CN113150365B - Preparation of melamine aerogel and fiber type clay reinforced melamine composite aerogel by normal pressure drying method - Google Patents
Preparation of melamine aerogel and fiber type clay reinforced melamine composite aerogel by normal pressure drying method Download PDFInfo
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- CN113150365B CN113150365B CN202110581923.0A CN202110581923A CN113150365B CN 113150365 B CN113150365 B CN 113150365B CN 202110581923 A CN202110581923 A CN 202110581923A CN 113150365 B CN113150365 B CN 113150365B
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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
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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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
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
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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
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/05—Elimination by evaporation or heat degradation of a liquid phase
- C08J2201/0502—Elimination by evaporation or heat degradation of a liquid phase the liquid phase being organic
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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
- C08J2361/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08J2361/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08J2361/28—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with melamine
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/10—Silicon-containing compounds
Abstract
The invention belongs to the technical field of material manufacturing, and discloses a method for preparing melamine composite aerogel and fiber type clay reinforced melamine composite aerogel by a normal pressure drying method. The invention takes melamine resin as a main material, prepares melamine gel and fiber type clay composite reinforced melamine gel through solvent heat treatment under the acidic condition, and washes away a catalyst through an alcohol reagent to dry the melamine composite aerogel with complete blocks and good mechanical properties at normal pressure; the fiber type clay is adopted to reinforce the melamine composite aerogel, and the clay can form a double-network structure in a melamine gel network to obtain the aerogel with better mechanical property. The material can be carbonized to obtain self-supporting carbon aerogel, and can be used as catalyst loading, adsorption, energy storage, heat insulation and flame retardant materials and other fields. The invention has short gel time, adopts a normal pressure drying method as a drying process, does not use a large amount of organic solvent for solvent replacement, has simple preparation process and short preparation period, and can meet the requirement of large-scale production.
Description
Technical Field
The invention relates to the technical field of aerogel, in particular to a method for preparing melamine aerogel and fiber type clay reinforced melamine composite aerogel by a normal pressure drying method.
Background
Aerogel materials, also known as "solidified smoke," are light nanoporous solid materials that are formed by the interpolymerization of particles having two nanoscale levels to form a three-dimensional pore network structure, and that are filled with gaseous dispersion media in the network framework. Organic aerogels are a class of porous materials composed of high polymer molecules with a unique nanoporous and continuous three-dimensional network structure. The organic aerogel has wide application prospect in the fields of catalysts, carriers, high-efficiency heat insulation and the like. However, the high-porosity three-dimensional network structure of the organic aerogel causes low strength and high brittleness, and the adopted drying mode is usually a supercritical drying process which is expensive. The low strength and toughness of the pure organic aerogel and the inability to prepare large blocks by drying under normal pressure are the biggest bottlenecks that limit large-scale popularization and application.
The fiber clay is a one-dimensional nanometer natural silicate mineral (such as halloysite, sepiolite and attapulgite). Because the fiber type clay has a unique three-dimensional structure, the colloidal property is one of the main characteristics of the fiber type clay, and the fiber type clay can be dispersed in an alcohol solution with lower concentration to form a 'hackle type' rack-mounted reticular structure. The fiber type clay is very suitable for being used as a framework support of the organogel to prepare the composite gel with good mechanical property. Therefore, research and development of a preparation method of the organic/inorganic composite aerogel, which is feasible, simple in preparation process and high in mechanical strength of the product, has very important significance for industrial production of the product.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the problems in the prior art, the invention provides a method for preparing melamine aerogel and fiber type clay reinforced melamine composite aerogel by using a normal pressure drying method, and the material can be carbonized to obtain self-supporting carbon aerogel and can be used as catalyst loading, adsorption, energy storage, heat insulation and flame retardant materials and other fields. The invention has short gel time, adopts a normal pressure drying method as a drying process, does not use a large amount of organic solvent for solvent replacement, has simple preparation process and short preparation period, and can meet the requirement of large-scale production.
