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Catalytic preparation method of trifluoroethylamine compound

A technology of trifluoroethylamine and trifluoroacetaldehyde, which is applied in the field of preparation of 2,2,2-trifluoroethylamine compounds, can solve the problems of poor industrialization feasibility, difficult post-processing, and numerous steps, and reduce risks High reliability, high industrial production value, simple post-processing effect

Inactive Publication Date: 2018-12-28
张海英
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The raw material cost of this route is relatively cheap, but there are many steps, difficult post-processing, low overall yield, and poor industrialization feasibility

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] Preparation of ruthenium-containing mesoporous molecular sieve carrier

[0068] Stir and mix 1.0 mol sodium silicate solution and 0.2 mol dodecyltrimethylammonium bromide solution, adjust the pH to 7.5, and stir evenly until a gel is formed; drop 30 mmol ruthenium trichloride solution into the formed Stir in the silica gel until uniform, adjust the pH to 10 with ammonia water, and continue to stir at room temperature for 2 h. The obtained mixed gel is hydrothermally reacted in an autoclave at 135°C for 24 h. After the reaction is completed, cool to room temperature, filter the product, and Washed with water and dried to obtain the molecular sieve precursor, which was placed in a muffle furnace and heated to 550 °C for 5 h to obtain a ruthenium-containing mesoporous molecular sieve catalytic carrier.

[0069] Further, the desired catalyst can be loaded on the prepared ruthenium-containing mesoporous molecular sieve carrier according to the general molecular sieve loading...

Embodiment 2

[0071] Preparation of trifluoroethylamine

[0072] (1) 1600 grams of ammonia content is 30wt% ammoniacal liquor, and 600 grams of trifluoroacetaldehyde hydrate enters its corresponding thermoregulatory preheater to preheat to 25 ℃ by respective metering pumps, after preheating, pass through respective The outlet conduit enters the static mixer for mixing, and the reaction materials are mixed in the mixer for 10 minutes;

[0073] (2) the mixed reaction material enters the tubular fixed-bed reactor containing the ruthenium-containing mesoporous molecular sieve prepared by the above-mentioned embodiment and supports 3wt% palladium acetate catalyst, and simultaneously pumps trifluoroacetaldehyde by the metering pump connected to the reactor Hydrate equimolar equivalent ammonium formate solution, so that the reaction material undergoes condensation-reduction reaction in the presence of ammonia atmosphere and ammonium formate, adjust the reaction temperature to 30 ° C, control the f...

Embodiment 3

[0078] (1) From the trifluoroacetaldehyde storage tank, the trifluoroacetaldehyde gas metering pump of 5mol is mixed in the Venturi gas-liquid mixer containing the ammonia gas atmosphere of 28% ammonia solution, and the ammonia solution of the mixer Containing 20mol of ammonia, fully mixed to form a hydrate of trifluoroacetaldehyde and water in the mixer, thereby obtaining a mixed solution of trifluoroacetaldehyde hydrate-ammonia water;

[0079] (2) the mixed reaction material enters the tubular fluidized bed reactor filled with the ruthenium-containing mesoporous molecular sieve prepared in the above-mentioned embodiment 1 and supports three (triphenylphosphine) ruthenium dichloride catalysts, wherein the catalyst load is 5wt%, while pumping formic acid of trifluoroacetaldehyde hydrate 0.8 molar equivalent in the reactor through the metering pump connected to the reactor, adjust the reaction temperature to be 25 ° C, control the material flow rate so that the residence time of...

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PUM

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Abstract

The invention provides a preparation method of 2,2,2-trifluoroethylamine. Trifluoroformaldehyde or trifluoroacetaldehyde hydrate and ammonia water are taken as raw materials and subjected to reactionin the presence of a mesoporous molecular sieve supported catalyst and a suitable hydrogen donor, a product is subjected to secondary reduction, and trifluoroethylamine is prepared. The process does not need high temperature or high pressure, has mild reaction conditions, high conversion rate, few byproducts and low cost, is clean and environmentally friendly, conforms to the trend of green chemical industry nowadays and has higher industrial production value, and a catalyst is easy to recycle.

Description

technical field [0001] The invention relates to a preparation method of a 2,2,2-trifluoroethylamine compound, belonging to the fields of pharmaceutical intermediates and organic synthesis. Background technique [0002] Trifluoroethylamine, especially 2,2,2-trifluoroethylamine is an important organic intermediate, and derivatives based on trifluoroethylamine are also organic molecules with important biological activities, which can be used as fine chemical products or medicine or natural products Synthetic intermediates. For example, trifluoroethylamine derivatives can be used to synthesize highly active insecticides, acaricides and ovicides, as well as herbicides, and are widely used in pesticides, chemicals and other industries. In the field of medicine, it can also be used as a medicine intermediate to prepare medicines for treating diabetes instead of biguanide and its derivatives. [0003] Since 2,2,2-trifluoroethylamine derivatives have high biological activity and ar...

Claims

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Application Information

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IPC IPC(8): C07C209/26C07C211/15
CPCC07C209/26C07C211/15Y02P20/584
Inventor 张海英
Owner 张海英
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