CN113000006A - Magnesium hydroxide adsorption material, preparation method and application - Google Patents

Magnesium hydroxide adsorption material, preparation method and application Download PDF

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CN113000006A
CN113000006A CN202110256225.3A CN202110256225A CN113000006A CN 113000006 A CN113000006 A CN 113000006A CN 202110256225 A CN202110256225 A CN 202110256225A CN 113000006 A CN113000006 A CN 113000006A
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magnesium hydroxide
citrate
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deionized water
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王雪松
林芳洁
李�录
朱虎
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Fujian Normal University
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    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B01J20/041—Oxides or hydroxides
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    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
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Abstract

The invention provides a magnesium hydroxide adsorption material and a preparation method thereof, wherein the magnesium hydroxide adsorption material is hexagonal phase magnesium hydroxide, and the form of the magnesium hydroxide adsorption material is a coralline porous structure constructed by element nanosheets; the preparation method comprises the following steps: mixing magnesium oxide, citrate and deionized water, uniformly stirring, sealing in a high-pressure reaction kettle, and carrying out hydrothermal reaction to obtain a first suspension; separation and drying: and carrying out solid-liquid separation on the first suspension, and drying the precipitate obtained after separation to obtain the magnesium hydroxide adsorbing material. The magnesium hydroxide adsorption material is synthesized in one step through hydrothermal reaction of citrate, magnesium oxide and deionized water, has high specific surface area, high pore volume and stable surface structure, and can be applied to adsorption of cadmium ions and/or lead ions. The invention has the advantages of low investment, simple and convenient operation, no waste generation, environmental protection and wide application range.

Description

Magnesium hydroxide adsorption material, preparation method and application
Technical Field
The invention relates to the technical field of inorganic functional materials, in particular to a magnesium hydroxide adsorption material, a preparation method and application thereof.
Background
With the development of industry in recent decades, heavy metal pollution of water has become a worldwide environmental problem. Untreated industrial wastewater containing heavy metal ions such As Pb (II), Cd (II), As (V), Ni (II) and the like is discharged to the environment at will, resulting in serious environmental problems. The heavy metal ions are extremely stable, have extremely high toxicity, non-biodegradability and carcinogenicity, and are extremely harmful to human life and ecological systems. Therefore, the removal of heavy metal ions from industrial emissions is essential and urgent and is also required by law.
In the field of environmental remediation, Magnesium Hydroxide (MH) is called a green safe water treatment agent and can be used for neutralization of acid-containing wastewater, decolorization of dye wastewater, adsorption removal of heavy metal wastewater and the like. Generally the sorption effect of MH materials is determined by the large specific surface area, pore volume and surface defects. Although some magnesium oxide products have extremely high specific surface area and pore volume to satisfy the above requirements, the actual adsorption capacity is drastically reduced due to pore clogging caused by hydration in an actually used water environment. Essentially, the adsorption behavior of magnesium oxide is again based primarily on its surface hydration product MH. Therefore, the development of active MH adsorbents with stable structures is currently an effective heavy metal ion removal strategy.
The current synthesis of MH materials is mainly focused on Mg2+Wet precipitation of solutions, sol-gel methods, hydration of magnesium oxide, microemulsion methods, etc. However, most processes inevitably produce harmful by-products and are generally costly and difficult to mass produce. Even so, high specific surface, high pore volume active MH sorbents with good adsorptive properties are still difficult to obtain. Although some nano MH products have higher specific surface area and enough surface defects, the reduction of adsorption capacity caused by agglomeration is still difficult to solve and difficult to be practically applied. Application No.: 201510944007.3 and application No.: 200610041984.3 to U.S. patent applicationMH material with the same structure and a preparation process thereof.
Disclosure of Invention
In order to solve the problem that the adsorption capacity of the existing MH adsorption material is reduced after agglomeration, the inventor provides a magnesium hydroxide adsorption material with high specific surface area, high pore volume and stable structure and a preparation method thereof.
The inventor provides a magnesium hydroxide adsorption material which is hexagonal phase magnesium hydroxide and is in a coral-shaped porous structure constructed by element nanosheets.
The coralline porous structure is formed by self-assembling nanosheets obtained by recrystallization of magnesium hydroxide. The overall size of the coral-like structure is a few microns. (generally within 10 μm)
In the prior art, the nano particles have large specific surface area and high surface energy, so the nano particles tend to agglomerate together to form a whole and reduce the surface energy. If no design intervention is needed, in order to reduce the surface energy most efficiently, the nano particles can select the exposed maximum surface of the nano particles to be in contact stacking, so that a relatively compact aggregation structure is formed, the specific surface area is reduced to the maximum extent, and the surface energy is reduced. At the same time, the pore volume is necessarily lower due to its compact agglomerated structure.
