CN114408932A - Method for preparing silica-based aerogel balls with controllable particle size by continuous liquid phase polymerization - Google Patents
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Abstract
The invention relates to a method for preparing silica-based aerogel balls with controllable particle sizes by continuous liquid phase polymerization. Adding a silicon source, aldehyde, a silane coupling agent and an organic inorganic solvent serving as reaction solutions into an alkaline coagulating bath, preparing a silica-based wet gel ball by a continuous liquid phase polymerization method and a sol-gel method, and performing solvent replacement and drying treatment to obtain the silica-based aerogel ball with controllable particle size. The method has the advantages of simple process, easily obtained raw materials, controllable diameter of the obtained aerogel spherulites, excellent performance and capability of realizing continuous large-scale industrial production. The prepared silica-based aerogel balls have typical application in heat insulation, heat preservation, purification and adsorption functional fillers.
Description
Technical Field
The invention belongs to the field of preparation of new materials, and relates to a method for preparing silica-based aerogel spheres with controllable particle sizes by continuous liquid phase polymerization.
Background
The aerogel is a nano porous material with a three-dimensional nano net structure, has the structural characteristics of low density, high specific surface area, high porosity and the like, and has excellent functions of heat insulation, adsorption, catalysis, drug loading and the like, so that the aerogel is widely applied to the fields of aerospace military industry, building heat insulation, traffic transportation, daily heat preservation, environmental purification and the like. At present, SiO2Although the aerogel has already been industrialized, commercialized and engineering application, the aerogel still has international problems to be solved, such as high cost, poor mechanical properties (specifically, high brittleness, fragility, powder falling, slag falling and the like), low use temperature and the like, and the engineering application and the wide popularization of the key energy-saving environment-friendly new material, namely the aerogel, are greatly limited. And SiO2The aerogel product form is mainly block, powder, felt and the like, and is difficult to be applied in the engineering of the adsorption field. On one hand, a powder sample is difficult to recover, secondary pollution is caused, and if granulation is carried out, performance is greatly influenced; on the other hand, the interior of samples such as large-size blocks, felts and the like is difficult to contact with the adsorbent, so that waste is caused or the adsorption dynamic performance is poor. The silica-based aerogel ball shows special size and shape characteristics as a new aerogel product form, makes up for the application limit of aerogels in other forms, and provides possibility for engineering application of the aerogel in heat insulation and purification adsorption functional fillers. Patent No. CN202011488745.9 discloses a preparation method of graphene aerogel spheres capable of continuous mass production, but does not relate to the category of silica-based aerogel spheres. The patent with the application number of CN202010651923.9 discloses a method for preparing spherical SiO by a ball drop method2The method for preparing aerogel material adopts water glass as silicon source and prepares spherical SiO by a ball drop method2Aerogel materials, but the ball drop method has the defects of complex process, time and labor consumption, is difficult to quantitatively produce and is difficult to truly realize industrialization.
Disclosure of Invention
In order to improve the prior SiO2The invention provides a method for preparing aerogel balls with controllable particle size by continuous liquid phase polymerization, which has the defects of continuous large-scale production, uncontrollable particle size and the likeThe silica-based aerogel spheres of (1). The silica-based aerogel ball is prepared by adopting a continuous liquid phase polymerization method, has the characteristics of high sphericity, extremely low density, large specific surface area, low thermal conductivity and the like, has a controllable pore structure and surface chemical structure, has typical application in heat insulation and preservation and purification adsorption functional fillers, and makes up for the traditional SiO2The aerogel balls have the defects in synthesis process and practical engineering application.
