CN107266942A - A kind of enhanced aerogel powder and preparation method thereof - Google Patents

A kind of enhanced aerogel powder and preparation method thereof Download PDF

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CN107266942A
CN107266942A CN201610214815.9A CN201610214815A CN107266942A CN 107266942 A CN107266942 A CN 107266942A CN 201610214815 A CN201610214815 A CN 201610214815A CN 107266942 A CN107266942 A CN 107266942A
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aerogel powder
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resin
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CN107266942B (en
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卢锋
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NANJING WEICAI NEW ENERGY TECHNOLOGY Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28Compounds of silicon
    • C09C1/30Silicic acid
    • C09C1/3045Treatment with inorganic compounds
    • C09C1/3054Coating
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28Compounds of silicon
    • C09C1/30Silicic acid
    • C09C1/3072Treatment with macro-molecular organic compounds
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28Compounds of silicon
    • C09C1/30Silicic acid
    • C09C1/309Combinations of treatments provided for in groups C09C1/3009 - C09C1/3081
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    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/10Treatment with macromolecular organic compounds

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Abstract

The present invention discloses a kind of enhanced aerogel powder and preparation method thereof, it is characterised in that the enhanced aerogel powder is made up of aerogel powder and covering material.A kind of preparation method for enhanced aerogel powder that the present invention is provided, comprises the following steps:(1)Aerogel powder is modified;(2)Coat the preparation of slurry;(3)Cladding;(4)Solidification.The features such as a kind of enhanced aerogel powder that the present invention is provided and preparation method thereof has low cost, high efficiency, continuous production, aerogel powder is on the premise of the original excellent specific property of aeroge is retained, have the advantages that mechanical property is good, with huge application prospect.

