SILICON-ALUMINUM-IRON COMPOSITE MATERIAL, AND PREPARATION METHOD THEREFOR AND USE THEREOF

Abstract

The present disclosure discloses a silicon-aluminum-iron composite material and a preparation method therefor and use thereof, and belongs to the technical field of wastewater treatment. The silicon-aluminum-iron composite material comprises an inner core and an outer shell wrapping the inner core; the inner core is a silicon-aluminum-based hollow sphere; the outer shell contains iron element; and there are holes on the silicon-aluminum-iron composite material. The silicon-aluminum-iron composite material of the present disclosure improves the specific surface area of the silicon-aluminum-iron composite material through structural adjustment. When it is used to adsorb heavy metal ions, the adsorption sites are correspondingly increased, which finally improves the adsorption capacity for heavy metal ions.

Claims

1. A silicon-aluminum-iron composite material, comprising an inner core and an outer shell wrapping the inner core, wherein, the inner core is a silicon-aluminum-based hollow sphere; the outer shell contains iron element; and holes are distributed on the inner core and the outer shell.

2. The silicon-aluminum-iron composite material according to claim 1, wherein a particle size of the silicon-aluminum-iron composite material is 0.2-0.3 ?m.

3. The silicon-aluminum-iron composite material according to claim 1, wherein a pore volume of the silicon-aluminum-iron composite material is 0.55-0.7 cm.sup.3/g.

4. The silicon-aluminum-iron composite material according to claim 1, wherein a specific surface area of the silicon-aluminum-iron composite material is 40-42.5 m.sup.2/g.

5. A method for preparing the silicon-aluminum-iron composite material according to claim 1, comprising steps of: S1. mixing a silica-alumina powder and an alkaline solution for reaction to obtain a mixture wherein the alkaline solution is a mixed solution of NaOH and Na.sub.2CO.sub.3; and S2. adding iron salt to the mixture obtained in step S1, and reacting under ultraviolet irradiation.

6. The method according to claim 5, wherein in step S1, a concentration of the alkaline solution is 0.5-2 mol/L; optionally, in the alkaline solution, the molar ratio of NaOH to Na.sub.2CO.sub.3 is 2-3:1.

7. The method according to claim 5, wherein in step S1, the mass-volume ratio of the silica-alumina powder to the alkaline solution is 1 g:20-30 mL.

8. The method according to claim 5, wherein the silica-alumina powder is a mixture of aluminum oxide and silicon oxide; optionally, a molar ratio of the silica-alumina powder to the iron salt is 15-30:1.

9. An adsorbent, wherein a raw material for preparing the adsorbent comprises the silicon-aluminum-iron composite material according to claim 1.

10. Use of the adsorbent according to claim 9 in the treatment of heavy metal wastewater.

11. The method according to claim 5, wherein a particle size of the silicon-aluminum-iron composite material is 0.2-0.3 ?m.

12. The method according to claim 5, wherein a pore volume of the silicon-aluminum-iron composite material is 0.55-0.7 cm.sup.3/g.

13. The method according to claim 5, wherein a specific surface area of the silicon-aluminum-iron composite material is 40-42.5 m.sup.2/g.

14. An adsorbent, wherein a raw material for preparing the adsorbent comprises the silicon-aluminum-iron composite material according to claim 2.

15. An adsorbent, wherein a raw material for preparing the adsorbent comprises the silicon-aluminum-iron composite material according to claim 3.

16. An adsorbent, wherein a raw material for preparing the adsorbent comprises the silicon-aluminum-iron composite material according to claim 4.

17. An adsorbent, wherein a raw material for preparing the adsorbent comprises the silicon-aluminum-iron composite material prepared by the method according to claim 5.

