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Bifunctional heterogeneous Pd@MIL-101@SGO composite material as well as preparation method and application thereof

A bifunctional group and composite material technology, applied in the direction of ether preparation, alkylene oxide preparation ether, chemical instruments and methods, etc., can solve the problems of large environmental pollution and complicated methods, and achieve high application value, excellent catalytic activity, and good repeatability The effect of using the ability

Active Publication Date: 2020-05-15
LIAONING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing main way of synthesizing β-alkoxy alcohols is the synthesis of olefins through multi-step reactions, including the epoxidation of olefins and the alcoholysis of epoxides. The methods used at this stage are complicated and require the separation of intermediate products, causing great environmental pollution.

Method used

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  • Bifunctional heterogeneous Pd@MIL-101@SGO composite material as well as preparation method and application thereof
  • Bifunctional heterogeneous Pd@MIL-101@SGO composite material as well as preparation method and application thereof
  • Bifunctional heterogeneous Pd@MIL-101@SGO composite material as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1 Pd@MIL-101@SGO composite material

[0026] (1) The preparation method is as follows

[0027] 1. Preparation of sulfonated graphene oxide (SGO): Add 30g of graphite powder, 400mL of concentrated sulfuric acid and phosphoric acid mixture (volume ratio: 9:1), and 9g of potassium permanganate into an ice-cooled container, and mix well Afterwards, stir at 423K for 12 hours, after cooling to room temperature, introduce the suspension into a container containing 400 mL of ice water and 3 mL of hydrogen peroxide, stir at room temperature for 12 hours, wash with water, concentrated hydrochloric acid and ethanol in sequence, and filter , and dried under vacuum at 353K for 12h to obtain SGO as a solid.

[0028] 2. Preparation of MIL-101@SGO composite material: H 2 BDC (1.328g, 8mmol), Cr(NO 3 ) 3 9H 2 O (3.2g, 8mmol) and concentrated hydrochloric acid (0.789g) were dissolved in 40mL of ultrapure water, 0.4528g of SGO was added, after stirring, the suspension was ult...

Embodiment 2

[0035] Example 2 Catalytic function of Pd@MIL-101@SGO composite material for styrene synthesis of β-alkoxy alcohol by one-pot serial method

[0036] The Pd@MIL-101@SGO composite material prepared in Example 1 was used as a catalyst to catalyze the synthesis of β-alkoxy alcohols from styrene in a one-pot series method.

[0037] Method: Take 1mmol styrene, 2mmol tert-butyl hydroperoxide, 1mL methanol, 3mL water, and 50mg catalyst in a 10mL reaction tube, stir and heat at 343K. The experimental results were monitored by a gas chromatograph GC. As the reaction progressed, the yield of the reaction increased gradually, and the yield was close to 100% in 5 hours. The reaction formula is as follows:

[0038]

[0039] After the reaction was completed, the catalyst was separated by filtration, washed with water and methanol for several times, then filtered off and dried in vacuum. The recovered catalyst was used for the next cycle experiment. Such as image 3 As shown, the activit...

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Abstract

The invention relates to a bifunctional heterogeneous Pd@MIL-101@SGO composite material as well as a preparation method and application thereof. According to the technical scheme, the preparation method comprises the following steps: adding sulfonated graphene oxide (SGO), terephthalic acid, chromium nitrate nonahydrate, hydrochloric acid and water into a container, stirring, carrying out an ultrasonic treatment until turbid liquid is uniformly dispersed, sealing, putting into a drying oven, keeping at 473K for 8 hours, cooling to the room temperature, washing, filtering, drying to obtain a MIL-101@SGO composite material; slowly dropwise adding a methanol solution of sodium chloro-palladate into the MIL-101@SGO material, and carrying out reduction by using a reducing agent to obtain the Pd@MIL-101@SGO composite material. The Pd@MIL-101@SGO composite material is a bifunctional heterogeneous catalyst for catalyzing styrene to synthesize beta-alkoxyl alcohol by a one-pot series method.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a palladium-supported metal-organic framework and sulfonated graphene oxide composite material and its application in the reaction of catalyzing the synthesis of β-alkoxy alcohols by a one-pot series method of styrene. Background technique [0002] Palladium nanoparticles are an efficient heterogeneous catalyst with high catalytic activity. In recent years, palladium nanoparticles are often loaded on supports to catalyze various organic reactions. Metal-organic framework material is a kind of good carrier, which has ultra-high specific surface area, stable structure and good thermal stability. Compared with other porous material carriers, it has many advantages. However, it is difficult to directly introduce strong Bronsted acid groups on metal-organic frameworks, and the yield is low and it is not conducive to large-scale production. [0003] One-pot tandem reacti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J37/02B01J37/10B01J37/16C07C41/03C07C43/178C07D301/19C07D303/04
CPCB01J31/1691B01J31/2239B01J37/10B01J37/0201B01J37/16C07D301/19C07D303/04C07C41/03B01J2531/62B01J35/393B01J35/396C07C43/1782
Inventor 张渝阳汤宏李鑫周美丽吴琼刘大亮
Owner LIAONING UNIVERSITY