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Preparation method of anhydrous ammonium bifluoride and microchannel reaction device thereof

An anhydrous hydrogen fluoride, microchannel reaction technology, applied in chemical instruments and methods, ammonium halide, chemical/physical processes, etc., can solve the problems of large working environment pollution, complex equipment structure, waste of raw materials, etc., and achieve low labor intensity, The effect of small size and no material waste

Active Publication Date: 2016-04-13
衢州市鼎盛化工科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The invention proposes a method for preparing anhydrous ammonium bifluoride, which solves the problems of high energy consumption, large waste of raw materials, large pollution of working environment and uneven reaction in the prior art
[0004] The present invention also proposes a microchannel reaction device for preparing the above-mentioned anhydrous ammonium bifluoride, which solves the problems of complex equipment structure and high investment cost in the prior art

Method used

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  • Preparation method of anhydrous ammonium bifluoride and microchannel reaction device thereof
  • Preparation method of anhydrous ammonium bifluoride and microchannel reaction device thereof
  • Preparation method of anhydrous ammonium bifluoride and microchannel reaction device thereof

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preparation example Construction

[0031] The preparation method of anhydrous ammonium bifluoride of the present invention, wherein reaction raw material hydrogen fluoride and liquid ammonia are all in liquid phase; Reaction is carried out in two steps: the first step first liquid phase reaction, takes away most of reaction heat; The second step utilizes reaction heat, From the liquid phase reaction to the molten state; after cooling, anhydrous ammonium bifluoride is obtained. The adopted scheme is: a) React liquid hydrogen fluoride and liquid ammonia in the microchannel reactor in the heat exchange section of the microchannel reaction device to obtain a solution of ammonium bifluoride and hydrogen fluoride; the temperature of the microchannel reactor in the heat exchange section during the above reaction process Less than or equal to 90°C; (b) Input the solution of ammonium bifluoride and hydrogen fluoride obtained in step (a) into the microchannel reactor in the melting section, continue to feed liquid ammonia...

Embodiment 1

[0037] A kind of preparation method of anhydrous ammonium bifluoride, comprising: see attached figure 2 as shown,

[0038] a) Pass 710g of liquid hydrogen fluoride and 200g of liquid ammonia into the microchannel reactor in the heat exchange section of the microchannel reaction device to react to obtain a solution of ammonium bifluoride and hydrogen fluoride; wherein, the flow rate of hydrogen fluoride is 35-36g / min, and the liquid The flow rate of ammonia is 10-11g / min. During the above reaction process, the temperature of the microchannel reactor in the heat exchange section is controlled at 80-90° C. by circulating cooling water;

[0039] (b) Input the solution of ammonium bifluoride and hydrogen fluoride obtained in step (a) into the microchannel reactor in the melting section, continue to feed 103g of liquid ammonia, and the flow rate of liquid ammonia is 10-11g / min. React to obtain ammonium bifluoride in a molten state; during the reaction process, the temperature of ...

Embodiment 2

[0043] A kind of preparation method of anhydrous ammonium bifluoride, comprising: see attached figure 2 as shown,

[0044]a) Pass 750g of liquid hydrogen fluoride and 210g of liquid ammonia into the microchannel reactor in the heat exchange section of the microchannel reaction device to react to obtain a solution of ammonium bifluoride and hydrogen fluoride; wherein, the flow rate of hydrogen fluoride is 35-36g / min, and the liquid The flow rate of ammonia is 10-11g / min. During the above reaction process, the temperature of the microchannel reactor in the heat exchange section is controlled at 65-70° C. by circulating cooling water;

[0045] (b) Input the solution of ammonium bifluoride and hydrogen fluoride obtained in step (a) into the microchannel reactor in the melting section, continue to feed 120g of liquid ammonia, and the flow rate of liquid ammonia is 10-11g / min. React to obtain ammonium bifluoride in a molten state; during the reaction process, the temperature of t...

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Abstract

The invention provides a preparation method of anhydrous ammonium hydrogen fluoride and a micro-channel reaction device thereof. The preparation method comprises the following steps: reacting liquid-state hydrogen fluoride with liquid ammonia in a heat exchange section micro-channel reactor in the micro-channel reaction device to obtain solution of ammonium hydrogen fluoride and hydrogen fluoride; inputting the solution of ammonium hydrogen fluoride and hydrogen fluoride into a melting section micro-channel reactor; continuously introducing the liquid ammonia to react so as to obtain molten-state ammonium hydrogen fluoride; cooling. The reaction device comprises a micro-channel reactor, a melt output device and a cooler which are connected in sequence, wherein the micro-channel reactor comprises a heat exchange section micro-channel reactor and a melting section micro-channel reactor; the heat exchange section micro-channel reactor is connected with a cooling water inlet and a cooling water outlet respectively; the melting section micro-channel reactor is connected with a heat energy input device. The reactants are uniformly heated, the heat energy is controllable, the energy is saved, no pollution is caused, no material is wasted, and safety and reliability are realized. The equipment cost is low, and fully automatic and clean process production is realized.

Description

technical field [0001] The invention relates to the technical field of anhydrous ammonium bifluoride, in particular to a preparation method of anhydrous ammonium bifluoride and a microchannel reaction device thereof. Background technique [0002] The existing methods for preparing ammonium bifluoride are mainly two kinds: liquid phase method and gas phase method. Liquid phase method: Hydrogen fluoride and ammonia need to react in water to form a saturated solution of ammonium bifluoride. By cooling down, ammonium bifluoride crystals are crystallized, and solid-liquid separation is performed to obtain ammonium bifluoride finished product. Disadvantages: large amount of circulation, large waste of raw materials, large pollution of the working environment, high labor intensity of operators, and harsh working environment. Gas phase method: the reaction is carried out in the gaseous state, the reactor and heat exchange system are very large, the structure is complex, the investm...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01C1/16B01J19/00
Inventor 应盛荣姜战应悦
Owner 衢州市鼎盛化工科技有限公司