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Supramolecular ionic liquid catalyst, preparation method and application thereof

An ionic liquid and catalyst technology, applied in chemical instruments and methods, preparation of organic compounds, catalysts for physical/chemical processes, etc., can solve problems such as easy unloading, reduction of ionic liquid active component concentration contact area, affecting catalytic efficiency, etc.

Active Publication Date: 2021-09-14
抚顺东科新能源科技有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Purpose of the invention: the present invention provides a supramolecular ionic liquid catalyst and its preparation method and application. Reduced, affecting the problem of catalytic efficiency

Method used

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  • Supramolecular ionic liquid catalyst, preparation method and application thereof
  • Supramolecular ionic liquid catalyst, preparation method and application thereof
  • Supramolecular ionic liquid catalyst, preparation method and application thereof

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preparation example Construction

[0044] A preparation method of supramolecular ionic liquid catalyst, the steps are as follows:

[0045] Structural design and preparation routes of supramolecular ionic liquid catalysts, such as figure 1 shown. Among them, 1,4-bis(2-hydroxyethoxy)benzene is the raw material, and B, C, and D are intermediate products.

[0046] Step 1, Synthesis of Intermediate B

[0047] Synthesis of Intermediate B: Dissolve 1,4-bis(2-hydroxyethoxy)benzene and triphenylphosphine in anhydrous acetonitrile, 1,4-bis(2-hydroxyethoxy)benzene, triphenyl The mass ratio of phosphine and anhydrous acetonitrile is 3-5:8-10:100, cooled in an ice-water bath; under stirring, slowly add CBr 4 , CBr 4 The mass ratio with anhydrous acetonitrile is 1-2:10, and the mixture is stirred at room temperature for 12 hours; add cold water with a mass ratio of 1:1 to acetonitrile (temperature is lower than 10°C), and a white precipitate is precipitated. Suction filtration under reduced pressure, filter cake is coll...

Embodiment 1

[0063] Step 1, the synthesis of intermediate B1

[0064] Synthesis of intermediate B1: 1,4-bis(2-hydroxyethoxy)benzene (3g) and triphenylphosphine (10g) were dissolved in anhydrous acetonitrile (100g), and cooled in an ice-water bath. With stirring, slowly add CBr 4 (20g), the mixture was stirred at room temperature for 12h. Cold water (100 g) was added and a white precipitate precipitated. Suction filtration under reduced pressure, the filter cake was collected and dried to obtain white flaky solid B1.

[0065] Step 2, the synthesis of intermediate C1

[0066] Synthesis of intermediate C1: Add intermediate B1 (3 g), paraformaldehyde (1 g), CH 2 Cl 2 (100g), the mixture was cooled in an ice-water bath for 10 min under the protection of nitrogen (purity 99%), and BF was added 3 -Et 2 0 (3g), the mixture was stirred for 2.5h. The mixture was suction filtered, and the filtrate was washed with 2.5 mol / L NaOH solution (60 mL) and distilled water (30 mL) and then washed with...

Embodiment 2

[0072] Step 1, the synthesis of intermediate B2

[0073] Synthesis of intermediate B2: 1,4-bis(2-hydroxyethoxy)benzene (5g) and triphenylphosphine (8g) were dissolved in anhydrous acetonitrile (100g), and cooled in an ice-water bath. With stirring, slowly add CBr 4 (10g), the mixture was stirred at room temperature for 12h. Cold water (100 g) was added and a white precipitate precipitated. Suction filtration under reduced pressure, the filter cake was collected and dried to obtain white flaky solid intermediate B2.

[0074] Step 2, the synthesis of intermediate C2

[0075] Synthesis of intermediate C2: Add intermediate B2 (6 g), paraformaldehyde (2 g), CH 2 Cl 2 (100g), the mixture was cooled in an ice-water bath for 30 min under the protection of nitrogen (purity 99%), and BF was added 3-Et 2 0 (6g), the mixture was stirred for 2.5h. The mixture was filtered with suction, and the filtrate was washed with 2.5 mol / L NaOH solution (2 x 30 mL) and distilled water (1 x 30 ...

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Abstract

The invention relates to a supramolecular ionic liquid catalyst, a preparation method and application thereof. The catalyst has an LCST phase behavior, wherein the structure of the catalyst is that column [5] arene and an ionic liquid are bonded, and the structure of the catalyst is regulated by changing the active groups of the column [5] arene and the ionic liquid. The supramolecular ionic liquid catalyst is applied to catalysis of methanol ester exchange reaction to synthesize dimethyl carbonate. According to the invention, through fusion and dissociation of a supramolecular ionic liquid and a solvent at different temperatures, a catalytic system intelligently regulates and controls phase transition of the catalytic process according to temperature changes, so that it is guaranteed that catalytic active components make full contact with raw materials to achieve efficient catalysis, and the separation and recovery process of the catalyst and the product is simplified so as to save energy and consumption and achieve environmental protection.

Description

technical field [0001] The invention relates to a supramolecular ionic liquid catalyst, in particular to the supramolecular ionic liquid catalyst and its preparation method and the application of catalyzing methanol transesterification to synthesize dimethyl carbonate. Background technique [0002] As an important green and non-toxic chemical raw material, dimethyl carbonate (DMC) contains functional groups such as methyl, methoxy and carbonyl in its molecular structure, which can replace methyl halide and dimethyl sulfate for methylation Reagent, instead of highly toxic phosgene, it can be used as a carbonylation reagent, and it can also be used in the synthesis of resins and fine chemicals for transesterification with alcohols, esters and amino alcohols. In addition, due to its good compatibility, high oxygen content and low saturated vapor pressure, DMC can also be used as a low-toxic solvent and fuel additive. [0003] In recent years, my country's industry mainly uses ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02C07C68/065C07C69/96
CPCB01J31/0281C07C68/065C07C69/96Y02P20/54
Inventor 郭立颖刘勇徐仕睿郑荣荣丁继宇王海玥布凡聪徐铁军宋晓慧马智慧左小青
Owner 抚顺东科新能源科技有限公司
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