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Process for preparation of iron sulfide

A protective atmosphere and mixture technology, applied in the field of FeS preparation, can solve the problems of expensive raw material processing equipment, high control requirements, and poor process, and achieve the effect of easy production equipment, simple equipment, and low cost

Inactive Publication Date: 2008-11-26
GRIMAT ENG INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the reaction between Fe powder and sulfur is a strongly exothermic reaction, persulfides are easily generated during the reaction or local overheating "sintering" occurs during the reaction, which prevents the further progress of the reaction, resulting in a non-stoichiometric FeS product.
Another method precipitation method is to adopt divalent iron salts such as ferrous sulfate and sulfur ion to generate ferrous sulfide precipitation in aqueous solution, but because moist ferrous sulfide is very easy to oxidize in the air to generate ferric oxide and sulfur, so In this method, the air must be isolated during the sedimentation, filtration and drying process, and the process is not easy to control and has high requirements.
[0004] In addition to the several methods for the synthesis of FeS materials described above, some other special preparation methods have been reported in the literature, such as microemulsion method, homogeneous precipitation method, glow discharge method, etc. Although these methods have high purity FeS products , but the raw materials and processing equipment are relatively expensive, and the production capacity is low, so it will not be mentioned here

Method used

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  • Process for preparation of iron sulfide
  • Process for preparation of iron sulfide

Examples

Experimental program
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Effect test

Embodiment 1

[0026] will analyze pure FeSO 4 ·7H 2 O5.117g is mixed with activated carbon 0.883g evenly, is packed in the quartz glass tube, after vacuumizing, at a pressure of 10 4 Under the protection of Pa nitrogen gas, put the quartz tube into the tubular resistance furnace, raise the temperature to 300°C at a rate of 10°C / min, keep it warm for 30min, and vacuum again, at a pressure of 1.5×10 4 Under the protection of nitrogen in Pa, the temperature was raised to 800°C at a rate of 7°C / min, and the product was naturally cooled after 6 hours of constant temperature to obtain the product. The purity of the product was >98.5%. It was FeS with a single phase space group of P63 / mmc. figure 1 .

Embodiment 2

[0028] According to the same material and steps of the embodiment, the pure FeSO 4 ·7H 2 O5.001g is mixed with graphite 0.862g evenly, and the temperature is 120 ℃, and the vacuum is 133Pa under the condition of vacuum drying for 3 hours, after drying, the material is packed into a quartz glass tube, and after vacuuming, the 4 Under the protection of Pa nitrogen, put the quartz tube into the tubular resistance furnace, raise the temperature to 300°C at a rate of 13°C / min, keep it warm for 30min, and vacuum again, at 2×10 4 Under the protection of nitrogen in Pa, the temperature rises to 800°C at a rate of 8°C / min, the temperature is maintained for 6 hours, and then naturally cooled to obtain the product. The purity is the same as in Example 1. It is FeS with a single phase space group of P63 / mmc, XRD diffraction pattern See figure 2 .

Embodiment 3

[0030] will analyze pure FeSO 4 ·7H 2 Mix O5.000g with 0.723g of activated carbon evenly, put it into a quartz glass tube, and vacuumize it under a pressure of 2×10 4 Under the protection of Pa nitrogen, put the quartz tube into the tubular resistance furnace, raise the temperature to 300°C at a rate of 10°C / min, keep it warm for 40min, and vacuum again, at a pressure of 5×10 4 Under the protection of Pa nitrogen, the temperature was raised to 800° C. at a rate of 7° C. / min, kept at a constant temperature for 6 hours, and then naturally cooled to obtain the product. The purity was the same as in Example 1, and it was FeS with a single phase space group of P63 / mmc.

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Abstract

The invention discloses a method for synthesizing ferrous sulfide material, which adopts green vitriol and carbon powder as raw materials that are evenly mixed and then synthesized by high-temperature solid-phase reaction under the protection of inert gases to obtain the product of the invention. The obtained ferrous sulfide powder by adopting the method of the invention has high purity, single phase, simple preparation conditions and low cost, which can be synthesized in batch.

Description

technical field [0001] The present invention relates to a kind of preparation method of FeS, adopts FeSO 4 ·7H 2 The ferrous sulfide product is obtained by mixing O and C in a sealed container through high-temperature solid phase synthesis, which belongs to the technical field of new material preparation. Background technique [0002] Ferrous sulfide has a phosphorus sheet structure similar to molybdenum disulfide or graphite, with low hardness and a melting point as high as 1100 °C. It is an antiferromagnetic semiconductor material, which is easy to slide along the bottom surface for plastic deformation. It has good plastic deformation ability and good lubricating performance, so it is widely used in industry. It is often used as solid lubricant, electrode and treatment containing Cr ( VI) waste water, etc. In addition, ferrous sulfide is often used as an electrode material in secondary molten salt lithium batteries. With the development of society, FeS will also receiv...

Claims

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Application Information

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IPC IPC(8): C01G49/12
Inventor 夏雯蒋文全傅钟臻于丽敏张文广
Owner GRIMAT ENG INST CO LTD
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