Method for preparing nano-tubular sodium titanate/titanci acid

Abstract

A method for preparing nano pipe sodium titanate / metatitanic acid, comprising the following steps: (1) mixing the compound containing titanium with the strong alkaline solution with the wight proportion being 20-80%; (2) heating and backflowing in the microwave oven for 10 minitues-20 hours; (3) cooling and depositing the reacted mixing liquid, washing the deposite to make the pH be 6-8, separating and getting the nano pipe sodium titanate, immersing the product got in the above reaction in strong acid for 3-72 hours, washing, drying and getting the nano pipe metatitanic acid. The invention is characterized by the temperated reacting condition, fast reaction velocity, high performance and cost ratio of the product and being suited to produced industrially.

Description

technical field

[0001] The invention relates to a method for preparing sodium titanate and titanic acid with nanotube structure by using microwave radiation as a heating source. Background technique

[0002] Nanotube sodium titanate / titanic acid has excellent optical and electrical properties, certain mechanical properties and large specific surface area, especially high visible light response, good fluorescence effect and enhanced electroluminescent performance. With ion exchange properties, it can be widely used in catalysts or catalyst supports, solar cells, sensor devices, optical devices; additives for ceramics, paint coatings, fabrics and plastics, and preparation of other titanate nanotubes by ion exchange; can As a recovery agent for silver ions; it can also be used as a chromatographic support for the analysis of lower alkanes. Traditional nanotube sodium titanate / titanic acid preparation methods include template method, sintering method, hydrothermal method, low t...

Examples

Embodiment 1

[0019] Embodiment 1, get 5g TiO 2 (anatase titanium dioxide powder produced by Zhoushan Tomorrow Chemical Plant), slowly add the polytetrafluoroethylene container that fills 100ml concentration and be the NaOH solution of 40% (weight percentage concentration), place in microwave oven, be set to medium low heat (750W , work for 10s, stop for 12s) Stir with a mechanical stirrer, add a reflux condenser, react for 6 hours, cool and settle, pour out the supernatant, wash with distilled water until the pH value is 6.0-8.0, filter, and dry to obtain nano The tube sodium titanate product is then soaked in 0.1M hydrochloric acid for 8 hours, filtered, washed, and dried to obtain the nanotube titanate product.

Embodiment 2

[0020] Embodiment 2, take 5g of metatitanic acid slurry with a water content of 50%, slowly add it into a polytetrafluoroethylene container filled with 100ml of NaOH solution with a concentration of 40% (weight fraction), place it in a microwave oven, set it to medium-low Fire (same as above), stir with a mechanical stirrer, add a reflux condenser, react for 6 hours, cool and settle, pour out the supernatant, wash with distilled water until the pH value is 6.0-8.0, filter, and dry to obtain titanium nanotubes Sodium acid product, then soaked in 0.1M hydrochloric acid for 8 hours, filtered, washed, and dried to obtain nanotube titanic acid product.

Embodiment 3

[0021] Embodiment 3, get reagent grade TiO 2 1g, slowly add 100ml of NaOH solution with a concentration of 40% (weight fraction) into a polytetrafluoroethylene container, place it in a microwave oven, set it to medium heat (750W, work for 12s, stop for 10s), stir with a mechanical stirrer , and add a reflux condenser, react for 6 hours, cool and settle, pour out the supernatant, wash with distilled water until the pH value is 6.0-8.0, filter, and dry to obtain the nanotube sodium titanate product, and then use 0.1M hydrochloric acid Soak for 8 hours, filter, wash and dry to obtain the nanotube titanic acid product.

technical field

[0001] The invention relates to a method for preparing sodium titanate and titanic acid with nanotube structure by using microwave radiation as a heating source. Background technique

[0002] Nanotube sodium titanate / titanic acid has excellent optical and electrical properties, certain mechanical properties and large specific surface area, especially high visible light response, good fluorescence effect and enhanced electroluminescent performance. With ion exchange properties, it can be widely used in catalysts or catalyst supports, solar cells, sensor devices, optical devices; additives for ceramics, paint coatings, fabrics and plastics, and preparation of other titanate nanotubes by ion exchange; can As a recovery agent for silver ions; it can also be used as a chromatographic support for the analysis of lower alkanes. Traditional nanotube sodium titanate / titanic acid preparation methods include template method, sintering method, hydrothermal method, low t...

Examples

Embodiment 1

[0019] Embodiment 1, get 5g TiO 2 (anatase titanium dioxide powder produced by Zhoushan Tomorrow Chemical Plant), slowly add the polytetrafluoroethylene container that fills 100ml concentration and be the NaOH solution of 40% (weight percentage concentration), place in microwave oven, be set to medium low heat (750W , work for 10s, stop for 12s) Stir with a mechanical stirrer, add a reflux condenser, react for 6 hours, cool and settle, pour out the supernatant, wash with distilled water until the pH value is 6.0-8.0, filter, and dry to obtain nano The tube sodium titanate product is then soaked in 0.1M hydrochloric acid for 8 hours, filtered, washed, and dried to obtain the nanotube titanate product.

Embodiment 2

[0020] Embodiment 2, take 5g of metatitanic acid slurry with a water content of 50%, slowly add it into a polytetrafluoroethylene container filled with 100ml of NaOH solution with a concentration of 40% (weight fraction), place it in a microwave oven, set it to medium-low Fire (same as above), stir with a mechanical stirrer, add a reflux condenser, react for 6 hours, cool and settle, pour out the supernatant, wash with distilled water until the pH value is 6.0-8.0, filter, and dry to obtain titanium nanotubes Sodium acid product, then soaked in 0.1M hydrochloric acid for 8 hours, filtered, washed, and dried to obtain nanotube titanic acid product.

Embodiment 3

[0021] Embodiment 3, get reagent grade TiO 2 1g, slowly add 100ml of NaOH solution with a concentration of 40% (weight fraction) into a polytetrafluoroethylene container, place it in a microwave oven, set it to medium heat (750W, work for 12s, stop for 10s), stir with a mechanical stirrer , and add a reflux condenser, react for 6 hours, cool and settle, pour out the supernatant, wash with distilled water until the pH value is 6.0-8.0, filter, and dry to obtain the nanotube sodium titanate product, and then use 0.1M hydrochloric acid Soak for 8 hours, filter, wash and dry to obtain the nanotube titanic acid product.

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