Method for synthesizing tellurium molybdate magnesium single crystal micro powder by using supercritical water system

A supercritical water and powder technology, applied in the directions of single crystal growth, single crystal growth, chemical instruments and methods, etc., to achieve the effect of simplifying synthesis steps, simple reaction equipment, and simple reaction process

Inactive Publication Date: 2013-04-10
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the singleness and deficiency of existing synthesis technology, the purpose of the invention is to provide a kind of

Method used

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  • Method for synthesizing tellurium molybdate magnesium single crystal micro powder by using supercritical water system
  • Method for synthesizing tellurium molybdate magnesium single crystal micro powder by using supercritical water system
  • Method for synthesizing tellurium molybdate magnesium single crystal micro powder by using supercritical water system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1. Ingredients

[0028] Weigh 0.1200 g of magnesium oxide, 0.4318 g of molybdenum trioxide and 0.4788 g of tellurium dioxide and disperse them into 50 ml of ultrapure water. It was then sealed into a reaction vessel (capacity 100 ml).

[0029] 2. Constant temperature reaction

[0030] Put the sealed reaction kettle into a muffle furnace to heat, so that the internal temperature of the reaction vessel is 380°C, the pressure in the reaction vessel is 24±0.2MPa, and the reaction is performed at constant temperature for 1 hour.

[0031] 3. Cooling

[0032] After the constant temperature reaction is over, turn off the power directly to cool down the furnace, let the reaction kettle cool down to room temperature (20-25°C) naturally, and take the reaction kettle out of the muffle furnace.

[0033] 4. Washing

[0034] The product was taken out from the reaction kettle, filtered through a vacuum filtration device, and washed at least three times with deionized water to obtai...

Embodiment 2

[0039] 1. Ingredients

[0040] Weigh 0.1200 g of magnesium oxide, 0.4318 g of molybdenum trioxide and 0.4788 g of tellurium dioxide and disperse them into 50 ml of ultrapure water. It was then sealed into a reaction vessel (capacity 100 ml).

[0041] 2. Constant temperature reaction

[0042] Put the sealed reaction kettle into a muffle furnace and heat it so that the internal temperature of the reaction vessel is 380° C., the pressure in the reaction vessel is 23-24 MPa, and the reaction is carried out at constant temperature for 2 hours.

[0043] 3. Cooling

[0044] After the constant temperature reaction is over, turn off the power to cool down the muffle furnace, let the reaction kettle cool down to room temperature (20-25°C) naturally, and take the reaction kettle out of the muffle furnace.

[0045] 4. Washing

[0046] The product was taken out from the reaction kettle, filtered through a vacuum filtration device, and washed at least three times with ethanol to obtain ...

Embodiment 3

[0051] 1. Ingredients

[0052] Weigh 0.1200 g of magnesium oxide, 0.4318 g of molybdenum trioxide and 0.4788 g of tellurium dioxide and disperse them into 50 ml of ultrapure water. It was then sealed into a reaction vessel (capacity 100 ml).

[0053] 2. Constant temperature reaction

[0054] Put the sealed reaction kettle into a resistance furnace and heat it so that the internal temperature of the reaction vessel is 380° C. and the pressure in the reaction vessel is 24-25 MPa, and the reaction is performed at a constant temperature for 4 hours.

[0055] 3. Cooling

[0056] After the constant temperature reaction is over, the reactor is naturally cooled to room temperature (20-25°C), and the reactor is taken out from the resistance furnace.

[0057] 4. Washing

[0058] Take out the product from the reaction kettle, filter the product through a vacuum filtration device (the pore size of the filter membrane is 0.025-0.5 microns), wash with deionized water until the pH of the w...

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Abstract

The invention discloses a method for synthesizing a tellurium molybdate magnesium single crystal micro powder by using a supercritical water system. With solid magnesium oxide powder, a tellurium dioxide powder and a molybdenum trioxide powder as raw materials and high temperature and high pressure water as a reaction medium, the tellurium molybdate magnesium single crystal micro powder material is synthesized in a sealed pressure container within a condition range of 380 DEG C and 23-25 MPa. The tellurium molybdate magnesium single crystal micro powder material synthesized by the method disclosed by the invention has the advantages of pure phase, comparatively structured particle morphology, particle size range of 15-50 microns, uneasily agglomerated particles and better dispersity. The synthesizing method disclosed by the invention is also suitable for synthesizing a plurality of multibasic oxide single crystal micro materials containing the molybdenum and tellurium and provides a simple, convenient, rapid, safe and environment-friendly preparation process route for novel multibasic oxides containing the molybdenum and tellurium.

Description

technical field [0001] The invention relates to a magnesium tellurium molybdate MgTeMoO 6 (abbreviated as MTM) single-crystal micron powder synthesis method, in particular to a method for synthesizing single-crystal micron powder of magnesium tellurium molybdate in a supercritical water system. Background technique [0002] Magnesium tellurium molybdate MgTeMoO 6 (MTM for short) is a nonlinear optical material, and its bulk single crystal can be grown by flux method; at the same time, magnesium tellurium molybdate can be used as a catalyst for the catalytic oxidation of propylene and isobutylene to acrolein and methacrolein. At present, magnesium tellurium molybdate polycrystalline powder is generally synthesized by conventional solid-state reaction. There are a series of problems in the magnesium tellurium molybdate powder particles synthesized by conventional solid state reaction, such as uneven morphology, small specific surface area, serious agglomeration, etc. The cr...

Claims

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Application Information

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IPC IPC(8): C30B7/10C30B29/46
Inventor 李博陶绪堂陈丽丽
Owner SHANDONG UNIV
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