The magnesium hydroxide adsorption material is of a coral-shaped porous structure and is also of a stable structure formed by self-assembly stacking of a magnesium hydroxide product after recrystallization under the action of citrate; compared with the magnesium hydroxide adsorption material in the prior art, the structure has the advantages of large specific surface area, large pore volume and strong adsorption capacity.
Furthermore, the thickness of the elementary nano-sheet of the magnesium hydroxide adsorbing material is 20-40 nm.
Further, the specific surface area of the magnesium hydroxide adsorbing material is 45-170m2Per g, pore volume of 0.4-0.8cm3/g。
The inventor also provides a preparation method of the magnesium hydroxide adsorbing material, which comprises the following steps:
hydrothermal reaction: mixing magnesium oxide, citrate and deionized water, uniformly stirring, sealing in a high-pressure reaction kettle, and carrying out hydrothermal reaction to obtain a first suspension;
separation and drying: and carrying out solid-liquid separation on the first suspension, and drying the precipitate obtained after separation to obtain the magnesium hydroxide adsorbing material.
The inventor finds in the research that: the citrate can control the shape and size of the magnesium hydroxide in the reaction process, the self-assembly behavior of the nano magnesium hydroxide can be controlled according to different concentrations of the citrate, the formation of holes is promoted in the recrystallization process of the magnesium hydroxide, and the nano magnesium hydroxide with different porous structures and forms can be regulated and controlled through the concentration of the citrate.
The citrate can be derived from citric acid and soluble citrate.
In addition, after the solid-liquid separation is carried out on the reacted product, the citrate molecules cannot remain in the magnesium hydroxide adsorption material which is the final product, so the filtrate can be repeatedly and circularly used, no by-product is discharged in the whole process, and the method is simple and economical.
Further, the mass of the citrate is 5% -50% of the mass of the magnesium oxide.
Further, the hydrothermal reaction step comprises hydrothermal reaction at the temperature of 160-200 ℃ for more than 4 h. The hydrothermal temperature has an effect on the morphology and size of the magnesium hydroxide.
Further, the mass ratio of the deionized water to the magnesium oxide is 45: 1.
Further, in the separation and drying step, the precipitate is dried for 12 hours at the temperature of 80 ℃ to obtain the magnesium hydroxide adsorbing material.
The inventor further provides the application of the magnesium hydroxide adsorbing material for adsorbing cadmium ions and/or lead ions.
The inventor also provides the application of the magnesium hydroxide adsorbing material as an adsorbing carrier for preparing a catalyst.
Compared with the prior art, the technical scheme has the advantages that the MH adsorption material is synthesized in one step through hydrothermal reaction of citrate, magnesium oxide and deionized water, has high specific surface area, high pore volume and stable surface structure, and can be applied to adsorption of cadmium ions and/or lead ions. When citrate (5 wt% to 50 wt%), the ratio thereofThe surface area is 45-170m2Per g, pore volume of 0.4-0.8cm3Has high specific surface area and pore volume in the/g range, and the specific surface area and the pore volume can be adjusted by controlling the addition amount of citrate and the hydrothermal temperature. Synthesized MH adsorbing material, Pb thereof2+The adsorption efficiency reaches nearly 100 percent, so that Cd is obtained2+The adsorption efficiency reaches more than 93 percent; in the presence of Na+、Ca2+、K+、Mg2+、Co2+、Ni2+Under the condition of coexisting cations, the adsorption efficiency can still be maintained above 90%. The invention has the advantages of low investment, simple and convenient operation, no waste generation, environmental protection and wide application range.
Drawings
Fig. 1 is an SEM image of the MH product of example 2 without citrate addition.
FIG. 2 is an SEM image of the product at different citrate dosages; wherein the amount of the citrate is a 5 wt%; b 10 wt%; c 15 wt%; d 20 wt%; e 25 wt%; f 30 wt%.
FIG. 3 shows the corresponding XRD of the product in FIG. 2 for different citrate dosages, wherein the citrate content is a 5 wt%; b 10 wt%; c 15 wt%; d 20 wt%; e 25 wt%; f 30 wt%.
FIG. 4 shows a definite adsorption time Pb2+Or Cd2+Removal efficiency map (25 ℃, 1000 mg/L).
FIG. 5 is a graph showing the effect of coexisting cations on adsorption efficiency.
