Immobilized type non-toxic catalyst and method for synthesizing N-phenylmaleimide and N-substitutional phenylmaleimide

A technology of phenyl substitution and catalyst, which is applied in the field of non-toxic catalysts and the preparation of fine organic compounds, can solve the problems of difficult acid wastewater treatment, unfavorable for large-scale production, unfavorable for environmental protection, etc., and achieves easy recycling and improved catalysis Active, reduce equipment corrosion effect

Inactive Publication Date: 2013-02-06
WUHAN NEW CONCEPT CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, this method still has some disadvantages that are not conducive to environmental protection, such as some difficult-to-treat acid waste water will be produced in the production, and orga

Method used

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  • Immobilized type non-toxic catalyst and method for synthesizing N-phenylmaleimide and N-substitutional phenylmaleimide

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Experimental program
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Effect test

Embodiment 1

[0039] Embodiment 1: A kind of preparation method of immobilized non-toxic catalyst, with 4A type zeolite molecular sieve carrier and zirconium organophosphine chelate aqueous solution as starting raw material, successively prepare through the following steps:

[0040] (1) In an environment of 20°C, dilute 40 parts of an aqueous solution of zirconium organophosphine chelate with a concentration of 50% zirconium organophosphine chelate by weight ratio through 60 parts of clean tap water to obtain a concentration of zirconium organophosphine chelate of 20% % impregnating liquid, 6g4A type zeolite molecular sieve carrier is added in 36g prepared impregnating liquid and impregnated for 7 hours, and reaction is bonded, wherein the mass ratio of 4A type zeolite molecular sieve carrier and zirconium organophosphine chelate aqueous solution is 1:6 ;

[0041] (2) Filter and dehydrate the impregnated 4A zeolite molecular sieve carrier, dry the filtered carrier in a constant temperature ...

Embodiment 2

[0042] Embodiment 2: A kind of preparation method of immobilized non-toxic catalyst, with 4A type zeolite molecular sieve carrier and hafnium organophosphine chelate aqueous solution as starting raw material, successively prepare through following steps:

[0043] (1) In an environment of 30°C, dilute 45 parts of hafnium organophosphine chelate aqueous solution with a concentration of 50% hafnium organophosphine chelate by weight ratio through 55 parts of clean tap water to obtain a hafnium organophosphine chelate concentration of 25% Then, add the weighed 10g 4A type molecular sieve carrier into 50g of the prepared immersion liquid for immersion for 5 hours, and react to bond, wherein the mass ratio of the 4A type molecular sieve carrier to the immersion liquid is 1:5;

[0044] (2) Filter and dehydrate the impregnated 4A molecular sieve carrier, dry the filtrate in a constant temperature oven at 110°C for 4 hours, then place it in a muffle furnace, and raise the temperature to ...

Embodiment 3

[0045] Embodiment 3: A kind of preparation method of immobilized non-toxic catalyst, with 10X zeolite molecular sieve carrier and zirconium organophosphine chelate aqueous solution as starting raw material, successively prepare through the following steps:

[0046] (1) At 25°C, select 50g of zirconium organophosphine chelate aqueous solution with a zirconium organophosphine chelate concentration of 50% as the impregnation solution, and then add 5g of 10X zeolite molecular sieve carrier weighed into the prepared impregnation solution Immersed in medium for 6 hours, reaction bonding, wherein the mass ratio of 10X zeolite molecular sieve carrier to impregnating liquid is 1:10;

[0047] (2) Filter and dehydrate the impregnated 10X zeolite molecular sieve carrier, dry the filtered carrier in a constant temperature oven at 60°C for 6 hours, then place it in a muffle furnace, and raise the temperature to 300°C at a rate of 5°C / sec. Calcined for 6 hours to obtain a solid-supported non...

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Abstract

The invention provides an immobilized type non-toxic catalyst and a method for synthesizing N-phenylmaleimide and N-substitutional phenylmaleimide. The immobilized type non-toxic catalyst is formed by utilizing a porous zeolite molecular sieve as a carrier, impregnating the porous zeolite molecular sieve into water solution of titanium organic phosphonic chelate or zirconium organic phosphonic chelate or hafnium organic phosphonic chelate for 6-10 hours, reacting and bonding, drying and roasting. Pure products of the N-phenylmaleimide and N-substitutional phenylmaleimide are obtained by adding maleic anhydride and aniline or maleic anhydride and aniline derivatives into the immobilized type non-toxic catalyst as raw materials, sequentially acylating, dehydrating and cyclizing and recrystallizing. The immobilized type non-toxic catalyst is non-toxic and environment-friendly, the method of synthesizing the N-phenylmaleimide and N-substitutional phenylmaleimide is environment-friendly, convenient in operation procss and high in product purity and yield, and solvent used is non-toxic, convenient to recover and reusable.

Description

technical field [0001] The invention relates to a non-toxic catalyst and its application in the preparation of fine organic compounds, in particular to a solid-supported non-toxic catalyst and its synthesis of N-phenylmaleimide and N-phenyl-substituted maleimide methods in imine. Background technique [0002] N-phenylmaleimide compound (N-PMI for short) is an important organic chemical raw material. It is a five-membered ring monomer with a 1,2-disubstituted vinyl structure. In the process of processing, if it is embedded in the polymer chain, it can increase the internal rotation resistance of the chain, thereby improving the heat resistance, impact resistance, heat solubility and processability of the polymer. Therefore, it is used as a heat-resistant modifier for ABS resin (acrylonitrile-butadiene-styrene), polyvinyl chloride (PVC), polymethyl methacrylate (MMA); it can also be used as a A cross-linking agent; can prepare adhesives to improve the adhesion of metal and r...

Claims

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Application Information

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IPC IPC(8): B01J31/24C07D207/448C07D207/452
Inventor 祁正大王贤东
Owner WUHAN NEW CONCEPT CHEM
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