CN112044392A - Preparation method of magnesium modified nano silicon dioxide hollow sphere - Google Patents

Preparation method of magnesium modified nano silicon dioxide hollow sphere Download PDF

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CN112044392A
CN112044392A CN201910489244.3A CN201910489244A CN112044392A CN 112044392 A CN112044392 A CN 112044392A CN 201910489244 A CN201910489244 A CN 201910489244A CN 112044392 A CN112044392 A CN 112044392A
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magnesium
modified nano
silicon dioxide
hollow spheres
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赵文丽
孙姣
吉庆敏
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Nanjing University of Science and Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • 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
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28016—Particle form
    • B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • B01J20/28064—Surface area, e.g. B.E.T specific surface area being in the range 500-1000 m2/g
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds

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  • Organic Chemistry (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

The invention discloses a preparation method of a magnesium modified nano silicon dioxide hollow sphere. The method is carried out according to solid SiO2The molar ratio of the magnesium salt to the magnesium salt is 5-50: 1, in solid SiO2And adding magnesium salt into the suspension of the nano particles, uniformly dispersing by using ultrasonic waves, adding sodium borohydride, and carrying out hydrothermal reaction at 80-180 ℃ to obtain the magnesium modified nano silicon dioxide hollow spheres. The method is simple and controllable, the synthesis temperature is low, the prepared magnesium modified nano silicon dioxide hollow spheres are prepared by dissolving solid silicon oxide spheres in the presence of sodium borohydride to regenerate magnesium-containing silicon oxide hollow spheres, the magnesium modified nano silicon dioxide hollow spheres consist of magnesium silicate and regenerated silicon oxide, and the hollow spheres have high specific surface area and pore volume and can be used as an adsorbent applied to organic pollutantsAnd (4) processing.

