Preparation method of 1,1-difluoroethane

A technology of difluoroethane and difluorodichloroethylene, applied in the field 1, can solve the problems of low utilization rate of raw materials, influence on product yield, short reaction cycle, etc., and achieve simple preparation method, easy operation, and few side reactions Effect

Active Publication Date: 2012-12-26
SINOCHEM LANTIAN +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method produces a large amount of tar, which is difficult to dispose of and affects product yield
In addition, there are Russian invention patent RU341788, American invention patents US4766258 and US4968850, European patent EP637579, Japanese patents JP50-106904 and JP50-106905, etc., all of wh

Method used

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  • Preparation method of 1,1-difluoroethane
  • Preparation method of 1,1-difluoroethane
  • Preparation method of 1,1-difluoroethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Embodiment 1: Pd / AC-300 catalyst (sample A)

[0043] Grind the activated carbon and screen out 10-20 mesh as a carrier, weigh 100g of activated carbon, put it into 300ml of 10% hydrochloric acid solution, stir and reflux for 6 hours in a water bath at a temperature of 80°C, take it out, and wash the acid with distilled water The final activated carbon is washed to neutrality, and then dried at 100°C for use;

[0044] Weigh 0.13g PdCl 2 , dissolved in 2ml of concentrated hydrochloric acid, added 15g of distilled water to make PdCl 2 After fully dissolving, add 15g of acid-washed activated carbon to the above solution, impregnate for 24 hours, dry at 100°C, then roast at 300°C for 4 hours in an air atmosphere, cool and set aside, record as: 0.5% Pd / AC-300.

Embodiment 2

[0045] Embodiment 2: Pd-Ni / AC-300 catalyst (sample B)

[0046] Weigh 1.21g NiCl 2 ·6H 2 O, dissolved in 15g of distilled water, after fully dissolving, add 15g of activated carbon treated in Example 1, impregnate for 24h, dry at 100°C, then roast at 400°C for 4h in an air atmosphere, cool and set aside;

[0047] Weigh 0.09g PdCl 2 , dissolved in 2ml of concentrated hydrochloric acid, added 10g of distilled water to make PdCl 2 After fully dissolving, add 10g of activated carbon containing auxiliary agent Ni after the above treatment, impregnate for 24h, dry at 100°C, then roast at 300°C for 4h in air atmosphere, after cooling, record as: 0.5%Pd-2% Ni / AC-300.

Embodiment 3

[0048] Embodiment 3: Pd-Ni / AC-300 catalyst (sample C)

[0049] As in the method of Example 2, PdCl will be weighed 2 The amount of the catalyst was changed to 0.05g, and the rest of the preparation conditions were unchanged, and the prepared catalyst was recorded as: 0.3%Pd-2%Ni / AC-300.

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Abstract

The invention discloses a preparation method of 1,1-difluoroethane. Under the existence of a catalyst, difluoro dichloroethylene and hydrogen are subjected to a hydrodechlorination reaction, such that 1,1-difluoroethane is prepared. The catalyst is composed of a main catalyst, an auxiliary agent, and a carrier. The main catalyst is Pd, the auxiliary agent is one or more selected from La, Ce, Cu, Zn or Ni, and the caralyst is loaded on the carrier. The preparation method disclosed by the invention has the advantages of novel raw material route, mild reaction conditions, simple product post-treatment, high catalyst efficiency, and the like. A conversion rate upon a raw material FC-1112A can be higher than 90%, and a selectivity of HFC-152a can be higher than 90%.

Description

technical field [0001] The invention relates to a preparation method of 1,1-difluoroethane. Background technique [0002] HFC-152a, molecular structure: CH 3 -CHF 2 , chemical name: 1,1-difluoroethane, English name: 1,1-bifluoroethane, molecular weight: 66, boiling point: -24.7°C, ozone-depleting potential value ODP=0, global warming coefficient value GWP=0.03, yes An excellent ODS (Ozone Depleting Substances) substitute. Since the physical and thermodynamic properties of HFC-152a are very similar to those of some CFCs (such as CFC-12), it is attracting more and more attention as a substitute for CFC. In my country, as an environmentally friendly and energy-saving working fluid, HFC-152a is widely used in small refrigeration appliances (such as refrigerators, freezers, etc.), and is also used as a single working medium in air conditioners for vehicles or cars, and the demand continues to increase. [0003] According to existing reports, the synthetic methods of 1,1-diflu...

Claims

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Application Information

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IPC IPC(8): C07C19/08C07C17/23C07C17/354B01J23/44B01J23/89B01J23/63
Inventor 刘武灿石能富徐卫国张金柯
Owner SINOCHEM LANTIAN
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