 170 ℃, and carrying out heat preservation hydrothermal treatment for 3.0-4.0 h; after the heat preservation treatment is finished, cooling the product to room temperature, filtering, washing with distilled water for 3 times, drying at 105 ℃ for 3 hours, cooling the product to room temperature, and transferring to a muffle furnace; heating to 800 ℃ at the heating rate of 10 ℃/min, calcining the product for 2 h, and cooling to room temperature in the furnace to obtain the lanthanum phosphate three-dimensional nano particles.

2. The method for preparing lanthanum phosphate three-dimensional nanoparticles according to claim 1, wherein: the purity of the lanthanum phosphate three-dimensional nano particle product is 99.1-99.8%, the yield is 97-99%, and the average particle size is 45-55 nm.

Technical Field

The invention relates to a method for preparing lanthanum phosphate three-dimensional nanoparticles, in particular to a method for preparing lanthanum phosphate three-dimensional nanoparticles by using lanthanum oxide and sodium dihydrogen phosphate as reaction raw materials and acetic acid as a reaction promoter. The invention relates to the preparation of nano lanthanum phosphate in the technical field.

Background

Lanthanum phosphate is a functional material applied to the fields of rare earth luminescence, optical glass, catalysts and the like. Although more excellent physicochemical properties can be obtained after beneficial impurities are incorporated in the lanthanum phosphate matrix material. However, the shape and quality of the lanthanum phosphate matrix material have an important influence on the functional properties of the lanthanum phosphate functional material. Therefore, the preparation and regulation of the shape, size (especially nanoparticles) and the like of the lanthanum phosphate matrix become important research and development points for preparing lanthanum phosphate functional materials.

Lanthanum phosphate has inherent characteristics of easy agglomeration and difficult crystallization, so that the preparation of lanthanum phosphate three-dimensional nanoparticles is one of the technical problems of the current lanthanum phosphate matrix material preparation.

Disclosure of Invention

Aiming at the technical problem in the current lanthanum phosphate preparation, the invention provides a preparation method of lanthanum phosphate three-dimensional nanoparticles with good dispersibility.

The invention relates to a method for preparing lanthanum phosphate three-dimensional nanoparticles, which takes lanthanum oxide and sodium dihydrogen phosphate as reaction raw materials and acetic acid as a reaction promoter to prepare the lanthanum phosphate three-dimensional nanoparticles. The method specifically comprises the following steps:

in a 100L hydrothermal reaction kettle, controlling the volume sum of acetic acid and deionized water to be 70.00L, sequentially adding 2.140mol of lanthanum oxide, 8.340 mol of sodium dihydrogen phosphate, 2.80-3.20L of acetic acid and 67.20-66.80L of deionized water, and uniformly mixing. Heating to 110-120 ℃, reacting for 12-14 h at constant temperature, then heating to 170 ℃, and carrying out heat preservation hydrothermal treatment for 3.0-4.0 h. After the heat preservation treatment is finished, cooling the product to room temperature, filtering, washing with distilled water for 3 times, drying at 105 ℃ for 3 hours, cooling the product to room temperature, and transferring to a muffle furnace; heating to 800 ℃ at the heating rate of 10 ℃/min, calcining the product for 2 h, and cooling to room temperature in the furnace to obtain the lanthanum phosphate three-dimensional nano particles.

The purity of the lanthanum phosphate three-dimensional nano particle product is 99.1-99.8%, the yield is 97-99%, and the average particle size is 45-55 nm.

The invention has the beneficial effects that: 1) high purity and high yield. The purity of the lanthanum phosphate three-dimensional nano particle reaches 99.1-99.8%, and the yield reaches 97-99%. 2) The particle size is fine. The average grain diameter of the lanthanum phosphate three-dimensional nano-particles is 45 nm-55 nm. 3) The dispersion performance is good. The lanthanum phosphate three-dimensional nano particles are not easy to agglomerate and have good fluidity. 4) Is green and environment-friendly. The preparation process takes water as a reaction medium, does not use toxic and harmful reagents, and has the advantages of environment-friendly reaction raw materials and products and no waste gas and waste residue.

Drawings

FIG. 1 is an XRD pattern of a lanthanum phosphate three-dimensional nanoparticle of the present invention;

FIG. 2 is an SEM image of three-dimensional lanthanum phosphate nanoparticles of the present invention.

Detailed Description

The method for preparing lanthanum phosphate three-dimensional nanoparticles according to the present invention is further described with reference to the following specific examples.