Novel Method for Extracting Ultra High Purity Alumina from Wastewater

Abstract

An object of the present invention is to provide a novel method for extracting ultra high purity alumina from wastewater. Wastewater is recycled, filtered, concentrated and pretreated in order to mix with alkali solution and extraction agent PX-17, undergoing 2 times of purification, adding control agent SX-1 and high temperature heat treatment to finally obtain ultra high purity nano-alumina particles which purity reaches as 99.999% and particle size reaches as 20-200 nm.

Claims

1. A novel method for extracting ultra high purity nano-alumina from wastewater, characterized in that it comprises the following steps: (1) filter the raw material waste containing aluminum (Al.sup.3+) by Teflon mesh, and concentrate it to maintain aluminum ions (Al.sup.3+) mass fraction of 3%˜18%; Then, the concentrated solution is dropped into the alkaline solution while the alkali mass fraction reaches 10%˜60%. (2) add extraction agent PX-17 into mixed solution and stir, during extraction process, keep the pH value always at 1-9, maintain the temperature at 10° C.˜90° C.; add extraction agent PX-17 in the preliminary extraction for a secondary extraction, the initial dosage is 1˜5 g/L, and stirring time is 30 min˜5 h in the preliminary extraction; the second dosage is 0.1˜3 g/L, and stirring time is 0.5 h˜5 h in the secondary extraction. (3) add the control agent SX-1 into above extract solution and stir, dosage is 0.1˜5 g/L, stir for 1 h˜24 h at 20° C.˜280° C.; and add the alkali solution under the pH value as 1 to 10 to precipitate the aluminum hydroxide; then cooling, filtering and washing with ultra-pure water for 3˜5 times, drying under 80° C.˜120° C. to obtain pure aluminum hydroxide precursor. (4) heat the pure aluminum hydroxide precursor under 600° C.˜1200° C. for 0.5˜4 hours; then obtain the ultra high purity nano alumina by cooling down under a certain temperature. Wherein the waste water in step (1) contains the surface treatment waste liquid of various aluminum, aluminum plate, aluminum wire, aluminum foil, aluminum brick and aluminum alloy.

2. The novel method for extracting ultra high purity nano-alumina from wastewater according to claim 1, characterized in that the alkaline solution in step (1) includes one or more of sodium hydroxide solution, potassium hydroxide solution, carbonate soda solution, potassium carbonate solution, calcium hydroxide solution and aqueous ammonia.

3. The novel method for extracting ultra high purity nano-alumina from wastewater according to claim 1, characterized in that the alkaline solution in step (3) includes one or more of sodium hydroxide solution, potassium hydroxide solution, carbonate soda solution, potassium carbonate solution, calcium hydroxide solution and aqueous ammonia.

4. The novel method, for extracting ultra high purity nano-alumina from wastewater according to claim 1 characterized in that the main components of contraction agent PX-17 in step (2) are giant porous ion exchange resin, macroporous, zeolite molecular sieve, activated carbon, porous carbon fiber, urea, porous alumina, the PX-17 component content is:as follows: giant porous ion exchange resins 18.5%˜22%, macroporous zeolite molecular sieve 10.5%˜14%, activated carbon 3.5%˜7%, porous activated carbon fibers 26.5%˜31%, urea 14%˜17%, and porous alumina 22.5% to 27%.

5. The novel method for extracting ultra high purity nano-alumina from wastewater according to claim 1, characterized in that the main components of contraction agent PX-17 in step (2) are giant porous ion exchange resin, macroporous zeolite molecular sieve, activated carbon, porous carbon fiber, urea, porous alumina, the PX-17 component content is as follows: giant porous ion exchange resins 19.0%˜20%, macroporous zeolite molecular sieve 10.8%˜12.5%, activated carbon 3.8%˜5.5%, porous activated carbon fibers 27%˜28.5%, urea 14.5%˜16%, and porous alumina 23% to 24.5%.

