CN117383571A - Modified inorganic silica gel and preparation process thereof - Google Patents

Modified inorganic silica gel and preparation process thereof Download PDF

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Publication number
CN117383571A
CN117383571A CN202311324449.9A CN202311324449A CN117383571A CN 117383571 A CN117383571 A CN 117383571A CN 202311324449 A CN202311324449 A CN 202311324449A CN 117383571 A CN117383571 A CN 117383571A
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parts
silica gel
graphene
modified
inorganic silica
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CN202311324449.9A
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赵志波
于秀暖
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Shandong Bangkai New Material Co ltd
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Shandong Bangkai New Material Co ltd
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Priority to CN202311324449.9A priority Critical patent/CN117383571A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/157After-treatment of gels
    • C01B33/158Purification; Drying; Dehydrating
    • C01B33/1585Dehydration into aerogels
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/182Graphene
    • C01B32/184Preparation
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/182Graphene
    • C01B32/194After-treatment
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/146After-treatment of sols
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/157After-treatment of gels

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Nanotechnology (AREA)
  • Silicon Compounds (AREA)

Abstract

The invention discloses modified inorganic silica gel which comprises the following components in parts by weight: 40-55 parts of sodium silicate, 30-40 parts of sulfuric acid, 3-8 parts of modified graphene, 3-5 parts of methanol, 1-5 parts of cobalt chloride and 1-5 parts of magnesium chloride. According to the invention, the organic active groups are grafted on the surface of the prepared silica gel by adding the modified graphene, the cobalt chloride and the magnesium chloride, so that the mechanical strength and the adsorption performance of the silica gel product are improved, and the silica gel product can be used as an adsorbent; meanwhile, the modified graphene not only maintains the characteristic of high specific surface area of the graphene, but also increases the dispersion capacity of the graphene oxide in the silica gel solution, and solves the problems of easy agglomeration and difficult dispersion of the graphene oxide.