Description

Preparation method of magnesium modified nano silicon dioxide hollow sphere
Technical Field
The invention relates to a preparation method of a magnesium modified nano silicon dioxide hollow sphere, belonging to the technical field of preparation of adsorption materials.
Background
Due to the unique structural characteristics of the hollow nano structure, the hollow nano structure is widely applied to the fields of catalysis, biological medicine, environmental treatment, energy storage and the like. Wherein, the hollow silica spheres have good mechanical property and thermal stabilityThe performance, porous silica hollow materials have been used in a variety of fields such as adsorption, drug delivery and catalysis. Successful application of the above relies to a large extent on the modification of the functional species of the hollow sphere, especially the composition of metal or metal oxide nanoparticles. The silicon-based material of the metal composite has the unique physical and chemical characteristics of the composite material. The hydrothermal method is one of the common methods for preparing the metal composite silicon oxide hollow sphere material. However, although this method is simple and easy to operate, there are some problems that are inevitable. For example, the temperature of the hollow spheres of the magnesium modified nano-silica prepared by the current hydrothermal synthesis is higher than 120 ℃, as reported in the literatures (Journal of Materials Chemistry B,2016,4(19):3257-3268 and Dalton Transactions,2013,42(24):8918-8925), even the temperature reaches 190 ℃ (chem. Asian J.2010,5, 1439-1444). In addition, the specific surface area of the synthesized magnesium modified nano-silica hollow sphere is lower (J.Phys.chem.C 2009,113, 10441-10445). Although the literature (chem. Eur. J.2010,16,3497-3503) reports that the specific surface area of the material reaches 521m2The material has weak adsorption capacity to methylene blue. In addition, the magnesium-containing silicon oxide hollow spheres synthesized by the method are all pure-phase magnesium silicate hollow spheres.
Disclosure of Invention
The invention aims to provide a preparation method of a magnesium modified nano silicon dioxide hollow sphere.
The technical scheme for realizing the purpose of the invention is as follows:
the preparation method of the magnesium modified nano silicon dioxide hollow sphere comprises the following steps:
by solid SiO2The molar ratio of the magnesium salt to the magnesium salt is 5-50: 1, in solid SiO2And adding magnesium salt into the suspension of the nano particles, uniformly dispersing by ultrasonic, adding sodium borohydride, carrying out hydrothermal reaction at 80-180 ℃, centrifuging after the reaction is finished, washing with water, and drying to obtain the magnesium modified nano silicon dioxide hollow spheres.
The solid SiO2The suspension of the nano particles is solid SiO2And (3) ultrasonically dispersing the nano particles in water to obtain a suspension, wherein the ultrasonic time is 10-30 min.
Preferably, after the magnesium salt is added, the ultrasonic dispersion time is 10-30 min.
In the invention, the solid SiO2The nano particles are prepared by a conventional method, and the diameter of the nano particles is 50 nm-900 nm.
Preferably, the magnesium salt is magnesium sulfate, magnesium chloride, magnesium nitrate, magnesium acetate, magnesium ethoxide or magnesium gluconate.
Preferably, the concentration of the sodium borohydride is 0.06 g/ml-0.2 g/ml.
Preferably, the hydrothermal reaction time is 0.5-48 hours.
Preferably, the concentration of the magnesium salt is 0.01mmol/ml to 0.1 mmol/ml.
Compared with the prior art, the invention has the following advantages:
the invention has lower hydrothermal temperature and is more economical and practical. In the synthesis process, sodium borohydride not only provides an alkaline environment for the reaction to promote the solid silicon oxide to be dissolved under the hydrothermal condition and in Mg2+In the presence of (B) and provide borate ion (BO)2 -) And participating in the silica reformation process to obtain the synthesized magnesium silicate and the resynthesized silica composite material, namely the magnesium silicate-silica composite hollow ball. The composite hollow sphere has higher specific surface area and pore volume, and the specific surface area reaches 600m2The water-soluble organic pollutant adsorbent can effectively adsorb organic pollutants.
Drawings
FIG. 1 is a schematic flow diagram of the process of the present invention.
FIG. 2 is a scanning electron micrograph of the magnesium-modified nano-silica hollow spheres prepared in the example.
FIG. 3 is a transmission electron micrograph of the magnesium-modified nano-silica hollow sphere prepared in the example.
FIG. 4 is a surface distribution diagram of oxygen, silicon and magnesium elements of the magnesium modified nano-silica hollow sphere prepared in example 1.
FIG. 5 is a scanning electron micrograph of the magnesium-modified nano-silica hollow spheres prepared in comparative example 1.
FIG. 6 is a scanning electron micrograph of the magnesium-modified nano-silica hollow spheres prepared in comparative example 2.
Table 1 is a table comparing the comprehensive adsorption performance data of the application examples and the comparative examples.
Detailed Description
The present invention will be described in more detail with reference to the following examples and the accompanying drawings.
Example 1
Step 1, preparing SiO2Suspension liquid: weigh 150mg of SiO2The size of the solid sphere nano-particles is about 450nm, the solid sphere nano-particles are placed in a beaker, 5mL of deionized water is added into the beaker, and the obtained solution is subjected to ultrasonic treatment for 10 minutes;
step 2, preparing magnesium chloride-SiO2Mixing the solution: adding 0.1mmol of magnesium chloride (MgCl) into the solution prepared in the step 12) Sonicating the solution for 10 minutes;
step 3, preparing the magnesium modified silicon dioxide hollow sphere: mixing the magnesium chloride-SiO prepared in the step 22The mixed solution was transferred to a 20mL capacity polytetrafluoroethylene-lined autoclave and 0.50g of NaBH was added thereto4And reacting at 80 ℃ for 12 hours;
and 4, centrifugally washing the obtained solution to be neutral, and then freezing and drying. The dried sample was a magnesium modified silica hollow sphere.
Table 1 is a table comparing the adsorption performance data of the magnesium modified silica hollow spheres obtained in example 1 with that of unmodified silica hollow spheres. As can be seen from Table 1, the adsorption performance of the magnesium modified silica hollow spheres on methylene blue is greatly improved to 370.45mg/g compared with that of unmodified silica hollow spheres.
Example 2
Similar to example 1, except that MgCl in step 2 of example 12Modified into magnesium acetate (C)4H6O4Mg), other conditions remained consistent.
Example 3
Similar to example 1, except that MgCl in step 2 of example 12Modified to magnesium nitrate (Mg (NO)3)2) Other conditions being kept consistent。
Example 4
Similar to example 1, except that the heating temperature in step 3 of example 1 was changed to 180 ℃, the other conditions were kept consistent.
Example 5
Similar to example 1, except that the heating time in step 3 of example 1 was changed to 8 hours, the other conditions were kept consistent.
Example 6
Similar to example 1, except that MgCl in step 2 of example 12The amount of addition was 0.05mmol, and the other conditions were kept the same.
Example 7
Similar to example 1, except that MgCl in step 2 of example 12The amount of addition was 0.5mmol, and the other conditions were kept the same.
FIG. 1 is a schematic flow chart of the present invention, which uses solid SiO2The magnesium modified silicon oxide hollow sphere is obtained by hydrothermal reaction in the presence of sodium borohydride. The composite material shows excellent adsorption performance to methylene blue.
Fig. 2 is a scanning electron micrograph of the magnesium-modified nano silica hollow spheres of examples 1, 2, 3,4, 5, 6 and 7, from which it can be seen that the composite material is a hollow sphere.
Fig. 3 is a transmission electron micrograph of the magnesium modified nano silica hollow spheres of examples 1, 2, 3,4, 5, 6 and 7, from which it can be seen that the hollow spheres consist of ultrathin nanosheets.
FIG. 4 is the surface distribution diagram of the oxygen, silicon and magnesium elements of the magnesium modified nano-silica hollow spheres of examples 1, 2, 3,4, 5, 6 and 7, and it can be seen that the three elements of oxygen, silicon and magnesium are uniformly distributed on the hollow spheres.
Comparative example 1
Similar to example 1, except that the heating temperature in step 3 of example 1 was changed to 60 ℃, the other conditions were kept consistent.
FIG. 5 is a scanning electron micrograph of the magnesium-modified nano-silica hollow sphere of comparative example 1,from the figure, the surface of the composite material is ultrathin nano-sheet but most of the composite material is still solid silica spheres, so that solid SiO with low temperature can be seen2The spheres are completely converted into hollow spheres.
Comparative example 2
Similar to example 1, except that the amount of magnesium chloride added in step 2 of example 1 was changed to 0.6mmol, the other conditions were kept the same.
Fig. 6 is a scanning electron micrograph of the magnesium-modified nano-silica hollow spheres of comparative example 2, from which it can be seen that when magnesium chloride is added in excess, transformed solid spheres and transformed hollow spheres with significant agglomeration are present.
The adsorbing materials prepared in the examples and the comparative examples were subjected to methylene blue adsorption experiments for the same reaction time, and after the mixture solution was filtered, UV-Vis measurements were rapidly performed, and the results of adsorption curve fitting are shown in table 1.
TABLE 1 Langmuir and Freundlich adsorption Curve parameters for methylene blue adsorption
Figure BDA0002086437400000041
In conclusion, the method has the advantages of simple and controllable process, lower synthesis temperature, economy and practicability. The magnesium modified nano silicon dioxide hollow sphere is prepared by dissolving solid silicon dioxide spheres under the action of sodium borohydride and synthesizing the silicon dioxide hollow sphere containing magnesium, and the composite hollow sphere is prepared from magnesium silicate and formed silicon dioxide and is synthesized for the first time. In addition, the magnesium modified nano silicon dioxide hollow sphere is composed of porous ultrathin nano sheets, has relatively high specific surface area and pore volume, has high adsorption capacity on organic dyes such as methylene blue, and can be repeatedly used.