6. The novel method for extracting ultra high purity nano-alumina from wastewater according to claim 1, characterized in that the main components of contraction agent PX-17 in step (2) are giant porous ion exchange resin, macroporous zeolite molecular sieve, activated carbon, porous carbon fiber, urea, porous alumina, the PX-17 component content is as follows: giant porous ion exchange resins 19.5%, macroporous zeolite molecular sieve 11%, activated carbon 4%, porous activated carbon fibers 27.5%, urea 14.8%, and porous alumina 23.9%.

7. The novel method for extracting ultra high purity nano-alumina from wastewater according to claim 1, characterized in that the main components of contraction agent SX-1 in step (3) includes one or more of mixed solution of polyvinyl pyrrolidone, polyethylene glycol-2000, gelatin, polyoxyethylene polyoxypropylene copolymers, Tween, polyvinyl-124, and aluminum hydroxide

8. The novel method, for extracting ultra high purity nano-alumina from, wastewater according to claim 1, characterized in that the ultra high purity nano-alumina in step (4) is taken out and pass through a fast cooling tunnel at a temperature of 0° C.˜4° C. for 15 min˜90 min.

9. The novel method for extracting ultra high purity nano-alumina from wastewater according to claim 1, characterized in that the purity of ultra-high purity nano-alumina is 99.992%˜99.999%.

10. The application of a novel method for extracting ultra high, purity nano-alumina from wastewater according to claim 1 for extracting the ultra-high purity nano alumina from waste water is applied for the retrieving of containing aluminum (Al.sup.3+) acidic wastewater.

Description

BRIEF DESCRIPTION OF THE INVENTION

[0025] FIG. 1 is a flow chat of a novel method for extracting ultra high purity nano-alumina from wastewater of the invention.

[0026] FIG. 2 is a X-ray Diffraction figure for ultra high purity nano-alumina made by example 5 of the invention.

[0027] FIG. 3 is a field emission scanning electron microscopy (FESEM) figure for ultra high purity nano-alumina made by example 5 of the invention.

[0028] FIG. 4 is the trace elements residual analysis (ICP-OES) result for ultra high purity nano-alumina made by example 1 of the invention.

[0029] FIG. 5 is the trace elements residual analysis (ICP-OES) result ultra high purity nano-alumina made by example 2 of the invention.

[0030] FIG. 6 is the trace elements residual analysis (ICP-OES) result for ultra high purity nano-alumina made by example 3 of the invention.

[0031] FIG. 7 is the trace elements residual analysis (ICP-OES) result for ultra high purity nano-alumina made by example 4 of the invention.

[0032] FIG. 8 is the trace elements residual analysis (ICP-OES) result for ultra high purity nano-alumina made by example 5 of the invention.

[0033] The embodiments of the present invention can be better understood by reference to the following examples which are offered by way of illustration. The present invention is not limited to the example given herein.

EXAMPLE 1

[0034] As shown in FIG. 1 and FIG. 4, the novel method for extracting ultra high purity nano-alumina from wastewater of the invention is as follows:

[0035] Step 1, filter the raw material waste containing aluminum (Al.sup.3+) by Teflon mesh, and concentrate it to maintain aluminum ions (Al.sup.3+) mass fraction of 5%; Then, the concentrated solution is dropped into the alkaline solution while the alkali mass fraction reaches 10%.

[0036] Step 2, add extraction agent PX-17 into mixed solution, during extraction process, keep pH value always at 3, maintain the temperature at 30° C.; add extraction agent PX-17 in the preliminary extraction for a secondary extraction, the initial dosage is 1.0 g/L, and stirring time is 0.5 h in the preliminary extraction; the second dosage is 1.2 g/L, and stirring time 0.5 h in the secondary extraction. Wherein the PX-17 component content is as follows: giant porous on exchange resins 18.5% macroporous zeolite molecular sieve 10.5%, activated carbon 5%, porous activated carbon fibers 28%, urea 14%, and porous alumina 24%.

