CN114408932B - Method for preparing silica-based aerogel balls with controllable particle size by continuous liquid phase polymerization - Google Patents
Method for preparing silica-based aerogel balls with controllable particle size by continuous liquid phase polymerization Download PDFInfo
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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. Silicon source, aldehyde, silane coupling agent and organic and inorganic solvent are taken as reaction solution, added into alkaline coagulating bath, and silica-based wet gel spheres are prepared by a continuous liquid phase polymerization method and a sol-gel method, and the silica-based aerogel spheres with controllable particle size are obtained by solvent replacement and drying treatment. The method has the advantages of simple working procedures, easily obtained raw materials, controllable particle size of the obtained aerogel balls, 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 and purification and adsorption function 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 balls with controllable particle sizes by continuous liquid phase polymerization.
Background
Aerogel is a nano porous material with a three-dimensional nano network structure, has the structural characteristics of low density, high specific surface area, high porosity and the like, and endows the material with excellent heat insulation, adsorption, catalysis, medicine carrying and other functions, so that the aerogel is widely applied to aerospace military industry, building heat insulation, transportation and the likeThe fields of daily heat preservation, environmental purification and the like. At present SiO 2 Although the aerogel has been industrialized, commercialized and engineering applied, the aerogel still has the international problems to be solved urgently, such as high cost, poor mechanical properties (such as large brittleness, fragility, powder and slag falling, etc.), low use temperature, and the engineering application and wide popularization of the aerogel, which is a key energy-saving and environment-friendly new material, are greatly limited. And SiO 2 Aerogel products are mainly in the form of blocks, powder, felt and the like, and are difficult to be applied in engineering in the adsorption field. On the one hand, the powder sample is difficult to recycle, secondary pollution can be caused, and if granulation can have great influence on the performance; on the other hand, the inside of samples such as large-size blocks and felts are difficult to contact with the adsorbent, so that waste or poor adsorption kinetics performance is caused. The silica-based aerogel balls are used as a novel aerogel product form, show special size and shape characteristics, make up the application limitation of other forms of aerogel, and provide possibility for the engineering application of the aerogel in heat insulation, heat preservation and purification and adsorption functional filler. Patent application number CN202011488745.9 discloses a preparation method of graphene aerogel balls capable of being continuously produced in large scale, but does not relate to the category of silica-based aerogel balls. Patent application number CN202010651923.9 discloses a ball-drop method for preparing spherical SiO 2 The method of aerogel material adopts water glass as silicon source, and adopts ball drop method to prepare spherical SiO 2 Aerogel materials, however, the ball drop method has the defects of complex process, time consumption and labor consumption, and difficult quantitative production, and is difficult to realize industrialization truly.
Disclosure of Invention
To improve the existing SiO 2 The invention provides a method for preparing silica-based aerogel balls with controllable particle sizes by continuous liquid phase polymerization, which is characterized by the defects of continuous mass production, uncontrollable particle sizes of the balls and the like. The silica-based aerogel balls are prepared by adopting a continuous liquid phase polymerization method, have the characteristics of high sphericity, extremely low density, large specific surface area, low heat conductivity and the like, have controllable pore structure and surface chemical structure, have typical application in heat insulation, heat preservation and purification and adsorption functional fillers, and make up for the traditional SiO 2 Air coagulationThe rubber ball has the defects of the synthetic process and the practical engineering application.
The technical scheme of the invention is as follows: a method for preparing silica-based aerogel balls with controllable particle size by continuous liquid phase polymerization comprises the following specific steps:
(1) Preparation of the 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 a prepolymerization reaction to obtain a silica-based reaction solution with 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 pH value of 8-12;
(3) Continuous liquid phase polymerization for preparing wet gel ball
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 heat for a certain time, separating and filtering, and washing with deionized water to obtain silica-based wet gel spheres;
(4) Aging and drying
And (3) replacing the silica-based wet gel spheres obtained in the step (3) with an organic solvent and drying to obtain silica-based aerogel spheres with controllable particle sizes.
Preferably, the silicon source in the step (1) is one of methyltrimethoxysilane, methyltriethoxysilane, trimethylmethoxysilane or dimethyldimethoxysilane; the aldehyde is one of formaldehyde, phthalic aldehyde, isophthalaldehyde, terephthalaldehyde 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 ultrasound, hydrothermal or microwave; the temperature of the 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 the 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, 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).
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 conditions for washing with 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 an average particle diameter of 50-3000 um, 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/cm 3 Apparent density of 0.05-0.08 g/cm 3 Specific surface area of 84-620 m 2 Per gram, the contact angle of water is 120-150 degrees, and the thermal conductivity is 0.022-0.037 W.m -1 ·K -1 。
The beneficial effects are that:
the method for preparing the silica-based aerogel balls with controllable particle size by continuous liquid phase polymerization has the following characteristics:
(1) The process is simple, the raw materials are easy to obtain, and the continuous liquid phase polymerization can truly realize continuous mass production.
(2) Compared with the bulk and powdery silicon-based aerogel materials, the silicon oxide-based aerogel balls overcome the problems of poor mechanical property, powder and slag falling, difficult recovery and the like of the traditional silicon-based aerogel materials, have the characteristics of good use, easy use, convenient recovery and the like, and show special size and shape characteristics as a novel aerogel product form.
