Preparation method of dinitroglycol guanidine

A technology of dinitroglycoguanidine and guanidine nitrate, which is applied in the direction of organic chemistry, can solve problems such as side reactions, and achieve the effects of increased yield, good economic benefits, and less impurity content

Inactive Publication Date: 2019-01-04
NANTONG TENDENCI CHEM
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Problems solved by technology

[0003] The technical problem to be solved by the present invention is that, aiming at the problem of side reactions in the process of preparing dinitroglycoguanidine in the prior art, the present invention provides a method of using ultrasonic low-temperature reaction to safely and efficiently convert nitroguanidine into Dinitroglyguanide method

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  • Preparation method of dinitroglycol guanidine

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Embodiment

[0024] This embodiment discloses a preparation method of dinitroglycoguanidine. The preparation method adopts ultrasonic and low-temperature dropwise addition. The specific steps of the preparation method are as follows:

[0025] Add 200g of concentrated sulfuric acid into a 500ml round bottom flask, the concentration of sulfuric acid is 98%, start stirring and slowly add 100g of guanidine nitrate, the feeding speed is controlled at 30min, and the feeding temperature does not exceed 30°C. After the addition of guanidine nitrate, slowly heat up to 40 ℃, heat preservation reaction for 0.5h, the material was added to 800g of ice water, rapidly stirred to cool down to 25 ℃, then filtered and washed with water to obtain nitroguanidine.

[0026] Add 174g of 40% glyoxal aqueous solution into a 500ml round-bottom flask, start stirring, slowly add 130g of nitroguanidine, and drop 52g of 35% hydrochloric acid at the same time, transfer the device to an ultrasonic system after the additio...

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Abstract

The invention discloses a preparation method of dinitroglycol guanidine. Dinitroglycol guanidine is prepared from guanidine nitrate, concentrated sulfuric acid, glyoxal and hydrochloric acid by an ultrasonic reaction, wherein the reaction comprises the following steps: guanidine nitrate is dehydrated by 98% concentrated sulfuric acid and processed by ice, guanidine nitrate is prepared and subjected to the ultrasonic reaction with glyoxal in presence of hydrochloric acid, dinitroglycol guanidine is generated and subjected to postprocessing of filtering, washing, recrystallization and drying, and solid dinitroglycol guanidine is obtained. Prepared dinitroglycol guanidine is high in purity, low in impurity content and high in molar yield, and has good economic benefit; the preparation methodis safe, environmentally friendly and applicable to industrial production.

Description

technical field [0001] The invention relates to the field of dinitroglycoguanidine production, in particular to a preparation method of dinitroglycoguanidine. Background technique [0002] In recent years, many natural products containing guanidine derivatives have been isolated from natural organisms, and many compounds containing guanidine have been found to have biological activity, and guanidine plays an important role in the activity. It is precisely because of the high biological activity of guanidine compounds that guanidine and its derivatives are widely used in clinical medicine, surfactants and pesticides. Dinitroglyguanidine is an important analogous precursor of the insecticide imidacloprid. The current existing methods have low yields and long acid catalysis time in the early stage. Therefore, the present invention has far-reaching significance for the insecticide imidacloprid. Contents of the invention [0003] The technical problem to be solved by the pre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/04
CPCC07D487/04
Inventor 张赟
Owner NANTONG TENDENCI CHEM
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