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Preparation method of 1, 3-diaminoguanidine monohydrochloride

A technology of diaminoguanidine and hydrochloride, which is applied in the fields of phosphate, phosphorus oxyacid, organic chemistry, etc., can solve the problems of high toxicity of dimethyl sulfate, long synthetic route, complicated operation, etc., and achieve the benefit of large-scale Industrialized production, improved production profit, high purity effect

Active Publication Date: 2015-02-25
甘肃汇能生物工程有限公司
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AI Technical Summary

Benefits of technology

This patented technology uses guanidinol or its salts together with other chemicals for producing various products such as pesticides that have low costs compared to traditional methods. It involves dissolving nitrogen oxide (NO) into an organic liquid called guanooline chloroformate, then adding it back again at room temperature under specific pH values. These reactions help reduce harmful waste generated during manufacturing processes while still achieving desired results. Additionally, this new technique allows for easy handling without causing any health hazards when treating certain types of pollution.

Problems solved by technology

Technical Problem: In this patented technical problem addressed in this patents, there have been many attempts at developing new ways to make aminoguanyl derivatives like guaidinetrins more stable without causing environmental concerns during manufacturing processes.

Method used

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  • Preparation method of 1, 3-diaminoguanidine monohydrochloride

Examples

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Embodiment 1

[0024] A kind of preparation method of 1,3-diaminoguanidine hydrochloride, concrete steps are as follows:

[0025] (1) Put guanidine hydrochloride (1Kg) and water (2Kg) into the reaction kettle, stir until the guanidine hydrochloride is completely dissolved, then add 1.0Kg of toluene (the mass ratio to water is 1:0.5), and then slowly add hydrazine hydrate ( 1.02Kg, the molar ratio of guanidine hydrochloride is 1:1.9,), the rate of addition is 2.0kg / h, after the dropwise addition, react at 60°C for 10h, adjust the pH to 2.5 with hydrochloric acid, let stand to separate the liquid, take the water layer and distill and concentrate There is a trace of precipitate in the water layer, and the concentrated solution is about (1.5Kg). In the reaction, the tail gas is passed into the tail gas absorption device, and the by-product ammonia produced in the reaction is absorbed by the three-level acid solution to obtain the ammonium salt solution. The acid solution Sequentially: mass fract...

Embodiment 2

[0028] A kind of preparation method of 1,3-diaminoguanidine hydrochloride, concrete steps are as follows:

[0029] (1) Put guanidine hydrochloride (10Kg) and aqueous solution (20Kg) into the reaction kettle, stir until the guanidine hydrochloride is completely dissolved, then add toluene (4Kg, the mass ratio to water is 1:0.2), and then slowly add hydrazine hydrate ( 10.4Kg, the molar ratio to guanidine hydrochloride is 1:2), the dropping rate is 2.5kg / h, after the dropwise addition, react at 70°C for 9h, adjust the pH to 2.5 with hydrochloric acid, let stand to separate the liquid, take the water layer and distill and concentrate to There is a small amount of precipitate in the water layer, and the concentrated solution is obtained about (15.1Kg). The by-product ammonia produced in the reaction absorbs the ammonium salt solution with a tertiary acid solution, and the acid solution is successively: mass fraction 85% phosphoric acid aqueous solution, mass fraction 50% phosphori...

Embodiment 3

[0032] A kind of preparation method of 1,3-diaminoguanidine hydrochloride, concrete steps are as follows:

[0033] (1) Put guanidine hydrochloride (1Kg) and water (4Kg) into the reaction kettle, stir until the guanidine hydrochloride is completely dissolved, then add toluene (1.6Kg, the mass ratio to water is 1:0.4), and then slowly add hydrazine hydrate dropwise (1.05Kg, molar ratio to guanidine hydrochloride 1:2.0), the dropping rate is 2.25kg / h, after the dropwise addition, react at 60°C for 10h, adjust the pH to 2.5 with hydrochloric acid, let stand to separate the liquid, take the water layer and distill and concentrate There is a trace of precipitate in the water layer, and about (2.5Kg) of the concentrated solution is obtained. In the reaction, the tail gas is passed into the tail gas absorbing device, and the by-product ammonia produced in the reaction is absorbed with a three-stage acid solution to obtain an ammonium salt solution. The acid solution Sequentially: mass...

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Abstract

The invention relates to a preparation method of 1, 3-diaminoguanidine monohydrochloride. The preparation method comprises the following steps of 1, dissolving guanidine hydrochloride as a raw material in water, adding a proper amount of toluene into the solution, dropwisely adding hydrazine hydrate into the mixed solution to cause a reaction lasting for 5-10h at a temperature of 50-110 DEG C, then adjusting a pH value to less than 3 by hydrochloric acid, carrying out standing liquid-separation, taking a water layer, and carrying out distillation concentration until the water layer produces a trace amount of precipitates, wherein a mass ratio of guanidine hydrochloride to water is 1: (2-6), a mass ratio of water to toluene is 1: (0.2-0.5) and a mole ratio of guanidine hydrochloride to hydrazine hydrate is 1: (1.9-2.5), and 2, slowly and dropwisely adding the concentrated solution obtained by the step 1 into a reactor with anhydrous ethanol along with stirring so that crystals are produced, washing the white crystals by cool water with a temperature of 1-6 DEG C and mass 2-3 times that of the concentrated solution, and carrying out drying to obtain a white solid object product, wherein a mass ratio of the concentrated solution to the anhydrous ethanol is 1: (3-5). The preparation method has the advantages of simple processes, mild conditions, high yield, high purity and environmental friendliness.

Description

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Claims

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Application Information

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Owner 甘肃汇能生物工程有限公司
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