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A kind of preparation method and preparation device of 3,5-dinitro-o-toluic acid

A technology of dinitro-o-toluic acid and o-toluic acid, which is applied in the preparation of nitro compounds, organic chemistry and other directions, can solve problems such as small axial back-mixing, and achieves reduction of side reactions, convenient operation and production. The effect of high process safety

Active Publication Date: 2019-05-07
ZHEJIANG RONGYAO CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Through the above technical scheme, the first tubular reactor and the second tubular reactor replace the tank reactor for nitration reaction, which can accurately control the reaction parameters, and the axial back mixing of reactants in the tube is small, which overcomes the existing reaction The technology has problems such as uneven local concentration, which significantly reduces side reactions; the tubular reaction adopts continuous operation mode, which makes it easier to realize process automation and higher safety in the production process; the preparation method is simple, the operation is convenient, the product yield is high, and it is suitable for industrialization Production

Method used

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  • A kind of preparation method and preparation device of 3,5-dinitro-o-toluic acid
  • A kind of preparation method and preparation device of 3,5-dinitro-o-toluic acid

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Embodiment 1

[0037]A preparation device for 3,5-dinitro-o-toluic acid, comprising a first metering tank 1, a second metering tank 2 and a third metering tank 3, the first metering tank 1, the second metering tank 2 and The third metering tank 3 is respectively connected with the first metering pump 5, the second metering pump 6 and the third metering pump 7 through pipelines, and the first metering pump 5 and the second metering pump 6 are connected to the first mixer 8 through pipelines, The first mixer 8 is connected with the first tubular reactor 10 by a pipeline, the third metering tank 3 is connected with a third metering pump 7 by a pipeline, and the third metering pump 7 and the first tubular reactor 10 are connected with a pipeline respectively. The second mixer 9, the second mixer 9 is connected with the second tubular reactor 11 through the pipeline, and the second tubular reactor 11 is connected with the receiving device 4 of the product through the pipeline, wherein the first tu...

Embodiment 2

[0040] Step 1: Weigh 10.0kg of o-toluic acid in a stirring tank; weigh 20.0kg of 1,2-dichloroethane, pour it into the weighed o-toluic acid and mechanically stir until it is completely dissolved, then transfer to In the first metering tank 1; Take by weighing 9.68 kg of 98% sulfuric acid 14.7kg, 95%-98% nitric acid in the second metering tank 2 and mix;

[0041] Step 2: Feed the materials in the first metering tank 1 and the second metering tank 2 respectively through the corresponding first metering pump 5 and the second metering pump 6 to the first mixer 8 for mixing, and the mixed liquid after uniform mixing enters The first tubular reactor 10 reacts, and the diameter of the first tubular reactor 10 is 1 mm, and the length of the tube is 5 m. The temperature of the first tubular reactor 10 is maintained at 40 ° C by the heat exchange device, and the reaction solution is in the first Reach the second mixer 9 after staying in the tubular reactor 10 for 2min;

[0042] Step 3:...

Embodiment 3

[0045] Step 1: Weigh 10.0kg of o-toluic acid in a stirring tank; weigh 60.0kg of 1,2-dichloroethane, pour it into the weighed o-toluic acid and mechanically stir until it is completely dissolved, then transfer to In the first metering tank 1; Take by weighing 98% sulfuric acid 110.3kg, 95%-98% nitric acid 15.1kg in the second metering tank 2 and mix;

[0046] Step 2: Feed the materials in the first metering tank 1 and the second metering tank 2 respectively through the corresponding first metering pump 5 and the second metering pump 6 to the first mixer 8 for mixing, and the mixed liquid after uniform mixing enters The first tubular reactor 10, the diameter of the first tubular reactor 10 is 30mm, and the length of the tube is 5m. The temperature of the first tubular reactor 10 is maintained at 83°C by the heat exchange device, and the reaction solution is in the first tubular reactor. After staying in the reactor 10 for 4min, it reaches the second mixer 9;

[0047] Step 3: W...

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Abstract

The invention discloses a preparation method and device for 3,5-binitro-o-methylbenzoic acid. According to the key point of the technical scheme, the device comprises a first measuring tank, a second measuring tank and a third measuring tank, wherein the first measuring tank and the second measuring tank are connected with a first measuring pump and a second measuring pump respectively through pipelines, the first measuring pump and the second measuring pump are respectively connected with a first mixer through pipelines, the first mixer is connected with a first tubular reactor through a pipeline, the third measuring tank is connected with a third measuring pump through a pipeline, the third measuring pump and the first tubular reactor are connected with a second mixture respectively through pipelines, the second mixer is connected with a second tubular reactor through a pipeline, and the second tubular reactor is connected with a product receiving device through a pipeline. The process for producing 3,5-binitro-o-methylbenzoic acid by virtue of the device is high in safety.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a preparation method and a preparation device of 3,5-dinitro-o-toluic acid. Background technique [0002] 3,5-Dinitro-o-toluic acid is an important intermediate for the synthesis of dinitrothamine (also known as globulin). Ammonium formate) is a broad-spectrum, efficient, safe, and non-residue anticoccidiostat, which can promote the growth of chickens in feed. It is effective against a variety of Eimeria in chickens, such as tender, poisonous, Brucella, heap-shaped, giant, etc. Eimeria and turkey coccidia. Especially for Eimeria tenabilis and Eimeria poisonous, it mainly inhibits the schizospores of the asexual cycle. The product is not only used for prevention, but also for treatment. The application of treatment dose has no adverse effect on the growth, development and hatching rate of eggs of chickens, and it also has a good effect on the prevention and treatment of coccidio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C201/08C07C205/57
CPCC07C201/08C07C205/57
Inventor 余志群王文佐苏为科陈建华陈仁尔
Owner ZHEJIANG RONGYAO CHEM
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