Preparation method of aluminum-vanadium-iron-manganese alloy

Abstract

The application provides a preparation method of an aluminum vanadium ferromanganese alloy and belongs to the field of materials. The method comprises the following steps: sequentially drying and sintering deactivated MnFe2O4 / chitosan composite microspheres to obtain MnFe2O4 powder; mixing the MnFe2O4 powder and vanadium pentoxide powder, and then sequentially performing combustion melting, casting, cooling and crushing to obtain flaky MnFe2VO9; and mixing the flaky MnFe2VO9, aluminum powder and calcium oxide to perform aluminothermic reaction to obtain the aluminum vanadium ferromanganese alloy. The deactivated MnFe2O4 / chitosan composite microspheres are used as raw materials, the water, chitosan and organic dyes in the composite microspheres are removed through drying and calcination, the MnFe2O4 powder and vanadium pentoxide powder are uniformly mixed, the flaky MnFe2VO9 is prepared through a melting method, the flaky MnFe2VO9 is used as raw material, the aluminum powder and calcium oxide are combined to prepare the aluminum vanadium ferromanganese alloy, and resource utilization is realized.

Description

Technical Field

[0001] This invention relates to the field of materials technology, and in particular to a method for preparing an aluminum-vanadium-iron-manganese alloy. Background Technology

[0002] With the rapid development of industry, water pollution has become a particularly prominent problem, especially the pollution of water bodies by organic dyes, such as azo dyes, anthracene dyes, indigo dyes, sulfur dyes, aryl methane fuels, cyanine dyes, phthalocyanine dyes, and hybrid dyes. These organic substances are difficult to degrade and spread rapidly after entering water bodies, seriously affecting the aquatic ecological environment.

[0003] For organic dye pollution in water bodies, magnetic MnFe2O4 / chitosan composite microspheres are often used as adsorbents. Chitosan in MnFe2O4 / chitosan composite microspheres is a microbially degradable natural polysaccharide derivative with good biocompatibility, non-toxicity, and easy degradation. The presence of hydroxyl and amino groups on the chitosan molecular chain makes it easy to chemically modify and endow it with various functions. It has been widely used in the fields of medicine, textiles, and daily chemicals, especially in the field of wastewater treatment, where it can be used as an adsorbent for organic wastewater. While maintaining the excellent adsorption performance of chitosan, MnFe2O4 / chitosan composite microspheres can be magnetically attracted to wastewater using a magnet. After the magnetically attracted MnFe2O4 / chitosan composite microspheres (containing organic dyes) are washed, the organic dye wastewater can be adsorbed 6 to 10 times until the MnFe2O4 / chitosan composite microspheres are poisoned and inactivated.

[0004] The poisoned and inactivated MnFe2O4 / chitosan composite microspheres contain 20-40 wt% organic dyes that cannot be removed by washing. Improper handling of MnFe2O4 / chitosan composite microspheres (containing organic dyes) can easily cause environmental pollution, and there is currently no effective treatment method. Summary of the Invention

[0005] In view of this, the purpose of this invention is to provide a method for preparing an aluminum-vanadium-iron-manganese alloy. This invention uses deactivated MnFe2O4 / chitosan composite microspheres as raw materials to prepare the aluminum-vanadium-iron-manganese alloy, achieving resource recycling.

[0006] To achieve the above-mentioned objectives, the present invention provides the following technical solution:

[0007] This invention provides a method for preparing an aluminum-vanadium-iron-manganese alloy, comprising the following steps:

[0008] The deactivated MnFe2O4 / chitosan composite microspheres were dried and sintered sequentially to obtain MnFe2O4 powder;

[0009] The MnFe2O4 powder and vanadium pentoxide powder were mixed and then subjected to combustion melting, casting, cooling and crushing in sequence to obtain flake MnFe2VO9;

[0010] The flake-shaped MnFe2VO9, aluminum powder, and calcium oxide are mixed and subjected to an aluminothermic reaction to obtain the aluminum-vanadium-iron-manganese alloy. The aluminum-vanadium-iron-manganese alloy comprises the following elements: vanadium: 10-15 wt%, iron: 11-30 wt%, manganese: 14-18 wt%, oxygen <0.06 wt%, nitrogen <0.02 wt%, and the balance aluminum.

