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Industrial catalysis method of synthetic nitro substitution compound

A synthetic method and industrial technology, applied in the field of nitro-substituted compounds, industrial catalysis for the synthesis of nitroguanidine, and the synthesis of nitroguanidine, which can solve the tedious crystallization process or post-processing steps, which are difficult to adapt to large-scale industrial production, Unsatisfactory product yield and other issues, to achieve the effect of efficient catalytic synthesis, broad industrialization prospects and technology transformation value, and reduce reaction time

Active Publication Date: 2014-05-14
辽宁森源化工股份有限公司
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  • Summary
  • 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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  • Industrial catalysis method of synthetic nitro substitution compound
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  • Industrial catalysis method of synthetic nitro substitution compound

Examples

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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, place them in a mortar, grind and mix uniformly, to obtain the catalyst used in all the following specific examples of the present invention.

Embodiment 1

[0032] Add 1000g of nitric acid with a mass concentration of 35% to the reactor filled with cooling water, maintain the temperature at 5-10°C, add 500g of guanidine nitrate to it in turn, add 25g of catalyst under stirring, and then add 25g of crown ether 18-crown- 6. Raise the temperature to 28℃, continue to stir the reaction for 30 minutes, the speed of the stirrer is 200r / min, then pour the reaction mixture into ice water, and a large amount of solids will precipitate out. After filtering and washing, the pure nitroguanidine can be obtained. The yield of guanidine 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 reactor with cooling water, maintain the temperature at 5-10℃, add 500g of guanidine nitrate to it in turn, add 25g of catalyst under stirring, and then add 10g of crown ether 15-crown- 5. Raise the temperature to 32℃, continue to stir the reaction for 40 minutes, the speed of the stirrer is 300r / min, then pour the reaction mixture into ice water, and a large amount of solids will precipitate out. After filtering and washing, the pure 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 method for synthesizing nitro substituted compounds, especially nitroguanidine, and more specifically to an industrial catalytic method for synthesizing nitroguanidine, belonging 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 used directly as chemical raw materials or as intermediates in the synthesis of a variety of organic compounds, thus having an important position and role. [0003] Among nitro compounds, nitroguanidine, also known as tropicite, is a white needle-like crystal with a very wide range of uses. First, nitroguanidine can be used as a raw material or intermediate for organic synthesis, for example, as an intermediate for imidacloprid and acetamiprid for the synthesis of N-nitroiminoimidazolidine; secondly, nitroguanidine can be reduced to prepare the corresponding aminoguanidine ,...

Claims

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Application Information

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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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