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3,5-diaminobenzoic acid preparation method

A technology of m-diaminobenzene and dinitrobenzoic acid, which is applied in the field of preparation of m-diaminobenzoic acid, can solve the problems of waste residue wastewater pollution, low yield, poor product quality, etc., and achieve high yield and short process route , no effect of three wastes pollution

Active Publication Date: 2009-02-11
内蒙古利元科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] This synthesis route is the iron powder reduction method route, the product quality of this method is poor, the yield is low, and there is a large amount of waste residue (iron slag) and waste water to pollute the environment

Method used

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  • 3,5-diaminobenzoic acid preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Put 300 ml of methanol as a solvent, 50 g of raw material 3,5-dinitroformic acid, and 0.25 g of Ni-Al type nickel as a catalyst into a 1-liter stainless steel high-pressure reactor, heat up at 20°C and feed hydrogen, control the hydrogen pressure at 2 MPa, react for 10 hours, discharge After pressing, the material is discharged and filtered, and the filtrate is separated from methanol to obtain the product m-diaminobenzoic acid. The content of chromatographic analysis is 95%, and the yield is 96%. The catalyst was washed with methanol for later use.

Embodiment 2

[0023] Use 300 milliliters of ethanol as solvent, get 50g raw material 3,5-dinitroformic acid, Ni-Al type nickel 3.5g, control hydrogen pressure 3MPa, react at 150 ℃ of temperature for 3 hours, operate with embodiment 1, obtain the product between two Aminobenzoic acid, the content of chromatographic analysis is 95%, and the yield is 97%.

Embodiment 3

[0025] Take 7.1gPaCl 3 , 304 g (NO 3 ) 3 ·6H 2 O was dissolved in 1.2 liters of distilled water and 20 milliliters of concentrated hydrochloric acid, heated to 50°C, and 500 milliliters of 30% sodium hydroxide was added for precipitation reaction. After 4 hours of reaction, solution 1 was obtained; distilled water was added to 90 grams of activated carbon, and the volume ratio was 1 : 2, stirring at 50°C until viscous slurry 2; adding solution 1 into slurry 2, reacting, reducing by passing through hydrogen, washing with methanol and water, and drying in vacuum at 120°C to obtain a catalyst activated carbon carrier.

[0026] Add 0.1 mole m-dinitrobenzoic acid (chemically pure), 100ml methanol (chemically pure) and 0.25 g of catalyst activated carbon carrier into the autoclave, feed hydrogen into the autoclave for 2 times, then pass into 0.3 mole of hydrogen, The reaction was carried out at a pressure of 1MPa, and the temperature was controlled at 80°C. After the system no lo...

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Abstract

The invention relates to a preparation method of 3, 5-diaminobenzoic acid, which is characterized in that: the 3, 5-dinitrobenzoic acid is taken as raw material, carbinol or ethanol as a solvent, and added with a catalyst; a reduction reaction is carried out between the 3, 5-dinitrobenzoic and hydrogen of theoretical reacting weight for 2-10 hours under the reaction pressure of 0.1 MPa to 5MPa as well as the reaction temperature of 20 DEG C to 150 DEG C, thereby obtaining crude product; the crude product is separated and removed off the solvent to obtain the 3, 5-diaminobenzoic acid product, wherein, the dosage ratio of materials is calculated on the basis of 1mol of 3, 5-dinitrobenzoic acid, the dosage of the carbinol or ethanol is 200ml to 1000ml, and the dosage of the catalyst is 0.5 percent to 10 percent of the weight of the 3, 5-dinitrobenzoic acid; the catalyst is either Raney nickel or an active carbon carrier. The method has short technological line, product purity up to 95 percent and yield rate over 96 percent and causes no 'three wastes' (waste gas, waste water and waste residues) pollution and the catalyst can be recovered for later use.

Description

technical field [0001] The invention relates to a method for preparing an organic intermediate, in particular to a method for preparing m-diaminobenzoic acid. Background technique [0002] m-diaminobenzoic acid is an important organic intermediate, which can be used as an intermediate in the synthesis of medicines and dyes, such as the synthesis of diatrizoic acid, reactive dyes, etc. These materials play an extremely important role in production and life. Important role, because m-diaminobenzoic acid has such a wide range of uses, its products and production methods have received widespread attention. At present, the main synthetic routes used to prepare m-diaminobenzoic acid are as follows: [0003] [0004] This synthesis route is the iron powder reduction method route, and this method product quality is poor, and yield is low, and there is a large amount of waste slag (iron slag) and waste water to pollute the environment. Contents of the invention [0005] The pur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/60C07C227/06
CPCY02P20/584
Inventor 罗俊龙
Owner 内蒙古利元科技有限公司
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