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A kind of synthetic method of 1,3,3,3-tetrafluoropropene

A technology of tetrafluoropropene and synthesis method, which is applied in the fields of halogen addition preparation, organic chemistry, dehydrohalogenation preparation, etc., to achieve the effects of less equipment investment, good selectivity and simple operation

Active Publication Date: 2019-05-14
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The selectivity of HFO-l234ze in this method is less, but it has some value for the co-production of HFO-1234vf

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0026] The present invention is a kind of synthetic method of 1,3,3,3-tetrafluoropropene, comprising the following steps:

[0027] (1) Add the mixture of elemental iodine, iodine pentafluoride and catalyst in the reactor, control the reaction temperature, feed trifluoropropene, when the system pressure is stable, stop the reaction to obtain 1,3,3,3-tetrafluoro -2-iodo-propane, the mass ratio of elemental iodine to iodine pentafluoride in the mixture is 1:0.4~0.5, after optimization, the mass ratio of elemental iodine to iodine pentafluoride is 1:0.44~0.48, elemental iodine and catalyst The mass ratio of the elemental iodine to the catalyst is 1:0.01~0.05. After optimization, the mass ratio of the elemental iodine to the catalyst is 1:0.02~0.03. By controlling the mass ratio of the elemental iodine to the catalyst, the quality of the reacted material is better and the reaction time is shorter. , to speed up the reaction rate, the reaction temperature is -15 to 35°C. After optim...

Embodiment 1

[0035] In a 10L horizontal reactor, drop into 8kg elemental iodine, 200g Sb, 50g of sodium iodide, after the nitrogen replacement is qualified, add 4.0kg of iodine pentafluoride (IF 5 ), the reaction temperature is 15°C, trifluoropropene is fed continuously or intermittently, and the reaction pressure is 0.3MPa. When the pressure is stable, stop feeding trifluoropropene. Warm up the reaction kettle to steam out 1,3,3,3-tetrafluoro-2-iodo-propane, pass through lye with a concentration of 15% and a temperature of 45°C, dry, condense, and collect to obtain 1,3,3,3-tetrafluoro The fluoropropylene product has a purity of 99.5% and a yield of 98.2%.

Embodiment 2

[0037] In a 10L horizontal reactor, drop into 8kg elemental iodine, 200g Sb, 50g of sodium iodide, after the nitrogen replacement is qualified, add 3.2kg of iodine pentafluoride (IF 5 ), the reaction temperature is 5°C, and trifluoropropene is fed continuously or intermittently, and the reaction pressure is 0.3MPa. When the pressure is stable, stop feeding trifluoropropene. Raise the temperature of the reaction kettle to steam out 1,3,3,3-tetrafluoro-2-iodo-propane, pass through the alkali solution with a concentration of 20% and a temperature of 45°C, dry, condense, and collect to obtain 1,3,3,3-tetrafluoro The fluoropropylene product has a purity of 99.4% and a yield of 97.3%.

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PUM

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Abstract

The invention discloses a synthetic method for 1,3,3,3-tetrafluoropropene. The synthetic method comprises the following steps: (1) adding a mixture of iodine, iodine pentafluoride and a catalyst into a reactor, controlling reaction temperature, introducing trifluoropropene, and stopping the reaction when system pressure is stable so as to obtain 1,3,3,3-tetrafluoro-2-iodopropane, wherein a mass ratio of iodine to iodine pentafluoride is 1: 0.4-0.5, a mass ratio of iodine to the catalyst is 1: 0.01-0.05, reaction temperature is -15 to 35 DEG C and reaction pressure is 0.1 to 0.6 MPa; and (2) evaporating the material 1,3,3,3-tetrafluoro-2-iodopropane in the reactor, introducing the evaporated 1,3,3,3-tetrafluoro-2-iodopropane into a reactor filled with alkali lye, carrying out a reaction at normal pressure, and subjecting a gas phase product to drying and compression so as to obtain the product 1,3,3,3-tetrafluoropropene, wherein reaction temperature is 35 to 80 DEG C. The method provided by the invention has the advantages of simple equipment, high operation security, high product purity, etc.

Description

technical field [0001] The invention relates to a synthesis method of 1,3,3,3-tetrafluoropropene. Background technique [0002] In the fluorine refrigeration industry, 1,3,3,3-tetrafluoropropene (HFO-1234ze), 2,3,3,3-tetrafluoropropene (HFO-1234yf), trifluoroiodomethane (FIC-l311) and l , 2,3,3,3-Pentafluoropropene (HFC-1225ye) and Ozone Depletion Potential (ODP) of 0, low greenhouse effect potential (GWP=6), is considered as the third generation refrigerant, as an alternative Widely used high-GWP 1,1,1,2-tetrafluoroethane (HFC-134a), l,1,1,2,2-pentafluoroethane (HFC-125) and other second-generation refrigerant replacement Taste. HFO-l234ze is non-toxic, non-flammable, and has relatively stable chemical properties. It is an important hydrofluoroolefin (HFOs) Ⅲ. It is widely used in foaming agent, refrigerant, aerosol propellant, cleaning agent, etc., and HFO-1234ze is an important chemical material intermediate. [0003] The synthesis methods of 1,3,3,3-tetrafluoropropen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/25C07C21/18
CPCC07C17/04C07C17/25C07C21/18C07C19/16
Inventor 耿为利周强王宗令吴庆吕秉达徐锋
Owner JUHUA GROUP TECH CENT
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