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A kind of synthetic method of tantalum alkoxide

A synthesis method and alkoxide technology, which is applied in the field of new synthesis of tantalum alkoxide as a raw material for the production of niobium compounds in the electronics industry, can solve the problems of low recovery rate, high cost, poor environment, etc., and achieve easy control, safety assurance, and low raw material price cheap effect

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

[0006] The purpose of the present invention is to solve the problems of long process flow, poor environment, high cost and low recovery rate in the synthesis process of tantalum alkoxide prepared by ammonia method in the prior art, and to provide a non-toxic, harmless and low-cost Inexpensive and high conversion tantalum alkoxide synthesis method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] A novel synthetic method of tantalum alkoxide, comprising the following steps:

[0039] 1) Under an argon atmosphere, add 50 grams of absolute ethanol and 500 milliliters of n-hexane into the reaction kettle, and stir evenly, then adjust the temperature of the entire reaction system and keep it at -10°C;

[0040] 2) Add 20 grams of sodium metal to the reaction kettle while stirring, and add it completely in 2 hours. During this process, keep the temperature of the reaction system at -10 ° C. After the addition, keep the temperature and reflux for 2 hours to obtain the mixture;

[0041] 3) Then add 50 grams of tantalum pentachloride tetrahydrofuran solution to the reaction kettle, and keep its temperature at -10°C, allow it to react for 4 hours, and then reflux for 6 hours;

[0042] 4) Return to room temperature and filter to obtain the filtrate, then heat the filtrate to 30°C, and decompress to 6000Pa to distill the solvent;

[0043] 5) After the solvent is evaporated ...

Embodiment 2

[0045] A novel synthetic method of tantalum alkoxide, comprising the following steps:

[0046] 1) Under a nitrogen atmosphere, add 40 grams of anhydrous methanol and 500 milliliters of n-hexane into the reaction kettle, and stir evenly, then adjust the temperature of the entire reaction system and keep it at -20°C;

[0047] 2) Add 20 grams of sodium metal to the reaction kettle while stirring, and add it completely in 3 hours. During this process, pay attention to keep the temperature of the reaction system at -20 ° C. After the addition, keep the temperature and reflux for 3 hours to obtain the mixture;

[0048]3) Then add 50 grams of tantalum pentachloride tetrahydrofuran solution to the reaction kettle, and keep its temperature at -20°C, allow it to react for 6 hours, and then reflux for 6 hours;

[0049] 4) Return to room temperature and filter to obtain the filtrate, then heat the filtrate to 50°C, and decompress to 3000Pa to distill off the solvent;

[0050] 5) After th...

Embodiment 3

[0052] A novel synthetic method of tantalum alkoxide, comprising the following steps:

[0053] 1) Under a nitrogen atmosphere, add 55 grams of anhydrous isopropanol and 500 milliliters of n-heptane into the reaction kettle, and stir evenly, then adjust the temperature of the entire reaction system and keep it at -20°C;

[0054] 2) Add 20 grams of sodium metal to the reaction kettle while stirring, and add it completely in 2 hours. During this process, keep the temperature of the reaction system at -20 ° C. After the addition, keep the temperature and reflux for 3 hours to obtain the mixture;

[0055] 3) Then add 50 grams of tantalum pentachloride tetrahydrofuran solution to the reaction kettle, and keep its temperature at -20°C, allow it to react for 5 hours, and then reflux for 8 hours;

[0056] 4) Return to room temperature and filter to obtain the filtrate, then heat the filtrate to 70°C, and decompress to 2000Pa to distill the solvent;

[0057] 5) After the solvent is eva...

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PUM

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Abstract

The invention discloses a novel synthesis method of tantalum alkoxide. The novel synthesis method comprises following steps: an anhydrous alkyl alcohol and alkane CnH(2n+2) (n is larger than or equal to 6) mixture is added to a reactor under inert atmosphere protection, metallic sodium is added under the stirring condition for a reaction, the temperature of a reaction system is kept at 0-30 DEG C, and heating reflux is performed for 2-3 h after addition; a tantalum pentachloride and tetrahydrofuran suspension is added dropwise to the system, the reaction is performed for 4-6 h at the temperature of 0-subzero 30 DEG C, and then the reflux reaction is performed for 6-10 h; filter residues are removed through filtering, a low-boiling-point solvent is obtained from an obtained filtrate through distillation under the pressure of 2,000-6,000 Pa, an obtained liquid is distilled under the pressure of 50-300 Pa, and tantalum alkoxide is obtained. The synthesis method solves the problems of long process, bad environment, high cost, low recovery rate and the like in a synthesis process of tantalum alkoxide prepared with an ammonia process in the prior art, and has the advantages that experimental steps are simple, the method is non-toxic and harmless, the cost is low, the conversion rate is high and the like.

Description

technical field [0001] The invention relates to the field of material production, in particular to a novel synthesis method for producing raw material tantalum alkoxide from niobium compounds used in the electronics industry. Background technique [0002] Tantalum pentoxide (Ta2O5) thin film has high dielectric constant (25-35), high refractive index and good chemical stability, it can be used as dielectric layer of capacitor in DRAM, MOS gate dielectric layer, thin film electroluminescent device Key materials for insulating layers, sensitive layers in biological and chemical sensors, and coatings. In particular, tantalum pentoxide is a high dielectric constant material, which is much higher than traditional silicon dioxide materials, so it can achieve a larger physical thickness at the same capacitance density, which can effectively reduce the leakage current of the device Density, improve the reliability and service life of the device. At present, tantalum pentoxide has ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/28C07C29/70C07C29/80C07C29/76
CPCC07C29/70C07C29/76C07C29/80C07C31/28
Inventor 不公告发明人
Owner JIANGSU SINOCOMPOUND CATALYST