The technical scheme is as follows: the invention provides a preparation method of melamine aerogel, which comprises the following steps: s1: adding melamine into an alcohol solution, stirring and dissolving, adding an acid catalyst, and stirring uniformly at room temperature to obtain melamine sol; s2: putting the melamine sol into a hydrothermal reaction kettle, and carrying out gel aging on the melamine sol at 80-160 ℃ for 6-24 h to obtain melamine gel; soaking the obtained melamine gel in an alcohol solution at 30-60 ℃, and washing off an acid catalyst; s3: and finally, drying the melamine gel obtained in the S2 in an oven at the normal pressure of 30-60 ℃ to obtain the melamine aerogel.
Preferably, in S1, the mass ratio of melamine to alcoholic solution is 0.1-0.5:3-10. Wherein the purity of the alcoholic solution is more than 99%.
Preferably, the alcohol solution is ethanol or isopropanol.
Preferably, the acid catalyst is hydrochloric acid, sulfuric acid or nitric acid.
The invention also provides a preparation method of the fiber type clay reinforced melamine composite aerogel, which comprises the following steps: s1: dispersing fiber type clay in an alcohol solution to prepare fiber type clay-alcohol slurry; s2: uniformly mixing the fiber clay-alcohol slurry and melamine, adding an acid catalyst, and uniformly stirring at room temperature to obtain a composite slurry; s3: putting the composite slurry into a hydrothermal reaction kettle, and performing gel aging at 80-160 ℃ for 6-24 h to obtain fiber type clay enhanced melamine gel; soaking the obtained fiber type clay-enhanced melamine gel in an alcohol solution at 30-60 ℃, and washing off an acid catalyst; s4: and finally, drying the fiber type clay-reinforced melamine gel obtained in the step S2 in an oven at the normal pressure of 30-60 ℃ to obtain the fiber type clay-reinforced melamine composite aerogel.
Preferably, in S2, the mass ratio of the melamine, the fibrous clay and the alcohol solution in the composite slurry is 0.1-0.5:0.06-0.7:3-10.
Preferably, the alcohol solution in S1 and S2 is both ethanol or isopropanol.
Preferably, the fibrous clay is halloysite, sepiolite or attapulgite.
Preferably, the acid catalyst is hydrochloric acid, sulfuric acid or nitric acid.
Has the beneficial effects that:
the invention takes melamine as a main material, prepares melamine gel through alcoholic solution heat treatment under the acidic condition, and washes away a catalyst through an alcohol reagent to dry the melamine aerogel with complete blocks and good mechanical properties.
The invention takes melamine resin as a main material to prepare fiber type clay reinforced melamine gel through solvent heat treatment under an acidic condition, and the unreacted catalyst is washed away by alcohol reagent, so that the fiber type clay reinforced melamine composite aerogel with complete blocks and good mechanical property can be dried. The fiber type clay reinforced melamine composite aerogel is adopted, and the clay can form a double-network structure in a melamine gel network to obtain the aerogel with better mechanical property.
Because the mechanical property of common carbon aerogel is poor, when the carbon aerogel is applied to an electrode material, the aerogel needs to be ground into powder, and then the electrode material is prepared by using a binder, and the binder is non-conductive, so that the property of the carbon aerogel is influenced. And the melamine aerogel and the compound aerogel of fibre type clay reinforcing melamine that this application was prepared can be carbonized into self-supporting carbon aerogel, because in the compound aerogel of attapulgite melamine gel, the fibrous bar form attapulgite is as the skeleton support of compound aerogel, forms two gel structures with the melamine granule, effectively improves the fragility of pure melamine aerogel. Compared with the prior art, the preparation method has the advantages that no adhesive is needed when the preparation method is applied to electrode materials, the preparation method has potential advantages in the fields of electrochemistry, catalysis and the like, and the preparation method can be used in the fields of catalyst loading, adsorption, energy storage, heat insulation and flame retardant materials and the like.
The invention has short gel time, adopts a normal pressure drying method as a drying process, does not use a large amount of organic solvent for solvent replacement, has simple preparation process and short preparation period, and can meet the requirement of large-scale production.
