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Methyl nitroguanidine and preparation method thereof

A technology of methyl nitroguanidine and nitroguanidine, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of reducing the yield of methyl nitroguanidine products, complex production process, etc., and achieves Low pollution, high reaction yield and convenient operation

Inactive Publication Date: 2009-10-28
NANTONG TENDENCI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current production process is complicated, and the product yield of methyl nitroguanidine after the reaction is reduced due to the limitation of the use of catalysts

Method used

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  • Methyl nitroguanidine and preparation method thereof
  • Methyl nitroguanidine and preparation method thereof
  • Methyl nitroguanidine and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] According to the molar ratio of reactant nitroguanidine, methylamine, water, sulfuric acid is: nitroguanidine: methylamine: water: sulfuric acid=1: 2: 10: 0.1.

[0017] Put a certain concentration of 800kg dilute sulfuric acid solution into a 1500L reaction kettle from the head tank, add alkylamine solution, adjust the pH value to 8.5, then put in 600kg of wet nitroguanidine, raise the temperature to 100°C, and add the remaining alkylamine solution, adjust the pH value at 10, and control the temperature at 70°C for about 5 hours. After the reaction, the temperature was lowered to 5° C., centrifugal dehydration was performed, and the filter cake was washed with cold water to obtain about 600 kg of crude methyl nitroguanidine.

[0018] Put the above-mentioned crude methyl nitroguanidine into a 1500L kettle with 800L of water, raise the temperature to 90°C, wait for the methylnitroguanidine to completely dissolve and filter, then cool the filtrate to 5°C in the crystalliza...

Embodiment 2

[0020] According to the mol ratio of reactant nitroguanidine, methylamine, water, sulfuric acid is: nitroguanidine: methylamine: water: sulfuric acid=1: 4: 15: 0.15.

[0021] Put a certain concentration of 800kg dilute sulfuric acid solution into a 1500L reactor from the head tank, add the alkylamine solution, adjust the pH value to 9.0, then put in 600kg of wet nitroguanidine, raise the temperature to 105°C, and add the remaining alkylamine solution, adjust the pH value at 11, and control the temperature at 75°C for 6 hours. After the reaction, the temperature was lowered to 5° C., centrifugal dehydration was performed, and the filter cake was washed with cold water to obtain about 600 kg of crude methyl nitroguanidine.

[0022] Put the above-mentioned crude methyl nitroguanidine into a 1500L kettle with 800L of water, raise the temperature to 90°C, wait for the methylnitroguanidine to completely dissolve and filter, then cool the filtrate to 5°C in the crystallization kettle...

Embodiment 3

[0024] According to the molar ratio of reactant nitroguanidine, methylamine, water, sulfuric acid is: nitroguanidine: methylamine: water: sulfuric acid=1: 6: 20: 0.25.

[0025] Put 800kg of dilute sulfuric acid solution of a certain concentration into a 1500L reaction kettle from the head tank, add alkylamine solution, adjust the pH value to 8.5, then put in 600kg of wet nitroguanidine, raise the temperature to 105°C, and add the remaining alkylamine solution, adjust the pH value at 10, and control the temperature at 80°C for 5 hours. After the reaction, the temperature was lowered to 5° C., centrifugal dehydration was performed, and the filter cake was washed with cold water to obtain about 600 kg of crude methyl nitroguanidine.

[0026] Put the above-mentioned crude methyl nitroguanidine into a 1500L kettle with 800L of water, raise the temperature to 90°C, wait for the methylnitroguanidine to completely dissolve and filter, then cool the filtrate to 5°C in the crystallizati...

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Abstract

The invention discloses methyl nitroguanidine and a preparation method thereof. Alkyl nitroguanidine is produced by the reaction of nitroguanidine, alkylamine and water under the condition of taking vitriol as a catalyst. The processing equipment is simple in structure and convenient to operate and has high reaction yield after taking the vitriol as the catalyst, little pollution and high product purity of over 98 percent generally.

Description

technical field [0001] The invention relates to a methyl nitroguanidine and a preparation method thereof. Background technique [0002] Methylnitroguanidine is a very important chemical raw material, mainly used as an intermediate for the insecticide thiaclonil. The current production process is complicated, and the product yield of methyl nitroguanidine after the reaction is reduced due to the limitation of the use of the catalyst. Contents of the invention [0003] The invention provides methyl nitroguanidine with simple process and high yield and a preparation method thereof. [0004] In order to solve the above technical problems, a kind of methyl nitroguanidine of the present invention and preparation method thereof, the structural formula of described methyl nitroguanidine is: [0005] [0006] R represents hydrogen or an alkyl chain of 1-8 carbon atoms. [0007] The preparation method of described a kind of methyl nitroguanidine, reacts and generates alkyl nit...

Claims

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Application Information

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IPC IPC(8): C07C279/36C07C277/08
Inventor 查志明
Owner NANTONG TENDENCI CHEM
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