Description

A kind of enhanced aerogel powder and preparation method thereof
Technical field
The present invention relates to the process for modifying surface field of inorganic nano porous material, more particularly to a kind of enhanced aerogel powder and preparation method thereof, belong to lightweight, insulation, fire prevention, sound insulation, explosion-proof, damping energy-absorbing material field.
Background technology
Aeroge is a kind of light-weight inorganic solid material with three-dimensional network skeleton structure and nanoscale hole hole, with high porosity, specific surface area, extremely low density and solid content, chemical inertness and noninflammability, the characteristics such as excellent lightweight, thermal insulation, fire prevention, sound insulation, damping energy-absorbing are shown, thermal conductivity factor can as little as below 0.015W/mK.
The composite with performances such as lightweight, thermal insulation, sound insulations can be made as Material claddings such as lightweight functional stuffing and concrete, resins in aerogel powder.However, the special architectural feature of aeroge causes the mechanical properties such as its fold resistance, compression strength relatively low, with easily being crushed in other materials recombination process;Further, since aeroge surface has a large amount of nanoscale hole holes, siphonage easily occurs when being contacted with solvent, so as to destroy aeroge nano-pore structure, causes its excellent specific property to be lost.
The content of the invention
It is an object of the invention to provide a kind of enhanced aerogel powder and preparation method thereof.
A kind of enhanced aerogel powder, is made up of aerogel powder and covering material.
In one of the embodiments, the covering material is aqueous adhesive.
In one of the embodiments, the aqueous adhesive is the one or more in organic adhesion agent, inorganic adhesive;The organic adhesion agent is the one or more in rosin resin, alkyd resin, acrylic resin, polyurethane resin, organic siliconresin, fluorocarbon resin, polyvinyl resin, polystyrene resin, Corvic, acrylic resin, acrylonitrile-butadiene-styrene resin etc.;The inorganic adhesive is the one or more in cement, gypsum, lime stone, waterglass, cupric oxide-phosphoric acid glue etc..
A kind of preparation method of enhanced aerogel powder of the present invention, comprises the following steps:
(1)Aerogel powder is modified;
(2)The preparation of aeroge composite mortar;
(3)Aeroge composite mortar is flowed continuously on ultrasonic atomization head so that aeroge composite mortar is dispersed into the atomization mass of aerogel powder Surface coating aqueous adhesive;
(4)Curing process.
In one of the embodiments, the step(1)Including hydrophobically modified step;The hydrophobically modified step is to carry out hydrophobically modified to aerogel powder in closed hydrophobic modifier gaseous environment;The hydrophobic modifier be trim,ethylchlorosilane, HMDS, HMDO, MTMS, MTES, dimethyldimethoxysil,ne, dimethyldiethoxysilane, γ-aminopropyltrimethoxysilane, gamma-aminopropyl-triethoxy-silane, γ-(The oxygen of 2,3- epoxies third)Propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, N-(β-aminoethyl)One or more in-gamma-aminopropyl-triethoxy-silane.
In one of the embodiments, the step(1)Also include surface hydrophilic modification step;The surface hydrophilic modification step is that hydrophobic aerogel powder surface is modified using surface hydrophilic modification solution;The surface hydrophilic modification solution is surfactant and the aqueous solution or the aqueous solution of low surface tension solvent of low surface tension solvent;The surfactant is the one or more in anionic surfactant, cationic surface active agent, amphoteric surfactant, nonionic surface active agent;The anionic surfactant is the one or more in fatty alcohol phosphates, aliphatic alcohol polyoxyvinethene phosphate salt, alkyl sulfate, fatty alcohol polyoxyethylene ether sulfate, fatty acid glyceride sulfate, sulphation ricinoleate, cycloalkanes sulfate, fatty acid amide alkyl sulfate, alkylbenzenesulfonate, alkylsulfonate, fatty acid methyl ester ethoxylate sulfonate, MES, aliphatic alcohol polyethenoxy ether carboxylate;The cationic surface active agent is aliphatic ammonium salt;The amphoteric surfactant is the one or more in alkyl amino acid, carboxylic acid group's glycine betaine, sulfobetaines, phosphate glycine betaine, alkyl hydroxy amine oxide;The nonionic surface active agent is the one or more in aliphatic polyester, APES, high-carbon fatty alcohol polyoxyethylene ether, polyoxyethylene carboxylate, fatty acid methyl ester ethoxylate, the oxireme addition product of polypropylene glycol, sorbitan ester, sucrose fatty ester, alkyl esteramides;The low surface tension solvent is one or more mixtures in acetone, n-hexane, pentane, normal heptane, ethanol, isopropanol, the tert-butyl alcohol, propane diols, glycerine.
In one of the embodiments, in the surface hydrophilic modification step, in addition to additional physical field action step;The additional physical field action step is one kind in far infrared radiation, stirring, ultrasonication, ball milling.
In one of the embodiments, the step(1)Also include drying process step;The drying process step is one kind in far-infrared ray drying, spray drying, microwave drying, constant pressure and dry, supercritical drying, subcritical drying, freeze-drying.
In one of the embodiments, the preparation of the aeroge composite mortar is by step(1)Modified aerogel powder, aqueous adhesive and water mixing, stirring.
In one of the embodiments, the curing process is the one or more in Heated by Far-Infrared Radiation, microwave heating, ultraviolet radiation, natural curing, steam curing, steam press maintenance.
Inner hydrophobic, the architectural feature of surface hydrophilic is presented in above-mentioned enhanced aerogel powder, can be on the premise of the original excellent specific property of aeroge be retained, have the advantages that high mechanical properties, particle diameter are uniform for micron order, particle diameter distribution, the fields such as coating, adhesive, insulating materials, concrete can be used for as functional stuffing;The present invention can realize it is continuous, stably, efficient industrial production.
Embodiment
In order to facilitate the understanding of the purposes, features and advantages of the present invention, the embodiment below to the present invention is described in detail.Many details are elaborated in the following description to fully understand the present invention.But the invention can be embodied in many other ways as described herein, those skilled in the art can make similar improvements without departing from the spirit of the invention, therefore the present invention is not limited to the specific embodiments disclosed below.