Detailed Description
To explain technical contents, structural features, and objects and effects of the technical solutions in detail, the following detailed description is given with reference to the accompanying drawings in conjunction with the embodiments.
In this embodiment, Xwt% citrate represents Xwt% by weight of magnesium oxide as citrate added during the preparation process.
Example 1 preparation of a Magnesium Hydroxide (MH) adsorbent material,
weighing the following raw materials in parts by weight: 1g of magnesium oxide, 0.2g of citrate and 45ml of deionized water, and the above substances are placed in a hydrothermal kettle and mixed uniformly. Placing the mixture in a blast drying oven, heating to 160 ℃ for hydrothermal reactionAnd 4 h. Taking out the reaction kettle, cooling to room temperature, filtering to obtain a white filter cake, washing, and drying at 80 ℃ for 12h to obtain the coralline porous MH adsorbing material (specific surface area of 159.3381 m)2Per g, pore volume of 0.746610cm3/g)
1. And (4) removing lead ions in the wastewater.
0.1g of MH adsorbing material prepared in the example 1 is weighed at room temperature and placed in a beaker containing 6000mg/L of 500-charge lead wastewater, the adsorption is carried out at the rotating speed of 20 r/min, the supernatant is taken for centrifugation and dilution after the adsorption balance is reached, the concentration of lead ions left after the adsorption is measured by ICP, and the lead adsorbing capacity is calculated to be 4535 mg/g.
2. And (5) removing cadmium ions in the wastewater.
0.1g of MH adsorbing material prepared in the example 1 is weighed at room temperature and placed in a beaker containing 6000mg/L of 500-charge cadmium wastewater, the adsorption is carried out at the rotating speed of 20 r/min, the supernatant is taken for centrifugation and dilution after the adsorption balance is reached, the concentration of the residual cadmium ions after the adsorption is measured by ICP, and the cadmium adsorption capacity is calculated to be 3530 mg/g.
Example 2 (comparative example)
The remaining conditions were unchanged compared to example 1, but no citrate was added. The result was hexagonal plate-like particles of only non-uniform size, see in particular FIG. 1(MH adsorbent material specific surface area 15.8125 m)2Per g, pore volume of 0.103080cm 3/g).
1. And (4) removing lead ions in the wastewater.
0.1g of MH adsorbing material in example 2 is weighed at room temperature and placed in a beaker containing 1000mg/L lead wastewater, the MH adsorbing material is adsorbed at the rotating speed of 20 r/min, supernatant is taken for centrifugation and dilution after the adsorption balance is achieved, the concentration of lead ions after the adsorption is measured by ICP, and the lead adsorbing capacity is calculated to be 917 mg/g.
2. And (5) removing cadmium ions in the wastewater.
0.1g of MH adsorbing material in the embodiment 2 is weighed at room temperature and placed in a beaker containing 1000mg/L of cadmium wastewater, the adsorption is carried out at the rotating speed of 20 r/min, the supernatant is taken for centrifugation and dilution after the adsorption balance is reached, the concentration of cadmium ions after the adsorption is measured by ICP, and the cadmium adsorption capacity is 176mg/g through calculation.
Figure BDA0002967358580000051
Figure BDA0002967358580000061
Example 3: (5 wt% citrate)
Compared with the embodiment 1, the process parameters are as follows: magnesium oxide 1g, citrate 0.05g, deionized water 45ml, hydrothermal temperature 180 DEG C
The final product was coralline porous magnesium hydroxide (specific surface area 47.5166 m)2Per g, pore volume of 0.412276cm3/g)
Example 4: (5 wt% citrate)
The technological parameters are as follows: magnesium oxide 1g, citrate 0.05g, deionized water 45ml, hydrothermal temperature 200 ℃ and coral-shaped porous MH product (specific surface area 48.3228 m)2Per g, pore volume of 0.42786cm3/g)
Example 5: (5 wt% citrate)
The technological parameters are as follows: magnesium oxide 1g, citrate 0.05g, deionized water 45ml, hydrothermal temperature 160 ℃ and obtaining coral porous MH product (specific surface area 45.5198 m)2Per g, pore volume of 0.396676cm3/g)
Example 6: (10 wt% citrate)
The technological parameters are as follows: magnesium oxide 1g, citrate 0.1g, deionized water 45ml, hydrothermal temperature 180 ℃ to finally obtain coralline porous MH adsorbing material (specific surface area 74.0877 m)2Per g, pore volume of 0.581121cm3/g)
Example 7: (10 wt% citrate)
