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Sulfonated phenolic resin and preparation and application as catalyst thereof

A technology of sulfonated phenolic resin and phenolic resin, applied in the catalytic synthesis of trioctyl citrate and tributyl citrate, the field of sulfonated phenolic resin solid acid catalyst, resin type solid acid catalyst, can solve the problem of thermal stability Poor performance, affecting the catalytic effect and other problems, to achieve the effect of low raw material cost, good catalytic effect and simple preparation

Inactive Publication Date: 2009-10-07
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, polystyrene-based sulfonated resins have a major disadvantage, that is, poor thermal stability, which affects their catalytic effect.

Method used

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  • Sulfonated phenolic resin and preparation and application as catalyst thereof
  • Sulfonated phenolic resin and preparation and application as catalyst thereof
  • Sulfonated phenolic resin and preparation and application as catalyst thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] Embodiment 1, the preparation of sulfonated phenolic resin catalyst

[0068] (1) Preparation of phenolic resin: join phenol in the formaldehyde solution of mass concentration 35~38%, make the molar ratio of phenol and formaldehyde be 1.5:1~2.5:1; 40-60% concentrated hydrochloric acid, heated to 90-110°C for 10-20 minutes; cooled after complete reaction, washed with distilled water, dried, and ground; extracted with ethanol for 20-30 hours to obtain phenolic resin;

[0069] (2) Sulfonation of phenolic resin: Add 2 to 3 times the volume of phenolic resin to dichloromethane into the self-made phenolic resin, and after swelling the phenolic resin for 2 to 3 hours, add concentrated sulfuric acid with the same volume as the resin, React at 80-100°C for 3-5 hours, raise the temperature to 100-120°C, and distill off the solvent dichloromethane completely; add oleum with a resin volume of 50-60% and a mass concentration of 30-60% to the remaining mixture , react at 100-120°C fo...

Embodiment 2

[0070] Embodiment 2, sulfonated phenolic resin catalyst catalytic synthesis trioctyl citrate

[0071] Add citric acid and n-octanol in a molar ratio of 1:5 to a two-necked flask with a water separator and a condenser, mix and heat to 80°C and reflux for about 15 minutes under stirring. When the citric acid is completely dissolved, measure the mixing The initial acid value of the solution; add a sulfonated phenolic resin catalyst with 4.5% citric acid mass to the mixed solution, control the temperature at 140°C, react for 5 hours, and separate the water produced by the reaction in time. After the reaction, take the reaction solution to measure the acidity. Value, calculate the esterification rate of trioctyl citrate: 96.0%.

Embodiment 3

[0072] Embodiment 3, sulfonated phenolic resin catalyst catalytic synthesis tributyl citrate

[0073] Add citric acid and n-butanol with a molar ratio of 1:5.5 into a two-necked flask with a water separator and a condenser, heat to 80°C after mixing, and reflux for about 15 minutes under stirring. When the citric acid is completely dissolved, Measure the initial acid value of the mixed solution; add a sulfonated phenolic resin catalyst with 3.8% citric acid mass to the mixed solution, control the temperature at 150°C, react for 6 hours, and separate the water produced by the reaction in time, and take the reaction solution after the reaction Measure the acid value and calculate the esterification rate of tributyl citrate: 99.0%.

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Abstract

The invention provides sulfonated phenolic resin. Firstly, phenolic resin is synthesized by raw materials of phenol and formaldehyde, and then the phenolic resin is sulfonated under proper conditions, thus obtaining the sulfonated phenolic resin. The catalytic activity center of the prepared phenolic resin is sulfonic group, and good thermal stability of the phenolic resin ensures that the acid activity center can play the catalyst role fully, thus deciding that the sulfonated phenolic resin is an acid catalyst with excellent properties. The sulfonated phenolic resin catalyst is used in the catalytic synthesis reaction of trioctyl citrate and tributyl citrate, and the result shows that the esterification rate of the tributyl citrate is 99 percent and that the esterification rate of the trioctyl citrate is more than 96.0 percent.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and relates to a resin-type solid acid catalyst, in particular to a sulfonated phenolic resin solid acid catalyst; the invention also relates to a preparation method of the resin-type solid acid catalyst and its use in catalytically synthesizing citric acid three Octyl esters and tributyl citrate applications. Background technique [0002] Citrate products are a new type of green plasticizer developed in recent years. They have the advantages of non-toxicity, good biodegradability, low volatility, anti-bacteria, and high plasticizing efficiency. They have been widely used in many fields. . my country is the world's largest producer of citric acid, and has unique advantages in the research and development of citric acid ester plasticizers and their downstream products. The key to developing citric acid esters is to increase the conversion rate, and the core technology to improve the co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/28C08G8/10C07C69/704B01J31/06
Inventor 常玥王勇刚查飞任小宁吕学谦
Owner NORTHWEST NORMAL UNIVERSITY
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