Drawings
Fig. 1 is a microscopic view of a melamine aerogel;
FIG. 2 is a microscopic view of a fibrous clay-reinforced melamine composite aerogel;
fig. 3 is a nitrogen adsorption and desorption curve of melamine aerogel and fiber type clay-reinforced melamine composite aerogel;
fig. 4 is a pore size distribution diagram of melamine aerogel and fiber type clay-reinforced melamine composite aerogel.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings.
Embodiment 1:
the embodiment provides a preparation method of melamine aerogel, which specifically comprises the following steps: 0.3g of melamine is added into 5mL ethanol, stirred and dissolved, then 0.2mL hydrochloric acid is added, and the mixture is stirred at a constant speed for 3 min at room temperature to obtain melamine sol. And (3) carrying out gel aging on the melamine sol in a hydrothermal reaction kettle for 20h at the temperature of 100 ℃ to obtain melamine gel. Soaking the obtained melamine gel in ethanol at 50 ℃, washing off unreacted hydrochloric acid in the melamine gel, and finally, carrying out normal pressure drying on the melamine gel in a baking oven at the temperature of 50 ℃ to obtain the melamine aerogel.
Embodiment 2:
the embodiment provides a preparation method of melamine aerogel, which specifically comprises the following steps: 0.3g of melamine is added into 6.0mL of isopropanol and stirred for dissolution, then 0.2mL hydrochloric acid is added and stirred at room temperature for 3 min at a constant speed to obtain melamine sol. And (3) carrying out gel aging on the melamine sol in a hydrothermal reaction kettle for 20h at the temperature of 80 ℃ to obtain melamine gel. Soaking the obtained melamine gel in isopropanol at 60 ℃, washing off unreacted hydrochloric acid in the melamine gel, and finally drying the melamine gel at normal pressure at the temperature of 60 ℃ in an oven to obtain the melamine aerogel.
Embodiment 3:
the embodiment provides a preparation method of melamine aerogel, which specifically comprises the following steps: 0.2g of melamine is added into 6.0mL isopropanol and stirred for dissolution, then 0.2mL of hydrochloric acid is added and stirred at room temperature for 3 min at a constant speed to obtain melamine sol. And (3) gel aging the melamine sol in a hydrothermal reaction kettle at 160 ℃ for 8 h to obtain melamine gel. Soaking the obtained melamine gel in ethanol at 50 ℃, washing off unreacted hydrochloric acid in the melamine gel, and finally drying the melamine gel at normal pressure at the temperature of 45 ℃ in an oven to obtain the melamine aerogel.
Embodiment 4:
this embodiment provides a preparation method of compound aerogel of fibre type clay reinforcing melamine, specifically is: 0.15g of halloysite was uniformly dispersed in 5ml of isopropanol to prepare a 3wt% fibrous clay-isopropanol slurry. 0.3g of melamine is added into 5mL and the fiber clay-isopropanol slurry is mixed evenly, then 0.2mL hydrochloric acid is added into the mixture and the mixture is stirred at room temperature for 3 min at a constant speed to obtain the composite slurry. And gel aging the composite slurry in a hydrothermal reaction kettle at 100 ℃ for 20 h. Soaking the obtained fiber type clay-enhanced melamine gel in isopropanol at 50 ℃, washing off unreacted hydrochloric acid, and finally drying the fiber type clay-enhanced melamine gel in a drying oven at 50 ℃ under normal pressure to obtain the fiber type clay-enhanced melamine composite aerogel.
Embodiment 5:
this embodiment provides a preparation method of a fiber type clay-reinforced melamine composite aerogel, specifically comprising: 0.18 g sepiolite was uniformly dispersed in 6 ml isopropanol to prepare a 3wt% fibrous clay-isopropanol slurry. 0.3g of melamine is added into 6.0mL and the fiber clay-isopropanol slurry is mixed evenly, then 0.2mL hydrochloric acid is added into the mixture and the mixture is stirred at a constant speed for 3 min at room temperature to obtain the composite slurry. The composite slurry is subjected to gel aging in a hydrothermal reaction kettle at 80 ℃ for 10 h. Soaking the obtained fiber type clay-enhanced melamine gel in ethanol at 60 ℃, washing off unreacted hydrochloric acid, and finally drying the fiber type clay-enhanced melamine gel in a drying oven at 40 ℃ normal pressure to obtain the fiber type clay-enhanced melamine composite aerogel.
