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Method for preparing dichlorofluoroethane by catalytic fluorination with vinylidene chloride

A technology of monofluorodichloroethane and vinylidene chloride, applied in catalyst activation/preparation, dehydrohalogenation preparation, chemical instruments and methods, etc., can solve the problem of increasing production energy consumption and cost, and improving the purity of monofluorodichloroethane. low conversion rate of vinylidene chloride, etc., to achieve the effects of inhibiting production, shortening reaction time, and excellent catalytic performance

Active Publication Date: 2017-09-29
ZHEJIANG SANMEI CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 1. The conversion rate of vinylidene chloride is relatively low, and the content of the by-product difluorochloroethane produced is relatively high, resulting in low purity of monofluorodichloroethane;
[0006] 2. Due to the low purity, purification operation is required after the reaction, thus increasing production energy consumption and cost
[0007] 3. The reaction rate is slow and the production efficiency is low;
[0008] 4. There are many chemical substances involved, and the amount of waste materials is large

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] First feed nitrogen into the reaction kettle, then take 10mol of vinylidene chloride and 11mol of anhydrous hydrogen fluoride, mix them and add them to an ultrasonic oscillator, and ultrasonically oscillate for 30 minutes; introduce the reaction solution into the reaction tank, turn on the blue light lamp and stirrer, The speed of the stirrer was kept at 800r / min, the reaction pressure was controlled at 0.3MPa, and the reaction was carried out for 45min to obtain a fluorodichloroethane product.

[0059] Based on the above-mentioned preparation process, the conversion rate of vinylidene chloride, the selectivity of fluorodichloroethane and the content of difluorochloroethane were detected respectively; the detection results are shown in Table 1:

[0060] Table 1 Example 1 detection result

[0061] Example 1

Embodiment 2

[0063] First feed nitrogen into the reaction kettle, then take 10mol vinylidene chloride and 12mol anhydrous hydrogen fluoride, mix them and add them to an ultrasonic oscillator, and ultrasonically oscillate for 30 minutes; introduce the reaction solution into the reaction tank, turn on the blue light lamp and stirrer, The speed of the stirrer was kept at 800r / min, the reaction pressure was controlled at 0.25MPa, and the reaction was carried out for 50min to obtain a fluorodichloroethane product.

[0064] Based on the above-mentioned preparation process, the conversion rate of vinylidene chloride, the selectivity of fluorodichloroethane and the content of difluorochloroethane were detected respectively; the detection results are shown in Table 2:

[0065] The test result of table 2 embodiment 2

[0066] Example 2

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PUM

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Abstract

The invention discloses a method for preparing dichlorofluoroethane by catalytic fluorination with vinylidene chloride. The method comprises the following steps: (1) preparing vinylidene chloride, namely preparing a carbon nitride catalyst, additionally chlorinating vinyl chloride and hydrogen chloride to generate 1,1-dichloroethane, and re-chlorinating the 1,1-dichloroethane to generate 1,1,1-trichloroethane; adding the carbon-nitride catalyst into the 1,1,1-trichloroethane, reacting at 550 DEG C to obtain vinylidene chloride, cooling, sealing and storing; (2) preparing anhydrous hydrogen fluoride; and (3) synthesizing dichlorofluoroethane, namely adding vinylidene chloride and anhydrous hydrogen fluoride into an ultrasonic oscillator for mixing, performing ultrasonic oscillation for 30 minutes to obtain a reacting liquid, putting the reacting liquid into a reaction kettle, and reacting under bluelight catalysis to generate the dichlorofluoroethane. The method can be used for effectively inhibiting production of byproduct dichlorofluoroethane, and has high vinylidene chloride conversion rate and high synthesizing speed, and the production efficiency can be improved.

Description

technical field [0001] The invention relates to a method for preparing organic matter, in particular to a method for preparing monofluorodichloroethane by catalytic fluorination of vinylidene chloride. Background technique [0002] Fluorodichloroethane, a high-purity liquid widely used in cleaning and solvent applications, has been designated as an ideal replacement for fully halogenated chlorofluorocarbons due to its low impact on the ozone layer, The market demand is huge. [0003] Fluorodichloroethane is synthesized by addition reaction of vinylidene chloride and anhydrous hydrogen fluoride as raw materials. Vinylidene chloride is also known as VDC, and its chemical structure is CH 2 =CCl 2 , is a colorless liquid with a strong pungent odor and is very volatile; due to the volatility of vinylidene chloride, it is difficult to preserve it in good condition. After a period of time, the weight of vinylidene chloride will be lost, resulting in waste. [0004] In the actual...

Claims

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Application Information

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IPC IPC(8): C07C19/12C07C17/087C07C19/045C07C17/10C07C19/05C07C17/25C07C21/08C01B7/19B01J27/24B01J37/03B01J37/08
CPCB01J27/24B01J37/036B01J37/082C01B7/193C01B7/195C07C17/087C07C17/10C07C17/25C07C19/045C07C19/05C07C21/08C07C19/12
Inventor 赵旭亮应俊吕赛伟
Owner ZHEJIANG SANMEI CHEM IND
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