(3) The silica-based aerogel balls prepared by the invention have controllable particle size and superhigh specific surface area, and can be used in heat insulation, heat preservation and purification adsorption functional fillers.
Drawings
FIG. 1 is a sample graph of silica-based aerogel spheres produced 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 produced in example 1.
Detailed Description
Example 1
At room temperature, 0.1mol of methyltrimethoxysilane, 0.1mol of phthalic aldehyde and 0.2mol of silane coupling agent KH550 are dissolved in 16mol of methanol, after being uniformly mixed, 8mol of acetic acid aqueous solution with the concentration of 1mmol/L is added, stirring is continued, ultrasound is carried out for 60min at 50 ℃, and the pre-polymerization reaction is carried out, thus obtaining the silicon oxide-based reaction solution with the pH 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 the coagulating bath at 70 ℃ and 10000rpm, preserving the heat for 30min at 70 ℃, separating and filtering, and washing with deionized water at 60 ℃ for 8min to obtain the silica-based wet gel spheres. And (3) replacing with methanol and spray-drying to obtain the silica-based aerogel balls with controllable particle sizes. Silica aerogel spheres having an average particle diameter of 50. Mu.m, an average sphericity of 0.99, a porosity of 95%, a pore diameter of 20nm and a bulk density of 0.01g/cm 3 Apparent density of 0.05g/cm 3 Specific surface area 620m 2 Water contact angle of 150 deg. and thermal conductivity of 0.022 W.m -1 ·K -1 Can be used as a filler for heat-insulating foaming plates of external walls of houses.
FIG. 1 is a sample graph of silica-based aerogel spheres produced in example 1. From the figure, it is clear that the sample is white spherical particles, the particle size distribution is uniform, the structure is uniform, and the sphericity is good.
FIG. 2 is an infrared spectrum of silica-based aerogel spheres prepared in example 1. 1023 and 787cm -1 The strong absorption peaks at the positions are respectively antisymmetric stretching vibration and symmetrical stretching vibration of Si-O-Si, which show that the preparationThe prepared sample contains a large number of Si-O-Si bonds, that is, the main component of the prepared sample is silicon oxide; 2973 and 1070cm -1 The peak at the site is Si-CH 3 The characteristic absorption peak of (2) shows that the hydrophobic functional group methyl in methyltrimethoxysilane is still connected with silicon atoms after the reaction is completed, so that the aerogel ball has excellent hydrophobicity.
FIG. 3 is a graph showing the particle size distribution of silica-based aerogel spheres produced in example 1. The measurement result of the laser particle sizer shows that: the particle size distribution of the prepared silica-based aerogel balls is uniform and concentrated, and the average particle size is 50um.
Example 2
At room temperature, 0.2mol of methyltriethoxysilane, 0.4mol of isophthalaldehyde and 0.2mol of silane coupling agent KH560 are dissolved in 16mol of ethanol, after being uniformly mixed, 8mol of oxalic acid aqueous solution with the concentration of 2mmol/L is added, stirring is continued, ultrasonic treatment is carried out for 50min at the temperature of 60 ℃, and a pre-polymerization reaction is carried out, so that a silicon oxide-based reaction solution with the pH of 4 is obtained. 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 the coagulating bath at 80 ℃ and a rotating speed of 100rpm, preserving the heat for 20min at 80 ℃, separating and filtering, and washing with deionized water at 70 ℃ for 6min to obtain the silica-based wet gel spheres. And (3) replacing by normal hexane and drying at normal pressure to obtain the silica-based aerogel balls with controllable particle size. Silica aerogel spheres having an average particle diameter of 3000um, an average sphericity of 0.87, a porosity of 85%, a pore diameter of 50nm and a bulk density of 0.03g/cm 3 Apparent density of 0.08g/cm 3 Specific surface area 84m 2 Water contact angle of 120 DEG, thermal conductivity of 0.037 W.m -1 ·K -1 Can be used as PM2.5 smoke purification and adsorption functional filler.
Example 3
1mol of trimethylmethoxysilane, 5mol of terephthalaldehyde and 5mol of silane coupling agent KH570 are dissolved in 20mol of isopropanol at room temperature, 10mol of carbonic acid water solution with the concentration of 5mmol/L is added to continuously stir after uniform mixing, hydrothermal reaction is carried out for 10min at the temperature of 100 ℃, and the silicon oxide-based reaction solution with the pH of 6 is obtained. 30ml of NaOH solution was dispersed at 90 ℃In 180ml of corn oil, the mixture was homogenized to give a coagulation bath with a pH of 12. Mixing the reaction solution with the coagulating bath at 80 ℃ and 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 spheres. And (3) ethanol replacement and vacuum drying are carried out to obtain the silica-based aerogel balls with controllable particle sizes. Silica aerogel spheres having an average particle diameter of 2000. Mu.m, an average sphericity of 0.90, a porosity of 90%, a pore diameter of 35nm and a bulk density of 0.028g/cm 3 Apparent density of 0.074g/cm 3 Specific surface area 247m 2 Water contact angle 136 DEG, thermal conductivity 0.032 W.m -1 ·K -1 Can be used as a filler with water treatment, purification and adsorption functions.
