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CN-121974310-A - Preparation method and device of nitrosyl fluoride

CN121974310ACN 121974310 ACN121974310 ACN 121974310ACN-121974310-A

Abstract

The invention relates to the field of special gas preparation, which comprises the steps of firstly mixing fluorine gas and inert gas to form first mixed gas, respectively precooling the first mixed gas and nitric oxide, and then introducing the first mixed gas and nitric oxide into a reaction container for reaction to generate nitrosyl Fluoride (FNO). Fluorine and inert gas are pre-mixed to reduce the heat of reaction, reduce the generation of nitrogen oxydifluoride (NOF 2 ), and the inert gas has a lower boiling point and is easy to remove in the subsequent separation process. The pre-cooling can further effectively reduce the reaction temperature and effectively improve the problem of aggravation of reaction heat caused by flow increase. The invention has simple and convenient process and solves the problems of complex process and high cost of the nitrosyl fluoride preparation in the prior art.

Inventors

  • YANG JUNHAO
  • RU GAOYI
  • HUANG NENGWU
  • XIE WUZHONG
  • CHEN ZHIWEI

Assignees

  • 广东华特气体股份有限公司

Dates

Publication Date
20260505
Application Date
20260211

Claims (8)

  1. 1. A preparation method of nitrosyl fluoride is characterized in that fluorine gas and inert gas are mixed to form first mixed gas, and the first mixed gas and nitric oxide are respectively precooled and then introduced into a reaction container to react to generate nitrosyl fluoride.
  2. 2. The method for preparing nitrosyl fluoride according to claim 1, wherein the inert gas is one or more of nitrogen, argon, helium and neon, and the pre-cooling temperature of the first mixed gas and the nitric oxide is-10 to-40 ℃.
  3. 3. The method for preparing nitrosyl fluoride according to claim 2, wherein the reaction vessel is cooled by a refrigerant, and the temperature of the refrigerant is controlled to be-5 to-30 ℃.
  4. 4. The method for preparing nitrosyl fluoride according to claim 3, wherein the nitric oxide and the first mixed gas are introduced into the reaction vessel for reaction under the condition that the volume flow rate is 50-300 sccm and the volume flow rate is 100-2500 sccm.
  5. 5. The method for producing nitrosyl fluoride according to any one of claims 1to 4, wherein the volume flow rate of the fluorine gas introduced into the first mixed gas is 1to 25% of the volume flow rate of the inert gas.
  6. 6. An apparatus for preparing nitrosyl fluoride, which is characterized by carrying out the preparation method of nitrosyl fluoride according to any one of claims 1 to 5, comprising the reaction vessel, a first feed pipe and a second feed pipe, The first feeding pipe and the second feeding pipe are respectively communicated with the reaction container and are used for introducing the nitric oxide and the first mixed gas.
  7. 7. The apparatus for preparing nitrosyl fluoride as set forth in claim 6, wherein a pre-cooling tube for pre-cooling, a flow control valve for controlling a flow rate of gas, and a pressure sensor for detecting a pressure are provided on the first feed tube and the second feed tube.
  8. 8. The apparatus for preparing nitrosyl fluoride as set forth in claim 7, wherein a cooling tube is provided inside the reaction vessel, and a thermometer and a pressure sensor are connected to the reaction vessel for detecting the temperature and pressure during the reaction.

Description

Preparation method and device of nitrosyl fluoride Technical Field The invention relates to the field of preparation of special gases, in particular to a preparation method and a device of nitrosyl fluoride. Background Nitrosyl Fluoride (FNO) is an important inorganic fluoride and a nitrosylating reagent, and has unique application in the fields of organic synthesis, energetic materials and special chemicals. The molecular structure of the catalyst has high reactivity of nitrogen-oxygen bond and fluorine atom, and can be used as efficient fluorinating agent and nitrating agent for preparing various nitro compounds, nitrous acid esters and fluorine-containing derivatives. The prior art discloses a preparation process for producing nitrosyl fluoride from more nitrite and hydrogen fluoride, which is a heterogeneous reaction with complex pretreatment, feeding and mixing processes of raw materials. The anhydrous hydrogen fluoride serving as a raw material has extremely strong corrosiveness and toxicity, has strict requirements on materials of reaction equipment, and has high equipment investment and maintenance cost. Therefore, a synthesis process of nitrosyl fluoride with simple preparation method and high reaction efficiency is needed. Disclosure of Invention The invention mainly aims to provide a novel preparation method of nitrosyl fluoride, which solves the problems of complex preparation process and high cost of nitrosyl fluoride in the prior art. In another aspect, an apparatus for preparing nitrosyl fluoride is provided for carrying out the process. A preparation method of nitrosyl fluoride comprises the steps of mixing fluorine gas and inert gas to form first mixed gas, respectively precooling the first mixed gas and nitric oxide, and then introducing the first mixed gas and nitric oxide into a reaction container for reaction. The fluorine gas and the inert gas are mixed firstly for diluting the fluorine gas, the reaction heat can be reduced by absorbing the heat by the inert gas and slowing down the reaction activity of the fluorine gas in the reaction, the generation of by-product oxydifluoride is reduced, in addition, the boiling point of the inert gas is lower, and the inert gas is easy to remove in the subsequent separation process. Preferably, the precooling temperature of the first mixed gas and the nitric oxide is-10 to-40 ℃. The first mixed gas and nitric oxide are pre-cooled in advance, so that the temperature of raw materials can be reduced, the reaction heat is reduced, and the flow rate is further selectively increased. Preferably, the reaction vessel is cooled by a refrigerant, and the temperature of the refrigerant is controlled to be-5 to-30 ℃. Preferably, the nitric oxide is introduced into the reaction vessel for reaction under the condition that the volume flow rate is 50-300 sccm and the volume flow rate of the first mixed gas is 100-2500 sccm. Preferably, the flow rate of the fluorine gas introduced into the first mixed gas is 1-25% of the volume flow rate of the nitrogen gas. When the fluorine content is relatively low, the safety is high, and the generated nitrosyl fluoride has fewer byproducts. An apparatus for preparing nitrosyl fluoride, comprising the reaction vessel, a first feed tube and a second feed tube, The first feeding pipe and the second feeding pipe are respectively communicated with the reaction container and are used for introducing the nitric oxide and the first mixed gas. The first feeding pipe and the second feeding pipe are provided with a pre-cooling pipe for pre-cooling, a flow control valve for controlling the flow of gas and a pressure sensor for detecting pressure. The reaction vessel is internally provided with a cooling pipe, and is connected with a thermometer and a pressure sensor for detecting the temperature and the pressure in the reaction process. The method has the beneficial effects that the nitrous acid fluoride is prepared by utilizing the mixed gas of nitric oxide, fluorine gas and inert gas through reaction, the preparation process is simple, the reaction is rapid, and the problems of complex reaction process and high cost in the prior art for preparing the nitrous acid fluoride are solved. A large amount of heat can be generated in the reaction process, so that the pressure of the reaction container is rapidly increased to generate a safety problem, and the reaction heat is rapidly removed through the mixing of fluorine gas and inert gas, so that the safety of the reaction is improved, and meanwhile, the reaction byproducts are reduced. In addition, the generation of by-product oxydifluoride can be further reduced by controlling the flow rate of fluorine gas. In addition, the reaction equipment is simple, the reaction can be completed without more devices and processes, and the reaction cost is low and controllable. Drawings In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior