Method for preparing fluorinated alkene by performing dehydrochlorination on chlorofluorocarbon under action of catalyst

A technology for dehydrochlorination and fluorine-containing olefins, which is applied in the direction of dehydrohalogenation preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of short service life of catalysts, high production costs, low yields, etc., and achieve reduction Operating cost, low specification requirement, effect of increased selectivity

Active Publication Date: 2013-12-04
山东华安近代环保科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Chinese patent (publication number: CN101772480) discloses a method of removing HCl by contacting HCFC-244bb with activated carbon at a certain temperature to obtain HFO-1234yf. The conversion rate can reach up to 80%, but there is no corresponding HFO-1234yf selective reporting
[0006] The above preparation method has high requirements on the purity of the raw material HCFC-244bb (generally, the purity of 244bb should be above 95%), while the raw material 2-chloro-1,1,1,2-tetrafluoropropane (abbreviated as HCFC-244bb) It is prepared by the addition of 2-chloro-3,3,3-trifluoropropene (abbreviated as HCFO-1233xf) and HF under the action of a catalyst, w

Method used

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  • Method for preparing fluorinated alkene by performing dehydrochlorination on chlorofluorocarbon under action of catalyst
  • Method for preparing fluorinated alkene by performing dehydrochlorination on chlorofluorocarbon under action of catalyst
  • Method for preparing fluorinated alkene by performing dehydrochlorination on chlorofluorocarbon under action of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0043] Example 1: Preparation of catalyst by impregnation method

[0044] (1) Add 11.0g magnesium nitrate (Mg(NO 3 ) 2 ), 24.0g ytterbium nitrate (Y 2 (NO 3 ) 3 ), 10.0g ferric chloride is dissolved in 80ml distilled water to make a solution, and then the specific surface area is 860m 2 / g of coal-based activated carbon was added as a carrier to the above solution. After being immersed for 8 hours, dried at 120°C for more than 12 hours, and then the precursor was calcined in a muffle furnace at 400°C for 6 hours to prepare a catalyst. :5%wt.Mg-1.5%wt.Y-3.0%wt.Fe / AC, spare.

[0045] (2) The preparation process of the catalyst is basically the same as (1), except that the magnesium nitrate is changed to cesium chloride, the ytterbium nitrate is changed to aluminum sulfate, the iron chloride is changed to lanthanum nitrate, the immersion time is changed to 6h, and the drying temperature Change to 80°C, change the calcination temperature to 450°C, and change the calcination time to 5h ...

Example Embodiment

[0066] Example 2:

[0067] A series of catalysts prepared in the examples were used as dehydrochlorination catalysts. A fixed-bed tubular reactor with a diameter of Φ38mm was filled with 60ml of catalyst. At a reaction temperature of 350°C to 850°C, 80wt.% of 2 -A mixture of chloro-1,1,1,2-tetrafluoropropane, 15wt.% of 2-chloro-3,3,3-trifluoropropene and 5wt.% of HF, passing through the catalyst bed with a residence time of 18s . The product was washed with water and alkali to remove HCl and HF, and then analyzed by gas chromatography. The analysis method was area normalization method. Before the reaction, the catalyst was kept at 400° C. for 2 hours in a hydrogen atmosphere, and then adjusted to the reaction temperature, the reaction materials were switched, and the reaction was performed for 10 hours. The reaction results are shown in Table 1.

[0068] Table 1 Reaction results of Example 2

[0069]

[0070] It can be seen from Table 1 that increasing the reaction temperature can...

Example Embodiment

[0071] Example 3:

[0072] This embodiment uses the same operating conditions as in Example 2, except that the composition of the reaction raw materials is changed to 85wt.% of 2-chloro-1,1,1,2-tetrafluoropropane and 10wt.% of 2-chloro -A mixture of 3,3,3-trifluoropropene and 5wt.% HF, the contact time was changed to 0.5s, 18s, 33s and 60s. The reaction results are shown in Table 2.

[0073] Table 2 Reaction results of Example 3

[0074]

[0075] It can be seen from Table 2 that extending the reaction contact time can significantly increase the conversion of raw materials, but will partially reduce the selectivity of the target product.

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Abstract

The invention belongs to the field of refrigerant, and provides a method for preparing fluorinated alkene by performing dehydrochlorination on chlorofluorocarbon under the action of a catalyst.According to the invention, the novel catalyst is prepared through an impregnation method, reaction of the catalyst and 2-chloro-l, 1, 2-tetrafluoro propane (HCFC-244bb) with lower purity is performed, and then high-temperature gas phase dehydrochlorination reaction is performed to prepare a fluorinated alkene product 2, 3, 3, 3-tetrafluoro propene. Through the adoption of the novel catalyst, the purity requirement on chlorofluoropropane is reduced, so that HCFC-244bb with the purity of 80 percent can be as a raw material, thereby effectively reducing the operating cost of the process; the halohydrocarbon conversion rate is high, and reach up to 60 percent, and the selectivity of the target fluorinated alkene is greater than 90 percent.

Description

technical field [0001] The invention belongs to the field of refrigerants and relates to a fluorine-containing olefin, in particular to a method for preparing fluorine-containing olefin by catalytic dehydrochlorination of chlorofluoroalkane. Background technique [0002] Hydrofluorocarbons (HFCs) are a class of compounds that are currently widely used as refrigerants. However, it has been found that such compounds have a high global warming potential (GWP), and a large amount of emission will cause global warming and aggravate the global greenhouse effect. It has been listed as one of the greenhouse gases by the Kyoto Protocol. For this reason, the world is actively looking for its environmentally friendly alternatives. Fluorine-containing olefins, especially hydrofluoroolefins (hydrofluoroolefins, HFO), such as 2,3,3,3-tetrafluoropropene (abbreviated as HFO-1234yf), are new types of olefins with zero ozone depletion potential (ODP) and low GWP value. Organic fluorides hav...

Claims

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Application Information

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IPC IPC(8): C07C21/18C07C17/25B01J23/83B01J23/10B01J23/78B01J23/86B01J23/26
Inventor 吕剑毛伟王博郝志军杜咏梅秦越杨志强马辉
Owner 山东华安近代环保科技有限公司
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