Preparation method of 2, 3, 3, 3-tetrafloropropylene

A technology of tetrafluoropropene and difluoromonochloromethane, which is used in the preparation of halogenated hydrocarbons, chemical instruments and methods, organic chemistry, etc., can solve the problems of complex separation mixture, many side reactions, short production cycle, etc., and avoid serious problems. The production of toxic perfluoroisobutene, the reduction of the probability of side reactions, and the effect of inhibiting carbon formation

Active Publication Date: 2014-06-04
SHANDONG DONGYUE POLYMER MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the reaction temperature of this method is as high as above 900°C, there are many side reactions and serious carbon formation, so the reaction pipeline needs to be dredged regularly, the production cycle is short, the efficiency is low, and the yield of this method is only 13%. Therefore, it is di

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0033] Example 1:

[0034] A method for preparing 2,3,3,3-tetrafluoropropene, using difluoromonochloromethane (R 22 ) And monochloromethane (methyl chloride) as raw materials, cracking reaction occurs under superheated steam dilution conditions to obtain 2,3,3,3-tetrafluoropropene. The chemical reaction equation is as follows:

[0035] 2CHClF 2 +CH 3 Cl→CF 3 CF=CH 2 +3HCl

[0036] Fill a steel cylinder with a volume of 8L with 16.8g of monochloromethane and 86.5g of difluorochloromethane

[0037] Add 6000g pure water into the jacketed reactor with a thermometer, pressure gauge, and pressure reducing valve with a volume of 10L. The ferrule is filled with heat-conducting silicone oil and connected to the circulating oil pump. Set the circulating oil pump temperature to 130°C to make the clamping The water vapor generated by the thermometer connected to the set of reaction kettles is passed into the tube furnace, where the temperature of the tube furnace is set to 1000°C, thereby genera...

Example Embodiment

[0041] Example 2: As described in Example 1, the difference is:

[0042] The reaction device is first fed with superheated steam to preheat the reaction pipeline. When the temperature meter connected to the reaction pipeline stabilizes at 700°C, adjust the flow rate of the volume flow meter connected to the steam pipeline to 209.2ml / s, and adjust the flow rate of the reaction raw materials. The meter flow rate is 41.8ml / s, and the reaction product mixed stream flows out of the reaction tube and enters the quenching device, the secondary alkaline washing device, and the drying device. The product stream obtained after drying is collected, and the mixed product is analyzed by gas chromatography 2,3,3,3 -The mass fraction of tetrafluoropropylene is 42.5%.

Example Embodiment

[0043] Example 3: As described in Example 1, the difference is:

[0044] The reaction device is first fed with superheated steam to preheat the reaction pipeline. When the temperature meter connected to the reaction pipeline stabilizes at 700°C, adjust the flow rate of the volumetric flow meter connected to the steam pipeline to 225.9ml / s, and adjust the flow rate of the reaction raw materials. The meter flow rate is 25.1ml / s, the reaction product mixed stream flows out of the reaction tube and then enters the quenching device, the secondary alkali washing device, and the drying device. The product stream obtained after drying is collected, and the mixed product is analyzed by gas chromatography 2,3,3,3 -The mass fraction of tetrafluoropropylene is 45.9%.

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Abstract

The invention provides a preparation method of 2, 3, 3, 3-tetrafloropropylene. The method comprises the following steps: with monochlorodifluoromethane and monochloro methane which are in a molar ratio of (0.5-4):1 as reaction raw materials, preheating the reaction raw materials, then mixing with superheated steam, wherein the volume ratio of the superheated steam to the reaction raw materials is (1-20):1, the temperature of the superheated steam is 900-1100 DEG C, the temperature in the reaction section is 600-1100 DEG C, and the stay time of reactants in the reaction section is 0.01-1s; and quenching, deacidifying, drying and rectifying and separating the product mixed flow to obtain 2, 3, 3, 3-tetrafloropropylene. The method provided by the invention overcomes the deficiency that a hollow tube is prone to carbonization in pyrolysis and side reactions are complex, the equipment maintenance rate is reduced, and meanwhile, the reaction period is prolonged, and the utilization ratio of the device is improved. The method provided by the invention has the characteristics of use of easily available raw materials, simple reaction process and the like. The obtained 2, 3, 3, 3-tetrafloropropylene has the advantages of zero ODP (Ozone Depletion Potential) and low GWP (Global Warming Potential), and is used as a substituent of automotive air conditionor refrigerant.

Description

technical field [0001] The invention relates to a method for preparing hydrofluoroolefins, in particular to a method for preparing 2,3,3,3-tetrafluoropropene (HFO-1234yf). technical background [0002] The "Montreal Protocol" has determined the phase-out schedule of HCFCs. With the phase-out of HCFCs, the third-generation fluorine-containing refrigerant HFCs, as a substitute for HCFCs, has attracted more and more attention. However, among many HFCs substitutes , although they all have ozone depletion potential (that is, ODP is zero) and have no detrimental effect on the ozone layer, many HFCs have high greenhouse effect potential, such as 1,1,1,2-tetrafluoroethane (HFC- 134a) has zero ODP, but its GWP is as high as 1300. As the greenhouse effect becomes more and more serious, people pay more attention to environmental issues. The European Union requires that the GWP value of all new vehicle refrigerants in its member states cannot exceed 150. In view of this, the Kyoto Proto...

Claims

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Application Information

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IPC IPC(8): C07C21/18C07C17/26
Inventor 韩春华张恒张永明魏茂祥董海红
Owner SHANDONG DONGYUE POLYMER MATERIAL
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