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Simple, efficient and energy-saving preparation method of niobic acid

A technology of niobic acid and niobate, applied in chemical instruments and methods, niobium compounds, inorganic chemistry, etc., can solve the problems of high synthesis purity, increase container volume, reduce energy consumption, etc., and achieve good application prospects and high production efficiency , low-cost effect

Active Publication Date: 2016-11-23
新沂肽科生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The strong corrosion of strong alkali on the container during high temperature treatment increases the preparation cost, and at the same time, impurities are brought into the product to affect the acidity and stability of the product niobic acid; the hydrothermal synthesis method reduces the reaction temperature, which reduces energy consumption, and at the same time compares High-temperature solid-phase synthesis has high purity and mature technology, but it requires pressure-resistant instruments
At the same time, because a large amount of water participates in the reaction process, the volume of the container is increased, and the energy consumption and equipment investment are correspondingly increased.
This method also has the disadvantage of low efficiency

Method used

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  • Simple, efficient and energy-saving preparation method of niobic acid
  • Simple, efficient and energy-saving preparation method of niobic acid
  • Simple, efficient and energy-saving preparation method of niobic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] ① Take 20g Nb 2 O 5 Mix with 21.8g KOH (Nb / K molar ratio 1:2.2) and grind uniformly. Add appropriate amount of water to adjust the mixture into a paste and squeeze it into sample strips. Place the sample strips on the honeycomb ceramic plate and heat it in a microwave for 5 minutes with a microwave power of 1 kW.

[0050] ② Take out the product obtained in step ①, cool and grind.

[0051] ③Dissolve the solid powder obtained in step ② in 500mL ultrapure water, filter out the insoluble matter, and use 3mol / L H for the filtrate 2 SO 4 Acidify to pH=4.6, and separate a gum.

[0052] ④ Take 500 mL of deionized water into the jelly obtained in step ③, stir evenly, and filter with suction.

[0053] ⑤ Take 500 mL of deionized water into the filter cake obtained in step ④, stir evenly, and filter with suction.

[0054] ⑥Repeat step ⑤3 times, until the final filtrate is neutral, and use BaCl 2 Solution detection The final filtrate until there is no SO in the filtrate 4 2- . The obtained ...

Embodiment 2

[0056] ① Take 20g Nb 2 O 5 Mix with 21.8g KOH (Nb / K molar ratio 1:2.2) and grind it evenly. Add appropriate amount of water to make the mixture into a paste and extrude it into sample strips. Place the sample strips on the honeycomb ceramic plate and heat for 10 minutes in the microwave. , Microwave power is 1kW.

[0057] ② Take out the product obtained in step ①, cool and grind.

[0058] ③Dissolve the solid powder obtained in step ② in 500mL ultrapure water, filter out the insoluble matter, and use 3mol / L H for the filtrate 2 SO 4 Acidify to pH=4.6, and separate a gum.

[0059] ④ Take 500 mL of deionized water into the jelly obtained in step ③, stir evenly, and filter with suction.

[0060] ⑤ Take 500 mL of deionized water into the filter cake obtained in step ④, stir evenly, and filter with suction.

[0061] ⑥Repeat step ⑤3 times, until the final filtrate is neutral, and use BaCl 2 Solution detection The final filtrate until there is no SO in the filtrate 4 2- . The obtained solid i...

Embodiment 3

[0063] ① Take 20g Nb 2 O 5 Mix with 21.8g KOH (Nb / K molar ratio 1:2.2) and grind it evenly. Add appropriate amount of water to make the mixture into a paste and extrude it into sample strips. Place the sample strips on the honeycomb ceramic plate and heat it in the microwave for 20 minutes , Microwave power is 1kW.

[0064] ② Take out the product obtained in step ①, cool and grind.

[0065] ③Dissolve the solid powder obtained in step ② in 500mL ultrapure water, filter out the insoluble matter, and use 3mol / L H for the filtrate 2 SO 4 Acidify to pH=4.6, and separate a gum.

[0066] ④ Take 500 mL of deionized water into the jelly obtained in step ③, stir evenly, and filter with suction.

[0067] ⑤ Take 500 mL of deionized water into the filter cake obtained in step ④, stir evenly, and filter with suction.

[0068] ⑥Repeat step ⑤3 times, until the final filtrate is neutral, and use BaCl 2 Solution detection The final filtrate until there is no SO in the filtrate 4 2- . The obtained solid...

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Abstract

The invention relates to a solid acid catalyst as well as a rapid and moderate preparation method of a non-crystalline niobium pentoxide material. Under a rapid and moderate condition, crystalline niobium pentoxide is transformed into niobate and then the energy-saving preparation of non-crystalline niobium pentoxide (niobic acid) is achieved; the preparation method has the significance of simplicity, high efficiency, energy saving and the like. The preparation method comprises the following steps: mixing crystalline niobium pentoxide as a raw material with an appropriate amount of potassium carbonate or potassium hydroxide; mixing with an appropriate amount of water to form a paste; placing the paste in a microwave field to receive radiation for a certain time, thereby transforming the crystalline niobium pentoxide into niobate; acidizing the niobate with dilute acid; and washing the acidized niobate, thereby obtaining the non-crystalline niobium pentoxide, namely niobic acid. The yield of niobic acid is 30%-85%.

Description

Technical field [0001] The invention relates to a simple, high-efficiency and energy-saving method to obtain amorphous niobium pentoxide (niobic acid) through niobate or polyniobate ( Nb 2 O 5 ·NH 2 O) method, its main content is to use microwave field radiation to replace the traditional high-temperature solid phase reaction or hydrothermal reaction method, the crystalline phase niobium pentoxide, alkali and water blend under the action of microwave field It is quickly converted into soluble niobate, and prepared by acidification, washing and other steps. The product can be used directly as a solid acid catalyst or react with oxalic acid, hydrogen peroxide, citric acid or tartaric acid to form a water-soluble complex as Preparation of precursors for niobium-based materials. Background technique [0002] Niobium oxide is usually Nb 2 O 5 It exists in the form, which is mainly obtained by separating other metals from niobite. According to the different production temperature, the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G33/00
Inventor 何杰王建李德威
Owner 新沂肽科生物科技有限公司