18. Use of the adsorbent according to claim 14 in the treatment of heavy metal wastewater.

19. Use of the adsorbent according to claim 15 in the treatment of heavy metal wastewater.

20. Use of the adsorbent according to claim 16 in the treatment of heavy metal wastewater.

Description

BRIEF DESCRIPTION OF DRA WINGS

[0073] The present disclosure will be further illustrated below in conjunction with the accompanying drawings and examples, in which:

[0074] FIG. 1 is a transmission electron microscope image of the silicon-aluminum-iron composite material obtained in Example 1 of the present disclosure.

DETAILED DESCRIPTION

[0075] The concept of the present disclosure and the technical effects produced thereby will be clearly and completely described below in conjunction with the examples, so as to fully understand the purpose, characteristics and effects of the present disclosure. Obviously, the described examples are only a part of the examples of the present disclosure, rather than all the examples. Based on the examples of the present disclosure, other examples obtained by those skilled in the art without creative efforts are all within the scope of protection of the present disclosure.

Example 1

[0076] In this example, a silicon-aluminum-iron composite material was prepared, and the specific process comprised:

[0077] S1. 1 g of silica-alumina powder was added to an alkaline solution and reacted at a rotating speed of 100 rpm for 1 h to obtain a mixture, wherein the silica-alumina powder was a mixture of silicon dioxide and aluminum oxide in a mass ratio of 1:1.2; and the alkaline solution was a mixture of 15 mL of NaOH solution with a concentration of 1 mol/L and 5 mL of Na.sub.2CO.sub.3 solution with a concentration of 1 mol/L; and

[0078] S2. 1 g of Fe(NO.sub.3).sub.3 was added to 100 mL of the mixture obtained in step S1, placed in a water bath and heated to 60? C., and then irradiated with ultraviolet rays for 6 h; after solid-liquid separation, the obtained solid was washed until pH=7 and dried at 60? C. for 12 h to obtain a silicon-aluminum-iron composite material, wherein the wavelength of ultraviolet rays was <400 nm, from a mercury lamp with a power of 1200 w.

[0079] The morphology of the silicon-aluminum-iron composite material obtained in this example was shown in FIG. 1.

Example 2

[0080] In this example, a silicon-aluminum-iron composite material was prepared, and the specific process comprised:

[0081] S1. 1 g of silica-alumina powder (same as Example 1) was added to an alkaline solution and reacted at a rotating speed of 120 rpm for 1.5 h to obtain a mixture, wherein the alkaline solution was a mixture of 15 mL of NaOH solution with a concentration of 1 mol/L and 7 mL of Na.sub.2CO.sub.3 solution with a concentration of 1 mol/L; and

[0082] S2. 1 g of Fe(NO.sub.3).sub.3 was added to 100 mL of the mixture obtained in step S1, placed in a water bath and heated to 70? C., and then irradiated with ultraviolet rays for 7 h; after solid-liquid separation, the obtained solid was washed to a neutral pH value and dried at 70? C. for 15 h to obtain a silicon-aluminum-iron composite material, wherein the wavelength of ultraviolet rays was <400 nm, from a mercury lamp with a power of 800 w.

Example 3

[0083] In this example, a silicon-aluminum-iron composite material was prepared, and the specific process comprised:

[0084] S1. 1 g of silica-alumina powder (same as Example 1) was added to an alkaline solution and reacted at a rotating speed of 160 rpm for 1.5 h to obtain a mixture, wherein the alkaline solution was a mixture of 18 mL of NaOH solution with a concentration of 1 mol/L and 8 mL of Na.sub.2CO.sub.3 solution with a concentration of 1 mol/L; and

[0085] S2. 1 g of Fe(NO.sub.3).sub.3 was added to 100 mL of the mixture obtained in step S1, placed in a water bath and heated to 60? C., and then irradiated with ultraviolet rays for 10 h; after solid-liquid separation, the obtained solid was washed to a neutral pH value and dried at 60? C. for 18 h to obtain a silicon-aluminum-iron composite material, wherein the wavelength of ultraviolet rays was <400 nm, from a mercury lamp with a power of 600 w.