[0011] Preferably, the deactivated MnFe2O4 / chitosan composite microspheres have a water content of 10-20 wt% and a MnFe2O4 content of 20-30 wt%.

[0012] Preferably, the sintering temperature is 600–800°C and the time is 1–3 hours.

[0013] Preferably, the sintering is carried out in an air atmosphere with a flow rate of 10-15 L / min.

[0014] Preferably, the sintering also produces exhaust gas, which is treated with a saturated calcium hydroxide solution.

[0015] Preferably, the combustion and melting temperature is 800–1100°C, and the time is 2–4 hours.

[0016] Preferably, the casting and cooling are carried out in a cooling pan, and the flow rate of the casting to the cooling pan is 4 to 8 kg / min.

[0017] Preferably, the diameter of the cooling plate is 2.5 to 3.5 m, the rotation speed is 2 to 5 rpm, the water inlet flow rate is 10 to 30 L / min, and the water inlet temperature is 5 to 15 °C.

[0018] Preferably, the diameter of the sheet-like MnFe2VO9 is less than 3 cm.

[0019] Preferably, the aluminothermic reaction occurs by igniting a magnesium strip.

[0020] This invention provides a method for preparing an aluminum-vanadium-iron-manganese alloy, comprising the following steps: drying and sintering deactivated MnFe2O4 / chitosan composite microspheres sequentially to obtain MnFe2O4 powder; mixing the MnFe2O4 powder and vanadium pentoxide powder and then sequentially subjecting them to combustion melting, casting, cooling and crushing to obtain flake-shaped MnFe2VO9; and mixing the flake-shaped MnFe2VO9, aluminum powder and calcium oxide to undergo an aluminothermic reaction to obtain the aluminum-vanadium-iron-manganese alloy, wherein the aluminum-vanadium-iron-manganese alloy comprises the following elements: vanadium: 10-15 wt%, iron: 11-30 wt%, manganese: 14-18 wt%, oxygen <0.06 wt%, nitrogen <0.02 wt%, and the balance aluminum.

[0021] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0022] This invention uses deactivated MnFe2O4 / chitosan composite microspheres as raw materials. By drying and calcining, the moisture, chitosan, organic dyes and other components are removed. MnFe2O4 powder and vanadium pentoxide powder are then mixed and prepared into flake MnFe2VO9 by melting. Using flake MnFe2VO9 as raw material, combined with aluminum powder and calcium oxide, an aluminum-vanadium-manganese-iron alloy is prepared, realizing the recycling of resources.

[0023] Furthermore, the preparation method provided by this invention can produce aluminum-vanadium-iron-manganese alloys with uniform composition, solving the problem of uneven alloy composition produced by the aluminothermic method. Detailed Implementation

[0024] This invention provides a method for preparing an aluminum-vanadium-iron-manganese alloy, comprising the following steps:

[0025] The deactivated MnFe2O4 / chitosan composite microspheres were dried and sintered sequentially to obtain MnFe2O4 powder;

[0026] The MnFe2O4 powder and vanadium pentoxide powder were mixed and then subjected to combustion melting, casting, cooling and crushing in sequence to obtain flake MnFe2VO9;

[0027] The flake-shaped MnFe2VO9, aluminum powder, and calcium oxide are mixed and subjected to an aluminothermic reaction to obtain the aluminum-vanadium-iron-manganese alloy. The aluminum-vanadium-iron-manganese alloy comprises the following elements: vanadium: 10-15 wt%, iron: 11-30 wt%, manganese: 14-18 wt%, oxygen <0.06 wt%, nitrogen <0.02 wt%, and the balance aluminum.