The technical scheme of the invention comprises the following steps: a method for preparing silica-based aerogel spheres with controllable particle sizes by continuous liquid phase polymerization comprises the following specific steps:
(1) preparation of reaction solution
Dissolving a silicon source, aldehyde and a silane coupling agent in an organic solvent, uniformly mixing, adding an acid solution, continuously stirring, pretreating for a period of time at a certain temperature, and carrying out prepolymerization reaction to obtain a silicon oxide-based reaction solution with the pH of 4-6;
(2) coagulation bath preparation
Dispersing the alkaline solution in oil at 25-90 ℃, and uniformly mixing to obtain a coagulating bath with the pH of 8-12;
(3) preparation of wet gel ball by continuous liquid phase polymerization
Mixing the reaction solution in the step (1) with the coagulating bath in the step (2) at a certain stirring rate at 70-90 ℃, preserving the temperature for a certain time, separating and filtering, and washing with deionized water to obtain silica-based wet gel balls;
(4) aging and drying
And (4) replacing and drying the silica-based wet gel ball obtained in the step (3) by using an organic solvent to obtain the silica-based aerogel ball with controllable particle size.
Preferably, the silicon source in step (1) is one of methyltrimethoxysilane, methyltriethoxysilane, trimethylmethoxysilane or dimethyldimethoxysilane; the aldehyde is one of formaldehyde, o-phthalaldehyde, m-phthalaldehyde, p-phthalaldehyde or glutaraldehyde; the silane coupling agent is one of a silane coupling agent KH550, a silane coupling agent KH560, a silane coupling agent KH570 or a silane coupling agent KH 791; the organic solvent is one of methanol, ethanol, isopropanol or acetonitrile; the acid solution is one of acetic acid aqueous solution, oxalic acid aqueous solution, carbonic acid aqueous solution, phosphoric acid aqueous solution or boric acid aqueous solution; the concentration of the acid solution is 1-10 mmol/L; the pretreatment mode is one of ultrasonic, hydrothermal or microwave; the temperature of pretreatment is 50-100 ℃; the pretreatment time is 10-60 min.
Preferably, the molar ratio of the silicon source, the aldehyde, the silane coupling agent, the solvent and the aqueous acetic acid solution in step (1) is 1: (1-10): (1-10): (20-200): (10-100).
Preferably, the alkaline solution in the step (2) is one of ammonia water, a urea solution, a NaOH solution or a KOH solution; the oil is one of methyl silicone oil, water-soluble silicone oil, corn oil, soybean oil or olive oil; the volume ratio of the alkaline solution to the oil is 1: (5-12).
Preferably, the stirring speed in the step (3) is 100-10000 rpm; the heat preservation time is 5-30 min, and the heat preservation temperature is 70-90 ℃; the washing conditions of the deionized water are as follows: the water temperature is 60-80 ℃, and the washing time is 1-10 min.
Preferably, the organic solvent in the step (4) is one of methanol, ethanol, acetonitrile, n-hexane or acetone; the drying mode is one of spray drying, normal pressure drying, vacuum drying or supercritical drying.
Preferably, the silica-based aerogel balls prepared in the step (4) have the average particle size of 50-3000 um, the average sphericity of 0.87-0.99, the porosity of 85-98%, the pore diameter of 20-50 nm and the bulk density of 0.01-0.03 g/cm3The apparent density is 0.05-0.08 g/cm3A specific surface area of 84 to 620m2A water contact angle of 120 to 150 DEG, a thermal conductivity of 0.022 to 0.037 W.m-1·K-1。
Has the advantages that:
the invention relates to a method for preparing silica-based aerogel balls with controllable particle size by continuous liquid phase polymerization, which has the following characteristics:
(1) the process is simple, the raw materials are easy to obtain, and continuous liquid phase polymerization can really realize continuous large-scale production.
(2) Compared with block-shaped and powdery silicon-based aerogel materials, the silicon oxide-based aerogel balls overcome the problems of poor mechanical property, powder falling, slag falling, difficulty in recycling and the like of the traditional silicon-based aerogel materials, have the characteristics of good use, easiness in use, convenience in recycling and the like, and show special size and shape characteristics as a new aerogel product form.
(3) The silica-based aerogel ball prepared by the invention has controllable particle size and ultrahigh specific surface area, and can be used in fillers with heat insulation, heat preservation, purification and adsorption functions.
Drawings
FIG. 1 is a sample graph of silica-based aerogel spheres made in example 1.
