CN114835128A - Preparation method of epoxy resin grafted modified silicon dioxide aerogel - Google Patents
Preparation method of epoxy resin grafted modified silicon dioxide aerogel Download PDFInfo
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- CN114835128A CN114835128A CN202210603683.4A CN202210603683A CN114835128A CN 114835128 A CN114835128 A CN 114835128A CN 202210603683 A CN202210603683 A CN 202210603683A CN 114835128 A CN114835128 A CN 114835128A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/157—After-treatment of gels
- C01B33/158—Purification; Drying; Dehydrating
- C01B33/1585—Dehydration into aerogels
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/157—After-treatment of gels
- C01B33/159—Coating or hydrophobisation
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B80/00—Architectural or constructional elements improving the thermal performance of buildings
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Abstract
The invention discloses a preparation method of epoxy resin grafted modified silicon dioxide aerogel, which comprises the following steps: (1) dispersing an organosilane coupling agent into a methanol solvent, adding deionized water and a gel promoter, mixing, and heating and hydrolyzing to obtain a silicon dioxide prepolymerization solution; (2) uniformly mixing the silicon dioxide pre-polymerization solution and the epoxy resin solution, placing the mixture in a water bath, standing and placing gel to form silicon dioxide in-situ grafting modified gel; (3) and placing the silica in-situ graft modified gel into a methanol solution for aging and replacement, and then drying to obtain the epoxy resin graft modified silica aerogel. According to the invention, the silica gel cluster solution is subjected to in-situ grafting modification by epoxy resin, and the epoxy group, the hydroxyl group and the silicon hydroxyl group are subjected to cross-linking polymerization to form the three-dimensional network structure silica hybrid alcogel through self-assembly, so that the integrity of the surface void structure of the silica aerogel is improved, the surface defect is reduced, and the strength of the three-dimensional network structure is improved.
Description
Technical Field
The invention belongs to the technical field of aerogel preparation, and particularly relates to a preparation method for modifying silicon dioxide aerogel.
Background
Silica aerogel is a lightweight insulating material with a unique nanoporous three-dimensional network structure. Because a large number of silicon hydroxyl groups exist on the inner surface of the silica aerogel prepared by the conventional method, the silicon hydroxyl groups not only can cause extra shrinkage of a gel block body due to polycondensation, but also can absorb and store water in air to crack and break the aerogel, so that the acoustic, optical, electrical, thermal, mechanical and other properties of the aerogel are seriously influenced, and the application occasions of the aerogel are limited.
At present, the hydrophobic modification of silicon dioxide aerogel is mainly divided into an in-situ polymerization method and a surface post-treatment modification method. The in-situ polymerization method, namely the co-precursor method, is to carry out co-hydrolysis reaction on a modifier containing hydrophobic groups and a silane solution, catalyze gel and dry to obtain the silica aerogel with hydrophobicity. For example: A.V. Rao and the like research the aerogel prepared by adding different modifiers into various silicon source precursors, and the research finds that: the quality of the hydrophobic performance of the aerogel depends on the number of the alkyl groups which are added and act in the organosilane serving as the combined precursor, and the organosilane modified material with monoalkyl trialkoxy is added, so that the contact angle is small, the hydrophobicity is poor, and the light transmittance is the best; by adding organosilane modified material with trialkyl, the density of aerogel material can be reduced, the volume shrinkage is reduced, the hydrophobic property is greatly improved, and the hydrophobic stable temperature is increased (more than 300 ℃); the hydrophobic stability temperature of the organosilane modified material with the phenyltrialkoxy can reach more than 550 ℃. However, trialkyl organosilane modified aerogels absorb more water than monoalkyl organosilane modified materials (except for HMDZ) when used for long periods.
The surface post-treatment method refers to the reaction of a modifier with hydroxyl groups on the surface of silica gel. For example, chinese patent CN107117932A discloses a hydrophobic agent and a method for preparing aerogel thermal insulation felt using the hydrophobic modifier, chinese patent CN11960424A discloses a method for preparing a super-hydrophobic spherical silica aerogel material, chinese patent CN113416028A discloses a process for producing a water-resistant aerogel thermal insulation material, chinese patent CN108017062A discloses a hydrophobic silica aerogel and a method for preparing the same, both of which describe the modification of aerogel, but the surface post-treatment method reported in the above patent is a reaction between the modifier and hydroxyl groups on the surface of silica aerogel, the water-proofing capability of the aerogel material prepared by the method has timeliness, if in a humid environment for a long time, the voids of the outer surface structure of the aerogel can store certain moisture, and the structure partially collapses after diffusion. Therefore, there is an urgent need for improvement of silica aerogel modification methods to obtain aerogels with good processing properties.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a preparation method of an epoxy resin graft modified silica aerogel.