[0028] In this invention, deactivated MnFe2O4 / chitosan composite microspheres are dried and sintered sequentially to obtain MnFe2O4 powder.

[0029] In this invention, the deactivated MnFe2O4 / chitosan composite microspheres preferably contain organic dyes. This invention does not have a special limitation on the source of the deactivated MnFe2O4 / chitosan composite microspheres, and sources well known to those skilled in the art can be used, such as deactivated MnFe2O4 / chitosan composite microspheres after treating water bodies with organic dyes.

[0030] In this invention, the water content of the deactivated MnFe2O4 / chitosan composite microspheres is preferably 10-20 wt%, and the MnFe2O4 content is preferably 20-30 wt%.

[0031] In this invention, the drying temperature is preferably 70-90°C, more preferably 80-85°C, and the drying time is preferably 10 hours or more, more preferably 12 hours. The drying is preferably carried out in a drying oven. The purpose of the drying is to remove moisture and prevent agglomeration during the sintering process, which would prevent the MnFe2O4 and vanadium pentoxide powders from being mixed evenly.

[0032] In this invention, the sintering temperature is preferably 600-800℃, more preferably 700-750℃, and the sintering time is preferably 1-3h, more preferably 1.5-2h. The purpose of sintering is to burn the chitosan and organic dye in the MnFe2O4 / chitosan composite microspheres (containing organic dyes) at high temperature.

[0033] In this invention, the sintering is preferably carried out in an air atmosphere, providing oxygen, and the air flow rate is preferably 10-15 L / min, more preferably 12 L / min, to carry away the nitrogen oxides and sulfur oxides gases generated by combustion.

[0034] In this invention, the sintering is preferably carried out in a tube furnace.

[0035] In this invention, the sintering preferably also produces exhaust gas, which is preferably treated with a saturated calcium hydroxide solution.

[0036] After obtaining MnFe2O4 powder, the present invention mixes the MnFe2O4 powder and vanadium pentoxide powder and then sequentially performs combustion melting, casting, cooling and crushing to obtain flake MnFe2VO9.

[0037] In this invention, the preferred mass ratio of MnFe2O4 powder to vanadium pentoxide powder is 1.27:1, and the flake-shaped MnFe2VO9 is prepared according to the chemical mass ratio.

[0038] In this invention, the mixing is preferably carried out in a mixer, the mixing time is preferably 10-20 min, more preferably 12-15 min, and the speed of the mixer is preferably 15-30 rpm, more preferably 20-22 rpm, so as to fully mix the two powders.

[0039] In this invention, the combustion melting temperature is preferably 800-1100℃, more preferably 900-1050℃, and the time is preferably 2-4h, more preferably 2.5-3h. The purpose of the combustion melting is to melt the MnFe2O4 powder and vanadium pentoxide powder at high temperature, grow them in situ into MnFe2VO9, improve the uniformity of the aluminum-vanadium-iron-manganese alloy, and further burn off the unreacted organic matter in the MnFe2O4 powder to purify MnFe2O4.

[0040] In this invention, the casting and cooling are preferably carried out in a cooling pan, and the flow rate of the casting to the cooling pan is preferably 4 to 8 kg / min, more preferably 5 to 7 kg / min, and most preferably 6 kg / min, to prevent the flow rate from being too fast and causing the sheet-like MnFe2VO9 to be too thick, which would affect the aluminothermic reaction rate.