Description

Modified inorganic silica gel and preparation process thereof
Technical Field
The invention relates to the technical field of inorganic silica gel, in particular to modified inorganic silica gel and a preparation process thereof.
Background
The production process of inorganic silica gel is usually that sodium silicate and sulfuric acid with certain concentration are soaked in tap water for washing after gum making, aging and gum cutting, and then the silica gel product is obtained after drying. Silica gel is a porous structure material, sodium silicate reacts with sulfuric acid, dehydration condensation is carried out to form porous silica, sodium sulfate as a byproduct is remained in a silica gel micro pore canal, and the purpose of water washing in the production process is to wash out sodium sulfate in the silica gel, so that a stable framework structure is formed, and the quality of the silica gel is improved; the inorganic silica gel in the existing market has limited self adsorption capacity, poor use effect and poor durability.
Disclosure of Invention
The invention aims to provide modified inorganic silica gel and a preparation process thereof, so as to solve the problems in the background technology.
In order to achieve the above purpose, the present invention provides the following technical solutions:
the modified inorganic silica gel comprises the following components in parts by weight:
40-55 parts of sodium silicate, 30-40 parts of sulfuric acid, 3-8 parts of modified graphene, 3-5 parts of methanol, 1-5 parts of cobalt chloride and 1-5 parts of magnesium chloride.
Preferably, the composition comprises the following components in parts by weight:
42-53 parts of sodium silicate, 33-46 parts of sulfuric acid, 3-5 parts of modified graphene, 4-5 parts of methanol, 3-5 parts of cobalt chloride and 3-5 parts of magnesium chloride.
Preferably, the composition comprises the following components in parts by weight:
50 parts of sodium silicate, 40 parts of sulfuric acid, 4 parts of modified graphene, 5 parts of methanol, 4 parts of cobalt chloride and 4 parts of magnesium chloride.
Preferably, the preparation method of the modified graphene comprises the following steps:
dispersing graphene oxide in water, and preparing graphene oxide suspension with the concentration of 6mg/mL through ultrasonic dispersion; then adding aluminum hydroxide and a surfactant polyacrylamide into the obtained graphene oxide suspension; wherein, the mass ratio of the aluminum hydroxide, the graphene oxide and the polyacrylamide is 2:3:8, fully stirring, reacting for 5 hours at 50-80 ℃ to obtain a reaction solution after complete reaction; heating the obtained reaction solution to 90-95 ℃, adding reducing agent potassium borohydride, and fully reacting to obtain black flocculent precipitate; the mass of the reducing agent is 9 times of that of the graphene oxide; and then carrying out suction filtration, washing and drying on the black flocculent precipitate to obtain the modified graphene.
A preparation process of modified inorganic silica gel comprises the following steps:
firstly, hydrolyzing sodium silicate by sulfuric acid, and obtaining a preliminary inorganic silica gel solution through dehydration and crosslinking;
secondly, ultrasonically dispersing the modified graphene in methanol, then adding cobalt chloride and magnesium chloride to obtain a dispersed graphene solution, and adding the dispersed graphene solution into inorganic silicon;
thirdly, aging the inorganic silica gel in the second step, washing the aged inorganic silica gel with deionized water to obtain supernatant, clarifying, vacuum drying for 2h, and calcining in a muffle furnace at 450 ℃ for 0.5h to obtain the porous inorganic silica gel.
Preferably, the aging treatment in the third step specifically includes: stirring for 30min at the rotating speed of 200r/min, then heating to 60 ℃, and aging for 5h.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the organic active groups are grafted on the surface of the prepared silica gel by adding the modified graphene, the cobalt chloride and the magnesium chloride, so that the mechanical strength and the adsorption performance of the silica gel product are improved, and the silica gel product can be used as an adsorbent; meanwhile, the modified graphene not only maintains the characteristic of high specific surface area of the graphene, but also increases the dispersion capacity of the graphene oxide in the silica gel solution, and solves the problems of easy agglomeration and difficult dispersion of the graphene oxide.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The modified inorganic silica gel comprises the following components in parts by weight:
40-55 parts of sodium silicate, 30-40 parts of sulfuric acid, 3-8 parts of modified graphene, 3-5 parts of methanol, 1-5 parts of cobalt chloride and 1-5 parts of magnesium chloride.
Comprises the following components in parts by weight:
42-53 parts of sodium silicate, 33-46 parts of sulfuric acid, 3-5 parts of modified graphene, 4-5 parts of methanol, 3-5 parts of cobalt chloride and 3-5 parts of magnesium chloride.
Comprises the following components in parts by weight:
50 parts of sodium silicate, 40 parts of sulfuric acid, 4 parts of modified graphene, 5 parts of methanol, 4 parts of cobalt chloride and 4 parts of magnesium chloride.
The preparation method of the modified graphene comprises the following steps:
dispersing graphene oxide in water, and preparing graphene oxide suspension with the concentration of 6mg/mL through ultrasonic dispersion; then adding aluminum hydroxide and a surfactant polyacrylamide into the obtained graphene oxide suspension; wherein, the mass ratio of the aluminum hydroxide, the graphene oxide and the polyacrylamide is 2:3:8, fully stirring, reacting for 5 hours at 50-80 ℃ to obtain a reaction solution after complete reaction; heating the obtained reaction solution to 90-95 ℃, adding reducing agent potassium borohydride, and fully reacting to obtain black flocculent precipitate; the mass of the reducing agent is 9 times of that of the graphene oxide; and then carrying out suction filtration, washing and drying on the black flocculent precipitate to obtain the modified graphene.
A preparation process of modified inorganic silica gel comprises the following steps:
firstly, hydrolyzing sodium silicate by sulfuric acid, and obtaining a preliminary inorganic silica gel solution through dehydration and crosslinking;
secondly, ultrasonically dispersing the modified graphene in methanol, then adding cobalt chloride and magnesium chloride to obtain a dispersed graphene solution, and adding the dispersed graphene solution into inorganic silicon;
