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Preparation method of 1, 3-diamino guanidine hydrochloride

A technology of diaminoguanidine and hydrochloride, which is applied in the direction of organic chemistry, can solve the problems of unfavorable industrial production, high cost of cyanamide, and low yield, etc., so as to facilitate large-scale industrial production, reduce three wastes, and improve The effect of production profit

Active Publication Date: 2015-04-01
ANHUI UNIVERSITY OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method can effectively reduce the generation of by-product triaminoguanidine, but the synthetic route is long, the operation is complicated, and the yield is not very high.
Later, some domestic scholars used cyanamide and hydrazine hydrate to control a certain equivalent ratio reaction, and then added hydrochloric acid for neutralization to prepare 1,3-diaminoguanidine hydrochloride. However, due to the high cost of cyanamide, it is obviously not conducive to the market. Industrial production under competitive environment

Method used

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  • Preparation method of 1, 3-diamino guanidine hydrochloride

Examples

Experimental program
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Effect test

Embodiment 1

[0016] Embodiment 1: drop into sodium thiocyanate (1Kg) and aqueous solution (1Kg) in reaction kettle, then add dimethyl sulfate (0.780Kg), after room temperature reaction 5~6h, collect oil layer, obtain methyl thiocyanate ( 0.892Kg).

[0017] In another reaction kettle, add hydrazine hydrochloride (1.671g) and water (8Kg) to heat up to 30-40°C, then add methyl thiocyanate (0.892Kg), control the reaction temperature at 30-40°C, and react for 4-5 hours Then let it cool down. Filter, wash with cold water three times, and dry to obtain the white target product (1.435Kg, the total yield is 92.8%, and the purity by HPLC is 99.1%). The by-product methyl mercaptan was sequentially absorbed with saturated sodium hydroxide solution, 30% sodium hydroxide solution and 35% sodium bicarbonate solution to obtain sodium methyl mercaptan solution.

Embodiment 2

[0018] Example 2: Add sodium thiocyanate (10Kg) and aqueous solution (10Kg) into the reaction kettle, then add another raw material dimethyl sulfate (7.79Kg), react at room temperature for 5-6 hours, collect the oil layer to obtain thiocyanate Methyl ester (8.91Kg).

[0019] In another reaction kettle, add hydrazine hydrochloride (16.91Kg) and water (80Kg) to raise the temperature to 30-40°C, then add methyl thiocyanate (8.91Kg), use a water bath to control the reaction temperature at 30-40°C, and react 4 After ~5 hours, let it cool down. It was filtered, washed three times with cold water, and then dried to obtain the white target product (14.21Kg, the total yield was 91.7%, and the purity by HPLC was 98.3%). The by-product methyl mercaptan was sequentially absorbed with saturated sodium hydroxide solution, 30% sodium hydroxide solution and 35% sodium bicarbonate solution to obtain sodium methyl mercaptan solution.

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Abstract

The invention discloses a preparation method of 1, 3-diamino guanidine hydrochloride, and belongs to the technical field of preparation of nitrogenous organic compounds. The preparation method comprises steps as follows: sodium thiocyanate is dissolved in water, dimethyl sulfate is added, the mixture reacts a room temperature for 5-6 hours, water and oil are layered after reaction, and a collected oil layer is a primary product of methyl thiocyanate; and hydrazine dihydrochloride is mixed with water, methyl thiocyanate is added when the temperature rises to 30-40 DEG C, the mixture is kept warm and reacts for 4-5 hours, and suction filtration, cold water cleaning and drying are performed, so that a white 1, 3-diamino guanidine hydrochloride solid is obtained. According to the preparation method, sodium thiocyanate and hydrazine dihydrochloride are taken as raw materials, and water is taken as a solvent, so that the production cost can be reduced greatly; and sodium methyl mercaptide is obtained after a by-product of methyl mercaptan is absorbed by an alkaline solution and can be used as a basic material for an intermediate of pesticide, medicine, dye or the like, and large-scale industrial production is facilitated. The preparation method has the advantages that the process is simple, the condition is mild, the yield is high, the product purity is high, environmental protection is realized and the like.

Description

Technical field: [0001] The invention belongs to the technical field of nitrogen-containing organic matter preparation, and in particular relates to a preparation method of 1,3-diaminoguanidine hydrochloride. Background technique: [0002] Guanidine is a nitrogen-containing organic compound, also known as "aminocarbamidine" and "imide urea", which is strongly alkaline and hygroscopic. Guanidine is unstable under alkaline conditions and is easily hydrolyzed. Solid guanidine is generally used in the form of salts, such as guanidine hydrochloride, guanidine nitrate, guanidine carbonate, guanidine sulfate, and guanidine stearate. Guanidine compounds are widely used in medicine, agriculture, chemical industry and other industries due to their excellent properties such as strong alkalinity, high stability, and good biological activity, and their synthesis methods are also continuously improved and perfected. Aminoguanidine salts are divided into monoaminoguanidine salts, diaminog...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C281/16
Inventor 夏佳美张千峰申克静贾爱铨
Owner ANHUI UNIVERSITY OF TECHNOLOGY
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