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

A synthetic method, the technology of tetrafluoropropene, applied in two fields, can solve the problems of unreported, less research on the preparation of HFO-1234yf, etc., and achieve the effect of high yield

Inactive Publication Date: 2011-12-07
SHANDONG DONGYUE POLYMER MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] There are few domestic researches on the preparation of HFO-1234yf, and there are almost no reports in this area

Method used

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  • The synthetic method of 2,3,3,3-tetrafluoropropene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Example 1: Step a) Catalyst Ni-Cu-La for preparing 1,1,1,2,3,3-hexafluoropropane by hydrogenation reduction of 1,1,1,2,3,3-hexafluoropropene 2 o 3 / Al 2 o 3 Preparation of:

[0046] The first step is to impregnate the auxiliary agent, weigh La(NO 3 ) 3 ·nH 2 O2.40g is added to 24ml deionized water to prepare La(NO 3 ) 3 solution, add 25g20-40 purpose Al to the solution 2 o 3 , impregnated at room temperature for 40h, then dried overnight at 150°C, and calcined at 500°C for 5h.

[0047] In the second step of impregnation, weigh 29.72gNi(NO 3 ) 2 ·6H 2 O, 6.84gCu(NO 3 ) 2 ·3H 2 O, washed into 20ml deionized water, prepared into a mixed solution of the two, the solid prepared in the first step was added to the mixed solution for immersion, drying and calcination, and the treatment conditions were the same as the first step, thereby preparing the catalyst Ni -Cu-La 2 o 3 / Al 2 o 3

[0048] Take a certain amount of catalyst and put it into a reaction tub...

Embodiment 2

[0050] Embodiment 2: step a) catalyst Ni-Cu-CoO / TiO 2 Preparation of:

[0051] Weigh Co(NO 3 ) 2 ·6H 2 O2.22g is added to 12ml deionized water to prepare Co(NO 3 ) 2 Solution, add 25g 20-40 purpose TiO to the solution 2 , impregnated at room temperature for 40h, then dried overnight at 150°C, and calcined at 500°C for 5h.

[0052] In the second step of impregnation, weigh 7.43gNi(NO 3 ) 2 ·6H 2 O, 11.41gCu(NO 3 ) 2 ·3H 2 O, washed into 12ml deionized water, prepared into a mixed solution of the two, the solid prepared in the first step was added to the mixed solution for immersion, drying and calcination, and the treatment conditions were the same as the first step, thereby preparing the catalyst Ni -Cu-CoO / TiO 2 .

[0053] Catalyst reduction and hydrogenation activity testing methods are the same as in Example 1. Pass hydrogen-nitrogen mixed gas (wherein hydrogen volume ratio is 10%), program temperature reduction, from room temperature to 250 ° C, heating rate ...

Embodiment 3

[0054] Embodiment 3: step b) the preparation of the chromium oxide of catalyst fluorination

[0055] Prepare chromium hydroxide with chromium nitrate solution and ammonia water, filter, wash with water, dry at 90°C, use a tablet molding machine to make a cylindrical shape with a diameter of 3mm and a length of 3mm, and put it into a Hastelloy C-22 In the reaction tube, under nitrogen flow, heat at 450°C for 2h to activate it, then lower the temperature to 200°C, supply fluoride anhydride diluted with nitrogen, and perform fluorination treatment for 5h. Chromium trioxide fluoride is prepared.

[0056] 10 g of the catalyst fluorinated chromium trioxide arranged above was charged into a reaction tube made of Hastelloy C-22 with an inner diameter of 2 cm and a length of 40 cm, and heated to 400° C. while flowing nitrogen gas.

[0057] Change nitrogen into 1,1,1,2,3,3-hexafluoropropane, and pass it into the reaction tube at a flow rate of 30cc / min. The gas at the outlet of the rea...

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Abstract

The present invention provides a method for synthesizing 2,3,3,3-tetrafluoropropene, which uses hexafluoropropene as a starting material, and undergoes multi-step hydrogenation reduction, HF removal and other steps to obtain high-purity target product 2,3 , 3,3-Tetrafluoropropene. The raw material hexafluoropropylene of the method is easy to obtain, and can be prepared by existing methods in the art, and can also be purchased commercially. The prepared 2,3,3,3-tetrafluoropropene is an excellent refrigerant substitute and has the advantages of zero ozone depletion potential (ODP) and low greenhouse effect potential (GWP value of 4).

Description

technical field [0001] The invention relates to a synthesis method of refrigerant, in particular to a synthesis method of 2,3,3,3-tetrafluoropropene (HFO-1234yf). Background technique [0002] The "Montreal Protocol" has determined the phase-out schedule of HCFCs. At present, the substitutes of HCFCs are mainly HFCs and their mixtures, including R-32, R-134a, R-152a and so on. Although the ozone depletion potential (ODP) of HFCs is 0, it has a high greenhouse effect potential (GWP), and has been included in the annex of greenhouse gases by the "Kyoto Protocol". As the greenhouse effect becomes more and more serious, people pay more attention to environmental issues. From the perspective of environmental protection requirements, HFCs are far from ideal substitutes for HCFCs. In order to meet environmental protection requirements, a new generation of refrigerant substitutes is developing towards a low GWP value based on an ODP value of 0. In recent years, it has been found th...

Claims

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Application Information

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IPC IPC(8): C07C21/18C07C17/25
Inventor 韩春华张永明张恒高自宏陈越
Owner SHANDONG DONGYUE POLYMER MATERIAL
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