CN112538175A - Preparation method of high-strength gel material - Google Patents
Preparation method of high-strength gel material Download PDFInfo
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- CN112538175A CN112538175A CN202011410028.4A CN202011410028A CN112538175A CN 112538175 A CN112538175 A CN 112538175A CN 202011410028 A CN202011410028 A CN 202011410028A CN 112538175 A CN112538175 A CN 112538175A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- 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
- C01B33/152—Preparation of hydrogels
- C01B33/154—Preparation of hydrogels by acidic treatment of aqueous silicate solutions
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/04—Condensation polymers of aldehydes or ketones with phenols only
- C08J2361/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
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Abstract
The invention discloses a preparation method of a high-strength gel material, which mainly uses thermosetting resin as a main raw material, and the thermosetting resin is prepared into a solution with a certain viscosity. The curing agent and solution of the thermosetting resin is then slowly added with stirring. On one hand, the curing agent can react with the resin, so that the viscosity of the solution is continuously improved, on the other hand, the viscosity of the added solution can be continuously reduced, finally, the viscosity of the whole system is maintained in a stable state, and the sol is finally formed along with the continuous addition of the curing agent and the solution. The formed sol is further stood and reacted to finally form a high-strength gel material. The prepared gel material can be widely applied to various fields, such as phase change of building materials and slow release materials of energy storage materials.
Description
Technical Field
The invention relates to the technical field of gel preparation, in particular to a preparation method of a high-strength gel material.
Background
The traditional polymer hydrogel often shows poor mechanical properties such as fragility and low breaking strength due to single crosslinking mode, uneven network structure, overhigh water content and the like. Although hydrogels are structurally and compositionally similar to the soft tissues of the body, including cartilage, tendons, etc., there is still a large gap in mechanical properties compared to hydrogels, which greatly limits the practical applications of hydrogels, especially when the hydrogels are applied as load-bearing materials. In the last two decades, the improvement of the mechanical properties (strength, elongation at break and toughness) of polymer hydrogels has raised a hot tide in the scientific research community. At present, scientists have successfully developed various high-mechanical strength hydrogels, including double-network hydrogels, nano-composite hydrogels, topological structural hydrogels, and the like, through molecular and network design, improving the regularity of hydrogel networks, enhancing the degree of freedom of network cross-linking points, and the flexibility of polymer chain segments. In the United states, the high-strength hydrogels have high elongation at break (strain capacity), but the tensile strength at break is not high, which is a problem to be solved by the high-strength gel.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a high-strength gel material, which solves the problem that the breaking tensile strength of the existing hydrogel is not high.
In order to achieve the purpose, the invention is realized by the following technical scheme: a preparation method of a high-strength gel material is characterized by comprising the following steps: the method specifically comprises the following steps:
s1, dissolving the thermosetting resin in a solution with certain concentration and viscosity;
s2, stirring uniformly, and slowly dripping a curing agent solution with a certain concentration;
s3, the viscosity of the whole system can be maintained at a certain level by controlling the adding speed;
s4, stopping stirring when the content of the solvent in the final system reaches the expected concentration;
s5, standing the prepared sol at a certain temperature, so that the curing agent and the resin further react to finally form the high-strength thermosetting resin gel material.
Preferably, the thermosetting resin in step S1 mainly includes unsaturated polyester resin, epoxy resin, phenol resin, melamine formaldehyde resin, furan resin, acrylic resin, polyamide resin, polyurethane, polybutadiene resin, silicone resin, rosin, pitch, camphor. The solvent containing phenolic resin is selected from acetone, ethanol, benzene, toluene, ethyl acetate, solvent gasoline, cyclohexane, vegetable oil, etc.; the solvent of the melamine formaldehyde resin is selected from dilute acid; the organic silicon resin solvent is selected from ethanol, butanol, ethyl acetate, benzene, toluene, cyclohexanone, etc.; the solvent of furan resin is selected from organic solvents such as ester and ketone; the solvent of the epoxy resin is selected from benzene, toluene, xylene, ethanol, ethylene glycol, acetone, butanol, methyl ethyl ketone, cyclohexanone, ether alcohol, ethyl acetate and the like; the solvent of the polybutadiene resin is selected from water and the like; the solvent of the acrylic resin is selected from methanol, ethanol, ethylene glycol, isopropanol, dioxane, benzene, toluene, xylene, acetone, methyl ethyl ketone, cyclohexanone, butyl acetate, dichloroethane, ethyl acetate, chloroform, dichloroethane, glacial acetic acid, dioxanone, tetrahydrofuran, etc.; the solvent of the polyamide resin is selected from formic acid, concentrated sulfuric acid, dimethylformamide, m-cresol, phenol, ethanol/benzene mixed solvent and the like; the solvent of polyurethane is selected from methyl ethyl ketone, cyclohexanone, dimethylformamide, tetrahydrofuran, ethyl acetate, dioxane, etc.; the solvent of rosin is selected from ethanol, diethyl ether, acetone, benzene, toluene, carbon disulfide, dichloroethane, turpentine and alkali solution; the solvent of the asphalt is selected from benzene, toluene, xylene, carbon tetrachloride and chloroform; the solvent of Camphora is selected from ethanol, diethyl ether, acetone, chloroform, glacial acetic acid, benzene, etc.
