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Ionic liquid modified silica gel loaded aluminum chloride catalyst

A technology of ionic liquid and catalyst, which is applied in the field of preparation of phenylphosphine dichloride on liquid modified silica gel supported aluminum chloride catalyst, which can solve the problems of high requirements for reaction equipment and achieve simple post-processing, high yield and simple preparation Effect

Active Publication Date: 2020-09-22
SHANDONG DIAI BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the reaction needs to be carried out under high temperature and high pressure. Phosphorus trichloride is highly corrosive, and the requirements for reaction equipment are relatively high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] a. Mix and stir 25g of 1-ethyl-3-methylimidazolium tetrafluoroborate and 5g of 300-400 mesh silica gel evenly, heat to 120°C, keep stirring at this temperature for 2 hours, then cool to room temperature, the solid is precipitated, After filtering and drying, ionic liquid modified silica gel is obtained;

[0027] b. Add 3g of ionic liquid-modified silica gel to 15ml of ethanol, add 0.5g of aluminum chloride under stirring, continue stirring for 2 hours, remove ethanol under reduced pressure, heat the mixture to 120°C under nitrogen protection, and react for 10 hours to obtain a yellow powder , which is the ionic liquid modified silica gel supported aluminum chloride catalyst.

Embodiment 2

[0029] a. Mix and stir 30g of 1-butyl-3-methylimidazolium tetrafluoroborate and 3g of 300-400 mesh silica gel evenly, heat to 150°C, keep stirring at this temperature for 1 hour, then cool to room temperature, the solid is precipitated, After filtering and drying, ionic liquid modified silica gel is obtained;

[0030] b. Add 2g of ionic liquid-modified silica gel to 20ml of ethanol, add 2g of aluminum chloride under stirring, continue stirring for 2 hours, remove ethanol under reduced pressure, and heat the mixture to 160°C under nitrogen protection. After reacting for 5 hours, a yellow powder is obtained. That is, the silica gel supported aluminum chloride catalyst modified by the ionic liquid.

Embodiment 3

[0032] a. Mix 30g of 1-butyl-3-methylimidazolium bromide and 5g of 300-400 mesh silica gel and stir evenly, heat to 150°C, keep stirring at this temperature for 1 hour, then cool to room temperature, and the solid is precipitated, filtered, and dried After drying, the silica gel modified by ionic liquid is obtained;

[0033] b. Add 2g of ionic liquid-modified silica gel to 18ml of ethanol, add 1.5g of aluminum chloride under stirring, continue stirring for 1 hour, remove the ethanol under reduced pressure, heat the mixture to 150°C under the protection of nitrogen, and react for 5 hours to obtain a yellow powder , which is the ionic liquid modified silica gel supported aluminum chloride catalyst.

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PUM

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Abstract

The invention provides an ionic liquid modified silica gel loaded aluminum chloride catalyst for catalytic preparation of dichlorophenylphosphine. The preparation method comprises the following stepsof: a, uniformly mixing and stirring ionic liquid and silica gel, performing heating to 100-150DEG C, keeping the temperature, performing stirring for 1-2h, then conducting cooling to room temperature, and precipitating, filtering and drying the solid to obtain ionic liquid modified silica gel; and b, adding the ionic liquid modified silica gel obtained in the step a into ethanol, adding aluminumchloride under stirring, continuously performing stirring for 1-2h, removing ethanol under reduced pressure, heating the mixture to 120-160DEG C under the protection of nitrogen, and carrying out reaction for 5-10h to obtain yellow powder. The prepared catalyst has stable properties and high reaction activity, a high product yield (90% or above) can be achieved by using a very small amount of a catalyst in the preparation process of dichlorophenylphosphine, post-treatment of the catalyst is simple, the catalyst can be removed from the system only through filtration, and the catalyst can be reutilized after drying.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a liquid modified silica gel supported aluminum chloride catalyst and the use of the catalyst in preparing phenylphosphine dichloride. Background technique [0002] Phenyl dichloride phosphine (DCPP), also known as phenyl phosphine dichloride, is one of the most important monomers for the synthesis of aromatic organic phosphine compounds. It is also used for the preparation of flame retardants, plasticizers, pesticides, nylon stabilizers, Intermediates of dyes and photoinitiators. Among them, phosphine-based reactive flame retardants prepared from phenylphosphine dichloride are widely used in the preparation of permanent flame-retardant products from polyester resins. [0003] At present, the synthetic method of phenylphosphine dichloride mainly contains following several kinds: [0004] (1) Aluminum trichloride catalytic method. With aluminum trichloride as catalyst, benzene ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/52B01J31/02
CPCC07F9/52B01J31/0295B01J31/0284B01J2231/4277
Inventor 李娟
Owner SHANDONG DIAI BIOTECH CO LTD
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