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Method for nitrogen trifluoride production

A nitrogen trifluoride, perfluorocarbon technology, applied in the field of detailed description, can solve the problems of not easy to work, corrosion of metal reactors and components, and high cost of fluorine production

Inactive Publication Date: 2006-07-26
AIR PROD & CHEM INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Unfortunately, fluorine is expensive to produce and not easy to work with
Therefore, the failure of this method to utilize 100% of fluorine is economically unfavorable
Second, the cleaning of unreacted fluorine will produce toxic as OF 2 by-product of
It is difficult to associate these by-products with NF 3 Separation resulting in additional waste to be disposed of
Third, the reaction medium may severely corrode metal reactors and components at normal operating temperatures
Finally, the reaction between fluorine and ammonium ions may not be 100% selective to generate NF 3 , and may generate varying amounts of by-products such as N 2 and N 2 f 2

Method used

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  • Method for nitrogen trifluoride production

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Example 1: Fomblin at 96°C _ 25 / 6 Ammonium bifluoride in PFC solvent

[0043] 75 grams (1.32 m) of solid ammonium bifluoride (NH 4 + HF 2 - ) (referred to herein as ABF) and approximately 150 mL (286 g) of Fomblin _ 25 / 6 oil formed the reaction mixture. The reactor is equipped with cooling coils or baffles, thermocouple probes, F 2 Feed tube, into liquid NH 3 Feed tube, pressure gauge, exhaust port and gas propeller type agitator. The mixture was stirred at a speed greater than 1900 revolutions per minute (rpm) while externally heating the mixture to a working temperature of about 96°C. Once the operating temperature is reached, 100% concentration of fluorine gas is introduced into the mixture at a rate of 50 standard cubic centimeters (sccm) per minute (sccm), or about 2.2 mmol / min, through the inlet pipe, and is discharged directly from the reactor through the exhaust port product.

[0044] During discharge of the product from the exhaust port, the gaseous p...

Embodiment 2

[0046] Example 2: In Fomblin _ 25 / 6PFC solvent at 96°C - high F 2 ammonium bifluoride

[0047] Nitrogen trifluoride was prepared as described in Example 1, except that 75.4 grams (1.32 mol) of solid ABF and about 150 mL (289 g) of Fomblin _ The 25 / 6 oil was mixed in a Monel stirred reactor. Once at operating temperature, set F 2 (100% concentration) was fed into the stirred mixture through the dip tube at a rate of 73.3 sccm and the gaseous product exited the reactor directly through the opening in the headspace. On exiting the reactor, the gaseous products were treated and analyzed as described in Example 1. The fluorine feed was continued for approximately 260 minutes, and the composition of the gaseous products exiting the reactor was measured approximately every 20 minutes. After the first 180 minutes of reaction time, vent the reactor of fluorine, NF 3 , N 2 and N 2 The concentration of O reaches a "steady state" concentration. Under "steady state" conditions, th...

Embodiment 3

[0058] Example 3: In Fomblin _ Ammonium bifluoride in 25 / 6 PFC solvent at 115°C

[0059] This experiment was carried out as described in Example 1, except that 100.2 grams (1.76 mol) of solid ABF and about 200 mL (364 g) of Fomblin _ The 25 / 6 oil was mixed in a Monel stirred reactor. The mixture was heated externally until a working temperature of 114-115°C was reached. Once at operating temperature, set F 2 (100% concentration) was fed into the stirred mixture through a dip tube at a rate of 50 sccm and the gaseous product exited the reactor directly through an opening in the headspace. On exiting the reactor, the gaseous products were treated and analyzed as described in Example 1. At "steady state" the fluorine conversion was 98%. The normalized gaseous product composition is 94% NF 3 , 5%N 2 , and 1% N 2 O. NF 3 The yield is 92%.

[0060] Compared with Example 1, when the working temperature increases, NF 3 Yield decreased slightly.

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Abstract

A method for the production of nitrogen trifluoride from a fluorine reactant and an ammonium ion source that is dispersed within a liquid phase reaction mixture containing one or more perfluorocarbon fluids is disclosed herein. In one embodiment, the fluorine reactant is introduced to the reaction mixture at a temperature that ranges from 90 DEG C to 120 DEG C. In this embodiment, the percentage yield of nitrogen trifluoride may be about 80% or greater.

Description

[0001] Cross References to Related Applications [0002] This invention is a continuation-in-part of US Patent Application Serial No. 10 / 299,482, filed November 19, 2002, the disclosure of which is incorporated herein by reference. Background technique [0003] Nitrogen trifluoride (NF 3 ) is in great demand and growing. Nitrogen trifluoride can be used, for example, as an etchant or container cleaning gas. NF on an industrial scale 3 Usually obtained by fluorination of ammonium bifluoride / HF complex. There are two main methods for preparing such composites: direct fluorination (DF) and electrochemical fluorination (ECF). [0004] on NH 3 or NH 4 + Salts undergo direct fluorination to NF 3 In the process, there are competing reactions such as the following: [0005] <chemistry num="001"> <chem file="200310120959_cml001.xml" / > < / chemistry> (1) [0006] <chemistry num="002"> <chem file=...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/083C01B7/19
CPCC01B21/0835C01B7/191C01B21/083
Inventor R·G·西雷特B·A·坎皮恩G·A·库佩J·M·肖尔克
Owner AIR PROD & CHEM INC
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