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The preparation method of 2,3,3,3-tetrafluoropropene

A technology of tetrafluoropropene and pentafluoropropane, which is applied in the field of preparation of a substitute for refrigerant HFC-134a, can solve the problems of harsh reaction conditions, use of toxic organic solvents, and low yield, and achieves mild reaction conditions and high reaction efficiency. Ease of operation and high productivity

Active Publication Date: 2011-12-28
SHANDONG DONGYUE POLYMER MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the deficiencies in the prior art, such as the low yield of the synthesis method, the use of substances such as toxic organic solvents, and relatively harsh reaction conditions, the present invention provides a preparation method for 2,3,3,3-tetrafluoropropene (HFO-1234yf) method

Method used

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Embodiment 1

[0044] The preparation method of embodiment 1,2,3,3,3-tetrafluoropropene (HFO-1234yf)

[0045] (1) Fill the Ni / C catalyst in a tubular reactor with an inner diameter of 2 cm and a length of 40 cm, first fill it with nitrogen, then heat it with steam to 450 ° C, and after passing nitrogen for one hour, pass CHCl 2 CF 2 CF 3 and H 2 Flow through the tube at a flow rate of 30cc / s, then raise the temperature to 500°C, and perform gas chromatographic analysis on the gas samples at the outlet of the reaction tube at the two temperatures. The obtained results are listed in Table 1.

[0046] (2) Using a mixture of fluorinated alumina and chromium fluoride as a catalyst to prepare HFO-1234yf by deHF reaction:

[0047] Catalyst preparation: Fill the solids of 15-20 mesh alumina and 15-20 mesh chromium fluoride in a molar ratio of 1:1 into a tubular reactor, which is heated by steam outside the tubular reactor at 250°C The catalyst was dried by heating under nitrogen purge for 20 mi...

Embodiment 2

[0058] Example 2. Phase studies of mixtures of HF and HFO-1234yf

[0059] A phase study was performed on a composition consisting essentially of HF and HFO-1234yf where the composition was varied and the vapor pressure was measured at 9.3 and 44.4°C. From the phase study data, the azeotrope composition at other temperatures and pressures was calculated. Table 4 provides the experimental and calculated azeotrope compositions for HF and HFO-1234yf at specified temperatures and pressures.

[0060] Table 4

[0061]

[0062]

Embodiment 3

[0063] Example 3, Experimental Research on the Dew Point and Bubble Point Vapor Pressure of HFO-1234yf

[0064] The dew point and bubble point vapor pressures of the compositions described herein, HFO-1234yf, were calculated from measured and calculated thermodynamic properties, and the near-azeotrope range was determined by such that the difference between the dew point pressure and bubble point pressure (based on the bubble point pressure) was equal to or less than a percent Table 5 summarizes the minimum and maximum concentrations of HFO-1234yf expressed (mole percent, % mole) for the three species.

[0065] table 5

[0066]

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Abstract

The invention provides a preparation method of tetrafluoropropene HFO-1234yf, comprising the following steps of: using pentafluoropropane chloride and H2 as reaction raw materials or using perfluoropropane as a reaction raw material, firstly forming 1,1,1,2,2-perfluoropropane intermediate product fluid, and then removing HF under the action of an HF-removing catalyst to prepare 2,3,3,3-tetrafluoropropene (HFO-1234yf). CHxCl3-xCFD2cfCFDx3 is used as an original raw material so as to overcome the defect that raw materials are not easily available; in addition, the reaction is easy to operate and the output is high. The prepared HFO-1234yf has advantages of zero ODP and low GWP, and can be used as an ideal substitute for new-generation automobile air conditioner refrigerant.

Description

technical field [0001] The invention relates to a preparation method of a substitute for refrigerant HFC-134a, in particular to the synthesis and separation of 2,3,3,3-tetrafluoropropene. Background technique [0002] In recent years, the problem of global warming has become increasingly serious, and reducing greenhouse gas emissions has become one of the focuses of global environmental protection. According to the fluorinated greenhouse gas (F-gas) regulations passed by the European Union in 2004, starting from January 1, 2011, the European Union will prohibit the use of refrigerants with a GWP (Global Greenhouse Effect Potential) greater than 150 in new automotive air conditioners. (R134aGWP is 1300 and will be disabled). All new cars will phase out refrigerants with high global warming potential (GWP) and ozone layer depletion potential (ODP) for 6 years from January 1, 2011 to January 1, 2017. Refrigerants with a GWP greater than 150 will be phased out in proportion to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C21/18C07C17/25
Inventor 张永明韩春华张恒高自宏陈越
Owner SHANDONG DONGYUE POLYMER MATERIAL
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