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Method for synthesizing 2,3,3,3-tetrafluoropropene

A synthetic method, fluorine and chlorine technology, applied in 2 fields, can solve the problems such as the difficulty of catalyst preparation, achieve the effect of major industrial application prospects, easy to obtain, and less by-products

Active Publication Date: 2011-09-28
泉州宇极新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Doulas A et al. with CX 3 CF 2 CH 3 (HCFC-242) as raw material to synthesize HFO-1234yf (see US 2996555 for details), CX 3 CF 2 CH 3 X in (HCFC-242) is F, Cl, Br, and the transformation rate of this preparation method raw material is 60%, but this process catalyst preparation is relatively difficult
[0004] In summary, the process of preparing HFO-1234yf is a systematic process. Among the various process routes for preparing HFO-1234yf, CX 3 CCl=CClX (X=F, Cl), CCl 2 =CClCH 2 Cl, CX 3 CF 2 CH and CF 3 CF 2 CH 2 The process route starting from Cl as the raw material has more commercial advantages, but these synthesis patents are mainly controlled by some international fluorine chemical giants. Domestic research institutions have also begun to study the preparation of HFO-1234yf, but there is almost no such aspect report

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) The raw material DMF (1.25 grams), carbon tetrachloride (45.21 grams), ethylene (15.43 grams) that the telomerization reaction is used are added successively to volume is 120ml, in the stainless steel container that valve is housed, concussion shakes up, as Mix raw materials; (2) in the reactor of the PFE pipe material of 15 inches in length, 1 / 8 inch in diameter, the composite metal filler of iron, chromium, nickel is filled inside, is heated to 120 ℃ in the electric furnace; (3) uses metering Pump mixes raw material with the flow rate of 0.2 milliliters / minute and squeezes in the reactor, and reaction pressure is 0.6Mpa, (4) after reacting 10min, cold trap collects reaction product, measures product composition with GC, and wherein TCP selectivity is 96.5%, Based on carbon tetrachloride, the yield of TCP is 68.2%, and the purity of TCP is 99% after purification by distillation under reduced pressure. (5) Add TCP in a 2L high-pressure reactor with a stirring device...

Embodiment 2

[0037] (1) Add 1.25 grams of DMF, 45.21 grams of carbon tetrachloride, and 15.43 grams of ethylene in a stainless steel container with a volume of 120 ml, and shake it well as a mixed raw material; (2) 15 inches in length and 1 in diameter / 8-inch PFE pipe reactor, filled with iron, chromium, nickel composite metal filler, heated to 120 ° C in an electric furnace; (3) use a metering pump to drive the mixed raw materials into the In the reactor, the reaction pressure is 0.8MPa, (4) after reacting for 30min, the cold trap collects the reaction product, and measures the product composition with GC, wherein the TCP selectivity is 97.6%, and in terms of carbon tetrachloride, the productive rate of TCP is 72.4% %; The reacted mixture reclaims unreacted raw material and cocatalyst by the method for distillation, and underpressure distillation obtains the TCP that purity is 99%. (5) Add TCP in a 2L autoclave with stirring device, and chlorine gas is added to the autoclave through a po...

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PUM

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Abstract

The invention relates to a method for synthesizing 2,3,3,3-tetrafluoropropene, and belongs to the field of fluorine-containing refrigerants. The method comprises the following steps of: performing telomerization on carbon tetrachloride (CCl4) and ethylene serving as raw materials to generate CCl3CH2CH2Cl, chlorinating to obtain CCl3CHClCH2Cl, and performing fluorine-chlorine exchange and HF removal under the catalytic condition to obtain a final product HFO-1234yf. The raw materials are low-cost and readily available, so raw material cost in the process of producing the HFO-1234yf is reduced; the previous two steps in the method are liquid phase reaction, the reaction temperature is low, and reaction pressure is close to normal pressure; the subsequent two steps are gas phase continuous reaction, pressure and temperature are relatively low, and reaction conditions are easy to control, so equipment is relatively simple; in addition, the conversion rate in each step of the preparation method is high, a few byproducts are generated, and the yield of the target product is high, so the method has a wide industrial application prospect.

Description

technical field [0001] The invention belongs to the field of environment-friendly fluorine-containing refrigerants, and in particular relates to a new synthesis method of 2,3,3,3-tetrafluoropropene. Background technique [0002] Fluorinated refrigerants for industrial applications require short atmospheric survival time (ALT), low atmospheric ozone depletion potential (ODP) and greenhouse effect potential (GWP), non-toxic, non-flammable, non-explosive, chemical and thermal stability Better, it can adapt to different working temperature ranges. 2,3,3,3-Tetrafluoropropene (HFO-1234yf), as a single working refrigerant, has excellent environmental parameters and good cooling effect, and if HFO-1234yf is used as an automobile refrigerant, the original vehicle refrigerant can continue to be used Air-conditioning systems, so HFO-1234yf is considered to be a potential new-generation automotive refrigerant substitute, and has been accepted by automakers in Western Europe. [0003] ...

Claims

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Application Information

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IPC IPC(8): C07C21/18C07C17/35
Inventor 周晓猛贾晓卿鲍鹏
Owner 泉州宇极新材料科技有限公司
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