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A kind of method of synthesizing phthalimide by means of urea choline chloride eutectic

A technology of phthalimide and choline chloride, which is applied in organic chemistry and other fields, and can solve problems such as pollution and environmental discharge

Active Publication Date: 2021-12-21
河北寰烯科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The object of the present invention is to provide a kind of method by means of urea choline chloride eutectic compound synthetic phthalimide, to overcome xylene, kerosene or N that exist in the traditional phthalimide production, Issues such as N-dimethylformamide VOCs emission and environmental pollution

Method used

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  • A kind of method of synthesizing phthalimide by means of urea choline chloride eutectic

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Effect test

Embodiment 1

[0014] 100 kilograms of urea and choline chloride molar ratio are 2:1 urea-choline chloride deep eutectic solvent and industrial grade purity 99% phthalic anhydride 57 kilograms are added in the reactor 1, rely on the reactor jacket steam to make the reactor The inner material is heated to 130°C and reacted for 2 hours. During the reaction, urea is added twice, 16 kg each time, and phthalimide is gradually precipitated as white crystals; after that, the temperature is lowered to about 60°C, and the material is sent to the centrifuge. Filtration in the filter filter 2; the filtrate is pumped into the reaction kettle 1 for recycling; the filter cake is washed with water in the washing kettle 3, and then sent to the dryer 4 for drying to obtain 54.5 kg of phthalimide products with a purity of more than 98% .

Embodiment 2

[0016] 100 kilograms of urea and choline chloride molar ratio are 2:1 urea-choline chloride deep eutectic solvent and industrial grade purity 99% phthalic anhydride 57 kilograms are added in the reactor 1, rely on the reactor jacket steam to make the reactor Heat the material inside to 132°C and react for 2 hours. During the reaction, add urea twice, 15 kg each time, and phthalimide is gradually precipitated as white crystals; after that, the material is sent to the centrifugal filter for filtration 2 Filtration; the filtrate is pumped into the reaction kettle 1 for recycling; the filter cake is washed with water in the washing kettle 3, and then sent to the drier 4 for drying to obtain 53 kilograms of phthalimide products with a purity of more than 98%.

Embodiment 3

[0018] 100 kilograms of urea and choline chloride molar ratio are 2:1 urea-choline chloride deep eutectic solvent and industrial grade purity 99% phthalic anhydride 57 kilograms are added in the reactor 1, rely on the reactor jacket steam to make the reactor Heat the material inside to 133°C and react for 2 hours. During the reaction, add urea twice, 15 kg each time, and phthalimide gradually precipitates as white crystals; then cool down to about 60°C, and send the material into the centrifuge Filtration in the filter filter 2; the filtrate is pumped into the reaction kettle 1 for recycling; the filter cake is washed with water in the washing kettle 3, and then sent to the dryer 4 for drying to obtain 52 kg of phthalimide products with a purity of more than 98% .

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Abstract

The invention uses phthalic anhydride as raw material, urea-choline chloride deep eutectic solvent as solvent, urea raw material and catalyst, and synthesizes phthalimide at relatively low temperature. This method overcomes the shortcomings of using solvents such as xylene, kerosene or N,N-dimethylformamide in the traditional process, and the solvent urea-choline chloride deep eutectic solvent can be recycled and reused, and the new process can reduce VOCs emissions. The crude phthalimide product is filtered, washed with water, and dried to obtain a phthalimide product with a certain purity. The process is simple in operation and mild in conditions. The low-temperature reaction reduces the decomposition of urea, avoids the loss of raw materials caused by the sublimation of phthalic anhydride and the volatilization of urea, and reduces the production cost. The product yield exceeds 93%, and the purity reaches more than 98%. Compared with similar processes, it has obvious advantages.

Description

technical field [0001] The invention belongs to the technical field of clean organic synthesis, in particular to a method for synthesizing phthalimide by means of urea choline chloride eutectic. Background technique [0002] According to the systematic nomenclature, phthalimide is 1,3-isoindoline-1,3-dione (isoindoline-1,3-dione), which is the downstream product of phthalic anhydride, because the H on N-H in its structure is very active and contains aromatic hydrocarbon structure , Widely used in dyes, pesticides, medicine, rubber, spices and other industries. Phthalimide has abundant downstream products, which can be used to synthesize various fine chemicals such as phenylpeptide, indigo, phthalonitrile, folpet, imidophos and mefenamic acid, nearly 30% of which are used in Synthetic herbicides or plant growth regulators. Anthranilic acid can be produced through Hofmann degradation reaction, amino acid, phthalamide, halogenated phthalimide and standard reagent potassium sa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D209/48
CPCC07D209/48
Inventor 冯树波孟祥鑫韩桂强
Owner 河北寰烯科技有限公司
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