[0041] In this invention, the diameter of the cooling plate is preferably 2.5-3.5 m, more preferably 2.8-3 m, the rotation speed is preferably 2-5 rpm, more preferably 3-3.5 rpm, the water inlet flow rate is preferably 10-30 L / min, more preferably 18-20 L / min, and the water inlet temperature is preferably 5-15℃, more preferably 10-12℃. This prevents the flake-like MnFe2VO9 from becoming too thick while achieving rapid cooling of the molten flake-like MnFe2VO9. The parameters of the cooling plate are preferably such that the rapid cooling is guaranteed to reduce the temperature from 800-1100℃ to below 80℃ within 30 seconds, thereby reducing the crystallinity of the flake-like MnFe2VO9 and increasing the aluminothermic reaction rate.

[0042] In this invention, the diameter of the flake-shaped MnFe2VO9 is preferably less than 3 cm to prevent the diameter of the flake-shaped MnFe2VO9 from being too large, which would affect the uniformity of the mixing process of the flake-shaped MnFe2VO9, aluminum powder, and calcium oxide.

[0043] After obtaining flake-shaped MnFe2VO9, the present invention mixes the flake-shaped MnFe2VO9, aluminum powder and calcium oxide and performs an aluminothermic reaction to obtain the aluminum-vanadium-iron-manganese alloy. The aluminum-vanadium-iron-manganese alloy comprises the following elements: vanadium: 10-15 wt%, iron: 11-30 wt%, manganese: 14-18 wt%, oxygen <0.06 wt%, nitrogen <0.02 wt%, and the balance aluminum.

[0044] In this invention, the preferred weight ratio of the flake MnFe2VO9, aluminum powder, and calcium oxide is (16-24):(20-23):(2-3). The calcium oxide acts as a slag-forming agent in the aluminothermic reaction. Due to its low density, it will not enter the alloy system and forms an alumina-calcium oxide binary slag system with the reduction product alumina, thereby reducing the viscosity of alumina and effectively separating the alumina from the outside of the alloy.

[0045] In this invention, the mixing is preferably carried out in a mixer for 3 to 5 minutes, more preferably for 4.5 minutes.

[0046] In this invention, the aluminothermic reaction is preferably initiated by igniting a magnesium strip.

[0047] To further illustrate the present invention, the preparation method of the aluminum-vanadium-iron-manganese alloy provided by the present invention will be described in detail below with reference to examples, but these should not be construed as limiting the scope of protection of the present invention.

[0048] Example 1

[0049] A method for preparing an aluminum-vanadium-iron-manganese alloy includes the following steps:

[0050] 190 kg of deactivated MnFe2O4 / chitosan composite microspheres (containing organic dyes) were dried in a forced-air drying oven at 80 °C for 12 h to obtain 164 kg of dried MnFe2O4 / chitosan composite microspheres (containing organic dyes). This material was transferred to a tube furnace and held at 750 °C for 1.5 h with air introduced at a flow rate of 12 L / min. After sintering, 45.9 kg of MnFe2O4 powder was obtained. The MnFe2O4 powder and 36... 16 kg of vanadium pentoxide powder was mixed in a mixer at 20 rpm for 15 min. The mixture was then transferred to a combustion kiln and melted at 900 °C for 2.5 h. After complete melting, the molten mixture was poured onto a cooling pan with a diameter of 2.8 m at a rotation speed of 3 rpm, a solution flow rate of 5 kg / min, a water inlet flow rate of 20 L / min, and an inlet water temperature of 12 °C. After cooling, the mixture was crushed by a crusher to obtain 82 kg of flake MnFe2VO9.

[0051] 82 kg of flake MnFe2VO9, 68.9 kg of aluminum powder, and 10.3 kg of calcium oxide were mixed in a mixer for 4.5 minutes, then loaded into a furnace and compacted. The furnace charge was ignited with magnesium strips to induce an aluminothermic reaction. After cooling, 89.8 kg of aluminum-vanadium-manganese-iron alloy was obtained.

[0052] The tested content is as follows:

[0053] Vanadium: 12.9 wt%, Iron: 27.8 wt%, Manganese: 13.7 wt%, Oxygen: 0.032 wt%, Nitrogen <0.015 wt%, the remainder being aluminum and unavoidable impurities.

