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Novel method for synthesizing polyethoxy acrylate with fluorenyl structure by using immobilized catalyst

A technology of ethoxylated acrylic acid and immobilized catalyst, which is applied in the direction of preparation of organic compounds, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problem of non-conformity with sustainable green and environmental protection chemical industry development, increase of solid waste and liquid Waste, unable to recycle and reuse problems, etc., to achieve the effect of easy separation, pollution reduction and high yield

Inactive Publication Date: 2021-06-25
沧州临港丰亚化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalyzer that this method uses is p-toluenesulfonic acid, but p-toluenesulfonic acid is as a kind of organic strong acid soluble in water, can't recycle and reuse, and reaction yield is only about 75%~85%, and production cost is on the high side, not only increases The amount of solid waste and liquid waste in the reaction is reduced, resulting in waste of resources and pollution to the environment, which does not meet the requirements of sustainable green and environmentally friendly chemical development.

Method used

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  • Novel method for synthesizing polyethoxy acrylate with fluorenyl structure by using immobilized catalyst
  • Novel method for synthesizing polyethoxy acrylate with fluorenyl structure by using immobilized catalyst
  • Novel method for synthesizing polyethoxy acrylate with fluorenyl structure by using immobilized catalyst

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Prepare a solid-supported catalyst: use diatomaceous earth as a carrier, load phosphotungstic acid, and the mass percentage of phosphotungstic acid is 20%;

[0035] 100.0g 10-ethoxy bisphenol fluorene, 25.0g immobilized phosphotungstic acid catalyst, 0.15g p-hydroxyanisole and 0.15g sodium hypophosphite were added to a 500ml four-necked round bottom flask with magnetic stirring, and then Add 225g of toluene solvent and 75g of cyclohexane solvent, start stirring, heating and dissolving, after slowly adding 25.5g of acrylic acid dropwise, raise the temperature to 95-105°C for reflux and water separation, react for 4 hours, cool down to 55°C and filter, collect The solid-supported phosphotungstic acid catalyst is reserved for the next use, add 60ml deionized water and wash 5 times until neutral, add 10g anhydrous sodium sulfate, stir and dry for 2 hours, then membrane filter, add 0.02g p-hydroxybenzoic acid to the filtrate Distillation under reduced pressure after the ethe...

Embodiment 2

[0037] Preparation of immobilized catalyst: use white clay as a carrier, load silicotungstic acid, and the mass percentage of silicotungstic acid is 25%;

[0038] Add 240g of 10-ethoxy bisphenol fluorene, 54g of solid-supported silicotungstic acid catalyst, 0.3g of p-hydroxyanisole and 0.3g of sodium hypophosphite into a 1000ml three-neck round bottom flask with magnetic stirring, and then add 450g of toluene Solvent, 150g cyclohexane solvent, start stirring and heating, raise the temperature to 80°C and stir for 20 minutes, after slowly adding 63g of acrylic acid dropwise, quickly raise the temperature to reflux and water separation, react for 4.5 hours, cool down to about 60°C, filter, collect Immobilized silicotungstic acid catalyst for reuse next time, add 300ml of deionized water to wash 7 times until neutral, add 15g of anhydrous sodium sulfate, stir for 15 minutes, let stand for 5 hours, membrane filter, filter the filtered reaction solution Add 0.06g of p-hydroxyanisol...

Embodiment 3

[0040] Prepare the immobilized catalyst: use white clay as the carrier, load silicomomolybdic acid, and the mass percentage of silicomomolybdic acid is 30%;

[0041]Add 350g of 10-ethoxy bisphenol fluorene, 80g of immobilized silicomolybdic acid catalyst, 0.25g of p-hydroxyanisole and 0.35g of sodium hypophosphite into a 2000ml glass bottle with stirring, then add 1050g of toluene solvent, and open Stir and heat, slowly add 93g of acrylic acid, after the addition, quickly raise the temperature to 110°C and reflux, divide the water, react for 6 hours, cool down to about 55°C, filter, collect the immobilized silicon molybdenum acid for next use, add 350ml to remove Ionized water, stirred for 5 minutes, separated after standing for 25 minutes, washed with water for 6 times until neutral, added 20g of anhydrous sodium sulfate, stirred for 3 hours, then membrane filtered, and added 0.1g of p-hydroxyanisole to the filtrate to reduce Pressure distillation, steamed toluene to obtain 3...

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Abstract

The invention relates to the technical field of novel functional materials with high refractive index, and in particular, relates to a novel method for synthesizing polyethoxy acrylate with a fluorenyl structure by using an immobilized catalyst; the catalyst is easy to recover and can be repeatedly used for multiple times, the reaction operation is simple and convenient, the temperature controllability is strong, the yield is high, the production cost is reduced, the production efficiency is improved, environmental pollution is reduced, and green chemical production requirements are met. The method comprises the following steps: S1, sequentially adding a reaction solvent, a reaction main material, an immobilized catalyst and a polymerization inhibitor into a reactor, uniformly stirring and mixing, reacting, and cooling to obtain a first liquid; S2, adding acrylic acid into the first liquid, carrying out reflux reaction, carrying out water separation treatment, and cooling to obtain a second liquid; S3, filtering the second liquid to obtain a third liquid; S4, washing the third liquid with deionized water until the third liquid is neutral to obtain a fourth liquid; and S5, adding a drying agent into the fourth liquid for drying treatment, filtering and distilling the solvent to obtain a product.

Description

technical field [0001] The invention relates to the technical field of high-refractive-index functional new materials, in particular to a novel method for synthesizing fluorenyl-structured polyethoxy acrylate compounds with immobilized catalysts. Background technique [0002] High-performance functional material products are the frontier direction of new material research. Due to their structural characteristics, the application of fluorene-based products in the field of high-performance new materials has attracted increasing attention. Polyacrylic resin, epoxy acrylic resin and other optical resin polymer materials with fluorene structure as the skeleton, because of their super toughness and excellent insulation, chemical resistance, wear resistance, heat resistance (glass The melting temperature reaches 350°C), high optical anisotropy, good impact resistance, excellent transparency and formability, long service life, light weight and simple production, etc., has become a n...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/54B01J31/18
CPCC07C67/08B01J27/188B01J27/19C07C2603/18C07C69/54
Inventor 张绍中李小勇冯博李世兰陈鹏苏联刘艳艳周小野
Owner 沧州临港丰亚化工有限公司
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