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A kind of synthetic method of niobium alkoxide

A synthesis method and technology of alkoxide, applied in metal alkoxide preparation, organic chemistry, etc., can solve the problems of low recovery rate, poor environment, high cost, etc., and achieve the effects of saving raw materials, high concentration, and increasing yield

Active Publication Date: 2020-06-09
JIANGSU SINOCOMPOUND CATALYST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of this invention is to provide a novel synthetic method of niobium alkoxide to solve the shortcomings of long flow process, poor environment, high cost and low recovery rate in the current ammonia method for niobium alkoxide synthesis process, and it has the advantages of reaction and The distillation conditions are stable and easy to control, no toxic and harmful gases are generated during the synthesis process, the raw materials are cheap, and the reaction yield and production efficiency are high.

Method used

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  • A kind of synthetic method of niobium alkoxide

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Under an argon atmosphere, add 50 grams of absolute ethanol and 500 milliliters of n-hexane into the reaction kettle, add 20 grams of sodium metal into the reaction kettle under stirring conditions, keep the temperature at -10°C during the addition, and maintain the system after adding Temperature reaction for 2 hours, then heating and reflux for 2 hours; then add 45 grams of niobium pentachloride tetrahydrofuran solution, maintain the system temperature at -10°C during the addition process, keep -10°C for 2 hours after the addition, and then reflux for 4 hours; Return to room temperature and filter. The temperature of the filtrate is raised to 30°C, and then the pressure is reduced to 7000Pa to distill off the solvent. After the solvent was evaporated to dryness, the temperature was raised to 80° C., and the pressure was reduced to below 300 Pa, and the product niobium ethoxide was obtained by vacuum distillation. The weight of the niobium ethoxide was measured to be 48...

Embodiment 2

[0035] Under an argon atmosphere, add 40 grams of anhydrous methanol and 500 milliliters of n-hexane to the reaction kettle, and add 20 grams of sodium metal to the reaction kettle under stirring conditions, and keep the temperature at -20 ° C during the addition. temperature for 3 hours, then heated to reflux for 3 hours. Then add 45 grams of niobium pentachloride tetrahydrofuran solution, maintain the temperature of the system at -20°C during the addition process, keep at -20°C for 2 hours after the addition, and then reflux for 8 hours. Return to room temperature and filter. The temperature of the filtrate is first raised to 50 ° C, and then the pressure is reduced to 6000 Pa to distill off the solvent. After the solvent was evaporated to dryness, the temperature was raised to 100° C., and the pressure was reduced to 250 Pa, and the product was distilled under reduced pressure to obtain the product niobium methoxide. The product niobium methoxide was measured to be 35 grams...

Embodiment 3

[0037] Under a nitrogen atmosphere, add 55 grams of anhydrous isopropanol and 500 milliliters of n-hexane into the reaction kettle, add 20 grams of sodium metal into the reaction kettle under stirring conditions, keep the temperature at -30°C during the addition, and keep The system temperature was reacted for 2 hours, and then heated to reflux for 2 hours. Then add 45 grams of niobium pentachloride tetrahydrofuran solution, maintain the temperature of the system at -30°C during the addition process, keep at -30°C for 2 hours after the addition, and then reflux for 10 hours. Return to room temperature and filter. The temperature of the filtrate is first raised to 60 ° C, and then the pressure is reduced to 5000 Pa to distill off the solvent. After the solvent was evaporated to dryness, the temperature was raised to 120° C., and the product was distilled under reduced pressure to 200 Pa to obtain the product niobium isopropoxide, which was measured to be 50 grams, and the calcu...

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Abstract

The invention discloses a novel synthesis method of niobium alkoxide. The method includes: 1) preparing the following raw materials: anhydrous alcohol, an alkane mixture, metal sodium and a niobium pentachloride.tetrahydrofuran suspension; 2) carrying out reaction on anhydrous alcohol, the alkane CnH2n+2 mixture and metal sodium reaction under certain condition; 3) adding the niobium pentachloride.tetrahydrofuran suspension for reaction; and 4) pressure reduced rectification and pressure reduced distillation so as to obtain the product niobium alkoxide. The synthesis method provided by the invention solves the disadvantages of long process, poor environment, high cost, low recovery rate and the like in existing synthesis process of niobium alkoxide by ammonia technique, and has the advantages of smooth reaction and distillation conditions, easy control, no production of toxic and harmful gas during synthesis, cheap raw materials, and high reaction yield and production efficiency, etc. Also, the synthesis reaction has a total yield up to 89%, and the raw material alkane is non-toxic, can be reused and does not generate any waste. Therefore, the method not only is suitable for laboratory synthesis, but also is suitable for large-scale synthesis.

Description

technical field [0001] The invention relates to the field of material production, in particular to a novel synthesis method for producing raw material niobium alkoxides from niobium compounds used in the electronics industry. Background technique [0002] Niobium pentoxide thin film has excellent optical properties, and its optical waveguide loss is small, so it has been widely used in waveguide devices. Utilizing its strong ultraviolet absorption ability, it can be used as a protective film for ultraviolet sensitive materials, and can prepare films with different refractive indices with silicon dioxide. Niobium pentoxide thin film is also an electrochromic material with excellent performance. Some studies believe that the electrochromic performance of niobium pentoxide thin film is comparable to that of tungsten oxide, which has been widely studied and applied to a certain extent; there are also researchers Niobium oxide is considered to be a complementary electrochromic g...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/70C07C31/28
CPCC07C29/70C07C31/28
Inventor 不公告发明人
Owner JIANGSU SINOCOMPOUND CATALYST