Claims (8)

1. The preparation method of the magnesium modified nano silicon dioxide hollow sphere is characterized by comprising the following steps:
by solid SiO2The molar ratio of the magnesium salt to the magnesium salt is 5-50: 1, in solid SiO2Adding into suspension of nanoparticlesAnd uniformly dispersing the magnesium salt by ultrasonic, adding sodium borohydride, carrying out hydrothermal reaction at 80-180 ℃, centrifuging after the reaction is finished, washing with water, and drying to obtain the magnesium modified nano-silica hollow sphere.
2. The method of claim 1, wherein the solid SiO is2The suspension of the nano particles is solid SiO2And (3) ultrasonically dispersing the nano particles in water to obtain a suspension, wherein the ultrasonic time is 10-30 min.
3. The preparation method according to claim 1, wherein the ultrasonic dispersion time is 10-30 min after the magnesium salt is added.
4. The method of claim 1, wherein the solid SiO is2The diameter of the nano-particles is 50 nm-900 nm.
5. The method according to claim 1, wherein the magnesium salt is magnesium sulfate, magnesium chloride, magnesium nitrate, magnesium acetate, magnesium ethoxide, or magnesium gluconate.
6. The method according to claim 1, wherein the concentration of sodium borohydride is 0.06g/ml to 0.2 g/ml.
7. The preparation method according to claim 1, wherein the hydrothermal reaction time is 0.5 to 48 hours.
8. The method according to claim 1, wherein the concentration of the magnesium salt is 0.01mmol/ml to 0.1 mmol/ml.
CN201910489244.3A 2019-06-06 2019-06-06 Preparation method of magnesium modified nano silicon dioxide hollow sphere Pending CN112044392A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113181879A (en) * 2021-05-21 2021-07-30 福州大学 Preparation method and application of hollow carbon-based magnesium silicate microsphere adsorbent
CN115770546A (en) * 2022-11-25 2023-03-10 南京信息工程大学 Porous magnesium silicate adsorbent and preparation method thereof
RU2816067C1 (en) * 2023-07-03 2024-03-26 Федеральное государственное бюджетное учреждение науки Ордена Трудового Красного Знамени Институт химии силикатов им. И.В. Гребенщикова Российской академии наук (ИХС РАН) Method of obtaining sorbent

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CN107500303A (en) * 2017-08-14 2017-12-22 曲阜师范大学 A kind of mesoporous magnesium silicate microballoon and its hydro-thermal thermal transition preparation method
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113181879A (en) * 2021-05-21 2021-07-30 福州大学 Preparation method and application of hollow carbon-based magnesium silicate microsphere adsorbent
CN115770546A (en) * 2022-11-25 2023-03-10 南京信息工程大学 Porous magnesium silicate adsorbent and preparation method thereof
RU2816067C1 (en) * 2023-07-03 2024-03-26 Федеральное государственное бюджетное учреждение науки Ордена Трудового Красного Знамени Институт химии силикатов им. И.В. Гребенщикова Российской академии наук (ИХС РАН) Method of obtaining sorbent

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Application publication date: 20201208