The technological parameters are as follows: magnesium oxide 1g, citrate 0.1g, deionized water 45ml, hydrothermal temperature 200 ℃ and coral-shaped porous MH product (specific surface area 76.3500 m)2Per g, pore volume of 0.603726cm3/g)
Example 8: (10 wt% citrate)
The technological parameters are as follows: magnesium oxide 1g, citrate 0.1g, deionized water 45ml, hydrothermal temperature 160 ℃ to finally obtain coralline porous MH product (specific surface area 73.0800 m)2Per g, pore volume of 0.577126cm3/g)
Example 9: (15 wt% citrate)
The technological parameters are as follows: magnesium oxide 1g, citrate 0.15g, deionized water 45ml, hydrothermal temperature 200 ℃ and finally obtaining coral porous MH adsorbing material (specific surface area 136.8818 m)2Per g, pore volume of 0.724537cm3/g)
Example 10: (15 wt% citrate)
The technological parameters are as follows: magnesium oxide 1g, citrate 0.15g, deionized water 45ml, hydrothermal temperature 180 ℃ to finally obtain coralline porous MH product (specific surface area 125.1238 m)2Per g, pore volume of 0.704482cm3/g)
Example 11: (15 wt% citrate)
The technological parameters are as follows: magnesium oxide 1g, citrate 0.15g, deionized water 45ml, hydrothermal temperature 160 ℃ to finally obtain coralline porous MH adsorbing material (specific surface area 112.2178 m)2Per g, pore volume of 0.651182cm3/g)
Example 12: (20 wt% citrate)
The technological parameters are as follows: magnesium oxide 1g, citrate 0.2g, deionized water 45ml, hydrothermal temperature 200 ℃ and coral-shaped porous MH product (specific surface area 169 m)2Per g, pore volume of 0.793223cm3/g)
Example 13: (20 wt% citrate)
The technological parameters are as follows: magnesium oxide 1g, citrate 0.2g, deionized water 45ml, hydrothermal temperature 180 ℃ to finally obtain coralline porous MH adsorbing material (specific surface area 163.8446 m)2Per g, pore volume of 0.764223cm3/g)
Example 14: (25 wt% citrate)
The technological parameters are as follows: magnesium oxide 1g, citrate 0.25g, deionized water 45ml, hydrothermal temperature 160 ℃ and finally obtaining coral porous MH adsorbing material (specific surface area 142.3248 m)2Per g, pore volume of 0.734267cm3/g)
Example 15: (25 wt% citrate)
The technological parameters are as follows: magnesium oxide 1g, citrate 0.25g, deionized water 45ml, hydrothermal temperature 180 ℃ to finally obtain coralline porous MH product (specific surface area 145.1231 m)2Per g, pore volume of 0.743325cm3/g)
Example 16: (25 wt% citrate)
The technological parameters are as follows: magnesium oxide 1g, citrate 0.25g, deionized water 45ml, hydrothermal temperature 200 ℃ and finally obtaining coral-shaped porous MH adsorption material (specific surface area 146.2256 m)2Per g, pore volume of 0.748952cm3/g)
Example 17: (30 wt% citrate)
The technological parameters are as follows: magnesium oxide 1g, citrate 0.3g, deionized water 45ml, hydrothermal temperature 160 ℃ and obtaining coral porous MH product (specific surface area 134.8248 m)2Per g, pore volume of 0.693644cm3/g)
Example 18: (30 wt% citrate)
The technological parameters are as follows: magnesium oxide 1g, citrate 0.3g, deionized water 45ml, hydrothermal temperature 180 ℃ to finally obtain coralline porous MH product (specific surface area 137.1256 m)2Per g, pore volume of 0.705236cm3/g)
Example 19: (30 wt% citrate)
The technological parameters are as follows: magnesium oxide 1g, citrate 0.3g, deionized water 45ml, hydrothermal temperature 200 ℃ and finally obtaining coral-shaped porous MH adsorption material (specific surface area 139.5568 m)2Per g, pore volume of 0.717532cm3/g)
Example 20: (40 wt% citrate)
The technological parameters are as follows: magnesium oxide 1g, citrate 0.4g, deionized water 45ml, hydrothermal temperature 160 ℃ to finally obtain coralline porous MH adsorbing material (specific surface area 121.1314 m)2Per g, pore volume of 0.607056cm3/g)
Example 21: (50 wt% citrate)
The technological parameters are as follows: magnesium oxide 1g, citrate 0.5g, deionized water 45ml, hydrothermal temperature 160 ℃ to finally obtain coralline porous MH adsorbing material (specific surface area 109.7073 m)2Per g, pore volume of 0.539270cm3/g)
From the above example data, it can be seen that when the amount of citrate is 20 wt%, the specific surface area and pore volume of the obtained MH adsorbent material product are the largest. The higher the hydrothermal temperature is, the maximum specific surface area and pore volume of the obtained MH adsorbing material product is obtained. When the addition amount of the citrate (5 wt% -50 wt%) is different, the specific surface area is 45-170m2Per g, pore volume of 0.4-0.8cm3Controllable in the range of/g.