FIG. 2 is an infrared spectrum of silica-based aerogel spheres prepared in example 1.
FIG. 3 is a graph showing the particle size distribution of silica-based aerogel spheres obtained in example 1.
Detailed Description
Example 1
At room temperature, 0.1mol of methyltrimethoxysilane, 0.1mol of o-phthalaldehyde and 0.2mol of silane coupling agent KH550 are dissolved in 16mol of methanol, after uniform mixing, 8mol of acetic acid aqueous solution with the concentration of 1mmol/L is added for continuous stirring, and the mixture is subjected to ultrasonic treatment at 50 ℃ for 60min for prepolymerization reaction to obtain a silicon oxide-based reaction solution with the pH value of 5. 10ml of urea solution was dispersed in 120ml of aqueous silicone oil at 50 ℃ and mixed uniformly to obtain a coagulation bath having a pH of 8. Mixing the reaction solution with a coagulating bath at 70 ℃ and the rotation speed of 10000rpm, preserving the temperature for 30min at 70 ℃, separating and filtering, and washing with deionized water at 60 ℃ for 8min to obtain the silica-based wet gel ball. And performing methanol replacement and spray drying to obtain the silica-based aerogel balls with controllable particle size. The average particle diameter of silica-based aerogel spheres is 50um, the average sphericity is 0.99, the porosity is 95 percent, the pore diameter is 20nm, and the bulk density is 0.01g/cm3Apparent density of 0.05g/cm3Specific surface area 620m2G, water contact angle of 150 degrees, thermal conductivity of 0.022 W.m-1·K-1It can be used as the heat-insulating foaming board filler of the outer wall of the house.
FIG. 1 is a sample graph of silica-based aerogel spheres made in example 1. It is clear from the figure that the sample is white spherical particles, uniform in particle size distribution, uniform in structure and good in sphericity.
FIG. 2 is an infrared spectrum of silica-based aerogel spheres prepared in example 1. 1023 and 787cm-1The strong absorption peaks are antisymmetric stretching vibration and symmetric stretching vibration of Si-O-Si respectively, which shows that the prepared sample contains a large amount of Si-O-Si bonds, namely the main component of the prepared sample is silicon oxide; 2973 and 1070cm-1Has a peak of Si-CH3The characteristic absorption peak shows that the hydrophobic functional group methyl in the methyltrimethoxysilane is still connected with the silicon atom after the reaction is finished, so that the aerogel ball has excellent hydrophobicity.
FIG. 3 is a graph showing the particle size distribution of silica-based aerogel spheres obtained in example 1. The measurement results of the laser particle size analyzer show that: the prepared silica-based aerogel balls are uniform and concentrated in particle size distribution, and the average particle size of the silica-based aerogel balls is 50 microns.
Example 2
At room temperature, 0.2mol of methyl triethoxysilane, 0.4mol of isophthalaldehyde and 0.2mol of silane coupling agent KH560 are dissolved in 16mol of ethanol, uniformly mixed, added with 8mol of oxalic acid aqueous solution with the concentration of 2mmol/L and continuously stirred, and subjected to ultrasonic treatment at 60 ℃ for 50min to perform prepolymerization reaction, so as to obtain a silica-based reaction solution with the pH value of 4. 10ml of ammonia water was dispersed in 100ml of methyl silicone oil at 25 ℃ and mixed uniformly to obtain a coagulation bath having a pH of 10. Mixing the reaction solution with a coagulating bath at 80 ℃ and the rotating speed of 100rpm, preserving the heat for 20min at 80 ℃, separating and filtering, and washing for 6min by deionized water at 70 ℃ to obtain the silica-based wet gel ball. And (3) replacing by normal hexane and drying at normal pressure to obtain the silica-based aerogel balls with controllable particle size. The average particle diameter of silica-based aerogel spheres is 3000um, the average sphericity is 0.87, the porosity is 85 percent, the pore diameter is 50nm, and the bulk density is 0.03g/cm3Apparent density of 0.08g/cm3Specific surface area 84m2G, water contact angle of 120 degrees, thermal conductivity of 0.037 W.m-1·K-1And can be used as PM2.5 flue gas purification adsorption functional filler.
