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Normal pressure alcohol heating process of synthesizing nanometer barium titanate powder with metatitanic acid as material

A technology of barium titanate and metatitanate, applied in titanium compounds, chemical instruments and methods, calcium/strontium/barium compounds, etc., to achieve the effect of simple process, high purity and energy saving

Inactive Publication Date: 2006-05-17
CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Alcohol thermal method can change the thermodynamic properties of the system and the grain morphology in hydrothermal system, and there is no report on the preparation of barium titanate by alcohol thermal method under normal pressure

Method used

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  • Normal pressure alcohol heating process of synthesizing nanometer barium titanate powder with metatitanic acid as material
  • Normal pressure alcohol heating process of synthesizing nanometer barium titanate powder with metatitanic acid as material
  • Normal pressure alcohol heating process of synthesizing nanometer barium titanate powder with metatitanic acid as material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] A three-necked flask of 100 ml is fixed on a heat-collecting constant temperature magnetic stirrer, and a condenser tube, a thermometer, and a constant-pressure dropping funnel are installed on the three-necked flask. Under normal pressure, put 25.2g (0.08mol) of barium hydroxide and 10ml of ethanol into a three-necked flask, beat 9.79g (0.1mol) of metatitanic acid in 15ml of ethanol and pour it into a constant pressure dropping funnel, and heat it in an oil bath with a magnetic force Stir. The temperature was raised to 40°C, and the reaction was timed for 6 hours.

[0017] After the reaction is finished, the reaction liquid is filtered and processed to obtain the product. The titanium-barium ratio of the chemically analyzed product is 1.12, and the XRD analyzed product is a cubic phase, see attached figure 1 , lattice parameter a=4.0286, and a small amount of BaTi 2 o 5 . According to the Scherrer formula, the average primary particle diameter of the barium titana...

Embodiment 2

[0019] A three-necked flask of 100 ml is fixed on a heat-collecting constant temperature magnetic stirrer, and a condenser tube, a thermometer, and a constant-pressure dropping funnel are installed on the three-necked flask. Under normal pressure, put 31.5g (0.1mol) of barium hydroxide and 60ml of ethylene glycol into a three-necked flask, beat 9.79g (0.1mol) of metatitanic acid in 15ml of ethylene glycol and inject it into a constant pressure dropping funnel. The oil bath was heated with magnetic stirring. The temperature was raised to 60°C, and the reaction was timed for 6 hours.

[0020] After the reaction is finished, the reaction liquid is filtered and processed to obtain the product. The titanium-barium ratio of the chemically analyzed product is 1.03, and the XRD analyzed product is a cubic phase, see attached figure 2 . Character parameter a=4.046, according to the Scherrer formula, the average primary particle size is calculated to be 10nm.

Embodiment 3

[0022] A three-necked flask of 100 ml is fixed on a heat-collecting constant temperature magnetic stirrer, and a condenser tube, a thermometer, and a constant-pressure dropping funnel are installed on the three-necked flask. Under normal pressure, put 9.79g (0.1mol) of metatitanic acid and 40ml of propanol into a three-necked flask to make a slurry, then purify 37.8g (1.2mol) of octahydrate barium hydroxide in 30ml of propanol and inject it under constant pressure while hot In the dropping funnel, the oil bath was heated with magnetic stirring. The temperature was raised to 80°C, and the reaction was timed for 10 hours.

[0023] After the reaction is finished, the reaction liquid is filtered and processed to obtain the product. The titanium-barium ratio of the chemical analysis product is 1.00, and the XRD analysis product is a cubic phase, see image 3 . According to the Scherrer formula, the average primary particle size is calculated to be 10nm.

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Abstract

The present invention discloses one fast, simple and cheap barium titanate preparing process. Under normal pressure, metatitanic acid, barium hydroxide and alcohol are mixed and reacted for certain time to obtain precipitate, and the precipitate is treated and dried to obtain high purity superfine barium titanate powder. The preparation path has cheap material, mild reaction condition, relaxed requirement on equipment, reaction side product being water, simple technological process, easy operation and excellent utility.

Description

technical field [0001] The invention relates to a method for preparing barium titanate, and more specifically relates to a method for synthesizing barium titanate powder in one step by using metatitanic acid as a raw material in an alcohol-thermal method under normal pressure. Background of the invention [0002] There are many preparation methods for barium titanate. From the types of raw materials, CN1273562A discloses a method of using TiCl 4 A method for preparing barium titanate as a raw material. However, this method uses the volatile TiCl 4 , causing certain harm to the human body and the environment, and the introduction of mineralizers increases the post-processing steps. "J.Eur.Ceram.Soc.." 1998, 18(4): 279-286 uses titanium alkoxide as raw material to synthesize barium titanate. Although there are some improvements in the raw materials, the titanium alkoxide still has certain damage to the human body, and the titanium alkoxide is exp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/00C01F11/00C04B35/468
Inventor 王公应冯秀丽王越曾毅
Owner CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI