Spherical zirconium silicate nanometer crystal preparation method

A zirconium silicate and nanocrystal technology, applied in nanotechnology, chemical instruments and methods, silicon compounds, etc., can solve the problems of high preparation temperature and short preparation time, and achieve low reaction temperature, short reaction period and convenient operation. Effect

Active Publication Date: 2012-06-20
江苏华莱明新能源科技有限公司
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  • Application Information

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Problems solved by technology

Jiang Weihui et al. (Chinese patent 200710108375.X) used commercially pure anhydrous zirconium tetrachloride and ethyl orthosilicate as precursors, and synthesized it by non-hydrolytic sol-gel me

Method used

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  • Spherical zirconium silicate nanometer crystal preparation method

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Experimental program
Comparison scheme
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Example Embodiment

[0015] Example 1:

[0016] 1) Respectively analyze pure ZrOCl 2 ·8H 2 O, NaSiO 3 ·9H 2 O and polyvinylpyrrolidone (PVP) are added into distilled water and stirred evenly to make ZrOCl 2 Precursor A with a molar concentration of 0.05mol / L, in which ZrOCl 2 ·8H 2 O: NaSiO 3 ·9H 2 The molar ratio of O is 2:9, ZrOCl 2 ·8H 2 The molar ratio of O:PVP is 1:9;

[0017] 2) Add analytically pure LiF to the precursor solution A to control LiF: NaSiO 3 ·9H 2 The molar ratio of O is 2:9 and stir to obtain solution B;

[0018] 3) Pour solution B into an Erlenmeyer flask and place it in an ultrasonic generator with a natural frequency of 80kHz, turn on the ultrasonic generator, control the temperature of the water bath of the reaction system at 30℃, control the reaction time at 5h, and select the ultrasonic power as 200W, the whole reaction should be reacted under ultrasonic initiation, and after the reaction, cool to room temperature to obtain solution C;

[0019] 4) Pour solution C into the hydrot...

Example Embodiment

[0021] Example 2:

[0022] 1) Respectively analyze pure ZrOCl 2 ·8H 2 O, NaSiO 3 ·9H 2 O and polyvinylpyrrolidone (PVP) are added into distilled water and stirred evenly to make ZrOCl 2 Precursor A with a molar concentration of 0.03mol / L, where ZrOCl 2 ·8H 2 O: NaSiO 3 ·9H 2 The molar ratio of O is 3:7, ZrOCl 2 ·8H 2 The molar ratio of O:PVP is 1.5:6;

[0023] 2) Add analytically pure LiF to the precursor solution A to control LiF: NaSiO 3 ·9H 2 The molar ratio of O is 4:7 and stir to obtain solution B;

[0024] 3) Pour solution B into an Erlenmeyer flask and place it in an ultrasonic generator with a natural frequency of 80kHz. Turn on the ultrasonic generator. The temperature of the water bath of the reaction system is controlled at 40℃, the reaction time is controlled at 3h, and the ultrasonic power is selected as 300W, the whole reaction should be reacted under ultrasonic initiation. After the reaction, it should be cooled to room temperature to obtain solution C;

[0025] 4) Pour...

Example Embodiment

[0027] Example 3:

[0028] 1) Respectively analyze pure ZrOCl 2 ·8H 2 O, NaSiO 3 ·9H 2 O and polyvinylpyrrolidone (PVP) are added into distilled water and stirred evenly to make ZrOCl 2 Precursor A with a molar concentration of 0.09mol / L, where ZrOCl 2 ·8H 2 O: NaSiO 3 ·9H 2 The molar ratio of O is 4:5, ZrOCl 2 ·8H 2 The molar ratio of O:PVP is 3:4;

[0029] 2) Add analytically pure LiF to the precursor solution A to control LiF: NaSiO 3 ·9H 2 The molar ratio of O is 6:5 and stir evenly to obtain solution B;

[0030] 3) Pour solution B into an Erlenmeyer flask and place it in an ultrasonic generator with a natural frequency of 80kHz, turn on the ultrasonic generator, control the temperature of the water bath of the reaction system at 50℃, control the reaction time at 1.5h, and select the ultrasonic power The temperature is 400W, and the reaction should be initiated by ultrasonic during the whole reaction. After the reaction, it is naturally cooled to room temperature to obtain soluti...

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Abstract

A spherical zirconium silicate nanometer crystal preparation method includes steps of adding ZrOCl2 8H2O, Na2SiO3 9H2O and PVP (polyvinyl pyrrolidone) into distilled water to obtain precursor liquid A, and adding LiF into the precursor liquid A to obtain liquor B; filling the liquor B in an ultrasonic generator to realize reaction under ultrasonic initiation, and naturally cooling to reach room temperature after reaction to obtain liquor C; pouring the liquor C into a hydrothermal reactor, then sealing the hydrothermal reactor, placing the hydrothermal reactor into a microwave hydrothermal reaction instrument, and naturally cooling to reach the room temperature after reaction to obtain liquor D; and collecting the liquor D by means of leaching of filter paper, then washing the collected liquor D by the aid of deionized water and anhydrous ethanol, and drying the washed liquor D in a draught drying cabinet to obtain spherical zirconium silicate nanometer crystals. Ultrasonic waves are adopted in a microwave hydrothermal method, so that the spherical zirconium silicate nanometer crystals with controllable crystalline forms and controllable sizes can be prepared at low temperature. Reactions are completed in liquid phase, accordingly, process equipment is simple, operation is convenient, raw materials can be obtained easily, preparation cost is low, distribution of grain sizes of the zirconium silicate crystals is narrow, the crystallize forms are controllable, reaction temperature is low, reaction period is short, and repeatability is good.

Description

technical field [0001] The invention belongs to the field of material chemical industry, and in particular relates to a method for preparing spherical zirconium silicate nanocrystals by combining ultrasonic waves with microwave hydrothermal heat. Background technique [0002] Zirconium silicate (ZrSiO 4 ) belongs to the tetragonal crystal system and is a silicate mineral with an island structure. Zirconium silicate can be used as a high-performance structural material (such as graphite, C / C composite materials and SiC structural ceramics, etc.) due to its high melting point, low thermal conductivity, low expansion coefficient, and excellent chemical and phase stability. High temperature oxidation resistant coating material. [0003] At present, the methods for preparing zirconium silicate crystals mainly include solid-state reaction method, precipitation method, hydrothermal method, and sol-gel method. The above methods generally require high temperature (such as 1300-160...

Claims

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Application Information

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IPC IPC(8): C01B33/20B82Y40/00
Inventor 曹丽云刘佳孙莹黄剑锋辛宇
Owner 江苏华莱明新能源科技有限公司
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