[0054] Example 2

[0055] 180 kg of deactivated MnFe2O4 / chitosan composite microspheres (containing organic dyes) were dried in a forced-air drying oven at 85°C for 10 h to obtain 153 kg of dried MnFe2O4 / chitosan composite microspheres (containing organic dyes). This material was transferred to a tube furnace and held at 800°C for 1.5 h with air introduced at a flow rate of 15 L / min. After sintering, 39.6 kg of MnFe2O4 powder was obtained. The MnFe2O4 powder, 3... 1.2 kg of vanadium pentoxide powder was mixed in a mixer at 22 rpm for 12 min. The mixture was then transferred to a combustion kiln and melted at 1050℃ for 2 h. After complete melting, the molten mixture was poured onto a cooling pan with a diameter of 3 m at a rotation speed of 3 rpm, a melt flow rate of 8 kg / min, a water inlet flow rate of 18 L / min, and an inlet water temperature of 10℃. After cooling, the mixture was crushed by a crusher to obtain 70.2 kg of flake MnFe2VO9.

[0056] 70.2 kg of flake MnFe2VO9, 59 kg of aluminum powder, and 8.9 kg of calcium oxide were mixed in a mixer for 4.5 min, then loaded into a furnace and compacted. The furnace charge was ignited with magnesium strips to induce an aluminothermic reaction. After cooling, 68 kg of aluminum-vanadium-manganese-iron alloy was obtained.

[0057] The tested content is as follows:

[0058] Vanadium: 13.4 wt%, Iron: 29.5 wt%, Manganese: 13.5 wt%, Oxygen: 0.022 wt%, Nitrogen <0.011 wt%, the remainder being aluminum and unavoidable impurities.

[0059] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. It should be noted that those skilled in the art can make various improvements and modifications without departing from the principles of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. A method for producing an aluminum ferrovanadium manganese alloy, characterized by, The method comprises the following steps: drying and sintering the inactivated MnFe2O4 / chitosan composite microspheres in sequence to obtain MnFe2O4 powder; mixing the MnFe2O4 powder and vanadium pentoxide powder, and then performing combustion melting, casting, cooling and crushing in sequence to obtain flaky MnFe2VO9; mixing the flaky MnFe2VO9, aluminum powder and calcium oxide to perform aluminothermic reaction to obtain the aluminum vanadium ferromanganese alloy, the aluminum vanadium ferromanganese alloy comprises the following contents of elements: vanadium 10-15wt%, iron 11-30wt%, manganese 14-18wt%, oxygen <0.06wt%, nitrogen <0.02wt% and the balance of aluminum.

2. The production method according to claim 1, characterized by, The water content of the inactivated MnFe2O4 / chitosan composite microspheres is 10-20wt%, and the content of MnFe2O4 is 20-30wt%.

3. The production method according to claim 1, characterized by, The sintering temperature is 600-800℃, and the time is 1-3h.

4. The production method according to claim 1 or 3, characterized by, The sintering is performed in an air atmosphere, and the flow rate of the air is 10-15L / min.

5. The production method according to claim 1 or 3, characterized by, The sintering also obtains tail gas, and the tail gas is treated by saturated calcium hydroxide solution.

6. The method of claim 1, wherein, The combustion melting temperature is 800-1100℃, and the time is 2-4h.

7. The preparation method according to claim 1, characterized in that, The casting and cooling are performed in a cooling disc, and the flow rate of the casting into the cooling disc is 4-8kg / min.

8. The method of claim 7, wherein, The diameter of the cooling disc is 2.5-3.5m, the rotating speed is 2-5rpm, the water inlet amount is 10-30L / min, and the water inlet temperature is 5-15℃.

9. The method of claim 1, wherein, The diameter of the flaky MnFe2VO9 is less than 3cm.

10. The method of claim 1, wherein, The aluminothermic reaction is ignited by a magnesium strip.