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Comprehensive utilization method of m-toluic acid nitration solid waste

A technology of m-toluic acid and toluic acid, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry and other directions, can solve the problems of low product selectivity and many nitrification by-products, etc., and achieve obvious economic value. , The effect of remarkable economic benefit and simple method

Active Publication Date: 2018-06-29
山东友道化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In summary, it can be seen that the existing nitration method of m-toluic acid has many by-products of nitration and low product selectivity.

Method used

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  • Comprehensive utilization method of m-toluic acid nitration solid waste
  • Comprehensive utilization method of m-toluic acid nitration solid waste
  • Comprehensive utilization method of m-toluic acid nitration solid waste

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] The composition of solid waste from the nitration reaction of m-methylbenzoic acid is: the mass percentage of 2-nitro-3-methylbenzoic acid is 10%, the mass percentage of 3-methyl-4-nitrobenzoic acid is 28%, The mass percentage of 2-nitro-5-methylbenzoic acid is 62%. In step (1), the solid waste of the nitrification reaction is dissolved and cleared with a NaOH aqueous solution with a concentration of 30% by mass, and the final pH is 12.8. Step (2) Use 25% concentrated hydrochloric acid to adjust the pH of the solution to 4.4 to obtain 51.8 g of 3-methyl-4-nitrobenzoic acid with a recovery rate of 92.6%. In step (3), 25% concentrated hydrochloric acid was used to adjust the pH of the solution to 3.2 to obtain 18.3 g of 2-nitro-3-methylbenzoic acid with a recovery rate of 91.5%. In step (4), 25% concentrated hydrochloric acid was used to adjust the pH of the solution to 1.2 to obtain 96.3 g of 2-nitro-5-methylbenzoic acid with a recovery rate of 77.7%. , The total recove...

Embodiment 2

[0041] The composition of the solid waste from the nitration reaction of m-methylbenzoic acid is: the mass percentage of 2-nitro-3-methylbenzoic acid is 15%, the mass percentage of 3-methyl-4-nitrobenzoic acid is 20%, The mass percentage of 2-nitro-5-methylbenzoic acid is 65%. Step (1) Use a KOH aqueous solution with a concentration of 20% by mass to dissolve the solid waste of the nitrification reaction, and the final PH=8.4. Step (2) Use 10% dilute nitric acid to adjust the pH of the solution to 4.0 to obtain 36.8 g of 3-methyl-4-nitrobenzoic acid with a recovery rate of 92.0%. Step (3) Use 10% dilute nitric acid to adjust the pH of the solution to 2.5 to obtain 28.5 g of 2-nitro-3-methylbenzoic acid with a recovery rate of 95.0%. Step (4) Use 10% dilute nitric acid to adjust the pH of the solution to 0.5 to obtain 94.9 g of 2-nitro-5-methylbenzoic acid with a recovery rate of 73.0%. , The total recovery rate of the three is 80.1%.

Embodiment 3

[0043] The composition of solid waste from the nitration reaction of m-methylbenzoic acid is: 2-nitro-3-methylbenzoic acid with a mass percentage of 20%, 3-methyl-4-nitrobenzoic acid with a mass percentage of 10%, The mass percentage of 2-nitro-5-methylbenzoic acid is 70%. Step (1) Use 15% NaHCO by mass percentage 3 The aqueous solution will dissolve the solid waste of the nitration reaction, and the final PH=7.5. Step (2) Use 50% phosphoric acid to adjust the pH of the solution to 5.5 to obtain 19.1 g of 3-methyl-4-nitrobenzoic acid with a recovery rate of 95.4%. Step (3) Use 50% phosphoric acid to adjust the pH of the solution to 4.0 to obtain 36.2 g of 2-nitro-3-methylbenzoic acid with a recovery rate of 90.5%. Step (4) Use 50% phosphoric acid to adjust the pH of the solution to 2.4 to obtain 116.2 g of 2-nitro-5-methylbenzoic acid with a recovery rate of 83.0%. , The total recovery rate of the three is 85.7%.

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Abstract

The invention discloses a comprehensive utilization method of m-toluic acid nitration solid waste. The method comprises the following steps: (1) dissolving the m-toluic acid nitration solid waste by alkaline water so as to be clarified, and controlling the pH value of the solution to be 7.5-13 to obtain a clarified solution; (2) adjusting the pH value of the clarified solution to be 4.0-5.5 with acid to obtain slurry, performing filtration to obtain a first filtrate and a first filter cake, and pulping and filtering the first filter cake with water to obtain a 3-methyl-4-nitrobenzoic acid product; (3) adjusting the pH value of the first filtrate to be 2.5-4.0 with acid, performing filtration to obtain a second filtrate and a second filter cake, and pulping and filtering the second filter cake with water to obtain a 2-nitro-3-toluic acid product; and (4) adjusting the pH value of the second filtrate to be 0-2.5 with acid, performing filtration to obtain a third filtrate and a third filter cake, and pulping and filtering the third filter cake with water to obtain a 2-nitro-5-toluic acid product. The method disclosed by the invention is simple, easy to operate and low in cost and especially has important significance of changing wastes into valuables and facilitating environmental protection.

Description

Technical field [0001] The invention relates to the field of fine chemical technology and environmental protection, in particular to a comprehensive utilization method of solid waste from the nitration reaction of m-toluic acid. Background technique [0002] 2-Nitro-3-methylbenzoic acid is the core starting material for the production of the blockbuster insecticides chlorantraniliprole and cyantraniliprole. The industrial production method is to use m-methyl benzoic acid as raw material and use nitric acid or mixed sulfur nitric acid as nitrating agent. The chemical reactions that occur are: [0003] [0004] The results of typical public information reports are listed as follows: [0005] Almog et al. (Urea nitrate and nitrourea. Powerful and regioselective aromatic nitration agents. From Tetrahedron Letters, 47(49), 8651-8652; 2006) used urea nitric acid or a mixture of nitrourea and sulfuric acid as the nitration agent. When nitrourea+concentrated sulfuric acid is used as the ni...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/16C07C205/57
CPCC07C201/16C07C205/57
Inventor 王勤波熊振华宗匡曾鹏曹金辉
Owner 山东友道化学有限公司
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