Preferably, the stirring speed in step S2 is at least 1000 rpm.
Preferably, the viscosity of the thermosetting resin solution in the step S3 is at least 30 mpa · S.
Preferably, the standing time of the resin in the step S5 is 4-48 h.
Advantageous effects
The invention provides a preparation method of a high-strength gel material. Compared with the prior art, the method has the following beneficial effects:
(1) the invention takes thermosetting resin as a main raw material, and prepares the gel material taking the thermosetting resin as the framework by controlling the reaction speed of the thermosetting resin in the middle of the solution and a curing agent, thereby fully playing the characteristic of higher strength of the thermosetting resin, and the material has higher strength performance.
(2) The invention uses the existing thermosetting resin and curing system in the market as main raw materials, and has the advantage of wide material source.
(3) The invention utilizes the thermosetting resin and the curing agent to cure in the solvent system to prepare the gel material, and has the characteristics of simpler production process and lower manufacturing cost.
Drawings
FIG. 1 is a graph showing the compression resilience of a phenolic resin gel according to the present invention;
FIG. 2 is a graph showing the compressive strength of the phenolic resin gel of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the embodiment of the present invention provides three technical solutions: a preparation method of a high-strength gel material specifically comprises the following steps:
example 1
Taking water glass as a raw material, putting 50g of the water glass in a reaction cup of a homogenizer, and adjusting the rotating speed to 2000 r/min. Weighing 5g of 98% sulfuric acid and 20g of distilled water, sequentially adding the sulfuric acid and the distilled water into a stirring reaction system, and standing and aging for 48 hours to obtain the nano-silica gel.
Example 2
Weighing 30g of phenolic resin with powdery alcohol-soluble phenolic resin as a raw material, adding 30g of alcohol, placing the phenolic resin in a magnetic stirrer at 70 ℃, stirring and dissolving at 800r/min, placing the dissolved solution in a reaction cup of a homogenizer, adjusting the rotating speed to 2000r/min, weighing 10g of sulfuric acid with the mass fraction of 98% and 30g of distilled water, sequentially adding the sulfuric acid and the distilled water into a stirring reaction system, placing the sol obtained by reaction in a 60 ℃ drying oven, heating for 5h, and then standing for 12h to obtain the phenolic resin gel.
Example 3
Taking water glass as a raw material, putting 50g of the water glass in a reaction cup of a homogenizer, and adjusting the rotating speed to 1500 r/min. Weighing 5g of sulfuric acid with the mass fraction of 98% and 20g of distilled water, and sequentially adding the sulfuric acid and the distilled water into a stirring reaction system to obtain the nano-silica gel.
Comparative experiment
Comparative example 1
Taking water glass as a raw material, putting 50g of the water glass in a reaction cup of a homogenizer, and adjusting the rotating speed to 1000 r/min. 5g of sulfuric acid with a mass fraction of 98% and 20g of distilled water were weighed and added to a reaction system under stirring in order that particle sedimentation occurred.
Comparative example 2
Taking water glass as a raw material, putting 50g of the water glass in a reaction cup of a homogenizer, and adjusting the rotating speed to 2000 r/min. 3g of 98% sulfuric acid and 20g of distilled water were weighed and added to a reaction system under stirring in this order, and no gel was formed.
Weighing 30g of phenolic resin with powdery alcohol-soluble phenolic resin as a raw material, adding 30g of alcohol, placing the phenolic resin in a magnetic stirrer at 70 ℃, stirring and dissolving at 800r/min, placing the dissolved solution in a reaction cup of a homogenizer, adjusting the rotating speed to 2000r/min, weighing 10g of sulfuric acid with the mass fraction of 98% and 40g of distilled water, sequentially adding the sulfuric acid and the distilled water into a stirring reaction system, placing the sol obtained by reaction in a 60 ℃ drying oven, heating for 5 hours, and then standing for 12 hours, wherein the sol cannot be formed.
In conclusion, when the stirring speed in S2 was not more than 1000 rpm and the viscosity in S3 was less than 30 mPas, the gel could not be formed normally.
