A method for preparing nitrogen trifluoride by ammonium bifluoride electrolysis

A nitrogen trifluoride and ammonium hydrogen fluoride technology, applied in the electrolysis process, electrolysis components, etc., can solve the problems of easy adhesion of anode gas and decrease of conduction current of electrolysis system, and achieve the effect of ensuring normal operation.

Active Publication Date: 2018-01-09
ZHEJIANG BRITECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the existing technology of ammonium bifluoride electrolysis to prepare nitrogen trifluoride, the anode effect is mainly due to the carbon-fluorine film on the surface of the carbon electrode. Although the carbon-fluorine film is conductive, the anode gas is easy to adhere to the carbon-fluorine film, causing the entire The conduction current of the electrolytic system drops sharply, and more efficient electrodes need to be found

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Step 1, preparation of conductive graphene-modified carbon electrode

[0024] Add 100Kg of conductive graphene to 1200Kg of methanol and 0.3Kg of 1-hexyl-3-methylpyridinium bromide, mix for 36 minutes to prepare a suspension, put the carbon electrode into the suspension and soak for 50h, and then place it in the 1100Kg Soak in an ammonia solution with a concentration of 20% by mass and 0.3Kg of 1-butyl-3-methylimidazole hydroxide for 50 hours, take it out and dry it to prepare a conductive graphene-modified carbon electrode, which is used as an electrolytic reaction anode.

[0025] Step 2, the preparation of nitrogen trifluoride

[0026] Hydrogen fluoride and ammonium fluoride are formulated into an electrolyte with a molar ratio (molten salt ratio) of 1.7:1 and continuously injected into the electrolytic cell. The anode of the electrolytic cell is the conductive graphene-modified carbon electrode in step 1. The electrolysis temperature is 110°C and the pressure is 0.00...

Embodiment 2

[0028] Step 1, preparation of conductive graphene-modified carbon electrode

[0029] Add 100Kg of conductive graphene to 1000Kg of methanol and 0.1Kg of 1-hexyl-3-methylpyridinium bromide, mix for 36 minutes to prepare a suspension, put the carbon electrode into the suspension and soak for 80h, and then place it in a 1000Kg Soak in an ammonia solution with a concentration of 10% by mass and 0.1Kg of 1-butyl-3-methylimidazole hydroxide for 80 hours, take it out and dry it to prepare a conductive graphene-modified carbon electrode, which is used as an electrolytic reaction anode.

[0030] Step 2, the preparation of nitrogen trifluoride

[0031] Hydrogen fluoride and ammonium fluoride are formulated into an electrolyte with a molar ratio (molten salt ratio) of 1:1 and continuously injected into the electrolytic cell. The anode of the electrolytic cell is the conductive graphene-modified carbon electrode in step 1. The electrolysis temperature is 80°C and the pressure is -0.01 MP...

Embodiment 3

[0033] Step 1, preparation of conductive graphene-modified carbon electrode

[0034] Add 100Kg of conductive graphene to 1500Kg of methanol and 0.5Kg of 1-hexyl-3-methylpyridinium bromide, mix for 36 minutes to prepare a suspension, put the carbon electrode into the suspension and soak for 20h, and then place it in the 1500Kg Soak in an ammonia solution with a concentration of 30% by mass and 0.5Kg of 1-butyl-3-methylimidazole hydroxide for 20 hours, take it out and dry it to prepare a conductive graphene-modified carbon electrode, which is used as an electrolytic reaction anode.

[0035] Step 2, the preparation of nitrogen trifluoride

[0036] Hydrogen fluoride and ammonium fluoride are formulated into an electrolyte with a molar ratio (molten salt ratio) of 3:1 and continuously injected into the electrolytic cell. The anode of the electrolytic cell is the conductive graphene-modified carbon electrode in step 1. The electrolysis temperature is 150°C and the pressure is 0.01MP...

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PUM

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Abstract

The invention relates to a method for preparing nitrogen trifluoride through electrolysis of ammonium bifluoride. The method comprises the steps that firstly, an electroconductive graphene modified carbon electrode is prepared and is adopted as an electrolysis reaction anode; hydrogen fluoride and ammonium fluoride are blended into an electrolyte according to the principle that the mole ratio (molten salt ratio) of hydrogen fluoride to ammonium fluoride is (1 to 3) to 1, the electrolyte is continuously injected into an electrolytic bath, the electrolysis temperature is 80 to 150 DEG C, the pressure is minus 0.01 to 0.01 MPa, the voltage is 5 to 10 V, a gas generated at the anode contains NF3, CF4, N2O and traces of impurities, the mixed gas is treated through a series of refining technologies known in the industry, including fluorine impurity removal and acid impurity removal, NF3 is adsorbed through a molecular sieve, NF3 is separated from CF4, NF3 is treated through water washing and alkali washing procedures, and a product is obtained through refining.

Description

technical field [0001] The invention relates to a method for preparing nitrogen trifluoride, in particular to a method for preparing nitrogen trifluoride by electrolysis of ammonium bifluoride. Background technique [0002] Preparation of NF by electrolysis 3 The anode material is mainly nickel, but the nickel anode corrodes faster, pollutes the electrolyte, and forms bottom slag at the bottom of the electrolytic cell. At the same time, the electrolysis process is accompanied by the electroplating process. Over time, nickel is electroplated to the cathode in the form of sponge nickel On the other hand, the cathode is thickened, and because of the uneven electroplating, the cathode is partially protruded. In order to prevent the gas generated by the tip of the cathode from entering the anode gas chamber and causing an explosion, when designing the electrolytic cell, the gap between the cathode and the apron has to be made The distance between them increases, which reduces th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B1/24
CPCC25B1/245
Inventor 陈刚李军张广第王宁周井森陈立峰孙立柱钱红东花永紧荀雨静
Owner ZHEJIANG BRITECH CO LTD
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