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A kind of preparation method of ammonium ferrocyanide hydrate

A technology of ammonium ferrocyanide and ferrocyanide, which is applied in the direction of ferricyanide and metal cyanide, can solve the problems of difficulty in improving product purity, strong concentrated hydrochloric acid, and complicated synthesis process, so as to improve yield and purity , mild reaction conditions and high reaction yield

Active Publication Date: 2020-02-07
GUANGDONG UNIV OF TECH
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Problems solved by technology

[0004] Although ammonium ferrocyanide has good solubility and can be used in various aspects, due to its complicated synthesis process, it is difficult to improve the purity of the product and lack of a detailed and systematic research system, it is difficult to industrialize, resulting in its high price in the market
For example, the introduction of ferrocyanide ion in the ninth volume of "Inorganic Chemistry Series" edited by Xie Gaoyang et al. is relatively concise. The synthesis of ferrocyanide ion is summarized in one sentence: its potassium salt reacts with hydrogen chloride in ether That is, or the reaction of potassium salt solution and concentrated hydrochloric acid; but the yield and purity of ammonium ferrocyanide obtained by these two methods are not high, because potassium ferrocyanide is insoluble in ether, the reaction is difficult to complete, ether Both concentrated hydrochloric acid and concentrated hydrochloric acid are highly volatile, and concentrated hydrochloric acid is highly corrosive, so this method is dangerous and toxic to a certain extent, and it is difficult to produce on a large scale
For the synthesis of ammonium ferrocyanide, bibliographical reports are even rarer, such as J. Balmaseda et al. in Journal of Physics and Chemistry of Solids 64 (2003) 685-693 report entitled Behavior of Prussian blue-based materials in presence of ammonia In the article, the synthesis of ammonium ferrocyanide is summarized in one sentence: ferrocyanide ion is a solid acid, which can be neutralized with ammonia water to obtain ammonium ferrocyanide; the reaction conditions are not mentioned, so the method is difficult to promote

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  • A kind of preparation method of ammonium ferrocyanide hydrate
  • A kind of preparation method of ammonium ferrocyanide hydrate

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[0023] The invention provides a kind of preparation method of ammonium ferrocyanide hydrate, comprising:

[0024] 1) mixing and reacting a metal salt of ferrocyanide, an aqueous hydrogen chloride solution, and a first solvent to obtain a ferrocyanide ion intermediate;

[0025] Wherein, the first solvent is a mixed solution of ether and water; the volume percentage of ether in the mixed solution of ether and water is 20% to 70%;

[0026] 2) Mixing and reacting the ferrocyanide ion intermediate, ammonia water and the second solvent to obtain ammonium ferrocyanide hydrate.

[0027] According to the present invention, the present invention mixes and reacts a metal salt of ferrocyanide, an aqueous hydrogen chloride solution, and a first solvent to obtain a ferrocyanide ion intermediate; wherein, the metal salt of ferrocyanide is preferably potassium ferrocyanide, One or more of sodium ferrocyanide and calcium ferrocyanide, more preferably potassium ferrocyanide, sodium ferrocyanid...

Embodiment 1

[0032] The synthetic steps of intermediate ferrocyanide ion:

[0033] (1) Weigh the raw material potassium ferrocyanide (126.7 g, 0.3 mol) into a dry 1000 mL double-necked round bottom flask.

[0034] (2) Measure diethyl ether (anhydrous, 100 mL) with a graduated cylinder and add it into a double-necked round bottom flask.

[0035] (3) Measure deionized water (300 mL) with a graduated cylinder and add it into a double-necked round bottom flask.

[0036](4) Stir at room temperature for 10 min, then place in a low temperature reactor, keep the low temperature, slowly add 25% aqueous hydrogen chloride solution (204.4 mL, 1.4 mol), and react at 15°C for 20 min. After the reaction was complete, a large amount of solids were precipitated. After vacuum filtration and washing with water for 3 times, 77 g of a white powdery product (ie intermediate ferrocyanide ion) was obtained, with a yield of 95% and a purity of 98%.

[0037] Synthetic steps of the product:

[0038] (1) The inter...

Embodiment 2

[0044] The synthetic steps of intermediate ferrocyanide ion:

[0045] (1) Weigh the raw material sodium ferrocyanide (179.21 g, 0.5 mol) into a dry 1000 mL double-necked round bottom flask.

[0046] (2) Measure diethyl ether (anhydrous, 150 mL) with a graduated cylinder and add it into a double-necked round bottom flask.

[0047] (3) Measure deionized water (350 mL) with a graduated cylinder and add it into a double-necked round bottom flask.

[0048] (4) Stir at room temperature for 10 min, then place in a low-temperature reactor, keep the low temperature, slowly add 36% aqueous hydrogen chloride solution (243 mL, 2.4 mol), and react at 10° C. for 25 min. After the reaction was complete, a large amount of solids precipitated out, filtered under reduced pressure, and washed with water three times to obtain 129 g of a white powdery product (ie intermediate ferrocyanide ion), with a yield of 96% and a purity of 98%.

[0049] Synthetic steps of the product:

[0050] (1) The in...

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Abstract

The invention provides a preparation method of ammonium ferrocyanide hydrate. Firstly, metal salt of ferrocyanide, a hydrogen chloride water solution and a first solvent are mixed to react, a ferrocyanide ion intermediate is obtained; then the ferrocyanide ion intermediate, ammonium hydroxide and a second solvent are mixed to react, and the ammonium ferrocyanide hydrate is obtained, wherein the first solvent is a mixed solution of diethyl ether and water, and the volume percentage of diethyl ether in the mixed solution of diethyl ether and water is 20%-70%. According to the preparation method of the ferrocyanide ion intermediate, the reaction condition is mild, the reaction yield is high, the purity of the obtained ferrocyanide ions is high, and the yield and the purity of the obtained ammonium ferrocyanide hydrate are both high.

Description

technical field [0001] The invention relates to the technical field of inorganic compound synthesis, in particular to a preparation method of ammonium ferrocyanide hydrate. Background technique [0002] Cyanide is an important gold leaching solvent in the gold industry. Most gold production enterprises use cyanide, and all kinds of cyanides involved in the gold industry are inorganic cyanides. Ferrocyanide in inorganic cyanide is an important raw material for electrode materials, coatings, catalysts, etc. It can be mainly used as a carburizing agent in the iron and steel industry to improve the surface hardness of steel parts; Cotton dyeing is carried out step by step to maintain the dyeing quality. It can be used as a coagulant in the pharmaceutical industry, which can achieve an ideal impurity removal process and improve the quality of medicines. The pigment industry is used as the main raw material for the production of pigment iron blue, and the chemical industry is us...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01C3/12
CPCC01C3/12C01P2002/72C01P2002/82C01P2006/80
Inventor 郑观生蒋银何军黄梦娇张华堂
Owner GUANGDONG UNIV OF TECH