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 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.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. A preparation method of a high-strength gel material is characterized by comprising the following steps: the method specifically comprises the following steps:
s1, dissolving the thermosetting resin in a solution with certain concentration and viscosity;
s2, stirring uniformly, and slowly dripping a curing agent solution with a certain concentration;
s3, the viscosity of the whole system can be maintained at a certain level by controlling the adding speed;
s4, stopping stirring when the content of the solvent in the final system reaches the expected concentration;
s5, standing the prepared sol at a certain temperature, so that the curing agent and the resin further react to finally form the high-strength thermosetting resin gel material.
2. The method of claim 1, wherein the gel material is selected from the group consisting of: the thermosetting resin in the step S1 mainly contains unsaturated polyester resin, epoxy resin, phenol resin, melamine formaldehyde resin, furan resin, acrylic resin, polyamide resin, polyurethane, polybutadiene resin, silicone resin, rosin, pitch, and camphor. The solvent containing phenolic resin is selected from acetone, ethanol, benzene, toluene, ethyl acetate, solvent gasoline, cyclohexane, vegetable oil, etc.; the solvent of the melamine formaldehyde resin is selected from dilute acid; the organic silicon resin solvent is selected from ethanol, butanol, ethyl acetate, benzene, toluene, cyclohexanone, etc.; the solvent of furan resin is selected from organic solvents such as ester and ketone; the solvent of the epoxy resin is selected from benzene, toluene, xylene, ethanol, ethylene glycol, acetone, butanol, methyl ethyl ketone, cyclohexanone, ether alcohol, ethyl acetate and the like; the solvent of the polybutadiene resin is selected from water and the like; the solvent of the acrylic resin is selected from methanol, ethanol, ethylene glycol, isopropanol, dioxane, benzene, toluene, xylene, acetone, methyl ethyl ketone, cyclohexanone, butyl acetate, dichloroethane, ethyl acetate, chloroform, dichloroethane, glacial acetic acid, dioxanone, tetrahydrofuran, etc.; the solvent of the polyamide resin is selected from formic acid, concentrated sulfuric acid, dimethylformamide, m-cresol, phenol, ethanol/benzene mixed solvent and the like; the solvent of polyurethane is selected from methyl ethyl ketone, cyclohexanone, dimethylformamide, tetrahydrofuran, ethyl acetate, dioxane, etc.; the solvent of rosin is selected from ethanol, diethyl ether, acetone, benzene, toluene, carbon disulfide, dichloroethane, turpentine and alkali solution; the solvent of the asphalt is selected from benzene, toluene, xylene, carbon tetrachloride and chloroform; the solvent of Camphora is selected from ethanol, diethyl ether, acetone, chloroform, glacial acetic acid, benzene, etc.
3. The method of claim 1, wherein the gel material is selected from the group consisting of: the stirring speed in the step S2 is at least 1000 rpm.
4. The method of claim 1, wherein the gel material is selected from the group consisting of: the viscosity of the thermosetting resin solution in the step S3 is at least 30 mpa · S.
5. The method of claim 1, wherein the gel material is selected from the group consisting of: the standing time of the resin in the step S5 is 4-48 h.
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| CN202011410028.4A CN112538175A (en) | 2020-12-03 | 2020-12-03 | Preparation method of high-strength gel material |
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| CN202011410028.4A CN112538175A (en) | 2020-12-03 | 2020-12-03 | Preparation method of high-strength gel material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113604117A (en) * | 2021-06-23 | 2021-11-05 | 杭州日耀涂料有限公司 | Preparation method of thermosetting resin |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1347599A (en) * | 1971-06-22 | 1974-02-27 | Matsushita Electric Ind Co Ltd | Method of making resin encapsulated electrical coil |
| CN108212032A (en) * | 2018-01-18 | 2018-06-29 | 航天特种材料及工艺技术研究所 | A kind of shape memory aerogel material and preparation method thereof |
| CN110218294A (en) * | 2019-06-24 | 2019-09-10 | 哈尔滨工业大学 | A kind of degradable imine based epoxy resin curing agent and its preparation method and application |
-
2020
- 2020-12-03 CN CN202011410028.4A patent/CN112538175A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1347599A (en) * | 1971-06-22 | 1974-02-27 | Matsushita Electric Ind Co Ltd | Method of making resin encapsulated electrical coil |
| CN108212032A (en) * | 2018-01-18 | 2018-06-29 | 航天特种材料及工艺技术研究所 | A kind of shape memory aerogel material and preparation method thereof |
| CN110218294A (en) * | 2019-06-24 | 2019-09-10 | 哈尔滨工业大学 | A kind of degradable imine based epoxy resin curing agent and its preparation method and application |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113604117A (en) * | 2021-06-23 | 2021-11-05 | 杭州日耀涂料有限公司 | Preparation method of thermosetting resin |
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Application publication date: 20210323 |