Taking the hydrothermal temperature of 160 ℃ as an example, the corresponding specific surface area and pore structure parameters are shown in table 1, and the final product of the MH adsorbing material is shown in figure 2, wherein the thickness of the coral thin slices is 20-40nm, and the dimension of the whole plane is measured in micron order (1-10 um). The corresponding XRD is shown in figure 3, and from figure 3, the product is assigned to the hexagonal magnesium hydroxide (JCPDS 44-1482), and no impurity peak of citrate appears, which indicates that the product is pure magnesium hydroxide.
TABLE 1 ratio table and pore parameter statistical table of MH adsorption material
Figure BDA0002967358580000111
MH (20 wt%) vs. Pb as prepared in example 12+And Cd2+Has excellent adsorption removal capability, as shown in FIG. 4, and can remove Pb within 60min2+The adsorption efficiency reaches nearly 100 percent, so that Cd is obtained2+The adsorption efficiency reaches more than 93 percent. Meanwhile, the anti-interference performance is strong, as shown in figure 5, the anti-interference performance is shown in the presence of Na+、Ca2+、K+、Mg2+、Co2+、Ni2+Under the condition of coexisting cations, the adsorption efficiency can still be maintained above 90 percent,
it is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or terminal that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or terminal. Without further limitation, an element defined by the phrases "comprising … …" or "comprising … …" does not exclude the presence of additional elements in a process, method, article, or terminal that comprises the element. Further, herein, "greater than," "less than," "more than," and the like are understood to exclude the present numbers; the terms "above", "below", "within" and the like are to be understood as including the number.
It should be noted that, although the above embodiments have been described herein, the invention is not limited thereto. Therefore, based on the innovative concepts of the present invention, the technical solutions of the present invention can be directly or indirectly applied to other related technical fields by making changes and modifications to the embodiments described herein, or by using equivalent structures or equivalent processes performed in the content of the present specification and the attached drawings, which are included in the scope of the present invention.

Claims (10)

1. The magnesium hydroxide adsorbing material is characterized by being hexagonal-phase magnesium hydroxide, and the form of the magnesium hydroxide adsorbing material is a coral-shaped porous structure constructed by element nanosheets.
2. The magnesium hydroxide adsorbent material according to claim 1, wherein the magnesium hydroxide adsorbent material has elementary nanosheets having a thickness of 20-40 nm.
3. The magnesium hydroxide adsorbent material according to claim 1, wherein the magnesium hydroxide adsorbent material has a specific surface area of 45 to 170m2Per g, pore volume of 0.4-0.8cm3/g。
4. A method for preparing a magnesium hydroxide adsorbent material according to any one of claims 1 to 3, comprising the steps of:
hydrothermal reaction: mixing magnesium oxide, citrate and deionized water, uniformly stirring, sealing in a high-pressure reaction kettle, and carrying out hydrothermal reaction to obtain a first suspension;
separation and drying: and carrying out solid-liquid separation on the first suspension, and drying the precipitate obtained after separation to obtain the magnesium hydroxide adsorbing material.
5. The preparation method according to claim 4, wherein the citrate accounts for 5-50% of the magnesium oxide by mass.
6. The preparation method as claimed in claim 4, wherein the hydrothermal reaction step comprises a hydrothermal reaction at 160-200 ℃ for more than 4 h.
7. The preparation method according to claim 4, wherein the mass ratio of the deionized water to the magnesium oxide is 45: 1.
8. The preparation method according to claim 4, wherein in the separation and drying step, the precipitate is dried at 80 ℃ for 12 hours to obtain the magnesium hydroxide adsorbing material.
9. Use of the magnesium hydroxide adsorbent material according to any one of claims 1 to 3 for adsorbing cadmium ions and/or lead ions.
10. Use of the magnesium hydroxide adsorbent material according to any one of claims 1 to 3 as an adsorbent support for the preparation of a catalyst.
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CN102050472A (en) * 2009-10-28 2011-05-11 中国科学院过程工程研究所 Method for preparing submicron flaky magnesium hydroxide from magnesium oxide
CN104437345A (en) * 2014-11-15 2015-03-25 中国科学院过程工程研究所 Solvent-thermal preparation method of porous ferroferric oxide adsorption material

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