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Catalyst for synthesizing salicylic acid through phenol carboxylation reaction and preparation method

A technology of phenol carboxyl group and catalyst, which is applied in the field of catalyst and preparation of phenol carboxylation reaction to synthesize salicylic acid, which can solve the problems of low reaction activity, harsh reaction conditions and high reaction efficiency, and achieve strong solubility, simple recycling and catalytic highly active effect

Active Publication Date: 2020-09-08
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalyst adopted in the present invention overcomes the problems of previous inorganic salt catalysts such as potassium carbonate with low reactivity and harsh reaction conditions. At the same time, compared with other ionic liquid catalysts, the MOFs immobilized ionic liquid catalyst has high reaction efficiency and magnetic nano-core The existence of the catalyst is more convenient for recovery and reuse, so the stability of the catalyst is better

Method used

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  • Catalyst for synthesizing salicylic acid through phenol carboxylation reaction and preparation method
  • Catalyst for synthesizing salicylic acid through phenol carboxylation reaction and preparation method
  • Catalyst for synthesizing salicylic acid through phenol carboxylation reaction and preparation method

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Experimental program
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Effect test

Embodiment 1

[0029] Preparation of [Bmim]Br / AlBr 3 : Step 1 {[Bmim]Br}: Weigh 64.12g (0.78mol) of 1-methylimidazole into a 500ml three-necked flask, and stir rapidly at a constant temperature of 70°C. Slowly add 117.87 g (0.858 mol) of n-bromobutane dropwise into the three-necked flask with a constant pressure dropping funnel for 1 h. After the dropwise addition, the mixture was refluxed at 70° C. for 10 h. After the reaction was completed, cool to room temperature to obtain the crude product [Bmim]Br, which was transferred to a separatory funnel, washed (3 times) with 30ml ethyl acetate, and then the product was rotary evaporated at 60°C for 30min to remove residual ethyl acetate. ester. The remaining product was transferred to a beaker and placed in a vacuum drying oven at a temperature of 65°C, and dried to constant weight to obtain the finished product of 1-methyl-3-n-butylimidazole bromide ([Bmim]Br). Step 2 {[Bmim]Br / AlBr 3}: Weigh 50g of prepared [bmim]Br into a 250ml single-nec...

Embodiment 2

[0031] Preparation of Fe 3 o 4 @Zn-ZIF-8: Weigh 1.77g of zinc nitrate hexahydrate and dissolve it in 60.5ml of anhydrous methanol to obtain solution 1; weigh 9.85g of 2-methylimidazole and dissolve it in 60.5ml of anhydrous methanol to obtain a solution 2; After mixing solution 1 with solution 2, add 0.08g Fe 3 o 4 Disperse into the mixed liquid, stir magnetically at 50°C for 4h; after the reaction, centrifuge at 8000r.p.m, and wash with methanol three times; the obtained solid is vacuum-dried at 80°C overnight, and ground to obtain Fe3O4@Zn-ZIF-8 . Such as figure 2 Shown is Fe3O4@Zn-ZIF-8 obtained in the present invention. Example 3

Embodiment 3

[0032] Preparation of [Bmim]Br / AlBr3-Fe 3 o 4 @Zn-ZIF-8: Dissolve 0.4g of ionic liquid [Bmim]Br / AlBr3 in 5ml of anhydrous methanol, and weigh 0.63g of Fe 3 o 4 @ZIF-8 added [Bmim]Br / AlBr 3 After ultrasonic treatment for 10 minutes, seal it with plastic wrap and place it in a ventilated place for immersion for 24 hours, then separate the catalyst with a magnet, dry it in a vacuum oven at 80°C overnight, and place the solid catalyst in a muffle furnace for calcination at 220°C After grinding, the recyclable MOFs immobilized ionic liquid catalyst [Bmim]Br / AlBr3-Fe3O4@Zn-ZIF-8 was obtained. Such as image 3 Shown is [Bmim]Br / AlBr3-Fe3O4@Zn-ZIF-8 obtained in the present invention.

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Abstract

The invention provides a catalyst for synthesizing salicylic acid through phenol carboxylation reaction and a preparation method. The catalyst is a novel recyclable MOFs immobilized ionic liquid catalyst. The catalytic active component is Lewis acidic ionic liquid, and the carrier is a magnetic core-shell MOFs nano composite material Fe3O4@ZIFs. The method comprises the following steps of: firstly, epitaxially growing a magnetic core-shell composite material carrier (Fe3O4@ZIFs) of a ZIFs shell layer on magnetic Fe3O4 nanoparticles by adopting a one-pot method, then synthesizing an ionic liquid catalyst with a Lewis acid active site by a two-step method, and immobilizing the ionic liquid catalyst with the Lewis acid active site on the surface of Fe3O4@ZIFs by an impregnation method. The catalyst has good catalytic performance on the reaction of preparing salicylic acid through phenol carboxylation, is high in recoverability by means of an external magnetic field effect, still keeps high catalytic activity after being recycled, the product selectivity is high, and the technological process is green and environment-friendly, therefore the catalyst is a novel green chemical catalyticmaterial with industrial application prospects.

Description

technical field [0001] The invention belongs to the field of salicylic acid synthesis, and in particular relates to a catalyst for synthesizing salicylic acid by phenol carboxylation and a preparation method. Background technique [0002] Salicylic acid (Salicylic Acid), also known as o-hydroxybenzoic acid. As an important pharmaceutical synthesis intermediate, its industrial synthesis is mainly based on the Kolbe-Schmitt reaction. This is a way to use CO 2 The industrial synthesis method as a reactant, that is, the process of introducing a carboxyl group on an aromatic ring through an electrophilic substitution reaction between carbon dioxide and phenol. It is divided into gas-solid phase reaction and gas-liquid phase reaction, and the method widely used in industry is the former. The method uses phenol as a raw material, undergoes an acid-base neutralization reaction with sodium hydroxide to generate sodium phenate, and then introduces carbon dioxide under a certain pre...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07C51/15C07C65/10H01F1/113
CPCB01J31/1691C07C51/15H01F1/113B01J2531/26C07C65/10Y02P20/54Y02P20/584
Inventor 李乃旭石闻卿周建成陈聪阚道琴王楠王可
Owner SOUTHEAST UNIV
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