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Solid acid catalyst for preparation of sodium isophthalate diethylene glycol 5-sulfonate via direct esterification and preparation and application of solid acid catalyst

A technology of diethylene glycol isophthalate and solid acid catalyst is applied in the directions of catalyst activation/preparation, physical/chemical process catalyst, sulfonate preparation, etc., and can solve the problems of inflammability, toxicity, explosion danger and the like, achieve good catalytic performance

Active Publication Date: 2017-08-11
UNIV OF JINAN +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There are two processes for the preparation of SIPE: the first is to use sodium dimethyl sulfonate (PM) and ethylene glycol to transesterify, but methanol needs to be removed, which is highly dangerous, and if the recovered methanol is Do not deal with environmental pollution, CN204999829 U discloses a system for continuously synthesizing the third monomer ethylene glycol isophthalate-5-sodium sulfonate, wherein it is mentioned that the batch process carries out transesterification, and the by-product methanol is volatile , poisonous, flammable, and explosive, requiring multiple nitrogen replacements, which not only consumes a large amount of nitrogen, but also increases the danger of the production process; the second production process is to combine isophthalic acid-5-sodium sulfonate and ethylene glycol Direct esterification produces SIPE, without the risk of methanol removal, high safety, lower cost of polyester products and reduction of industrial pollution, CN 101265218 A discloses a direct esterification of isophthalic acid-5-sulfonate to prepare in- The method of diethylene glycol phthalate-5-sulfonate, in the esterification process, because the generation of water will affect the activity of traditional catalyst tetrabutyl titanate or isopropyl titanate, making it hydrolyzed and affecting the catalytic Performance, the acid value can only be reduced to 0.85 after 15 hours of reaction, and the catalyst is difficult to separate from the product because it can be dissolved in the product after the reaction, thus affecting the dyeing performance of SIPE as the third monomer participating in polyester synthesis

Method used

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  • Solid acid catalyst for preparation of sodium isophthalate diethylene glycol 5-sulfonate via direct esterification and preparation and application of solid acid catalyst
  • Solid acid catalyst for preparation of sodium isophthalate diethylene glycol 5-sulfonate via direct esterification and preparation and application of solid acid catalyst
  • Solid acid catalyst for preparation of sodium isophthalate diethylene glycol 5-sulfonate via direct esterification and preparation and application of solid acid catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Dissolve 0.17g of cetyltrimethylammonium bromide in 250.00g of water, add 10.15g of montmorillonite, stir at 70°C for 18h, cool to room temperature, wash and filter, and dry at 80°C for 12h to obtain organically modified montmorillonite Soil (organic soil); preparation of suspension A: add 1.25g of tetrabutyl titanate and 10.00g of organic soil to 50.00g of ethanol, and stir evenly; preparation solution B: mix 0.05g of concentrated hydrochloric acid, 5.25g of water, Mix 50g of ethanol evenly; drop solution B into suspension A at a constant speed, and then stir the mixture at 20°C for 12 hours, then at 70°C for 12 hours; cool the mixed suspension of A and B to room temperature, wash and filter, The filter cake was dried at 110°C for 6h, and calcined at 500°C for 4h to obtain solid acid catalyst a.

[0031] figure 1 In the preparation process of the obtained solid acid catalyst, the XRD spectrum of montmorillonite, organoclay, and catalyst; after organic modification and...

Embodiment 2

[0034] Dissolve 0.26g of dodecyltrimethylammonium bromide in 500.00g of water, add 13.55g of montmorillonite, stir at 80°C for 10h, cool to room temperature, wash and filter, and dry at 80°C for 12h to obtain organically modified montmorillonite soil (organic soil). Preparation of suspension A: Add 1.66g of tetrabutyl titanate and 10.00g of organic soil to 100.00g of ethanol, and stir evenly; preparation of solution B: Mix 0.12g of concentrated hydrochloric acid, 7.05g of deionized water, and 20.00g of anhydrous Ethanol mixed well. The solution B was dropped into the suspension A at a constant speed, and the mixed solution was stirred at 45°C for 6h and at 20°C for 12h after the dripping was completed. The mixed suspension of A and B was cooled to room temperature, washed and filtered, the filter cake was dried at 80°C for 12h, and calcined at 700°C for 2h to obtain solid acid catalyst b.

[0035] Add 80.25g of isophthalic acid-5-sodium sulfonate, 400.50g of ethylene glycol,...

Embodiment 3

[0037]Dissolve 0.18g of dodecyldimethylbenzyl ammonium chloride in 300.00g of water, add 10.00g of montmorillonite, stir at 50°C for 24h, cool to room temperature, wash and filter, and dry at 80°C for 12h to obtain organically modified Montmorillonite (organic soil). Preparation of suspension A: Add 1.28g of isopropyl titanate and 10.00g of organic soil to 80.00g of ethanol, and stir evenly; preparation of solution B: Mix 0.06g of concentrated hydrochloric acid, 4.08g of deionized water, and 40.00g of anhydrous Ethanol mixed well. Add solution B to suspension A at a constant speed, and then mix the solution at 50°C for 4 hours and at 30°C for 8 hours. The mixed suspension of A and B was cooled to room temperature, washed and filtered, the filter cake was dried at 120°C for 6h, and calcined at 600°C for 3h to obtain solid acid catalyst c.

[0038] Add 80.25g of isophthalic acid-5-sodium sulfonate, 160.09g of ethylene glycol, 0.82g of sodium acetate, and 2.18g of catalyst c in...

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Abstract

The invention discloses synthesis and application of a solid acid catalyst and particularly relates to a solid acid catalyst for preparation of sodium isophthalate diethylene glycol 5-sulfonate via direct esterification and preparation and application of the solid acid catalyst; the solid acid catalyst comprises an inorganic lamellar structure material and an intercalation element; the inorganic lamellar structure material may be one or any of montmorillonite, mica, purified bentonite, kaolin, graphite, hydrotalcite and a tetravalent metallic insoluble salt; and the intercalation element may be one or any of Ti, O, H and C. The solid acid catalyst has high catalytic activity in the production of sodium isophthalate diethylene glycol 5-sulfonate from 5-sulfoisophthalic acid monosodium salt and diethylene glycol via direct esterification, the catalyst is easy to separate from the product after reaction, and the catalyst is reusable after being activated.

Description

technical field [0001] The invention belongs to the technical field of environmental protection catalysts, and in particular relates to a solid acid catalyst for preparing diethylene glycol isophthalate-5-sodium sulfonate through direct esterification, a preparation method and application thereof. Background technique [0002] Diethylene glycol isophthalate-5-sodium sulfonate (SIPE) is a very important chemical raw material, which can improve the processing and dyeing performance of polyester polyester, and participate in the modification of polyester as a polyester dyeing modifier. It is especially widely used in the synthesis of normal pressure cationic dyeable polyester, high temperature and high pressure cationic dyeable polyester and alkali soluble polyester. [0003] There are two processes for the preparation of SIPE: the first is to use sodium dimethyl sulfonate (PM) and ethylene glycol to transesterify, but methanol needs to be removed, which is highly dangerous, an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/10B01J21/06B01J21/16B01J37/08B01J37/04B01J35/02C07C303/28C07C309/73B01J35/00
CPCC07C303/28B01J21/063B01J21/16B01J27/10B01J37/04B01J37/082B01J35/00B01J35/30C07C309/73
Inventor 杨成杨皓孙恺宋瑶瑶
Owner UNIV OF JINAN
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