Embodiment 6:
this embodiment provides a preparation method of a fiber type clay-reinforced melamine composite aerogel, specifically comprising: 0.24 g attapulgite is evenly dispersed in 6 ml ethanol to prepare 4wt% fiber type clay-ethanol slurry. 0.2g of melamine is added into 6.0mL and the fiber clay-ethanol slurry is mixed evenly, then 0.2mL hydrochloric acid is added into the mixture and the mixture is stirred at room temperature for 3 min at a constant speed to obtain the composite slurry. The composite slurry is subjected to gel aging of 8 h in a hydrothermal reaction kettle at 160 ℃. Soaking the obtained fiber type clay-enhanced melamine gel in ethanol at 50 ℃, washing off unreacted hydrochloric acid, and finally drying the fiber type clay-enhanced melamine gel in a drying oven at the normal pressure of 45 ℃ to obtain the fiber type clay-enhanced melamine composite aerogel.
The micro-morphology, nitrogen adsorption and desorption capacity and pore size distribution of the melamine aerogel obtained in embodiments 1 to 3 and the fiber type clay-reinforced melamine composite aerogel obtained in embodiments 4 to 6 were respectively tested, and the micro-morphology results are shown in fig. 1 and 2, the nitrogen adsorption and desorption curves are shown in fig. 3, and the pore size distribution is shown in fig. 4.
Fig. 1 and 2 show the micro-topography of the melamine aerogel and the fiber-type clay-reinforced melamine composite aerogel in embodiments 1 and 4
Fig. 3 shows nitrogen adsorption and desorption curves of the melamine aerogel and the fiber type clay-reinforced melamine composite aerogel according to the embodiments 2 and 5.
Fig. 4 shows the pore size distribution diagrams of the melamine aerogel and the fiber-type clay-reinforced melamine composite aerogel according to embodiments 3 and 6.
The above embodiments are merely illustrative of the technical concepts and features of the present invention, and the purpose of the embodiments is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (4)
1. The preparation method of the fiber type clay reinforced melamine composite aerogel is characterized by comprising the following steps:
s1: dispersing fiber type clay in an alcohol solution to prepare fiber type clay-alcohol slurry;
s2: uniformly mixing the fiber clay-alcohol slurry and melamine, adding an acid catalyst, and uniformly stirring at room temperature to obtain a composite slurry; in the composite slurry, the mass ratio of the melamine to the fibrous clay to the alcoholic solution is 0.1-0.5:0.06-0.7:3-10;
s3: putting the composite slurry into a hydrothermal reaction kettle, and performing gel aging at 80-160 ℃ for 6-24 h to obtain fiber type clay enhanced melamine gel; soaking the obtained fiber type clay-enhanced melamine gel in an alcohol solution at 30-60 ℃, and washing off an acid catalyst;
s4: and finally, drying the fiber type clay-reinforced melamine gel obtained in the step S2 in an oven at the normal pressure of 30-60 ℃ to obtain the fiber type clay-reinforced melamine composite aerogel capable of being carbonized into the self-supporting carbon aerogel.
2. The method for preparing the fiber type clay-reinforced melamine composite aerogel according to claim 1, wherein the alcohol solution in S1 and S2 is ethanol or isopropanol.
3. The preparation method of the fiber type clay-reinforced melamine composite aerogel according to claim 1 or 2, wherein the fiber type clay is halloysite, sepiolite or attapulgite.
4. The method for preparing the fiber type clay-reinforced melamine composite aerogel according to claim 1 or 2, wherein the acid catalyst is hydrochloric acid, sulfuric acid or nitric acid.
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