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Preparation of Novel Thermosensitive Ionic Liquid and Its Catalytic Synthesis of Chloroacetate

A technology of liquid and acid ions, applied in chemical instruments and methods, preparation of organic compounds, preparation of sulfonic acid, etc., can solve the problem of no relevant reports on esterification performance, achieve high catalytic performance, good universality, and simplified separation The effect of the process

Inactive Publication Date: 2021-06-11
LIAONING INST OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Wu et al. found that the imidazole-based ionic liquid based on phosphotungstovanadium ternary heteropolyacid can undergo a reversible phase transition process below 100 °C, and is a gel electrolyte with temperature control properties (Wu, X. F., Huang, T. P., Tong X., et al. RSC. Adv. ,2015,5(28):21973-21977), but its esterification performance has not been reported

Method used

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  • Preparation of Novel Thermosensitive Ionic Liquid and Its Catalytic Synthesis of Chloroacetate
  • Preparation of Novel Thermosensitive Ionic Liquid and Its Catalytic Synthesis of Chloroacetate
  • Preparation of Novel Thermosensitive Ionic Liquid and Its Catalytic Synthesis of Chloroacetate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1 (preparation of heteropolyacid ionic liquid)

[0025] The preparation of heteropolyacid ionic liquid is divided into four steps, which are:

[0026] Step 1: Dissolve 0.066 mol (8.00g) of 1,3-propane sultone and 0.066 mol (6.6g) of triethylamine in 13mL of anhydrous acetone, and slowly add the acetone solution of triethylamine to 1 , 3-Propane sultone in acetone solution, added dropwise within 1h. The mixed solution was stirred at 50°C for 4h, during which a white precipitate was formed. Filter under reduced pressure, wash with a small amount of anhydrous acetone three times, and dry the product under vacuum at 60°C for 12 hours to obtain TEAPS as a white powder.

[0027] Step 2: Dissolve 0.09mol (30g) sodium tungstate in 37 ml water and stir until the solid is completely dissolved. Then, 1 mL of 85% phosphoric acid was added dropwise while stirring to adjust the pH to 9. Then glacial acetic acid was added dropwise under vigorous stirring to adjust the p...

Embodiment 2

[0030] Example 2 (heteropolyacid ionic liquid catalyzed synthesis of n-amyl chloroacetate reaction example)

[0031] Weigh 0.16mol (15.4g) of chloroacetic acid and 0.2g of catalyst into a three-neck flask, measure 20.6mL (alcohol-acid ratio: 1.2) of n-pentanol and 10mL of water-carrying agent benzene, add saturated saline to the water separator device. Heat with an electric heating electromagnetic stirrer, control the temperature of the reaction liquid phase at 140°C, and reflux for 2 hours. Then the reaction product is cooled, the esterification product is separated from the heteropolyacid ionic liquid catalyst, and the esterification product and the catalyst are obtained by filtration. The catalyst can be recycled and reused after washing and drying, and the filtrate can be collected by normal pressure distillation. Aqueous benzene, unreacted alcohol, and then n-amyl chloroacetate can be obtained, and the reaction esterification rate is 98.75%.

Embodiment 3

[0032] Example 3 (Example of repeated use performance investigation of the synthesis of n-pentyl chloroacetate by heteropolyacid ionic liquid catalysis)

[0033] Weigh 15.4g of chloroacetic acid and 0.2g of catalyst into a three-necked flask, measure 20.6mL (alcohol-acid ratio: 1.2) of n-amyl alcohol and 10mL of water-carrying agent benzene, and add saturated saline to the water separator. Heat with an electric heating electromagnetic stirrer, control the temperature of the reaction liquid phase at 140°C, and reflux for 2 hours. Then the reaction product is cooled, the esterification product is separated from the catalyst, and the esterification product and the catalyst are obtained by filtration. The filtrate is distilled under normal pressure to collect water-carrying agent benzene and unreacted alcohol, and then n-amyl chloroacetate can be obtained. Measure the esterification rate; the catalyst can be used for the next reaction after being washed and dried, and reused four ...

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Abstract

The invention discloses an acid-functionalized-temperature-controlled ternary heteropolyacid ionic liquid, a preparation method, and an esterification method for catalytically synthesizing chloroacetate. The structural formula of the heteropolyacid ionic liquid is shown in (I). The ionic liquid has temperature response characteristics during the esterification reaction of chloroacetic acid and alcohol. It is mixed with the reactant at the reaction temperature. When the reaction temperature drops to room temperature, the ionic liquid and the product quickly separate into two phases. The catalyst and the reaction product can be quickly separated by filtration. The ionic liquid not only has the advantages of convenient recovery and no waste acid discharge, but also has the characteristics of high esterification efficiency and good reusability. (I).

Description

technical field [0001] The invention relates to the preparation of an acid-functionalized-temperature-controlled ternary heteropolyacid ionic liquid and a method for catalytically synthesizing chloroacetate, and belongs to the technical field of the synthesis of functionalized ionic liquids and their organic-catalyzed esterification reactions. Background technique [0002] Chloroacetate is an important organic synthesis intermediate, widely used in medicine, pesticide, plasticizer and other fields. Concentrated sulfuric acid is often used as a catalyst in traditional organic ester production methods. The disadvantages are many side reactions, low product purity, difficult separation and recovery of catalysts, serious equipment corrosion, and environmental pollution caused by a large amount of acidic wastewater in post-treatment. In order to solve the above problems, researchers have studied a variety of heterogeneous catalysts to replace sulfuric acid, such as ion exchange r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C303/22C07C309/14B01J31/18C07C67/08C07C69/63
CPCB01J27/188B01J31/0285B01J31/0298C07C67/08C07C303/22C07C309/14C07C69/63
Inventor 鄢景森吴庆银鄂永胜王泽青贺凤伟王强代文双吴治本徐鹏飞
Owner LIAONING INST OF SCI & TECH
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