Example 3
At room temperature, dissolving 1mol of trimethylmethoxysilane, 5mol of terephthalaldehyde and 5mol of a silane coupling agent KH570 in 20mol of isopropanol, uniformly mixing, adding 10mol of a 5mmol/L carbonic acid water solution, continuously stirring, carrying out hydrothermal reaction at 100 ℃ for 10min, and carrying out prepolymerization reaction to obtain a silicon oxide-based reaction solution with the pH value of 6. 30ml of NaOH solution was dispersed in 180ml of corn oil at 90 ℃ and mixed well to obtain a coagulation bath with pH 12. Mixing the reaction solution with a coagulating bath at 80 ℃ and the rotation speed of 1000rpm, preserving the heat at 80 ℃ for 10min, separating and filtering, and washing with deionized water at 70 ℃ for 6min to obtain the silica-based wet gel ball. And performing ethanol replacement and vacuum drying to obtain the silica-based aerogel balls with controllable particle size. The average particle diameter of the silica-based aerogel spheres is 2000um, the average sphericity is 0.90, the porosity is 90 percent, the pore diameter is 35nm, and the bulk density is 0.028g/cm3Apparent density of 0.074g/cm3Specific surface area 247m2G, water contact angle 136 DEG, thermal conductivity 0.032 W.m-1·K-1It can be used as water treatment purifying adsorption function filler.
Example 4
At room temperature, 0.5mol of dimethyl dimethoxysilane, 5mol of formaldehyde and 5mol of silane coupling agent KH791 are dissolved in 60mol of acetonitrile, mixed uniformly, added with 30mol of phosphoric acid aqueous solution with the concentration of 8mmol/L and stirred continuously, and subjected to a prepolymerization reaction at 80 ℃ for 20min to obtain a silicon oxide-based reaction solution with the pH value of 4. 40ml of KOH solution was dispersed in 320ml of soybean oil at 60 ℃ and mixed well to obtain a coagulation bath having a pH of 12. Mixing the reaction solution with a coagulating bath at 70 ℃ and 2000rpm, keeping the temperature at 70 ℃ for 15min, separating and filtering, and washing with deionized water at 60 ℃ for 10min to obtain the silica-based wet gel ball. And performing acetonitrile replacement and supercritical drying to obtain the silica-based aerogel balls with controllable particle size. The average particle diameter of the silica-based aerogel spheres is 1000um, the average sphericity is 0.92, the porosity is 92 percent, the pore diameter is 34nm, and the bulk density is 0.022g/cm3Apparent density of 0.062g/cm3Specific surface area 287m2G, water contact angle of 134 degrees, and heat conductivity of 0.026 W.m-1·K-1Can be used for purifying atmosphereAnd (4) adsorbing functional filler.
Example 5
At room temperature, 0.5mol of methyltriethoxysilane, 4mol of glutaraldehyde and 3mol of silane coupling agent KH550 are dissolved in 100mol of ethanol, after uniform mixing, 50mol of boric acid aqueous solution with the concentration of 10mmol/L is added for continuous stirring, and the mixture is subjected to a prepolymerization reaction at 100 ℃ for 10min to obtain a silica-based reaction solution with the pH value of 5. 50ml of ammonia water was dispersed in 500ml of olive oil at 40 ℃ and mixed well to obtain a coagulation bath having a pH of 10. Mixing the reaction solution with a coagulating bath at 90 ℃ under the high-speed shearing dispersion condition that the rotating speed is 6000rpm, preserving the heat for 5min at 90 ℃, separating and filtering, and washing for 1min by deionized water at 80 ℃ to obtain the silica-based wet gel ball. And performing acetone replacement and supercritical drying to obtain the silica-based aerogel spheres with controllable particle size. The average grain diameter of the silica-based aerogel spheres is 500um, the average sphericity is 0.96, the porosity is 98 percent, the pore diameter is 25nm, and the bulk density is 0.017g/cm3Apparent density of 0.052g/cm3Specific surface area 433m2G, water contact angle of 142 DEG, thermal conductivity of 0.023 W.m-1·K-1And can be used as the filler of the heat-insulating foaming plate of the petroleum pipeline.
