Brphinsted-Lewis acidic ionic liquid and application thereof in rosin polymerization reaction

An acidic ionic liquid and reaction technology, which is applied in the fields of chemical modification of natural resin, organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, etc., can solve equipment corrosion and environmental pollution, solid acid catalyst structure Carbon, affecting product quality and other issues, to achieve the effect of good quality, no loss of acidity, and easy operation

Inactive Publication Date: 2008-06-04
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to overcome the severe environmental pollution existing in the use of existing acidic catalysts, catalyst residues affecting product quality, difficult separation of products with liquid acid, serious equipment corrosion and environmental pollution, serious carbonation of solid acid catalysts, and difficult Recycling and other disadvantages provide a recyclable and environmentally friendly process production route for the synthesis of polymerized rosin

Method used

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  • Brphinsted-Lewis acidic ionic liquid and application thereof in rosin polymerization reaction
  • Brphinsted-Lewis acidic ionic liquid and application thereof in rosin polymerization reaction

Examples

Experimental program
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Effect test

Embodiment 1

[0012] Dissolve 27.2g of 1,4-butane sultone in 136g of ethyl acetate, raise the temperature to 40°C, and add 16.4g of N-methylimidazole dropwise. Washed with ethyl acetate and dried at 100° C. to obtain 42.7 g of white solid 1-(4-sulfonic acid) butyl-3-methylimidazole inner salt, yield 98%. Take 21.8 g of 1-(4-sulfonic acid) butyl-3-methylimidazolium inner salt, dissolve it in 43.6 g of water, add 9.9 g of hydrochloric acid with a mass concentration of 37%, dropwise, and react at 90°C for 3 hours Afterwards, dehydration under reduced pressure gave 24.4g pale yellow viscous liquid acidified internal salt, chlorinated 1-(4-sulfonic acid) butyl-3-methylimidazolium salt, yield 94%; Under nitrogen protection, 12.8g Mix 1-(4-sulfonic acid)butyl-3-methylimidazolium chloride with 10g zinc chloride and react at 100°C until the zinc chloride dissolves to obtain 22.8g Brnsted-Lewis acidic ionic liquid 1 -(4-sulfonic acid)butyl-3-methylimidazolium chloride zincate. Get 1.3g 1-(4-sulfon...

Embodiment 2

[0014] Mix 12.8g of 1-(4-sulfonic acid) butyl-3-methylimidazolium chloride with 9.8g of cuprous chloride, and react at 100°C under nitrogen protection until the cuprous chloride is dissolved to obtain 22.6g Brnsted-Lewis acidic ionic liquid 1-(4-sulfonic acid) butyl-3-methylimidazolium chlorocuprousate. Get 1.8g 1-(4-sulfonic acid) butyl-3-methylimidazolium chloride cuprous acid salt, 5g rosin and 40g cyclohexane react under reflux after 5 hours, cool to room temperature product, separate upper layer liquid, The upper layer liquid was decompressed to remove the solvent to obtain a polymerized rosin product with a softening point of 121°C (ring and ball method).

Embodiment 3

[0016] Dissolve 24.4g of 1,3-propane sultone in 200g of ethyl acetate, raise the temperature to 40°C, add 22g of N-propylimidazole dropwise, after the dropwise addition, keep the reaction for 4 hours, filter, and filter the cake with ethyl acetate After washing and drying at 100°C, 45 g of white solid 1-(3-sulfonic acid)propyl-3-propylimidazole inner salt was obtained, with a yield of 97%. Take 23.2 g of 1-(3-sulfonic acid) propyl-3-propyl imidazole inner salt, dissolve it in 55 g of water, add 9.9 g of hydrochloric acid with a mass concentration of 37%, and after the addition is completed, react at 90°C for 2 hours , dehydration under reduced pressure to get 24.7g pale yellow viscous liquid acidified inner salt, chlorinated 1-(3-sulfonic acid) propyl group-3-propylimidazolium salt, yield 92%; 13.4g chlorinated 1-(3 -sulfonic acid) propyl group-3-propylimidazolium salt mixed with 11g cupric chloride, under nitrogen protection, react until cupric chloride dissolves at 110 ℃, ob...

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Abstract

The invention discloses a preparation technology for a catalyst, in particular to a BrPhinsted-Lewis acid ionic liquid catalyst and an application thereof in reaction of rosin polymerization. The specific preparation method is that: alkyl sultone is reacted with equimolar N-alkyl imidazole or pyridine or trialkylamine to obtain inner salt; the inner salt is reacted with equimolar hydrochloric acid or hydrobromic acid and then dehydrated to obtain acidized inner salt; the acidized inner salt is reacted with Lewis with the mol ratio 1:1.1-2.5 to obtain the BrPhinsted-Lewis acid ionic liquid; the BrPhinsted-Lewis acid ionic liquid is used as catalyst in polymerized rosin preparation technique. Compared with the prior art, the product generated from rosin polymerization reaction does not interblend with the ionic liquid catalyst, is self-layered, and emerges from solvent directly, thus obtaining the aim product. The BrPhinsted-Lewis acid ionic liquid catalyst has the advantages of stable performance and recycling use; with industrial application value and no environmental pollution, the invention belongs to environment friendly technique.

Description

technical field [0001] The invention relates to the technical field of catalyst manufacture, more specifically to a Brönsted-Lewis acidic ionic liquid catalyst and its application in rosin polymerization. Background technique [0002] Polymerized rosin is one of the important rosin modified products. Because of its high softening point, excellent oxidation resistance, high viscosity (in organic solvents), no crystallization, and low acid value, it is widely used in papermaking, paint, rubber, Plastics, electrical appliances, medicine, pesticides, printing and dyeing, ink and other fields have been widely used. At present, the industrial use of sulfuric acid as a catalyst to prepare polymerized rosin; Catalyst for polymerization reaction; CN 101,582B uses zinc chloride / hydrochloric acid composite catalyst system to catalyze the preparation of polymerized rosin. Most of these processes have the following disadvantages: the acidic nature of the acidic catalyst itself makes it...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09F1/04B01J31/04
Inventor 于世涛刘仕伟刘福胜解从霞季开慧
Owner QINGDAO UNIV OF SCI & TECH
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