Example 4

[0086] In this example, a silicon-aluminum-iron composite material was prepared, and the specific process comprised:

[0087] S1. 1 g of silica-alumina powder (same as Example 1) was added to an alkaline solution and reacted at a rotating speed of 200 rpm for 2 h to obtain a mixture, wherein the alkaline solution was a mixture of 22 mL of NaOH solution with a concentration of 1 mol/L and 8 mL of Na.sub.2CO.sub.3 solution with a concentration of 1 mol/L; and

[0088] S2. 1 g of Fe(NO.sub.3).sub.3 was added to 100 mL of the mixture obtained in step S1, placed in a water bath and heated to 90? C., and then irradiated with ultraviolet rays for 12 h; after solid-liquid separation, the obtained solid was washed to a neutral pH value and dried at 90? C. for 24 h to obtain a silicon-aluminum-iron composite material, wherein the wavelength of ultraviolet rays was <400 nm, from a mercury lamp with a power of 300 w.

Example 5

[0089] In this example, the silicon-aluminum-iron composite material obtained in Example 1 was used as an adsorbent to carry out the treatment of manganese-containing heavy metal wastewater, and the specific steps were:

[0090] 100 mL of wastewater with a manganese ion concentration of 50 mg/L was added with 2.5 g of the silicon-aluminum-iron composite material obtained in Example 1. Under the conditions of room temperature and atmospheric pressure (25? C., 1 atmosphere), pH 3 and a speed of 120 rpm, the adsorption was performed under stirring for 4 h. After filtration, a purified aqueous solution and a waste adsorbent were obtained.

Example 6

[0091] In this example, the silicon-aluminum-iron composite material obtained in Example 2 was used as an adsorbent to carry out the treatment of manganese-containing heavy metal wastewater, and the specific steps were:

[0092] 100 mL of wastewater with a manganese ion concentration of 60 mg/L was added with 3 g of the silicon-aluminum-iron composite material obtained in Example 2. Under the conditions of room temperature and atmospheric pressure (25? C., 1 atmosphere), pH 5 and a speed of 140 rpm, the adsorption was performed under stirring for 4.5 h. After filtration, a purified aqueous solution and a waste adsorbent were obtained.

Example 7

[0093] In this example, the silicon-aluminum-iron composite material obtained in Example 3 was used as an adsorbent to carry out the treatment of manganese-containing heavy metal wastewater, and the specific steps were:

[0094] 100 mL of wastewater with a manganese ion concentration of 80 mg/L was added with 3.5 g of the silicon-aluminum-iron composite material obtained in Example 3. Under the conditions of room temperature and atmospheric pressure (25? C., 1 atmosphere), pH 6 and a speed of 160 rpm, the adsorption was performed under stirring for 5 h. After filtration, a purified aqueous solution and a waste adsorbent were obtained.

Example 8

[0095] In this example, the silicon-aluminum-iron composite material obtained in Example 4 was used as an adsorbent to carry out the treatment of manganese-containing heavy metal wastewater, and the specific steps were:

[0096] 100 mL of wastewater with a manganese ion concentration of 100 mg/L was added with 4.0 g of the silicon-aluminum-iron composite material obtained in Example 4. Under the conditions of room temperature and atmospheric pressure (25? C., 1 atmosphere), pH 6 and a speed of 180 rpm, the adsorption was performed under stirring for 6 h. After filtration, a purified aqueous solution and a waste adsorbent were obtained.

Example 9

[0097] In this example, the waste adsorbent obtained in Example 5 was used to carry out the treatment of manganese-containing heavy metal wastewater, and the specific steps were:

[0098] 100 mL of wastewater with a manganese ion concentration of 100 mg/L was added with 4.5 g of the waste adsorbent obtained in Example 8. Under the conditions of room temperature and atmospheric pressure (25? C., 1 atmosphere), pH 5 and a speed of 140 rpm, the adsorption was performed under stirring for 4.5 h. After filtration, a purified aqueous solution and a waste adsorbent were obtained.