Claims (7)
1. A method for preparing silica-based aerogel spheres with controllable particle sizes by continuous liquid phase polymerization comprises the following specific steps:
(1) preparation of reaction solution
Dissolving a silicon source, aldehyde and a silane coupling agent in an organic solvent, uniformly mixing, adding an acid solution, continuously stirring, pretreating for a period of time at a certain temperature, and carrying out prepolymerization reaction to obtain a silicon oxide-based reaction solution with the pH of 4-6;
(2) coagulation bath preparation
Dispersing the alkaline solution in oil at 25-90 ℃, and uniformly mixing to obtain a coagulating bath with the pH of 8-12;
(3) preparation of wet gel ball by continuous liquid phase polymerization
Mixing the reaction solution in the step (1) with the coagulating bath in the step (2) at a certain stirring rate at 70-90 ℃, preserving the temperature for a certain time, separating and filtering, and washing with deionized water to obtain silica-based wet gel balls;
(4) aging and drying
And (4) replacing and drying the silica-based wet gel ball obtained in the step (3) by using an organic solvent to obtain the silica-based aerogel ball with controllable particle size.
2. The method according to claim 1, wherein the silicon source in step (1) is one of methyltrimethoxysilane, methyltriethoxysilane, trimethylmethoxysilane or dimethyldimethoxysilane; the aldehyde is one of formaldehyde, o-phthalaldehyde, m-phthalaldehyde, p-phthalaldehyde or glutaraldehyde; the silane coupling agent is one of a silane coupling agent KH550, a silane coupling agent KH560, a silane coupling agent KH570 or a silane coupling agent KH 791; the organic solvent is one of methanol, ethanol, isopropanol or acetonitrile; the acid solution is one of acetic acid aqueous solution, oxalic acid aqueous solution, carbonic acid aqueous solution, phosphoric acid aqueous solution or boric acid aqueous solution; the concentration of the acid solution is 1-10 mmol/L; the pretreatment mode is one of ultrasonic, hydrothermal or microwave; the temperature of pretreatment is 50-100 ℃; the pretreatment time is 10-60 min.
3. The method according to claim 1, wherein the molar ratio of the silicon source, the aldehyde, the silane coupling agent, the solvent and the aqueous acetic acid solution in step (1) is 1: (1-10): (1-10): (20-200): (10-100).
4. The method of claim 1, wherein the alkaline solution in step (2) is one of ammonia, urea solution, NaOH solution or KOH solution; the oil is one of methyl silicone oil, water-soluble silicone oil, corn oil, soybean oil or olive oil; the volume ratio of the alkaline solution to the oil is 1: (5-12).
5. The method according to claim 1, wherein the stirring rate in the step (3) is 100 to 10000 rpm; the heat preservation time is 5-30 min, and the heat preservation temperature is 70-90 ℃; the washing conditions of the deionized water are as follows: the water temperature is 60-80 ℃, and the washing time is 1-10 min.
6. The method according to claim 1, wherein the organic solvent in the step (4) is one of methanol, ethanol, acetonitrile, n-hexane or acetone; the drying mode is one of spray drying, normal pressure drying, vacuum drying or supercritical drying.
7. The method according to claim 1, wherein the silica-based aerogel balls prepared in step (4) have an average particle size of 50-3000 μm, an average sphericity of 0.87-0.99, a porosity of 85-98%, a pore diameter of 20-50 nm, and a bulk density of 0.01-0.03 g/cm3The apparent density is 0.05-0.08 g/cm3A specific surface area of 84 to 620m2A water contact angle of 120 to 150 DEG, a thermal conductivity of 0.022 to 0.037 W.m-1·K-1。
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