Example 4
At room temperature, 0.5mol of dimethyl dimethoxy silane, 5mol of formaldehyde and 5mol of silane coupling agent KH791 are dissolved in 60mol of acetonitrile, after being uniformly mixed, 30mol of phosphoric acid aqueous solution with the concentration of 8mmol/L is added, stirring is continued, and the mixture is subjected to microwave for 20min at 80 ℃ to perform a prepolymerization reaction, so that a silica-based reaction solution with the pH of 4 is obtained. 40ml of KOH solution was dispersed in 320ml of soybean oil at 60℃and mixed uniformly to give a coagulation bath having a pH of 12. Mixing the reaction solution with the coagulating bath at 70 ℃ and 2000rpm, preserving 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 spheres. And performing acetonitrile replacement and supercritical drying to obtain the silica-based aerogel balls with controllable particle sizes. Silica-based aerogel spheres having an average particle diameter of 1000. Mu.m, an average sphericity of 0.92, a porosity of 92%, a pore diameter of 34nm and a bulk density of 0.022g/cm 3 Apparent density of 0.062g/cm 3 Specific surface area 287m 2 Water contact angle 134 deg. and thermal conductivity 0.026W.m -1 ·K -1 Can be used as an atmospheric purification and adsorption functional filler.
Example 5
Dissolving 0.5mol of methyltriethoxysilane, 4mol of glutaraldehyde and 3mol of silane coupling agent KH550 in 100mol of ethanol at room temperature, adding 50mol of boric acid aqueous solution with the concentration of 10mmol/L, continuously stirring, performing hydrothermal reaction at 100 ℃ for 10min, and performing prepolymerization reactionA silica-based reaction solution having a pH of 5 was obtained. 50ml of ammonia water was dispersed in 500ml of olive oil at 40℃and mixed uniformly to obtain a coagulation bath having a pH of 10. Mixing the reaction solution with the coagulating bath at 90 ℃ under the high-speed shearing dispersion condition with the rotating speed of 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 spheres. And (3) performing acetone replacement and supercritical drying to obtain the silica-based aerogel balls with controllable particle sizes. Silica-based aerogel spheres having an average particle diameter of 500. Mu.m, an average sphericity of 0.96, a porosity of 98%, a pore diameter of 25nm and a bulk density of 0.017g/cm 3 Apparent density of 0.052g/cm 3 Specific surface area 433m 2 Water contact angle 142 deg. and thermal conductivity 0.023 W.m -1 ·K -1 The foaming material can be used for the heat-insulating foaming plate filler of petroleum pipelines.
Claims (6)
1. A method for preparing silica-based aerogel balls with controllable particle size by continuous liquid phase polymerization comprises the following specific steps:
(1) Preparation of the 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 a prepolymerization reaction to obtain a silica-based reaction solution with pH of 4-6; wherein the temperature of the pretreatment is 50-100 ℃; the pretreatment time is 10-60 min;
(2) Coagulation bath preparation
Dispersing the alkaline solution in oil at 25-90 ℃ and uniformly mixing to obtain a coagulating bath with pH value of 8-12; wherein the alkaline solution is one of ammonia water, 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);
(3) Continuous liquid phase polymerization for preparing wet gel ball
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 heat for a certain time, separating and filtering, and washing with deionized water to obtain silica-based wet gel spheres;
(4) Aging and drying
And (3) replacing the silica-based wet gel spheres obtained in the step (3) with an organic solvent and drying to obtain silica-based aerogel spheres with controllable particle sizes.
2. The method of claim 1, wherein the silicon source in step (1) is one of methyltrimethoxysilane, methyltriethoxysilane, trimethylmethoxysilane, or dimethyldimethoxysilane; the aldehyde is one of formaldehyde, phthalic aldehyde, isophthalaldehyde, terephthalaldehyde 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.
3. The method according to claim 1, wherein the molar ratio of the silicon source, aldehyde, silane coupling agent, solvent, aqueous acetic acid solution in step (1) is 1: (1-10): (1-10): (20-200): (10-100).
4. The method according to claim 1, wherein the stirring rate in the step (3) is 100 to 10000rpm; the heat preservation time is 5-30 min, and the heat preservation temperature is 70-90 ℃; the conditions for washing with deionized water are as follows: the water temperature is 60-80 ℃, and the washing time is 1-10 min.
5. The method according to claim 1, wherein the organic solvent in 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.
6. The method according to claim 1, wherein the silica-based aerogel balls obtained in the step (4) have an average particle diameter of 50 to 3000. Mu.m, an average sphericity of 0.87 to 0.99, a porosity of 85 to 98%, a pore diameter of 20 to 50nm, and a bulk density of 0.01 to 0.03g/cm 3 Apparent density of 0.05-0.08 g/cm 3 Specific surface area of 84-620 m 2 Per gram, the contact angle of water is 120-150 degrees, and the thermal conductivity is 0.022-0.037 W.m -1 ·K -1 。
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