thirdly, aging the inorganic silica gel in the second step, washing the aged inorganic silica gel with deionized water to obtain supernatant, clarifying, vacuum drying for 2h, and calcining in a muffle furnace at 450 ℃ for 0.5h to obtain the porous inorganic silica gel.
The method comprises the following steps: the aging treatment in the third step comprises the following specific steps: stirring for 30min at the rotating speed of 200r/min, then heating to 60 ℃, and aging for 5h.
Example 1:
the modified inorganic silica gel comprises the following components in parts by weight:
40 parts of sodium silicate, 30 parts of sulfuric acid, 3 parts of modified graphene, 3 parts of methanol, 1 part of cobalt chloride and 1 part of magnesium chloride.
The preparation method of the modified graphene comprises the following steps:
dispersing graphene oxide in water, and preparing graphene oxide suspension with the concentration of 6mg/mL through ultrasonic dispersion; then adding aluminum hydroxide and a surfactant polyacrylamide into the obtained graphene oxide suspension; wherein, the mass ratio of the aluminum hydroxide, the graphene oxide and the polyacrylamide is 2:3:8, fully stirring, reacting for 5 hours at 50-80 ℃ to obtain a reaction solution after complete reaction; heating the obtained reaction solution to 90-95 ℃, adding reducing agent potassium borohydride, and fully reacting to obtain black flocculent precipitate; the mass of the reducing agent is 9 times of that of the graphene oxide; and then carrying out suction filtration, washing and drying on the black flocculent precipitate to obtain the modified graphene.
A preparation process of modified inorganic silica gel comprises the following steps:
firstly, hydrolyzing sodium silicate by sulfuric acid, and obtaining a preliminary inorganic silica gel solution through dehydration and crosslinking;
secondly, ultrasonically dispersing the modified graphene in methanol, then adding cobalt chloride and magnesium chloride to obtain a dispersed graphene solution, and adding the dispersed graphene solution into inorganic silicon;
thirdly, aging the inorganic silica gel in the second step, washing the aged inorganic silica gel with deionized water to obtain supernatant, clarifying, vacuum drying for 2h, and calcining in a muffle furnace at 450 ℃ for 0.5h to obtain the porous inorganic silica gel.
The method comprises the following steps: the aging treatment in the third step comprises the following specific steps: stirring for 30min at the rotating speed of 200r/min, then heating to 60 ℃, and aging for 5h.
Example 2:
the modified inorganic silica gel comprises the following components in parts by weight:
55 parts of sodium silicate, 40 parts of sulfuric acid, 8 parts of modified graphene, 5 parts of methanol, 5 parts of cobalt chloride and 5 parts of magnesium chloride.
The preparation method of the modified graphene comprises the following steps:
dispersing graphene oxide in water, and preparing graphene oxide suspension with the concentration of 6mg/mL through ultrasonic dispersion; then adding aluminum hydroxide and a surfactant polyacrylamide into the obtained graphene oxide suspension; wherein, the mass ratio of the aluminum hydroxide, the graphene oxide and the polyacrylamide is 2:3:8, fully stirring, reacting for 5 hours at 50-80 ℃ to obtain a reaction solution after complete reaction; heating the obtained reaction solution to 90-95 ℃, adding reducing agent potassium borohydride, and fully reacting to obtain black flocculent precipitate; the mass of the reducing agent is 9 times of that of the graphene oxide; and then carrying out suction filtration, washing and drying on the black flocculent precipitate to obtain the modified graphene.
A preparation process of modified inorganic silica gel comprises the following steps:
firstly, hydrolyzing sodium silicate by sulfuric acid, and obtaining a preliminary inorganic silica gel solution through dehydration and crosslinking;
secondly, ultrasonically dispersing the modified graphene in methanol, then adding cobalt chloride and magnesium chloride to obtain a dispersed graphene solution, and adding the dispersed graphene solution into inorganic silicon;
thirdly, aging the inorganic silica gel in the second step, washing the aged inorganic silica gel with deionized water to obtain supernatant, clarifying, vacuum drying for 2h, and calcining in a muffle furnace at 450 ℃ for 0.5h to obtain the porous inorganic silica gel.
The method comprises the following steps: the aging treatment in the third step comprises the following specific steps: stirring for 30min at the rotating speed of 200r/min, then heating to 60 ℃, and aging for 5h.
Example 3:
the modified inorganic silica gel comprises the following components in parts by weight:
comprises the following components in parts by weight:
50 parts of sodium silicate, 40 parts of sulfuric acid, 4 parts of modified graphene, 5 parts of methanol, 4 parts of cobalt chloride and 4 parts of magnesium chloride.
The preparation method of the modified graphene comprises the following steps:
dispersing graphene oxide in water, and preparing graphene oxide suspension with the concentration of 6mg/mL through ultrasonic dispersion; then adding aluminum hydroxide and a surfactant polyacrylamide into the obtained graphene oxide suspension; wherein, the mass ratio of the aluminum hydroxide, the graphene oxide and the polyacrylamide is 2:3:8, fully stirring, reacting for 5 hours at 50-80 ℃ to obtain a reaction solution after complete reaction; heating the obtained reaction solution to 90-95 ℃, adding reducing agent potassium borohydride, and fully reacting to obtain black flocculent precipitate; the mass of the reducing agent is 9 times of that of the graphene oxide; and then carrying out suction filtration, washing and drying on the black flocculent precipitate to obtain the modified graphene.
A preparation process of modified inorganic silica gel comprises the following steps:
firstly, hydrolyzing sodium silicate by sulfuric acid, and obtaining a preliminary inorganic silica gel solution through dehydration and crosslinking;
secondly, ultrasonically dispersing the modified graphene in methanol, then adding cobalt chloride and magnesium chloride to obtain a dispersed graphene solution, and adding the dispersed graphene solution into inorganic silicon;
thirdly, aging the inorganic silica gel in the second step, washing the aged inorganic silica gel with deionized water to obtain supernatant, clarifying, vacuum drying for 2h, and calcining in a muffle furnace at 450 ℃ for 0.5h to obtain the porous inorganic silica gel.
The method comprises the following steps: the aging treatment in the third step comprises the following specific steps: stirring for 30min at the rotating speed of 200r/min, then heating to 60 ℃, and aging for 5h.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.

