CN1594449A

CN1594449A - Process for the preparation of iron blue

Info

Publication number: CN1594449A
Application number: CN 200410012417
Authority: CN
Inventors: 杨柳; 董文娟; 董川
Original assignee: Shanxi University
Current assignee: Shanxi University
Priority date: 2004-07-14
Filing date: 2004-07-14
Publication date: 2005-03-16
Anticipated expiration: 2024-07-14
Also published as: CN1252191C

Abstract

The invention discloses a process for the preparation of iron blue by using ferric nitrate, hexacyanoferrate (II) as raw material, through grinding, water scrubbing, stewing, filtering, abandoning filter liquor, and drying the blue deposition.

Description

Preparation method of iron blue

The technical field is as follows:

the invention relates to a preparation method of an iron compound, and particularly belongs to a preparation method of iron blue.

Background art:

iron blue, also known as prussian blue or hua blue. The iron blue is mainly used for paint, printing ink and paper, can also be used as pigment of crayons, watercolors and oil colors, and is widely applied in the industrial aspect. It is believed that its main component is iron (III) Fe (III) hexacyanoferrate (II)₄[Fe(CN)₆]₃·xH₂And O. The iron in the cation may be partially substituted with an alkali metal or ammonium ion. The industrial production of iron blue is carried out by preparing white slurry of precipitate from ferrous salt and potassium ferrocyanide, and oxidizing the precipitate in acidic medium.

When sodium ferrocyanide is used as a raw material, ammonium sulfate or ammonium chloride is added to produce white slurry, which is then oxidized in an acidic medium. (see "pigment technology" (second edition) Fine chemical industry publishing Co., Ltd. Fujian Wu Shenniang Processations)

The existing industrial production method needs to prepare white slurry and perform acidity adjustment and oxidation procedures, and if the white slurry is not uniform, the acidity is not properly adjusted or the oxidation is not complete, the quality of the product is greatly influenced.

The invention content is as follows:

the invention aims to provide a preparation method of iron blue, which has the advantages of simple production process, less pollution and low cost.

The invention provides a preparation method of iron blue, which takes ferric nitrate and hexacyanoferrate (II) acid salt (such as potassium hexacyanoferrate (II) or sodium hexacyanoferrate (II) and the like) as raw materials and obtains a crude product by grinding; washing with water, standing, filtering, removing filtrate, and drying blue precipitate to obtain the final product; the reaction formula is as follows:

wherein M is K⁺、Na⁺、NH₄ ⁺

The raw material formula (weight percentage) is as follows:

20 to 80 percent of ferric nitrate,

20 to 80 percent of hexacyanoferrate (II) acid salt;

preferably:

40 to 60 percent of ferric nitrate,

40 to 60 percent of hexacyanoferrate (II) acid salt;

compared with the existing industrial method, the method of the invention has the following advantages: 1. the method adopting the solid phase reaction has the biggest characteristics of simple raw materials and no need of acidity adjustment and oxidation procedures, thereby simplifying the production process, shortening the flow, saving the time, improving the production efficiency, saving the energy and greatly reducing the cost. 2. The main raw materials are ferric nitrate and hexacyanoferrate (II) (namely the yellow blood salt), and the price is low. 3. The production process needs less equipment, and the used separation reagent is water, so that the method is clean and environment-friendly.

The implementation mode is as follows:

example 1: weighing 4.04g of ferric nitrate nonahydrate and 4.22g of potassium hexacyanoferrate (II) trihydrate, mixing and grinding uniformly, adding 250ml of distilled water for dissolving, standing for 3 days at room temperature, filtering, discarding filtrate, and drying the obtained precipitate to obtain 2.98g of iron blue, wherein the yield is 96.94%. The process flow comprises the following steps:

example 2: 3.03g of ferric nitrate nonahydrate and 4.22g of potassium hexacyanoferrate trihydrate (II) are weighed, mixed and ground uniformly, then 250ml of distilled water is added for dissolving, the mixture is kept stand for 2 days at room temperature, the filtrate is removed, and the obtained precipitate is dried to obtain 2.34g of iron blue, wherein the yield is 93.31%.

Example 3: weighing 4.04g of ferric nitrate nonahydrate and 3.16g of potassium hexacyanoferrate trihydrate (II), mixing and grinding uniformly, adding 250ml of distilled water for dissolving, standing for 1 day at room temperature, filtering, discarding filtrate, and drying the obtained precipitate to obtain 2.00g of iron blue, wherein the yield is 87.08%.

Example 4: weighing 4.04g of ferric nitrate nonahydrate and 4.84g of sodium hexacyanoferrate (II) decahydrate, mixing and grinding uniformly, adding 250ml of distilled water for dissolving, standing for 2 days at room temperature, filtering, discarding filtrate, and drying the obtained precipitate to obtain 2.76g of iron blue, wherein the yield is 95.12%.

Claims

1. A preparation method of iron blue is characterized in that iron nitrate and hexacyanoferrate (II) are used as raw materials, and crude products are obtained by grinding; washing with water, standing, filtering, removing filtrate, and drying blue precipitate to obtain the final product;

the raw material formula (weight percentage) is as follows:

20 to 80 percent of ferric nitrate,

20 to 80 percent of hexacyanoferrate (II) acid salt.

2. The method according to claim 1, wherein the salt of iron (II) hexacyanide is potassium hexacyanide iron (II), sodium hexacyanide iron (II) or ammonium hexacyanide iron (II).

3. The process for preparing ferric blue according to claim 1, wherein the raw material formula (weight percentage) is preferably:

40 to 60 percent of ferric nitrate,

40 to 60 percent of hexacyanoferrate (II) acid salt.