A preparation method of epoxy resin graft modified silicon dioxide aerogel comprises the following steps:
(1) dispersing an organosilane coupling agent into a methanol solvent, adding deionized water and a gel promoter, mixing, heating and hydrolyzing, heating in a water bath at 40-70 ℃ for 1-3h to obtain a silica prepolymerization solution, wherein the mass percentages of the organosilane coupling agent, the methanol, the deionized water and the gel promoter are 12.3%, 85.9%, 1.7% and 0.1%; the organosilane coupling agent comprises one or two of tetraethoxysilane, methyl orthosilicate, poly tetraethoxysilane and poly methyl orthosilicate; the gel promoter comprises one or two of hydrochloric acid, oxalic acid, phosphoric acid, citric acid and boric acid;
(2) uniformly mixing the silica pre-polymerization solution and the epoxy resin solution, specifically, dropwise adding the epoxy resin solution into the silica pre-polymerization solution, stirring for 1-5min, placing the solution in a water bath, standing and placing the solution for 3-15min for gelation, wherein the temperature in the water bath is 20-30 ℃, and forming silica in-situ grafting modified gel; the epoxy resin comprises one or two of bisphenol A epoxy resin, bisphenol F epoxy resin, polyphenol glycidyl ether epoxy resin and aliphatic glycidyl ether epoxy resin; the dosage of the epoxy resin is 2-14wt% of the total mass of the organosilane coupling agent, the methanol, the deionized water and the gel accelerator, because if the dosage of the epoxy resin is less than the range, the polymerization gel can not be promoted, if the dosage of the epoxy resin is more than the range, the gel speed is too high to control, and the heat insulation performance is deteriorated after the density is increased;
(3) and placing the silica in-situ graft modified gel into a methanol solution for aging and replacement for 12-24h, and then drying to obtain the epoxy resin graft modified silica aerogel.
According to the preparation method of the epoxy resin graft modified silica aerogel, deionized water and acid are used for catalyzing and hydrolyzing an organosilane coupling agent, namely Si-O-R is hydrolyzed into Si-O-H under an acidic condition, wherein a small part of Si-O-H is polymerized with Si-O-Si, so that an acidic uniform silica micelle solution is obtained. Under the condition of existence of a large amount of silicon hydroxyl, mixing with an epoxy resin solution, dehydrating by polymerization of the hydroxyl on the epoxy resin and the silicon hydroxyl, and grafting to a silicon dioxide micelle; simultaneously, under the nucleophilic action of silicon hydroxyl, epoxy groups on the epoxy resin are subjected to ring opening and are subjected to etherification cross-linking polymerization reaction with silicon hydroxyl groups on the silica micelles to promote the micelles to grow into complete colloidal particles, so that silica in-situ graft modified gel is formed, and the epoxy resin graft modified silica aerogel is finally obtained through aging, replacement and supercritical drying
Compared with the prior art, the preparation method of the epoxy resin grafted modified silicon dioxide aerogel has the beneficial effects that: 1. according to the invention, the silica gel cluster solution is subjected to in-situ grafting modification by epoxy resin, and the epoxy group, the hydroxyl group and the silicon hydroxyl group are subjected to cross-linking polymerization to form the three-dimensional network structure silica hybrid alcohol gel through self-assembly, so that the integrity of the surface void structure of the silica aerogel is improved, the surface defect is reduced, and the strength of the three-dimensional network structure is improved;
2. the modified silicon dioxide hybrid alcohol gel contains hydrophobic groups such as aromatic hydrocarbon structures and the like, and is favorable for improving the hydrophobicity, water resistance and acid and alkali resistance of the silicon dioxide aerogel;
3. according to the composite material, the epoxy resin in-situ graft modification is adopted to enhance the hydrophobic property and the structural strength of the silica aerogel, and the silica aerogel and the epoxy resin are self-assembled to form the three-dimensional network structure gel, so that compared with the traditional one-step method or acid-base two-step method, the surface modification process flow is simplified, the whole operation step is simple, the implementation condition is mild, and the prepared material has good performance.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings.
FIG. 1 is a sample diagram of an in situ graft-modified silica aerogel in example 1 of the present invention;
FIG. 2 is a comparative photograph showing water drop patterns of silica aerogel and epoxy resin graft-modified silica aerogel in example 1 of the present invention;
FIG. 3 is a weight chart of the epoxy resin graft modified silica aerogel in example 2 of the present invention subjected to pressures of 50, 100, and 200 times.
