Method for preparing ferriferrous oxide microwave adsorbing material by utilizing copper-iron tailing pyrite cinder

A microwave absorbing material, the technology of ferric tetroxide, which is applied in ferrous oxides, chemical instruments and methods, iron oxide/iron hydroxide and other directions, can solve problems such as environmental pollution, and achieve high purity and strong magnetic properties. , the effect of high complex permittivity

Inactive Publication Date: 2012-10-10
WUHAN INSTITUTE OF TECHNOLOGY
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  • Abstract
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Problems solved by technology

[0004] The problem to be solved by the present invention is to provide a method for preparing iron ferric oxide microwave absorbing material by using the slag of acid production from copper-iron tailings in view of the above-mentioned prior art. The problem of environmental pollution caused by acid slag from copper and iron tailings also provides new raw materials and processes for the production of related iron-based microwave absorbing materials

Method used

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  • Method for preparing ferriferrous oxide microwave adsorbing material by utilizing copper-iron tailing pyrite cinder
  • Method for preparing ferriferrous oxide microwave adsorbing material by utilizing copper-iron tailing pyrite cinder
  • Method for preparing ferriferrous oxide microwave adsorbing material by utilizing copper-iron tailing pyrite cinder

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Experimental program
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Embodiment 1

[0025] Step 1: Mix sulfuric acid with a volume concentration of 75% and acid-making slag from delafossite tailings at a liquid-solid ratio (ml / g) of 1.5:1. After the slag is solidified into gray particles, it is put into a muffle furnace and aged at 300°C for 2 hours. Transfer the matured slag into a three-necked bottle, add an appropriate amount of water (the liquid-solid ratio (ml / g) is 1.65:1), heat in a water bath and maintain 80°C, and stir at a rate of 400r / min. After 2h, filter to obtain crude ferric sulfate solution.

[0026] Step 2: Add water to the crude ferric sulfate solution to dilute to Fe 3+ The concentration is 1.1mol / L. After stirring and heating up to 90°C, add pyrite concentrate according to the ratio of solid-liquid ratio (g / ml) of 1:1.5, adjust the stirring rate to 200r / min, react for about 3 hours, and filter A crude ferrous sulfate solution was obtained.

[0027] Step 3: Add NaOH solution dropwise to the crude ferrous sulfate solution filtrate to adju...

Embodiment 2

[0031] Step 1: Same as Step 1 in Example 1, the aging temperature is adjusted to 180° C., and the aging time is 2.5 hours.

[0032] Step 2: Dilute crude ferric sulfate with water to Fe 3+ The concentration is 1.1mol / L, after stirring and heating up to 90°C, press Fe:Fe 3+ = 1.2:2 molar ratio to add iron filings, adjust the stirring rate to 200r / min, react for about 3h, and filter to obtain crude ferrous sulfate solution.

[0033] Step 3~step 4: with the step 3~step 4 in the embodiment 1, make Fe 3 o 4 magnetic particles.

[0034] image 3 (a), (b) and (c) are the Fe that embodiment 2 makes respectively 3 o 4 Transmission electron microscope (JEM-100CX11 transmission electron microscope of JEOL Ltd.), scanning electron microscope and EDS elemental analysis diagram of magnetic particles (S-4800 cold field emission scanning electron microscope of Hitachi Electronics Co., Ltd.). image 3 (a) clearly shows that Fe 3 o 4 The magnetic particle size is about 200nm, from ima...

Embodiment 3

[0036] Step 1-Step 2: Same as Step 1-Step 2 in Example 1, the aging temperature was adjusted to 110° C., and the aging time was 3 hours to prepare a crude ferrous sulfate solution.

[0037] Step 3: Add sodium hydroxide dropwise to the crude ferrous sulfate solution to adjust the pH value to 5.5, and then add a small amount of polyacrylamide for flocculation and precipitation after filtration. After the precipitation is complete, filter to obtain a pure ferrous sulfate solution.

[0038] Step 4: with the step 4 in the embodiment 1, make Fe 3 o 4 magnetic particles.

[0039] Use the Nanjing University HH-50 hysteresis loop measuring instrument to measure and draw the Fe obtained in embodiment 3 at 300K 3 o 4 The hysteresis loop, such as Figure 4 Shown, the saturation magnetization of ferromagnets (M s ), residual magnetization (M r ) and coercivity (H c ) are 28.1, 3.0emu / g and 241.3Oe, respectively, with strong magnetic properties.

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Abstract

The invention relates to a method for preparing ferriferrous oxide microwave adsorbing material by utilizing copper-iron tailing pyrite cinder, comprising the following steps: the copper-iron tailing pyrite cinder is soaked by curing acid to obtain crude ferric sulphate solution; reduction reaction is carried out to obtain crude ferrous sulphate solution; purification and heating in water bath are carried out, NaOH solution is dropped to maintain reaction, air is blown in, reaction end point is recognized by measuring molar ratio Fe <3+> / Fe <2+>, magnetic adsorptive separation and drying are carried out for obtaining Fe3O4 magnetic particles; the obtained Fe3O4 magnetic particles is evenly stirred with melted ceresin wax, pressing and cooling are carried out for manufacturing the adsorbing material. The method has the beneficial effects that: 1) the iron recovery can reach about 80 percent by effectively extracting from the copper-iron tailing pyrite cinder; 2) the obtained Fe3O4 has high purity without impurities; 3) a new pathway for comprehensively utilizing the cinder is opened up, and a new raw material and a process are provided for the production of relative iron microwave adsorbing materials.

Description

technical field [0001] The invention relates to the field of secondary resource utilization and microwave-absorbing materials, in particular to a method for preparing ferroferric oxide microwave-absorbing materials by using acid-making slag from copper-iron tailings. Background technique [0002] Copper-iron tailings acid production slag is the final industrial waste residue after sulfuric acid is prepared from copper-iron tailings. At present, the annual output of cinder in our country is very large, and its iron content is generally 35-65%, which is a good secondary resource. However, most of it has not been effectively utilized. If the slag is used to recover valuable metals, the required investment is only 1 / 3 to 1 / 2 of the investment required for the construction of an equivalent amount of ore and non-ferrous metal mines, and the production cost is only equivalent to (or even lower than) the average Iron and steel and non-ferrous metallurgy industry, it can be seen tha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K3/00C01G49/08
Inventor 邹正宣爱国吴元欣闫志国何俊袁华杜治平田琦峰金放
Owner WUHAN INSTITUTE OF TECHNOLOGY
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