A kind of pd@mil-101 ​​composite material and its preparation method and application

A composite material and mixed liquid technology, applied in the preparation of halogenated hydrocarbons, chemical instruments and methods, hydrocarbons, etc., can solve the problems of difficult to protect catalysts, reflect selectivity, difficult to produce, etc., and achieve good reusability. , convenient purification and separation, the effect of improving yield

Active Publication Date: 2018-06-26
芜湖数字信息产业园有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Due to its high specific surface area, good atomic surface activity, and good recyclability, palladium nanoparticles have become a good choice for the study of Suzuki reaction heterogeneous catalysis, especially in recent years when palladium nanoparticles are loaded onto graphite. Dilute, graphene oxide, and functionalized graphene increase the specific surface area of ​​palladium nanoparticles, thereby improving the catalytic activity of the catalyst. However, these traditional catalyst supports are difficult to protect the catalyst during the catalytic reaction. Moreover, it is difficult to show selectivity in the catalytic process, so it is very meaningful to develop a palladium nanoparticle composite material that is selectively catalyzed for the Suzuki reaction.
[0004] 4-Bromobiphenyl is an important raw material in chemical synthesis and has very good application prospects, but it is difficult to produce or the yield is very low by traditional methods

Method used

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  • A kind of pd@mil-101 ​​composite material and its preparation method and application
  • A kind of pd@mil-101 ​​composite material and its preparation method and application
  • A kind of pd@mil-101 ​​composite material and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Example 1 Pd@MIL-101 composite material

[0022] (1) Preparation method

[0023] 1. Preparation of MIL-101 crystals: Weigh 4g of chromium nitrate nonahydrate and 1.312g of terephthalic acid in a 100mL hydrothermal synthesis reactor, add 540mL of acetic acid (99.5%) and 50mL of sub-boiling distilled water at the same time, and use a stirring rotor to Sealed and stirred for 30 minutes, after stirring evenly, the rotor was taken out, and the hydrothermal synthesis reaction kettle was placed in an oven at 200°C for 8 hours of reaction. After the reaction, remove the liquid in the solution, wash the solid particles with 10 mL of water and 10 mL of ethanol three times each, put the washed solid into 50 mL of N,N'-dimethylformamide (DMF), and statically Place overnight, and obtain MIL-101 crystals after filtration.

[0024] 2. Activation of MIL-101 crystals: put the MIL-101 crystals into a vacuum drying oven at 150° C. for 12 hours in vacuum to obtain activated MIL-101 cryst...

Embodiment 2

[0030] Example 2 Selective Catalysis of Pd@MIL-101 Composite for the Reaction of Phenylboronic Acid and 1,4-Dibromobenzene

[0031] The method is as follows: Weigh 3mmol (0.1825g) of phenylboronic acid, 3mmol (0.4146g) of potassium carbonate and 1.5mmol (0.354g) of 1,4-dibromobenzene, and dissolve them in 10mL of methanol solution to obtain a mixed solution; Add 53mg of Pd@MIL-101 composite material (1.44mg Pd) and 1.44mg of pure palladium nanoparticles prepared in Example 1, respectively, and then place them in 10mL eggplant-shaped reaction bottles, install the reaction device, and first insert the long needle Stretch below the liquid surface, pass nitrogen gas for 10 minutes to remove the oxygen contained in the solution, then pull out the needle to make the whole reactor airtight, and finally insert a needle above the condenser tube for full nitrogen protection, and react at a temperature of 80°C. After 24h, get reaction solution respectively and carry out gas chromatograph...

Embodiment 3

[0036] Example 3 Repeatability test of Pd@MIL-101 composite material

[0037] After the reaction in Example 2 was completed, the Pd@MIL-101 composite material was isolated, and the experiment in Example 2 was repeated 4 times. Through repeated experiments, the yield of the Pd@MIL-101 composite for the first four times of the reaction did not change much, with good catalytic activity and selectivity, and the yield of 4-bromobiphenyl for the fifth time was 50.33%. The yield of benzene was 13.26%. It proves that the Pd@MIL-101 composite material synthesized by the present invention has good reusability, is easy to separate from reactants, and does not interfere with the entire reaction system.

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Abstract

The invention relates to a Pd @MIL-101 composite and a preparation method and application thereof. According to the adopted technical scheme, palladium chloride is added to methyl alcohol while sodium chloride is added, ultrasonic dispersion is conducted, stirring is conducted for 10-20 hours, and sodium tetrachloropalladate is obtained; a sodium tetrachloropalladate solution is dropwise added into MIL-101 crystals slowly, pd<2+>@MIL-101 is obtained; a methanol solution of asaturated sodium borohydride is added to the pd<2+>@MIL-101, reduction is conducted under the condition of ice-water bath, and the Pd @MIL-101 composite is obtained. The synthesized Pd @MIL-101 composite has special selectivity catalytic activity for phenylboronic acid and 1,4-dibromo-benzene in a suzuki reaction, and the yield of an intermediate product 4-bromobiphenyl is effectively raised.

Description

technical field [0001] The invention belongs to the field of synthesis of precious metal-catalyzed organic matter. A novel metal-organic framework material (MIL-101) is used as a carrier, and palladium nanoparticles are loaded into it to form a new Pd@MIL-101 composite material, which has the final reaction product selection. Ability to generate 4-bromobiphenyl that is difficult to generate or has a very low yield by traditional methods. Background technique [0002] The reaction of halogenated aromatics and phenylboronic acid in the Suzuki reaction is the most extensive and important reaction method in the synthesis of symmetrical or unsymmetrical biphenyl compounds. Biphenyl compounds have become a very widely used organic compound due to their wide range of physical and chemical properties. Compounds have been used in many fields such as herbicides, drugs, and liquid crystal materials. It is precisely because of such a wide range of application prospects that the Suzuki r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22B01J35/10C07C25/18C07C17/263C07C15/14C07C1/32
Inventor 张渝阳崔晓骏罗艳娟韩正波
Owner 芜湖数字信息产业园有限公司
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