Claims (6)

1. The modified inorganic silica gel is characterized by comprising the following components in parts by weight:
40-55 parts of sodium silicate, 30-40 parts of sulfuric acid, 3-8 parts of modified graphene, 3-5 parts of methanol, 1-5 parts of cobalt chloride and 1-5 parts of magnesium chloride.
2. The modified inorganic silica gel according to claim 1, which comprises the following components in parts by weight:
42-53 parts of sodium silicate, 33-46 parts of sulfuric acid, 3-5 parts of modified graphene, 4-5 parts of methanol, 3-5 parts of cobalt chloride and 3-5 parts of magnesium chloride.
3. The modified inorganic silica gel according to claim 2, which comprises the following components in parts by weight:
50 parts of sodium silicate, 40 parts of sulfuric acid, 4 parts of modified graphene, 5 parts of methanol, 4 parts of cobalt chloride and 4 parts of magnesium chloride.
4. A modified inorganic silica gel as claimed in claim 3, wherein the preparation method of the modified graphene comprises the following steps:
dispersing graphene oxide in water, and preparing graphene oxide suspension with the concentration of 6mg/mL through ultrasonic dispersion; then adding aluminum hydroxide and a surfactant polyacrylamide into the obtained graphene oxide suspension; wherein, the mass ratio of the aluminum hydroxide, the graphene oxide and the polyacrylamide is 2:3:8, fully stirring, reacting for 5 hours at 50-80 ℃ to obtain a reaction solution after complete reaction; heating the obtained reaction solution to 90-95 ℃, adding reducing agent potassium borohydride, and fully reacting to obtain black flocculent precipitate; the mass of the reducing agent is 9 times of that of the graphene oxide; and then carrying out suction filtration, washing and drying on the black flocculent precipitate to obtain the modified graphene.
5. The process for preparing modified inorganic silica gel according to claim 1, comprising the steps of:
firstly, hydrolyzing sodium silicate by sulfuric acid, and obtaining a preliminary inorganic silica gel solution through dehydration and crosslinking;
secondly, ultrasonically dispersing the modified graphene in methanol, then adding cobalt chloride and magnesium chloride to obtain a dispersed graphene solution, and adding the dispersed graphene solution into inorganic silicon;
thirdly, aging the inorganic silica gel in the second step, washing the aged inorganic silica gel with deionized water to obtain supernatant, clarifying, vacuum drying for 2h, and calcining in a muffle furnace at 450 ℃ for 0.5h to obtain the porous inorganic silica gel.
6. The process for preparing modified inorganic silica gel according to claim 5, comprising the steps of: the aging treatment in the third step comprises the following specific steps: stirring for 30min at the rotating speed of 200r/min, then heating to 60 ℃, and aging for 5h.
CN202311324449.9A 2023-10-13 2023-10-13 Modified inorganic silica gel and preparation process thereof Pending CN117383571A (en)

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CN202311324449.9A CN117383571A (en) 2023-10-13 2023-10-13 Modified inorganic silica gel and preparation process thereof

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Application Number Priority Date Filing Date Title
CN202311324449.9A CN117383571A (en) 2023-10-13 2023-10-13 Modified inorganic silica gel and preparation process thereof

Publications (1)

Publication Number Publication Date
CN117383571A true CN117383571A (en) 2024-01-12

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