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Method for preparing low chlorine content tantalum niobium alkoxide

A chlorine content, tantalum-niobium technology, applied in the field of preparation of tantalum-niobium alkoxide, can solve the problems of poor safety, explosion, low yield of tantalum-niobium alkoxide, etc., to reduce heat generation, increase yield, and improve process safety sexual effect

Inactive Publication Date: 2008-08-06
NINGXIA ORIENT TANTALUM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method produces a large amount of ammonium chloride precipitation due to the use of directly neutralizing the precipitated hydrogen chloride gas in the solution, so that a part of tantalum ethoxide exists in the precipitation of ammonium chloride, resulting in a low yield of tantalum niobium alkoxide, and the traditional The method generates a large amount of heat in the reaction process, which has exceeded the flash point of alcohol and organic matter, so it is easy to catch fire or explode, and the safety is poor

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 358 grams (1 mole) of high-purity tantalum pentachloride at -20°C to a 4L flask, add 0.5L of anhydrous toluene at -20°C, and drop slowly under cooling conditions. Add 920 grams (20 moles) of absolute ethanol (controlling the addition amount per minute is 50 grams), then under the protection of an inert gas, the solution is heated and refluxed at 76-89 ° C for 2 hours, and no acid gas is released with pH test paper. Pass into 102 grams (6 moles) of ammonia gas in the middle, when the pH value of solution is alkaline. Use ordinary filter paper or filter cloth to filter. The filter cake is washed with absolute ethanol, the collected filtrate is subjected to ordinary distillation, and the ethanol and toluene collected at different temperatures are recycled. The remaining solution was distilled under reduced pressure, and the fractions at 40Pa to 1300Pa and 140 to 250°C were collected to obtain 365 grams of tantalum ethoxide, and the detected chloride ion content was 90...

Embodiment 2

[0023] Add 270 grams (1 mole) of high-purity niobium pentachloride at -20°C to a 10L flask, add 5L of anhydrous toluene at -20°C after freezing, and drop slowly under cooling conditions Add 276 grams (6 moles) of absolute ethanol (controlling the addition amount per minute is 50 grams), then under the protection of dry inert gas, the solution is heated to reflux, the temperature is controlled at 76 to 89 ° C, and heated to reflux for 3 to 4 hours. PH test paper confirms that no acidic gas is released, feeds 850 grams (50 moles) of ammonia gas in the solution, and the pH value of the solution is alkaline. Use ordinary filter paper or filter cloth to filter. The filter cake is washed with absolute ethanol, the filtrate is collected by ordinary distillation, excess ethanol and toluene are collected at different temperatures, and the ethanol and toluene are recycled. Carry out vacuum distillation on the remaining solution, collect the distillate at 40 to 1200Pa, 130 to 230°C, and...

Embodiment 3

[0025] Add 360 grams (1 mole) of high-purity tantalum pentachloride at -20°C to a 4L flask, add 0.5L of solvent gasoline at -20°C, and slowly add it dropwise under cooling conditions. 740 grams (10 moles) of anhydrous n-butanol, (controlling the amount added per minute is 50 grams), then the solution was heated and refluxed at 115-120 ° C for 2 hours, and checked with pH test paper to confirm that no acid gas was released. Feed 102 grams (6 moles) of ammonia gas, and the pH value of the solution is alkaline. Use ordinary filter paper or filter cloth to filter. The filter cake is washed with anhydrous n-butanol, and the collected filtrate is subjected to ordinary distillation, butanol and solvent gasoline collected at different temperatures, and the butanol and solvent gasoline are recycled. The remaining solution was distilled under reduced pressure, and the fractions at 40Pa to 1300Pa and 140 to 250°C were collected to obtain 490 grams of tantalum butoxide, and the detected ...

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Abstract

The invention relates to a method for preparing tantalum-niobium alkoxides with low chlorinity. The procedure comprises freezing chlorides of tantalum or niobium first and then adding a diluent frozen by the same means and adding alcohol compounds for reaction under cooling conditions; performing heating reflux in an inert gas atmosphere, pumping ammonia gas into the system and then filtering the reaction solution and distilling the filtrate to isolate the diluent and retain mother liquid of tantalum-niobium alkoxides in the distilling kettle; distilling the mother liquid of tantalum-niobium alkoxides under reduced pressure and collecting distillates obtained under 40-1,300Pa and at 130-250 DEG C; adding calcium oxide or magnesium oxide into the collected distillate mixture and performing reduced pressure distillation again so as to get tantalum-niobium alkoxides with low chlorinity. The invention removes partial chloride hydrogen from the solvent system by means of heating reflux, adopts low-temperature raw material (including tantalum chloride or niobium chloride and the diluent) as the initial raw material and further removes chlorine ions with calcium oxide in the end, thereby improving the yield of tantalum-niobium alkoxides, increasing the technology safety and, meanwhile, harvesting tantalum-niobium alkoxides with lower chlorinity.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a preparation method of tantalum-niobium alkoxide with low chlorine content. Background technique [0002] Tantalum niobium alkoxide specifically Ta(OR) 5 , Nb(OR) 5 , R represents methyl, ethyl, propyl, butyl, isobutyl. Tantalum niobium alkoxide is mainly used in various thin films, coatings and various functional materials. Because tantalum niobium alkoxide can be dissolved in organic solvents, and can also be miscible with other metal or non-metallic organic compounds, it is an important precursor for the preparation of nano-scale functional materials. Tantalum-niobium alkoxide is liquid at room temperature (25°C), and it can be converted into vapor when heated to 150°C to 200°C under high vacuum, which provides a good raw material for metal organic compound vapor deposition (MOCVD). Tantalum niobium alkoxide can also prepare various artificial crystals, such as ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/70C07C31/28
Inventor 王伟李彬鲁东葛力志郭涛
Owner NINGXIA ORIENT TANTALUM IND
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