Detailed Description
The following description of the embodiments of the present invention is provided for illustrative purposes, and other advantages and effects of the present invention will become apparent to those skilled in the art from the present disclosure.
It is to be noted that the term "comprises," "comprising," or any other variation thereof is intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus 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 apparatus.
Example 1
A preparation method of epoxy resin graft modified silicon dioxide aerogel comprises the following steps:
(1) dispersing poly (ethyl orthosilicate) into a methanol solvent, adding deionized water and 37% hydrochloric acid, mixing, putting into a water bath kettle, controlling the temperature in the water bath kettle to be 50 ℃, and carrying out hydrolysis reaction for 2 hours to obtain a silicon dioxide prepolymerization solution, wherein the mass percentages of the organosilane coupling agent, the methanol, the deionized water and the gel promoter are 12.3%, 85.9%, 1.7% and 0.1%;
(2) dripping 6wt% of bisphenol A epoxy resin solution into the silica prepolymerization solution, stirring for 5min to obtain a homogeneous system, placing in a water bath kettle, controlling the water bath temperature at 30 ℃, standing for 10min for gelation, and polymerizing to obtain three-dimensional network structure alcogel, namely silica in-situ graft modified gel;
(3) and placing the silicon dioxide in-situ grafting modified gel into a methanol solution for aging and replacement for 12h, and then drying by supercritical carbon dioxide to obtain the milky hydrophobic epoxy resin grafting modified silicon dioxide aerogel. Compared with unmodified silica aerogel, the method has the advantages that water drops are dripped on the surface of a sample, the structure collapses, and a white powder state is presented; and grafting the modified silica aerogel by using the epoxy resin, and dripping water beads on the surface of the sample to form water beads, which is shown in figure 2.
Example 2
A preparation method of epoxy resin graft modified silicon dioxide aerogel comprises the following steps:
(1) dispersing tetraethoxysilane into a methanol solvent, adding deionized water and 37% hydrochloric acid, mixing, putting into a water bath kettle, controlling the temperature in the water bath kettle to be 60 ℃, and carrying out hydrolysis reaction for 1.5 hours to obtain a silicon dioxide prepolymerization solution, wherein the mass percentages of the organosilane coupling agent, the methanol, the deionized water and the gel promoter are 12.3%, 85.9%, 1.7% and 0.1%;
(2) dripping 8wt% of bisphenol A epoxy resin solution into the silica prepolymerization solution, stirring for 1min to obtain a homogeneous system, placing in a water bath kettle, controlling the water bath temperature at 25 ℃, standing for 5min for gelation, and polymerizing to obtain three-dimensional network structure alcogel, namely silica in-situ graft modified gel;
(3) and placing the silica in-situ graft modified gel into a methanol solution for aging and replacement for 12h, and then drying by supercritical carbon dioxide to obtain the epoxy resin graft modified silica aerogel. The density test result is 222.2kg/m 3 The test weight of the sample is 1g, weights of 50g, 100g and 200g are applied, and the epoxy resin grafted modified silica aerogel sample block is not deformed and broken, as shown in figure 3
Example 3
A preparation method of epoxy resin graft modified silicon dioxide aerogel comprises the following steps:
(1) dispersing poly (ethyl orthosilicate) into a methanol solvent, adding deionized water and 37% hydrochloric acid, mixing, putting into a water bath kettle, carrying out hydrolysis reaction for 1h at the temperature of 65 ℃ in the water bath kettle, and obtaining a silicon dioxide prepolymerization solution, wherein the mass percentages of an organosilane coupling agent, methanol, deionized water and a gel promoter are 12.3%, 85.9%, 1.7% and 0.1%;
(2) dripping 10wt% of bisphenol A epoxy resin solution into the silica prepolymerization solution, stirring for 1min to obtain a homogeneous system, placing in a water bath kettle, controlling the water bath temperature at 30 ℃, standing for 3min for gelation, and polymerizing to obtain three-dimensional network structure alcogel, namely silica in-situ graft modified gel;
(3) and placing the silica in-situ graft modified gel into a methanol solution for aging and replacement for 24 hours, and then drying by supercritical carbon dioxide to obtain the hydrophobic epoxy resin graft modified silica aerogel. The density of the sample is increased, and the density test result is 260.3kg/m 3 The swatches exhibited slight cracking and increased strength.
