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Process for preparing high purity iron salt

A high-purity, iron salt technology, applied in chemical instruments and methods, iron compounds, inorganic chemistry, etc., can solve problems such as difficult removal, cumbersome procedures, and dangerous reduction steps, and achieve the effect of large-scale industrial production prospects.

Inactive Publication Date: 2011-09-14
北京金方博源科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The previous method is to make high-purity iron by electrolysis to remove various other elements associated with iron, such as nickel, arsenic, cobalt, manganese, etc. The cost is very high and it is not easy to remove these harmful impurities. Very active, easy to form iron oxide
It is more difficult to prepare oxygen-free iron salts such as anhydrous ferric chloride and ferric bromide
CN1231223 discloses a method for preparing high-purity iron powder. The method starts from ore dressing, removes other impurities in iron ore by adding collectors, inhibitors, regulators and highly corrosive hydrofluoric acid, and then Next, solid carbon and hydrogen are used for two-step deoxidation reduction to prepare iron powder with high purity. This method has cumbersome procedures, harsh conditions, and the reduction step is also very dangerous.
Although the iron prepared by this method has high purity, the cost is also high, and it can only be used in the production of special steel, and other heavy metals in it are still above 100ppm, which is difficult to meet the requirements of industries such as pharmaceuticals with a heavy metal content of less than 20ppm

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In a 1000ml reactor, add 200g of ferrocene, control the system pressure at -0.09MPa, heat to 180°C, use a 500ml receiver to receive the sublimated product, and obtain 190g of pure product, which is analyzed by atomic absorption for nickel , manganese, cobalt, arsenic, etc. are all lower than 1ppm.

[0023] In a 5000ml autoclave, add 190g of ferrocene sublimated in the previous step, replace it with high-purity nitrogen three times, fill it with 2.5MPa nitrogen, and then close the system, raise the temperature to 500°C at a speed of 5°C per minute, and After heat preservation for 8 hours, the system pressure can rise to 5.6 MPa at the highest, and after natural cooling, 170 g of black solid product is obtained, wherein iron accounts for 30% and carbon accounts for 70%.

[0024] Add 500ml of 20% dilute sulfuric acid into a 1000ml flask, then add 170g of the above-mentioned Fe / C powder in batches, filter and concentrate the crystals, and dry in vacuum below 50°C to obtain ...

Embodiment 2

[0026] In a 1000ml reactor, add 200g of methylferrocene, heat to 220°C, and use a 500ml receiver to receive the sublimated product to obtain 185g of pure product, which is analyzed by atomic absorption for nickel, manganese, cobalt, arsenic etc. are lower than 1ppm.

[0027] In a 5000ml autoclave, add 185g of methylferrocene sublimated in the previous step, replace it with high-purity nitrogen three times, fill it with 2.5MPa nitrogen, and then close the system, raise the temperature to 500°C at a speed of 5°C per minute, and Keep warm at high temperature for 8 hours, the system pressure can rise to 5.7MPa at the highest, and cool naturally to obtain 165g black solid product, wherein iron accounts for 32% and charcoal accounts for 68%.

[0028] Add 500ml of 20% dilute sulfuric acid into a 1000ml flask, then add 165g of the above-mentioned Fe / C powder in batches, filter and concentrate the crystals, and dry in vacuum below 50°C to obtain 230g of ferrous sulfate heptahydrate wit...

Embodiment 3

[0030] In the reaction tower of 1000ml, add 100g with the Fe / C powder that embodiment 1 method gains, replace 3 times with high-purity nitrogen, be heated to 320 ℃, pass into chlorine to generate the mixture of anhydrous ferric chloride and charcoal powder, the generated Ferric chloride is sublimated at this temperature, and 80g of anhydrous ferric chloride is received, with a content of 99.2%, and the contents of nickel, manganese, cobalt, arsenic, etc. are all less than 5ppm through atomic absorption analysis.

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Abstract

The invention provides a process for preparing high purity molysite. The process comprises that organic iron is utilized as raw material to sublime or distill and purify the organic iron, the organic iron is carbonized into Fe / C powder at certain temperature, relative molysite is generated by the reaction of Fe / C powder with different oxidants, or inorganic salt of iron is generated by reacting the purified organic iron with oxidants directly, and the high purity malysite is obtained by separating and purifying. The process of the invention is a very effective process to prepare high purity molysite, which has relatively large prospect of industrial production.

Description

technical field [0001] The invention relates to a method for preparing high-purity iron salts. The method uses organic iron as a raw material, undergoes sublimation or distillation purification, and then carbonizes to make Fe / C powder, and then reacts with an oxidant to make corresponding iron salts, or directly The purified organic iron is reacted with an oxidizing agent to form an inorganic iron salt, which is then separated and purified to obtain a high-purity iron salt. Background technique [0002] High-purity iron salts are mainly used in pharmaceuticals, reagents, standard substances and other fields. The previous method is to make high-purity iron by electrolysis to remove various other elements associated with iron, such as nickel, arsenic, cobalt, manganese, etc. The cost is very high and it is not easy to remove these harmful impurities. Very active, easy to generate iron oxide. It is more difficult to prepare oxygen-free iron salts such as anhydrous ferric chlo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G49/00
Inventor 王研刘林学
Owner 北京金方博源科技发展有限公司