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Synthesis method of 3,4-diaminotoluene

A technology of diaminotoluene and a synthesis method, applied in the field of organic synthesis, can solve the problems of low content of finished products, brown appearance, unstable quality, etc., and achieve the effects of reduced raw material cost, high product purity, and fewer reaction steps.

Inactive Publication Date: 2017-01-25
JIANGSU TIANJIAYI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above two methods for synthesizing 3,4-diaminotoluene are high in cost, serious in pollution, low in finished product content, brown in appearance, oxidized and discolored in the air, and unstable in quality

Method used

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  • Synthesis method of 3,4-diaminotoluene
  • Synthesis method of 3,4-diaminotoluene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 300 grams of o-nitro-p-toluidine to a 1500 ml three-necked flask equipped with a reflux condenser, then add 450 grams of methanol, stir, and heat the material to 50-55 ° C for 30 minutes to dissolve. Add the above-mentioned methanol solution of o-nitro-p-toluidine to a 1-liter autoclave, then add 30 grams of Ni catalyst, and replace with nitrogen and hydrogen. Start stirring and heat up to 60°C, start hydrogenation, control hydrogenation pressure 1-3MPa, temperature 65-75°C, maintain for 1 hour after hydrogenation, exhaust hydrogen, discharge, remove methanol under normal pressure, and then under reduced pressure The water was removed, and finally 233.6 g of 3,4-diaminotoluene was obtained through rectification under reduced pressure, with a content of 99.5% and a yield of 97%.

[0017] Concrete reaction steps are shown in formula (I):

[0018]

Embodiment 2

[0020] Add 300KG o-nitro-p-toluidine into a 1500L enamel reaction kettle equipped with a reflux condenser, then add methanol 450kg methanol, start stirring, and raise the temperature of the material to 50-50 to dissolve for 30 minutes. The above-mentioned methanol solution of o-nitro-p-toluidine was poured into a 1000-liter autoclave with a stainless steel pump, and then 30 kg of Ni catalyst was added, and replaced with nitrogen and hydrogen. Turn on stirring and heat up to 60°C, start hydrogenation, control hydrogenation pressure 1-3MPa, temperature 65-75°C, keep hydrogenation for 1 hour, exhaust hydrogen, discharge, methanol is removed under normal pressure, and then under reduced pressure The water was removed, and finally 233kg of 3,4-diaminotoluene was obtained through rectification under reduced pressure, with a content of 99.6% and a yield of 96.7%.

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Abstract

The invention relates to a synthesis method of 3,4-diaminotoluene. The synthesis method is characterized in that hydrogenation reduction reaction is performed by taking o-nitro-p-toluidine as a raw material under the action of a catalyst and an alcohol solvent to obtain 3,4-diaminotoluene, wherein the weight ratio of the solvent to o-nitro-p-toluidine is (1.5-3):1; and in the hydrogenation reduction reaction, the temperature is 65-85 DEG C and the pressure is 1.0-4.0 MPa. According to the synthesis method, o-nitro-p-toluidine is used as the raw material, a hydrogenation reduction process is adopted, the synthesis route is short, the product purity is high (99.5%) and the yield is high (96%-97%). Compared with the existing sodium sulfide reduction process and the ferrous powder reduction process, the synthesis method is less in reaction step, short in synthesis route, small in wastewater quantity (0.3 ton of wastewater is generated by the products per ton), high in product purity (99.5%) and stable in quality, obviously reduces the cost of the raw material and satisfies the demands of an anti-rusting agent and a corrosion inhibitor of high-quality and high-grade organic pigment disperse fluorescent yellow and synthesis metals (such as silver, copper, lead, nickel and zinc).

Description

technical field [0001] The invention relates to a synthesis method of 3,4-diaminotoluene, which belongs to the technical field of organic synthesis. Background technique [0002] 3,4-diaminotoluene (also known as 4-methyl-o-phenylenediamine) is an important organic intermediate used in the synthesis of high-grade organic pigments to disperse fluorescent yellow and in the synthesis of metals (such as silver, copper, lead, nickel, Zinc, etc.) antirust agent and corrosion inhibitor (5-methylbenzotriazole), widely used in antirust oil (grease) products, mostly used for copper and copper alloy vapor phase corrosion inhibitor circulating water treatment Agents, automotive antifreeze, polymer stabilizers, plant growth regulators, lubricating oil additives, ultraviolet absorbers, etc. [0003] In the prior art, the synthetic method of 3,4-diaminotoluene has two kinds, and a kind of is to adopt ortho-nitro-p-toluidine as raw material, through alkali sulfide reduction, after the redu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/36C07C211/51
CPCC07C209/36C07C211/51
Inventor 耿宏耿星辰
Owner JIANGSU TIANJIAYI CHEM CO LTD
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