Continuous production method for perfluoro tripropylamine

A technology of perfluorotripropylamine and its production method, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of amino compounds, etc., can solve the problems of many by-products, low yield, complicated perfluorotripropylamine equipment, etc., and achieve The effect of reducing breakage and improving productivity

Active Publication Date: 2013-06-12
苏州工业园区捷仕通医疗设备有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the electrolytic synthesis of perfluorotripropylamine has complicated equipmen

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0024] Example 1

[0025] A Monel alloy fluorination reactor with an inner diameter of 80 mm and a length of 200 mm was filled with spherical cobalt oxide with a diameter of 3 mm. The fluorination reactor is heated to 300°C, and a mixed gas of 50% fluorine-50% nitrogen is introduced for fluorination, so that the cobalt oxide is completely converted into cobalt trifluoride. Then the temperature of the fluorination reactor was maintained at 230°C; according to the molar ratio of fluorine gas to tripropylamine 10:1, 20% fluorine-nitrogen mixed gas and 10% tripropylamine-nitrogen mixed gas were continuously introduced to react, and the residence time was controlled 5 second. After 3 hours, neutralize the collected reaction product with 20% potassium hydroxide aqueous solution to a neutral pH value, and let it stand. After layering, take the organic phase and wash it three times with deionized water. Separate the organic phase with anhydrous sodium sulfate After drying, rectificatio...

Example Embodiment

[0026] Example 2

[0027] Using the same equipment as in Example 1, the fluorination reactor was heated to 300°C, and a 50% fluorine-50% nitrogen mixed gas was introduced for fluorination, so that the cobalt oxide was completely converted into cobalt trifluoride. Then the temperature of the fluorination reactor was maintained at 200°C; according to the molar ratio of fluorine gas to tripropylamine 12:1, 20% fluorine-nitrogen mixed gas and 15% tripropylamine-nitrogen mixed gas were continuously introduced to react, and the residence time was controlled to 5 second. After 3 hours, neutralize the collected reaction product with 20% potassium hydroxide aqueous solution to a neutral pH value, and let it stand. After layering, take the organic phase and wash it three times with deionized water. Separate the organic phase with anhydrous sodium sulfate After drying, carry out rectification and separation, and take the boiling point of 127~128℃ to obtain perfluorotripropylamine with a pu...

Example Embodiment

[0028] Example 3

[0029] Using the same equipment as in Example 1, the fluorination reactor was heated to 260°C, and a 50% fluorine-50% nitrogen mixed gas was introduced for fluorination, so that the cobalt oxide was completely converted into cobalt trifluoride. Then the temperature of the fluorination reactor was maintained at 260°C; 30% fluorine-nitrogen mixed gas and 20% tripropylamine-nitrogen mixed gas were continuously introduced in the ratio of fluorine gas to tripropylamine at a molar ratio of 16:1 to react, and the residence time was controlled to 5 second. After 3 hours, the collected reaction product was neutralized with 20% potassium hydroxide aqueous solution until the pH was neutral, and left to stand. After layering, the organic phase was taken and washed three times with deionized water, and the organic phase was separated out with anhydrous sodium sulfate After drying, carry out rectification and separation, and take the boiling point of 127~128℃ to obtain perf...

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PUM

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Abstract

The invention discloses a continuous production method for prefluoro tripropylamine. The continuous production method for prefluoro tripropylamine comprises the following steps of: (1) filling filler into a fluoration reactor, and then introducing fluorine mixed gas for fluoridizing; (2) adding tripropylamine into a tripropylamine vaporizer by a feeder; (3) introducing nitrogen into the tripropylamine vaporizer, diluting tripropylamine steam and continuously carrying the diluted tripropylamine into the fluoration reactor; (4) continuously introducing fluorine nitrogen mixed gas into the fluoration reactor to react with the diluted tripropylamine steam mixed gas continuously introduced into the fluoration reactor, and collecting reaction products; and (5) washing the reaction products with alkali, then washing with water, rectifying and purifying to finally obtain prefluoro tripropylamine. According to the continuous production method for prefluoro tripropylamine, fluorine simple substance or diluent fluorine gas is adopted as an activating agent, and feeding ratio of a fluoration agent to tripropylamine, reaction temperature and reaction time are accurately controlled, so that organic reactant is fluorated completely; and breakage of intramolecular C-C bonds is reduced to the utmost extent, and production efficiency of the prefluoro tripropylamine target product is improved.

Description

technical field [0001] The invention relates to a continuous production method of artificial blood raw materials and perfluorotripropylamine, a special working medium used in the manufacturing process of semiconductor devices. Background technique [0002] In the past, the preparation methods of perfluorotripropylamine include cobalt trifluoride fluorination method and electrolytic fluorination method. The cobalt trifluoride fluorination method needs to convert cobalt oxide or cobalt dioxide into cobalt trifluoride by fluorination first, and then cobalt trifluoride reacts with tripropylamine in the reactor to obtain a mixture containing perfluorotripropylamine; cobalt fluoride Continuous regeneration is required, the temperature of the reactor is difficult to control uniformly, the amplification is limited, the production cannot be carried out continuously, and it is not suitable for mass production. In addition, the electrolytic synthesis of perfluorotripropylamine is comp...

Claims

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Application Information

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IPC IPC(8): C07C211/15C07C209/74
Inventor 鲁俞方治文
Owner 苏州工业园区捷仕通医疗设备有限公司
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