Method for preparing large size beta-type ammonium tetramolybdate monocrystal particle

Patent metadata

Field	Value
Publication number	US-11859314-B2
Application number	US-202217834238-A
Country	US
Kind code	B2
Filing date	Jun 7, 2022
Priority date	Jun 9, 2021
Publication date	Jan 2, 2024
Grant date	Jan 2, 2024

Abstract

A method for preparing large size beta-type ammonium tetramolybdate monocrystal particle includes industrial ammonium molybdate, ammonia, de-ionized water are used to prepare ammonium molybdate solution with concentration of 0.2˜0.6 g/ml; pH is adjusted to 5˜7, temperature is adjusted to the first temperature of 70˜90° C. to obtain the first ammonium molybdate solution; beta-type ammonium tetramolybdate crystal seed is put into crystallization container, and the first ammonium molybdate solution is poured in the crystallization container, to form crystallization system; the crystallization system stands still at room temperature, naturally cooling, the beta-type ammonium tetramolybdate crystal seed grows into large size beta-type ammonium tetramolybdate monocrystal particle. A beta-type ammonium tetramolybdate crystal seed is obtained by constant-temperature crystallization at 70˜90° C. The obtained beta-type ammonium tetramolybdate crystal seed is put stewing in the first ammonium molybdate solution and is naturally cooling to produce large size beta-type ammonium tetramolybdate monocrystal particle forms.

First claim

The invention claimed is:

1. A method for preparing a large size beta-type ammonium tetramolybdate monocrystal particle, wherein, the method comprises:
industrial ammonium molybdate, ammonia water, and de-ionized water are used to prepare an ammonium molybdate solution with a concentration of 0.2˜0.6 g/ml; pH of the ammonium molybdate solution is adjusted to 5˜7, and temperature of the ammonium molybdate solution is adjusted to a first temperature of 70˜90° C. to obtain a first ammonium molybdate solution; and
a beta-type ammonium tetramolybdate crystal seed is put in a crystallization container, and the first ammonium molybdate solution is poured into the crystallization container to form a crystallization system; the crystallization system stands still at a room temperature, naturally cooling, and the beta-type ammonium tetramolybdate crystal seed grows up as a large size beta-type ammonium tetramolybdate monocrystal particle product,
wherein the beta-type ammonium tetramolybdate crystal seed is prepared by:
using industrial ammonium molybdate, ammonia water, and de-ionized water to prepare the ammonium molybdate solution with the concentration of 0.2˜0.6 g/ml;
adjusting the pH of the ammonium molybdate solution to 1˜2, adjusting the temperature of the ammonium molybdate solution to a second temperature of 70˜90° C. to obtain a second ammonium molybdate solution; and
stirring the second ammonium molybdate solution at a constant temperature of the second temperature, crystallizing at the constant temperature for 3˜5 mins, and filtering to obtain the beta-type ammonium tetramolybdate crystal seed.

2. The method for preparing the large size beta-type ammonium tetramolybdate monocrystal particle of claim 1 , wherein the pH of the ammonium molybdate solution is adjusted to 5˜7 by nitric acid, to obtain the first ammonium molybdate solution.

3. The method for preparing the large size beta-type ammonium tetramolybdate monocrystal particle of claim 1 , further comprising drying the obtained beta-type ammonium tetramolybdate crystal seed at a temperature not exceeding 60° C.

4. The method for preparing the large size beta-type ammonium tetramolybdate monocrystal particle of claim 1 , wherein the pH of the ammonium molybdate solution is adjusted by nitric acid to obtain the second ammonium molybdate solution.

5. The method for preparing the large size beta-type ammonium tetramolybdate monocrystal particle of claim 1 , wherein the first temperature and the second temperature are controlled to be the same.

6. The method for preparing the large size beta-type ammonium tetramolybdate monocrystal particle of claim 1 , wherein a particle size of the industrial ammonium molybdate is between 0.7˜1.1 μm, and D50 is 0.99 μm.

7. The method for preparing the large size beta-type ammonium tetramolybdate monocrystal particle of claim 1 , wherein the concentration of the first ammonium molybdate solution is controlled to be the same as the concentration of the second ammonium molybdate solution.

8. The method for preparing the large size beta-type ammonium tetramolybdate monocrystal particle of claim 1 , wherein the second ammonium molybdate solution is stirred at a constant temperature at a rate of 100 r/min.

Assignees

• Univ Zhengzhou

Inventors

• Wu Xiaochao
• Li Qingkui
• Zhang Jing
• Yang Kaijun
• Wang Chengduo
• He Jilin

Classifications

• C30B7/08 Primary

  by cooling of the solution · CPC title

• C30B33/02

  Heat treatment (C30B33/04, C30B33/06 take precedence) · CPC title

• C30B29/32 Primary

  Titanates; Germanates; Molybdates; Tungstates · CPC title

• C01G39/00

  Compounds of molybdenum · CPC title

• C30B7/04

  using aqueous solvents · CPC title