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Method for synthetizing 2-amino-1, 3, 5-benzenetricarboxylic acid and application thereof for preparation of NH2-MOF-808

A technology of NH2-MOF-808 and benzenetricarboxylic acid, which is applied in the preparation of nitro compounds, organic compounds, and cyanide reaction, etc. It can solve the problems of difficult control, high price, and difficult purification, and achieve easy operation , simple preparation process, simple and effective synthesis method

Inactive Publication Date: 2019-05-24
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The raw material 2-amino-1,3,5-trimethylbenzene required for this reaction is expensive and difficult to synthesize, and because the amide bond is easily hydrolyzed under alkaline heating conditions, it is easy to regenerate 2-amino-1,3,5 -Trimethylbenzene thus epoxidizes benzene, making the reaction difficult to control resulting in lower yields and difficult purification

Method used

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  • Method for synthetizing 2-amino-1, 3, 5-benzenetricarboxylic acid and application thereof for preparation of NH2-MOF-808
  • Method for synthetizing 2-amino-1, 3, 5-benzenetricarboxylic acid and application thereof for preparation of NH2-MOF-808
  • Method for synthetizing 2-amino-1, 3, 5-benzenetricarboxylic acid and application thereof for preparation of NH2-MOF-808

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A highly efficient synthetic method for 2-amino-1,3,5-benzenetricarboxylic acid, comprising the following steps:

[0036] Step 1: Weigh 7.9g of 3,5-dimethylbenzoic acid and dissolve it in 20mL of acetic acid solution, add 8.8mL of concentrated nitric acid, and heat to 80°C. Add 7.9 mL of concentrated sulfuric acid dropwise into the mixture with a dropping funnel, and react at 80°C for 30 minutes. After the reaction, collect the solid precipitate by filtration to obtain 2-nitro-3,5-dimethylbenzoic acid. The yield is 92%.

[0037] Step 2: Weigh 2g of 2-nitro-3,5-dimethylbenzoic acid obtained in step 1 and add it to 20mL of water, add 1.4g of sodium hydroxide, the pH of the test solution is alkaline, weigh 6.48g of permanganate Potassium was added three times in about 4 hours under ice bath conditions, and then reacted at 60°C for 10 hours. After the end, add ethanol to remove unreacted potassium permanganate and filter it with a sand core funnel. Take the filtrate and ad...

Embodiment 2

[0043] Efficient Synthesis of 2-Amino-1,3,5-Benzenetricarboxylic Acid and NH 2 -The preparation method of MOF-808, comprises the following steps:

[0044] Step 1: Weigh 7.9g of 3,5-dimethylbenzoic acid and dissolve it in 20mL of acetic acid solution, add 8.8mL of concentrated nitric acid, and heat to 80°C. Add 7.9 mL of concentrated sulfuric acid dropwise into the mixture with a dropping funnel, and react at 80°C for 30 minutes. After the reaction, collect the solid precipitate by filtration to obtain 2-nitro-3,5-dimethylbenzoic acid. The yield is 90%.

[0045] Step 2: Weigh 2g of 2-nitro-3,5-dimethylbenzoic acid obtained in step 1 and add it to 20mL of water, add 1.4g of sodium hydroxide, the pH of the test solution is alkaline, weigh 6.48g of permanganate Potassium was added three times in about 4 hours under ice bath conditions, and then reacted at 60°C for 10 hours. After the end, add ethanol to remove unreacted potassium permanganate and filter it with a sand core funne...

Embodiment 3

[0050] Efficient Synthesis of 2-Amino-1,3,5-Benzenetricarboxylic Acid and NH 2 -The preparation method of MOF-808, comprises the following steps:

[0051] Step 1: Weigh 7.9g of 3,5-dimethylbenzoic acid and dissolve it in 20mL of acetic acid solution, add 8.8mL of concentrated nitric acid, and heat to 80°C. Add 7.9 mL of concentrated sulfuric acid dropwise into the mixture with a dropping funnel, and react at 80°C for 30 minutes. After the reaction, collect the solid precipitate by filtration to obtain 2-nitro-3,5-dimethylbenzoic acid. The yield is 93%.

[0052] Step 2: Weigh 2g of 2-nitro-3,5-dimethylbenzoic acid obtained in step 1 and add it to 20mL of water, add 1.4g of sodium hydroxide, the pH of the test solution is alkaline, weigh 6.48g of permanganate Potassium was added three times in about 4 hours under ice bath conditions, and then reacted at 60°C for 10 hours. After the end, add ethanol to remove unreacted potassium permanganate and filter it with a sand core funne...

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Abstract

The invention belongs to the field of preparation and application of organic compounds and metal-organic framework compounds, and discloses a method for synthetizing 2-amino-1, 3, 5-benzenetricarboxylic acid and an application thereof for preparation of a photocatalysis NH2-MOF-808 material, the process comprises the following steps: (1) using 3, 5-dimethyl benzoic acid as a raw material, and preparing a precursor ligand 2-amino-1, 3, 5-benzene tricarbonic acid through the steps of nitration, oxidation, reduction and the like, wherein the process method is simple and feasible, the cost is lower, and the yield is high; (2) synthesizing an amino-substituted NH2-MOF-808 material by adopting a solvothermal method at a certain temperature, and carrying out catalytic degradation on rhodamine B (RhB) and methyl orange (MO) by simulating sunlight by using a xenon lamp. In addition, XRD, SEM, FT-IR and DRS technologies are used to carry out characterize tests on the structure and properties ofthe material. Due to the introduction of amino groups, NH2-MOF-808 has an enhanced adsorption property than MOF-808, and the light absorption range is expanded, making it potentially useful in the fields of adsorption, Lewis base catalysis, and photocatalysis.

Description

technical field [0001] The invention belongs to the field of preparation and application of organic compounds and metal-organic framework compounds, in particular to a synthesis method of 2-amino-1,3,5-benzenetricarboxylic acid and its use in the preparation of NH 2 -Use of MOF-808 material. Background technique [0002] As a unique type of organic-inorganic hybrid material with a complex porous network, MOFs have a wide variety of choices of central metal ions and organic ligands, and are favored because of their controllable high specific area and porous structure. It has attracted attention and is widely used in the fields of light, electricity, magnetism, gas storage, drug release, adsorption, and catalysis. In order to enhance the adsorption and catalytic performance of MOFs, purposefully design and synthesize MOFs containing unsaturated metal coordination sites or introduce uncoordinated -OH, -NH on MOFs ligands 2 ,-OCH 3 ,-NO 2 And other active groups are very eff...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/62C07C227/04C07C205/57C07C201/08C07C201/12C08G83/00B01J31/22C02F1/30C02F101/30
Inventor 王方平夏昌坤陈敏姜德立朱光辉
Owner JIANGSU UNIV
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