[0037] Step 3, add the control agent SX-1 into extract solution, dosage is 0.3 g/L, at 30° C. and stir for 24 h; and add the alkali solution under the pH value as 2 to precipitate the aluminum hydroxide; then cooling, filtering and washing with ultra-pure water for 3˜5 times, drying under 80° C. to obtain pure aluminum hydroxide precursor.

[0038] Step 4, heat the pure aluminum hydroxide precursor under 600° C. for 0.5 hours; then obtain the ultra high purity nano alumna by cooling down under 4° C.

[0039] Obtain the purity of 99.992% of ultra high purity nano alumina, and the particle size was 200 nm.

Example 2

[0040] As shown in FIG. 1 and FIG. 5, the novel method for extracting ultra high purity nano-alumina from wastewater of the invention is as follows:

[0041] Step 1, filter the raw material waste containing aluminum (Al.sup.3+) by Teflon mesh, and concentrate it to maintain aluminum ions (Al.sup.3+) mass fraction of 8%; Then, the concentrated solution, is dropped into the alkaline solution while the alkali mass fraction reaches 22%.

[0042] Step 2, add extraction agent PX-17 into mixed solution, during extraction process, keep pH value always at 5, maintain the temperature at 45° C.; add extraction agent PX-17 in the preliminary extraction for a secondary extraction, the initial dosage is 1.5 g/L, and stirring time is 1.5 h in the preliminary extraction; the second dosage is 2.4 g/L, and stirring time is 1.5 h in the secondary extraction. Wherein the PX-17 component content is as follows: giant porous ion exchange resins 18.5%, macroporous zeolite molecular sieve 11.5%, activated carbon 4.5%, porous activated carbon fibers 27%, urea 14.5%, and porous alumina 24%.

[0043] Step 3, add the control agent SX-1 into extract solution, dosage is 1.0 g/L, at 90° C. and stir for 18 h; and add the alkali solution under the pH value as 5 to precipitate the aluminum hydroxide; then cooling, filtering and washing with ultra-pure water for 3˜5 times, drying under 90° C. to obtain pure aluminum hydroxide precursor.

[0044] Step 4, heat the pure aluminum hydroxide precursor under 750° C. for 1.5 hours; then obtain the ultra high purity nano alumina by cooling down under 2° C.

[0045] Obtain the purity of 99.995% of ultra high purity nano alumina, and the particle size was 180 nm.

Example 3

[0046] As shown in FIG. 1 and FIG. 6, the novel method for extracting ultra high purity nano-alumina from wastewater of the invention is as follows:

[0047] Step 1, filter the raw material waste containing aluminum (Al.sup.3+) by Teflon mesh, and concentrate it to maintain aluminum ions (Al.sup.3+) mass fraction of 11%; Then, the concentrated solution is dropped into the alkaline solution while the alkali mass fraction reaches 34%.

[0048] Step 2, add extraction agent PX-17 into mixed solution, during extraction process, keep pH value always at 7, maintain the temperature at 60° C.; add extraction agent PX-17 in the preliminary extraction for a secondary extraction, the initial, dosage is 1.0 g/L, and stirring time is 2.5 h in the preliminary extraction; the second dosage is 1.0 g/L, and stirring time is 2.5 h in the secondary extraction. Wherein the PX-17 component content is as follows: giant porous ion exchange resins 20%, macroporous zeolite molecular sieve 11%, activated carbon 4%, porous activated carbon fibers 26.6%, urea 14.4%, and porous alumina 24%.

[0049] Step 3, add the control agent SX-1 into extract solution, dosage is 1.5 g/L, at 158° C. and stir for 12 h; and add the alkali solution under the pH value as 7 to precipitate the aluminum hydroxide; then cooling, filtering and washing with ultra-pure water for 3˜5 times, drying under 100° C. to obtain pure aluminum hydroxide precursor.