Example 4
A preparation method of epoxy resin graft modified silicon dioxide aerogel comprises the following steps:
(1) dispersing poly (methyl orthosilicate) and a methanol solvent, adding deionized water and 37% hydrochloric acid, mixing, putting into a water bath kettle, controlling the temperature in the water bath kettle to be 40 ℃, and carrying out hydrolysis reaction for 3 hours to obtain a silicon dioxide prepolymerization solution, wherein the mass percentages of the organosilane coupling agent, the methanol, the deionized water and the gel promoter are 12.3%, 85.9%, 1.7% and 0.1%;
(2) dripping 14wt% of bisphenol A epoxy resin solution into the silica prepolymerization solution, stirring for 3min to obtain a homogeneous system, placing in a water bath kettle, controlling the water bath temperature at 30 ℃, standing for 15min for gelation, and polymerizing to obtain three-dimensional network structure alcogel, namely silica in-situ graft modified gel;
(3) placing the silica in-situ grafting modified gel into a methanol solution for aging and replacement for 24 hours,and then drying the mixture by supercritical carbon dioxide to obtain the hydrophobic epoxy resin grafted modified silicon dioxide aerogel. The sample block cracks seriously and the density is increased, and the test result is 280.7kg/m 3 。
Other parts of the invention not described in detail are conventional techniques known to the person skilled in the art.
The scope of the present invention is not limited to the technical solutions disclosed in the embodiments, and any modifications, equivalent substitutions, improvements, etc. made to the above embodiments according to the technical spirit of the present invention fall within the scope of the present invention.
Claims (9)
1. A preparation method of epoxy resin graft modification silicon dioxide aerogel is characterized by comprising the following steps: the method comprises the following steps:
(1) dispersing an organosilane coupling agent into a methanol solvent, adding deionized water and a gel promoter, mixing, and heating and hydrolyzing to obtain a silicon dioxide prepolymerization solution;
(2) uniformly mixing the silicon dioxide pre-polymerization solution and the epoxy resin solution, placing the mixture in a water bath, standing and placing gel to form silicon dioxide in-situ grafting modified gel;
(3) and placing the silica in-situ graft modified gel into a methanol solution for aging and replacement, and then drying to obtain the epoxy resin graft modified silica aerogel.
2. The method for preparing the epoxy resin graft-modified silica aerogel according to claim 1, wherein: the mass percentages of the organosilane coupling agent, the methanol, the deionized water and the gel promoter are 12.3%, 85.9%, 1.7% and 0.1%.
3. The method for preparing the epoxy resin graft-modified silica aerogel according to claim 1, wherein: the heating hydrolysis in the step (1) is water bath heating, and the temperature is 40-70 ℃; the temperature in the water bath kettle in the step (2) is 20-30 ℃.
4. The method for preparing the epoxy resin graft-modified silica aerogel according to claim 1, wherein: the organosilane coupling agent comprises one or two of tetraethoxysilane, methyl orthosilicate, poly tetraethoxysilane and poly methyl orthosilicate.
5. The method for preparing the epoxy resin graft-modified silica aerogel according to claim 1, wherein: the gel accelerator comprises one or two of hydrochloric acid, oxalic acid, phosphoric acid, citric acid and boric acid.
6. The method for preparing the epoxy resin graft-modified silica aerogel according to claim 1, wherein: and (3) when the silica pre-polymerization solution and the epoxy resin solution are mixed in the step (2), dropwise adding the epoxy resin solution into the silica pre-polymerization solution, and stirring for 1-5min until the silica pre-polymerization solution and the epoxy resin solution are uniformly mixed.
7. The method for preparing an epoxy resin graft-modified silica aerogel according to claim 1 or 6, wherein: the epoxy resin comprises one or two of bisphenol A epoxy resin, bisphenol F epoxy resin, polyphenol glycidyl ether epoxy resin and aliphatic glycidyl ether epoxy resin.
8. The method for preparing the epoxy resin graft-modified silica aerogel according to claim 1, wherein: the dosage of the epoxy resin is 2-14wt% of the total mass of the organic silane coupling agent, the methanol, the deionized water and the gel accelerator.
9. The method for preparing the epoxy resin graft-modified silica aerogel according to claim 1, wherein: the hydrolysis time in the step (1) is 1-3 h; standing for 3-15min in the step (2); the aging time in the step (3) is 12-24 h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115571885A (en) * | 2022-10-31 | 2023-01-06 | 陕西科技大学 | Isocyanate grafted modified silica aerogel and preparation method thereof |
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