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A kind of industrial catalytic method of synthesizing nitro-substituted compound

An industrial and catalyst technology, applied in the field of chemical intermediate synthesis, can solve the problems of cumbersome crystallization treatment process or post-treatment steps, difficult to adapt to large-scale industrial production, unsatisfactory product yield and other problems, and achieves efficient catalytic synthesis, Broad industrialization prospects and technological transformation value, the effect of reducing reaction time

Active Publication Date: 2016-06-01
辽宁森源化工股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Although there are many synthesis processes or methods of nitroguanidine in the prior art, these methods involve complicated crystallization treatment or post-treatment steps, or adopt specific reactors (such as tubular reactors or microchannel reactions) device), or the use of high-concentration acid for the dehydration reaction has potential safety hazards, or the yield of the product is still unsatisfactory and other defects. These inherent drawbacks often increase the cost of production and waste industrial raw materials, thereby making the existing process The method is difficult to adapt to large-scale industrial production

Method used

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  • A kind of industrial catalytic method of synthesizing nitro-substituted compound
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  • A kind of industrial catalytic method of synthesizing nitro-substituted compound

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Effect test

preparation example 1

[0030] Weigh thiophene-3-boronic acid and CuCl according to the molar ratio of 1:1:1 2 And each component of ammonium chloride, it is placed in the mortar and grinds and mixes evenly, promptly obtains the catalyst that adopts in the following all specific embodiments of the present invention.

Embodiment 1

[0032] Add 1000g of nitric acid with a mass concentration of 35% to the reaction kettle with cooling water, maintain the temperature at 5-10°C, add 500g of guanidine nitrate in turn, add 25g of catalyst under stirring, and then add 25g of crown ether 18-crown- 6. Raise the temperature to 28°C, continue to stir the reaction for 30 minutes, and the speed of the stirrer is 200r / min, then pour the reaction mixture into ice water, and a large amount of solids are precipitated. After filtering and washing, the pure product of nitroguanidine, nitroguanidine can be obtained. The base guanidine yield was 98.8%, and the purity was 98.7% (HPLC).

Embodiment 2

[0034]Add 1200g of nitric acid with a mass concentration of 30% to the reaction kettle with cooling water, maintain the temperature at 5-10°C, add 500g of guanidine nitrate in turn, add 25g of catalyst under stirring, and then add 10g of crown ether 15-crown- 5. Raise the temperature to 32°C, continue to stir the reaction for 40 minutes, the stirrer speed is 300r / min, then pour the reaction mixture into ice water, a large amount of solids are precipitated, after filtering and washing, the pure nitroguanidine, nitroguanidine can be obtained. The yield of guanidine was 99.4%, and the purity was 98.9% (HPLC).

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Abstract

The invention relates to a synthetic nitro substitution compound, in particular to an industrial catalysis method of nitroguanidine. A novel ternary catalytic system is formed by screening out different kinds of component combinations, the reaction environment with low concentration nitric acid is achieved by using an additive, the nitroguanidine is used as raw materials, and the preparation for the nitroguanidine can be finished by the reaction with high yield within a short time, so that the utilization of high level of acid which has strong corrosion resistance and high volatilization can be avoided and production cost is reduced. Through the optimization of process parameters, the optimal technology of the industrial catalysis of the nitroguanidine which is suitable for being produced widely is explored, the reaction yield and material utilization rate are improved greatly, and application prospects and market value are wide.

Description

technical field [0001] The invention relates to a nitro-substituted compound, especially a method for synthesizing nitroguanidine, and more specifically relates to an industrial catalytic method for synthesizing nitroguanidine, which belongs to the field of chemical intermediate synthesis. Background technique [0002] Nitro-substituted compounds are an important class of organic compounds in organic chemistry. They can be directly used as chemical raw materials, or as intermediates for the synthesis of various organic compounds, thus playing an important role. [0003] Among the nitro compounds, nitroguanidine, also known as peridotite, is a white needle crystal with a wide range of uses. First of all, nitroguanidine can be used as a raw material or intermediate for organic synthesis, for example, as an intermediate of imidacloprid and acetamiprid for the synthesis of N-nitroiminoimidazolidine; secondly, nitroguanidine can be reduced to prepare the corresponding aminoguanid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C279/34C07C277/08
Inventor 章方军
Owner 辽宁森源化工股份有限公司
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