Comparative Example 1

[0099] In this comparative example, an adsorbent was prepared, and the difference between Comparative Example 1 and Example 4 was:

[0100] In step S2, ultraviolet irradiation was directly performed without adding Fe(NO.sub.3).sub.3.

Comparative Example 2

[0101] In this comparative example, the adsorbent obtained in Comparative Example 1 was used to carry out the treatment of manganese-containing heavy metal wastewater, and the specific difference between Comparative Example 2 and Example 8 was:

[0102] Instead of using the silicon-aluminum-iron composite material obtained in Example 4, the material obtained in Comparative Example 1 was used to prepare the adsorbent.

Test Example

[0103] In this test example, the silicon-aluminum-iron composite materials obtained in Examples 1 to 4 and the adsorbent prepared in Comparative Example 1 were tested for the physical and chemical performances.

[0104] The specific surface area and pore volume were tested by BET.

[0105] The particle size was tested by a Malvern particle size analyzer.

[0106] The adsorption capacity was tested and calculated by (c.sub.o?c.sub.e) v/m; where c.sub.0 represented the initial mass concentration of heavy metals in wastewater containing heavy metals; c.sub.e represented the concentration of heavy metals in wastewater containing heavy metals after adsorption equilibrium; v represented the volume (L) of wastewater containing heavy metals; and m represented the mass (g) of the adsorbent; and the test method for c.sub.0 and c.sub.e was ICP-OES.

[0107] The test results were shown in Table 1.

TABLE-US-00001 TABLE 1 Physical and chemical performances of materials obtained in Examples 1-4 and Comparative Example 1 Specific Particle Pore Adsorption surface size volume capacity Sample area (m.sup.2/g) (?m) (cm.sup.3/g) (mg/g) Example 1 40.3 0.24 0.67 107.2 Example 2 41.7 0.29 0.62 112.3 Example 3 42.1 0.26 0.58 115.4 Example 4 41.2 0.27 0.63 110.6 Comparative 35.1 0.43 0.42 82.5 Example 1

[0108] Table 1 showed that the silicon-aluminum-iron composite material provided by the present disclosure had smaller particle size, larger pore volume and specific surface area, and thus had a higher adsorption capacity than the adsorbent obtained in Comparative Example 1. It was indicated that the addition of iron salt can indeed lead to the formation of silicon-aluminum-iron composite material with a hollow core-shell structure, and this structure can indeed improve the adsorption capacity for manganese.

[0109] In this test example, the adsorption performance of each adsorbent in Examples 5-9 and Comparative Example 2 was also tested. The efficiency of manganese removal was calculated by: (manganese concentration in initial heavy metal wastewater-manganese concentration in aqueous solution after purification)/manganese concentration in initial heavy metal wastewater; and the test method of manganese concentration was ICP-OES. The test results showed that the efficiencies of manganese removal in Examples 5-8 and Comparative Example 2 were 99.72%, 99.91%, 99.99%, 99.95% and 87.5%, respectively. These results demonstrated that the adsorption performance of the silicon-aluminum-iron composite materials obtained in Examples 1-4 of the present disclosure for manganese was obviously better than that of the iron-free adsorbent obtained in Comparative Example 1. In Example 9, the waste adsorbent was used to remove manganese, with an efficiency of manganese removal being 95% and adsorption capacity being 95 mg/g, indicating that the waste adsorbent still had good ability for manganese removal.

[0110] The examples of the present disclosure have been described in detail above in conjunction with the drawings. However, the present disclosure is not limited to the above-mentioned examples, and various modifications can be made without departing from the purpose of the present disclosure within the scope of knowledge possessed by those of ordinary skill in the art. In addition, in the case of no conflict, the examples and the features in the examples of the present disclosure may be combined with each other.