[0050] Step 4, heat the pure aluminum hydroxide precursor under 900° C. for 2 hours; then obtain the ultra high purity nano alumina by cooling down under 2° C.

[0051] Obtain the purity of 99.994% of ultra high purity nano alumina, and the particle size was 150 nm.

Example 4

[0052] As shown in FIG. 1 and FIG. 7, the novel method for extracting ultra high purity nano-alumina from wastewater of the invention is as follows:

[0053] Step 1, filter the raw material waste containing aluminum (Al.sup.3+) by Teflon mesh, and concentrate it to maintain aluminum ions (Al.sup.3+) mass fraction of 14%; Then, the concentrated solution is dropped into the alkaline solution while the alkali mass fraction reaches 46%.

[0054] Step 2, add extraction agent PX-17 into mixed solution, during extraction process, keep pH value always at 8, maintain the temperature at 75° C.; add extraction agent PX-17 in the preliminary extraction for a secondary extraction, the initial dosage is 1.5 g/L, and stirring time is 3.5 h in the preliminary extraction; the second dosage is 4.5 g/L, and stirring time is 3.5 h in the secondary extraction. Wherein the PX-17 component content is as follows: giant porous ion exchange resins 18.5%, macroporous zeolite molecular sieve 10.7%, activated carbon 4.3%, porous activated carbon fibers 26.5%, urea 14%, and porous alumina 26%.

[0055] Step 3, add the control agent SX-1 into extract solution, dosage is 1.75 g/L, at 200° C. and stir for 6 h; continue add the alkali solution under the pH value as 8 to precipitate the aluminum hydroxide; then cooling, filtering and washing with ultra-pure water for 3˜5 times, drying under 110° C. to obtain pure aluminum hydroxide precursor.

[0056] Step 4, heat the pure aluminum hydroxide precursor under 1000° C. for 3 hours: then obtain the ultra high purity nano alumina by cooling down under 0° C.

[0057] Obtain the purity of 99.995% of ultra high purity nano alumina, and the particle size was 130 nm.

Example 5

[0058] As shown in FIG. 1 FIG. 2, FIG. 3 and FIG. 8, the novel method for extracting ultra high purity nano-alumina from wastewater of the invention is as follows:

[0059] Step 1, filter the raw material waste containing aluminum (Al.sup.3+) by Teflon mesh, and concentrate it to maintain aluminum ions (Al.sup.3+) mass fraction of 18%; Then, the concentrated solution is dropped into the ammonia solution while the alkali mass fraction reaches 60%.

[0060] Step 2, add extraction agent PX-17 into mixed solution, during extraction process, keep pH value always at 4, maintain the temperature at 90° C.; add extraction agent PX-17 in the preliminary extraction for a secondary extraction, the initial dosage is 2.0 g/L, and stirring time is 1 h in the preliminary extraction; the second dosage is 1.25 g/L, and stirring time is 1 h in the secondary extraction. Wherein the PX-17 component content is as follows: giant porous ion exchange resins 19.5%, macroporous zeolite molecular sieve 11%, activated carbon 4%, porous activated carbon fibers 27.5%, urea 14.8%, and porous alumina 23.2%.

[0061] Step 3, add the control agent SX-1 into extract solution, dosage is 1.8 g/L, at 280° C. and stir for 1 h; continue add the ammonia solution under the pH value as 8 to precipitate the aluminum hydroxide; then cooling, filtering and washing with ultra-pure water for 3˜5 times, drying under 120° C. to obtain pure aluminum hydroxide precursor.

[0062] Step 4, heat the pure aluminum hydroxide precursor under 1200° C. for 2 hours; then obtain the ultra high purity nano alumina by cooling down under 0° C.

[0063] Obtain the purity of 99.999% of ultra high purity nano alumina, and the particle size was 100 nm.