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Preparation method of solid acid catalyst and application of catalyst to synthetic reaction of diethylene glycol dibenzoate (DEDB)

A solid acid catalyst, solid technology, applied in the preparation of organic compounds, the preparation of carboxylate, chemical instruments and methods, etc., can solve the problems of complex preparation process, many side reactions, low product yield, etc. Simple, overcoming poor activity and high catalytic activity

Active Publication Date: 2011-09-07
XILONG SCI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The synthetic method of DEDB is to be raw material with benzoic acid and diethylene glycol, available vitriol oil or p-toluenesulfonic acid are catalyzer to prepare, but there are following shortcomings with above-mentioned two kinds of materials as catalyzer: the first, side reaction is many, It is difficult to refine the product, and the product yield is low: second, the equipment is seriously corroded; third, the discharge of three wastes is large, and the post-treatment is complicated; fourth, the color of the product is deep, which affects the appearance and quality
The catalyst uses a hydrothermal method that requires high temperature and high pressure, and the preparation process is complicated. Organic titanium esters and organic silicon esters are expensive raw materials, so the cost of the catalyst is high.
[0006] CN101407461A discloses a kind of preparation method of diethylene glycol dibenzoate, adopts heteropolyacid, toluenesulfonic acid, hydrochloric acid etc. as catalyst, but needs follow-up deacidification process
[0007] CN101492372A discloses a production method of diethylene glycol dibenzoate, using a composite catalyst, a mixture of tetraisopropyl titanate and a solid titanium-based compound, but does not disclose what the solid titanium-based compound is

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In a 10L stainless steel bucket, take 1.6kg of hydrated sodium silicate and put it into 6.4kg of water, stir and keep it warm at 80°C for 1 hour to prepare a 15% sodium silicate solution.

[0023] Take 1.5kg of zirconia, slowly add it to the sodium silicate solution under stirring, and keep stirring for 8 hours at 85°C, add ammonia water with a weight content of 30% to the reaction system, adjust the pH value of the solution to 10, filter, and solid After washing 5 times with water, the product was dried at 110° C. for 4 hours.

[0024] Under stirring, the obtained sample was completely submerged in ammonium bisulfate solution with a weight concentration of 28%, and the pH of the solution was adjusted to 8~9 with 30% ammonia water, stirred for 0.5 hours, and left to soak for 24 hours.

[0025] The supernatant was removed, filtered, and the solid was washed with water five times, dried at 110° C. for 4 hours, and cooled naturally.

[0026] Put the obtained solid into a ...

Embodiment 2

[0028] The main steps are the same as in Example 1, wherein the immersion time of the solid obtained in the mixed acid is 4 hours, and the obtained solid acid catalyst is designated as sample B.

Embodiment 3

[0030] The main steps are the same as in Example 1, wherein the immersion time of the obtained solid in the mixed acid is 2 hours, and the calcination temperature is 500 ° C. The obtained solid acid catalyst is designated as sample C.

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PUM

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Abstract

The invention discloses a SO4<2-> / ZrO2 / SiO2 solid acid catalyst for synthesizing DEDB (Diethylene Glycol Dibenzoate). A preparation method of the solid acid catalyst comprises the following steps of: adding zirconium oxide into a sodium silicate aqueous solution; stirring, preserving heat and drying; soaking in a NH4HSO4 or (NH4)2SO4 aqueous solution; drying; soaking a solid with sulfuric acid, boric acid or phosphoric acid; and baking at the temperature of 450-600 DEG C and cooling to obtain the solid acid catalyst. In the DEDB synthesis process, procedures such as neutralizing, water washing, decoloring and the like are eliminated, the yield of DEDB reaches 98.6 percent, and the esterification rate reaches 99.5 percent.

Description

technical field [0001] The invention relates to a preparation method and application of a catalyst, in particular to a preparation method of a solid acid catalyst suitable for producing diethylene glycol dibenzoate. Background technique [0002] Diethylene glycol dibenzoate (DEDB) is a new type of plasticizer. Foreign countries used this ester as a plasticizer in the 1970s for the molding and processing of PVC products. Compared with DOP, DEDB has the characteristics of good compatibility, good cold resistance, antistatic property, remarkable anti-pollution performance, outstanding thermal stability, low volatility, good resistance to light and discoloration, and low toxicity, so it has a very good market prospect. [0003] The synthetic method of DEDB is to be raw material with benzoic acid and diethylene glycol, available vitriol oil or p-toluenesulfonic acid are catalyzer to prepare, but there are following shortcomings with above-mentioned two kinds of materials as cat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/053C07C69/78C07C67/08
Inventor 赵书煌吴沐坚卢伟宁郑鹤立黄伟鹏庄景发李金荣章小亮
Owner XILONG SCI CO LTD
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