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Preparation method of guanidinium thiocyanate

A technology of guanidinium thiocyanate and thiocyanate, applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve problems such as high temperature and pressure, high equipment requirements, reduced production efficiency and economy , to achieve the effects of high production efficiency, good product quality and low product cost

Pending Publication Date: 2021-01-12
SUZHOU YACOO SCI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the guanidine carbonate as raw material is generally prepared by guanidine hydrochloride, and this causes the reduction of production efficiency and economy
[0007] As can be seen from the above-mentioned traditional technologies, among the currently known techniques for synthesizing guanidine thiocyanate: the direct synthesis method needs higher temperature and pressure, and requires high equipment; and the method of using carbonate exchange has efficiency and economy. sexual problems

Method used

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Examples

Experimental program
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Effect test

preparation example Construction

[0026] The invention provides a kind of preparation method of guanidinium thiocyanate, comprises following preparation steps:

[0027] Mix guanidine hydrochloride and thiocyanate in a solvent, react at 60°C-75°C for 2.5h-3.5h while stirring, then filter and crystallize to obtain guanidine thiocyanate.

[0028] Wherein, the molar ratio of described guanidine hydrochloride and described thiocyanate is 1:0.8-1.3; This thiocyanate is thiocyanate ion SCN - The resulting salt, in one embodiment, the thiocyanate is but not limited to alkali metal thiocyanate or ammonium thiocyanate; in this embodiment, the alkali metal thiocyanate is sulfur One of sodium cyanate, lithium thiocyanate, and potassium thiocyanate.

[0029] The weight ratio of the solvent to the guanidine hydrochloride is 8-10:9.5-10; the solvent is one or more combinations of water, alcohol solvents, and aprotic organic solvents. The alcoholic solvent is one of methanol, ethanol, and isopropanol; in this embodiment, th...

Embodiment 1

[0040] A kind of preparation method of guanidinium thiocyanate comprises following preparation steps:

[0041] Add 40g of water / 40g of acetone, 95g of guanidine hydrochloride, and 91g of ammonium thiocyanate to the reaction flask in sequence, turn on the stirring, raise the temperature to 70°C, react for 3 hours while stirring, and filter to obtain the reaction solution; add the above reaction solution to pre-cool In a reaction flask, stir overnight, and then filter to obtain a white solid; dissolve the above solid in 180g of water, heat to 50°C, add activated carbon, stir and filter to obtain a filtrate; place the above filtrate in a freezer overnight Afterwards, after filtering and drying, 79 g of guanidine thiocyanate was obtained, and its content was 99.2%.

Embodiment 2

[0043] A kind of preparation method of guanidinium thiocyanate comprises following preparation steps:

[0044] Add 50g of water / 50g of ethanol, 95g of guanidine hydrochloride, 107g of potassium thiocyanate, and 2.5g of diatomaceous earth in the reaction flask in sequence, turn on the stirring, heat up to 75°C, react for 3 hours while stirring, and filter to obtain the reaction solution; The reaction solution was added into a pre-cooled reaction flask, stirred overnight, and then filtered to obtain a white solid; the above solid was dissolved in 136g of water, heated to 50°C, then activated carbon was added, stirred and filtered to obtain a filtrate; After the filtrate was placed in the freezer overnight, it was filtered and dried to obtain 81 g of guanidine thiocyanate, with a content of 99.1%.

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PUM

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Abstract

The invention discloses a guanidinium thiocyanate preparation method, which comprises: mixing guanidine hydrochloride and a thiocyanate in a solvent, carrying out a reaction for 2.5 h to 3.5 h while stirring at a temperature of 60 DEG C to 75 DEG C, and conducting filtering and crystallizing to obtain guanidinium thiocyanate. A salt exchange method is adopted, guanidine hydrochloride is used as araw material to produce guanidinium thiocyanate instead of guanidine carbonate, the reaction process is lower than 80 DEG C, no gas is released in the preparation process, the method is superior to anexisting synthesis method, the preparation process is more controllable and environmentally friendly in the production process, the product cost is lower, the production efficiency is high, and the product quality is good.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of guanidine thiocyanate. Background technique [0002] Guanidine salts are widely used in the production of biomedicine, dyes and resin components. Free guanidine is a crystalline organic base that is as basic as sodium hydroxide. Free guanidine is not stable enough and not easy to store, so it is sold in the form of salt in practical application. Common guanidine salts include: guanidine hydrochloride, guanidine thiocyanate, guanidine carbonate, guanidine phosphate, etc. [0003] In specific applications, guanidinium salts are used as pH regulators for amino resins, antioxidants, resin stabilizers, and additives for washing wool surfactants. Guanidine phosphate is used as a flame retardant for wood, fiber, paper, etc. Guanidine stearate is used as soap filler, and aryl derivatives, such as symmetrical biphenylguanidine, are used as accelerator...

Claims

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Application Information

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IPC IPC(8): C07C279/02C07C277/00C07C277/06
CPCC07C277/00C07C277/06
Inventor 袁永坤曹丽辉
Owner SUZHOU YACOO SCI CO LTD