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Calcium fluoride based fluorinated catalyst and application thereof

A technology based on fluorination catalysts and catalysts, applied in the direction of physical/chemical process catalysts, organic chemistry, chemical instruments and methods, etc., can solve the problems of low catalytic activity of catalysts, poor catalytic activity, poor catalytic activity, etc., and achieve simple preparation process , less industrial waste, good catalytic activity effect

Active Publication Date: 2011-02-02
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Most of the gas-phase fluorination catalysts used in practice are chromium-containing catalysts. It has been proved that chromium compounds are toxic and will cause damage to the human digestive tract and kidneys, and high-valent chromium has a strong carcinogenic effect, and its production and use will harm people and the environment. cause harm,
[0008] In order to solve the above problems, a chromium-free fluorination catalyst is used to replace the chromium-containing fluorination catalyst. For example, Chinese patents CN107817A and CN1111606A disclose a chromium-free catalyst, which is to support zinc on alumina, halogenated aluminum oxide or aluminum oxyhalide, but This catalyst activity is relatively poor; Chinese patent CN1680029A discloses a kind of chromium-free catalyst, and this catalyst will antimony halide n Cl 5-n ) is supported on calcium fluoride, but the catalytic activity of the catalyst is low, and the antimony halide is easily lost during the fluorination reaction, and the catalyst has poor thermal stability
[0009] The currently reported chromium-free catalysts have poor catalytic activity and are easily lost, so they have no practical application value

Method used

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  • Calcium fluoride based fluorinated catalyst and application thereof
  • Calcium fluoride based fluorinated catalyst and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Implementation with reference to the mass percent composition of the following fluorination catalyst precursor:

[0034] FeCl 3 30.0%

[0035] NiCl 2 0.5%

[0036] CaCO 3 69.5%

[0037] Ferric chloride and NiCl 2 Dissolve in water to make impregnation solution, add CaCO 3 , impregnated for 1 hour, evaporated to dryness by rotary evaporation, and dried in an oven at 120°C for 8 hours to obtain a catalyst precursor, which was calcined in a muffle furnace at 450°C for 8 hours, and then loaded into a tubular reactor , the temperature was raised to 300°C, fluorinated with hydrogen fluoride gas for 1 hour, and then the temperature was raised to 400°C at a heating rate of 1°C / min, and the fluorination was continued for 8 hours to prepare a calcium fluoride-based fluorination catalyst.

[0038] In a nickel tube fixed-bed tubular reactor with an internal diameter of 38mm, 60ml of the above-mentioned calcium fluorid...

Embodiment 2

[0041] The preparation process of the catalyst is basically the same as in Example 1, except that the NiCl 2 Change to CoCl 2 , with reference to the mass percent composition of the following fluorination catalyst precursor:

[0042] FeCl 3 30.0%

[0043] CoCl 2 0.5%

[0044] CaCO 3 69.5%

[0045] The obtained catalyst precursor is roasted and fluorinated with HF to prepare a calcium fluoride-based fluorination catalyst.

[0046] In a nickel tube fixed-bed tubular reactor with an internal diameter of 38 mm, 60 ml of the above-mentioned prepared fluorination catalyst are charged, and HF and HCC-240fa are introduced to react, and the molar ratio of HF / HCC-240fa is controlled to be 10: 1. The contact time is 5.5 seconds, the reaction temperature is 200°C, and after 20 hours of reaction, the reaction product is washed with water and alkali to remove HCl and HF, and the conversion rate of HCC-240fa is 100% according to gas chromatography a...

Embodiment 3

[0048] The preparation process of the catalyst is basically the same as in Example 1, except that the NiCl 2 Change to ZnCl 2 , with reference to the mass percent composition of the following fluorination catalyst precursor:

[0049] FeCl 3 30.0%

[0050] ZnCl 2 0.5%;

[0051] CaCO 3 69.5%

[0052] The obtained catalyst precursor is roasted and fluorinated with HF to prepare a calcium fluoride-based fluorination catalyst.

[0053] Inside diameter is in the nickel tube fixed-bed tubular reactor of 38mm, the above-mentioned fluorination catalyst that packs into 60ml makes, feeds HF and tetrachloropropane to react, and the mol ratio of control HF / tetrachloropropane is 15: 1, The contact time is 3.2 seconds, the reaction temperature is 260°C, and after 20 hours of reaction, the reaction product is washed with water and alkali to remove HCl and HF, and the conversion rate of tetrachloropropane is 100% according to gas chromatography analys...

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Abstract

The invention discloses a calcium fluoride based fluorinated catalyst and application thereof. A precursor of the catalyst uses calcium carbonate as a carrier, ferric trichloride and a soluble salt of a cocatalyst selected from one of Ni<2+>, Co<2+>, Zn<2+>, Mn<2+>, or Cu<2+>, and the like are soaked. The precursor of the catalyst comprises the following components in percentage by mass of: 2.0-50.0 percent of ferric trichloride, 0-2.0 percent of cocatalyst and 48.0-98.0 percent of calcium carbonate, wherein the cocatalyst is an Ni<2+>, Co<2+>, Zn<2+>, Mn<2+>, or Cu<2+> soluble salt; and the precursor of the catalyst is roasted at a temperature of 400-500 DEG C, and the calcium fluoride based fluorinated catalyst is prepared by the fluorination of hydrogen fluoride gas at a temperature of350-450 DEG C. The prepared fluorinated catalyst has the characteristics of no chromium, environment protection, good catalysis activity, and the like, and is mainly used for preparing hydrogen fluroolefins or hydrogen fluro chloroalkene by halohydrocarbon.

Description

technical field [0001] The invention relates to a calcium fluoride-based fluorination catalyst and its application. In particular, it relates to a fluorination catalyst for the vapor phase fluorination of halocarbons to produce hydrofluoroolefins (HFOs) or hydrofluorochloroolefins (HCFOs). Background technique [0002] In the fluorine chemical industry, the method of gas-phase fluorinated halogenated hydrocarbons is often used to prepare fluorinated olefins and hydrofluorochloroolefins. This method has the advantages of simple equipment, easy continuous large-scale production, and safety. The fluorination catalyst plays a central role in the gas-phase fluorination of halogenated hydrocarbons. At present, the gas-phase fluorination catalysts used in industry are chromium-containing fluorination catalysts. [0003] Chinese patent CN94106793.9 has reported that Cr(NO 3 ) 3 and In(NO 3 ) 3 The mixture is prepared as a fluoride precursor, and after roasting and HF fluorinat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/20B01J27/128C07C21/18B01J27/138
Inventor 王博吕剑寇联岗马洋博郝志军张伟何飞刘波
Owner XIAN MODERN CHEM RES INST
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