A kind of embodiment of the enhanced aerogel powder of the present invention, is made up of aerogel powder and covering material.
In this way, aerogel powder will not be destroyed with other materials compound tense nano-porous structure by water equal solvent, and other materials can tile on aerogel powder surface, be aerogel powder and the compound offer precondition of other materials.
In the present embodiment, the covering material is aqueous adhesive.
So, the mechanical properties such as bending strength, the compression strength of aqueous adhesive are far above aeroge, the mechanical property of aerogel powder can be significantly improved on the premise of aeroge excellent properties are retained in aerogel powder Surface coating binder materials, expand the engineer applied of aerogel powder.
In the present embodiment, the aqueous adhesive is the one or more in organic adhesion agent, inorganic adhesive;The organic adhesion agent is the one or more in rosin resin, alkyd resin, acrylic resin, polyurethane resin, organic siliconresin, fluorocarbon resin, polyvinyl resin, polystyrene resin, Corvic, acrylic resin, acrylonitrile-butadiene-styrene resin etc.;The inorganic adhesive is the one or more in cement, gypsum, lime stone, waterglass, cupric oxide-phosphoric acid glue etc..
So, different aqueous adhesives has different mechanical property and different maintenances, curing process, generally compared with organic adhesion agent, the mechanical property of inorganic adhesive is higher, but maintenance, curing process complexity, cycle are long, the present invention according to needed for aerogel powder mechanical property and subsequently with the physical and chemical performance needed for other materials compound tense aerogel powder surface, select suitable aqueous adhesive or a variety of aqueous adhesives compounding cladding aerogel powder.
A kind of preparation method of enhanced aerogel powder, comprises the following steps:
(1)Aerogel powder is modified;
(2)The preparation of aeroge composite mortar;
(3)Aeroge composite mortar is flowed continuously on ultrasonic atomization head so that aeroge composite mortar is dispersed into the atomization mass of aerogel powder Surface coating aqueous adhesive;
(4)Curing process.
In addition, atomising head surfacing can have hydrophobic property.
So, utilize ultrasonic atomization technique and the hydrophobic technology of ultrasonic atomization head surface, aeroge composite mortar is flowed continuously on ultrasonic atomization head, using the hole explosion effect between composite mortar and air and ultrasonic atomization head surface hydrophobic property, the composite mortar around hole is ground into the atomization mass of micron-sized aeroge Surface coating aqueous adhesive;The enhanced aerogel powder of the architectural feature with inner hydrophobic, surface hydrophilic and Surface coating aqueous adhesive is made by above-mentioned steps by the present invention, the Material claddings such as functional stuffing and concrete, adhesive can be used as on the premise of nano-porous structure is not destroyed.
In the present embodiment, the step(1)Including hydrophobically modified step;The hydrophobically modified step is to carry out hydrophobically modified to aerogel powder in closed hydrophobic modifier gaseous environment;The hydrophobic modifier be trim,ethylchlorosilane, HMDS, HMDO, MTMS, MTES, dimethyldimethoxysil,ne, dimethyldiethoxysilane, γ-aminopropyltrimethoxysilane, gamma-aminopropyl-triethoxy-silane, γ-(The oxygen of 2,3- epoxies third)Propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, N-(β-aminoethyl)One or more in-gamma-aminopropyl-triethoxy-silane.
So, because in existing aeroge preparation method, precursor, displacement solvent and drying process have significant effect to the hydrophobicity of aeroge, if the surface of aeroge and the contact angle of water are more than 90 °, hydrophobically modified can not be carried out in advance, directly carry out surface hydrophilic modification;If the surface of aeroge and the contact angle of water are less than 90 °, need to carry out hydrophobically modified in advance;Hydrophobically modified is carried out to aerogel powder in closed hydrophobic modifier gaseous environment, modified effect except significantly improving aerogel powder, ensure that inside nano-porous structure is not destroyed outer during follow-up hydrophilic modifying, also significantly improves modification efficiency and production efficiency, reduces production cost.
In the present embodiment, the step(1)Also include surface hydrophilic modification step;The surface hydrophilic modification step is that hydrophobic aerogel powder surface is modified using surface hydrophilic modification solution;The surface hydrophilic modification solution is surfactant and the aqueous solution or the aqueous solution of low surface tension solvent of low surface tension solvent;The surfactant is the one or more in anionic surfactant, cationic surface active agent, amphoteric surfactant, nonionic surface active agent;The anionic surfactant is the one or more in fatty alcohol phosphates, aliphatic alcohol polyoxyvinethene phosphate salt, alkyl sulfate, fatty alcohol polyoxyethylene ether sulfate, fatty acid glyceride sulfate, sulphation ricinoleate, cycloalkanes sulfate, fatty acid amide alkyl sulfate, alkylbenzenesulfonate, alkylsulfonate, fatty acid methyl ester ethoxylate sulfonate, MES, aliphatic alcohol polyethenoxy ether carboxylate;The cationic surface active agent is aliphatic ammonium salt;The amphoteric surfactant is the one or more in alkyl amino acid, carboxylic acid group's glycine betaine, sulfobetaines, phosphate glycine betaine, alkyl hydroxy amine oxide;The nonionic surface active agent is the one or more in aliphatic polyester, APES, high-carbon fatty alcohol polyoxyethylene ether, polyoxyethylene carboxylate, fatty acid methyl ester ethoxylate, the oxireme addition product of polypropylene glycol, sorbitan ester, sucrose fatty ester, alkyl esteramides;The low surface tension solvent is the one or more in acetone, n-hexane, pentane, normal heptane, ethanol, isopropanol, the tert-butyl alcohol, propane diols, glycerine.
So, using the aqueous solution of the aqueous solution or low surface tension solvent of surfactant and low surface tension solvent, in hydrophilic modifying processing procedure is carried out to hydrophobic aerogel powder surface there is surface to cooperate with hydrophilic modifying effect, it is remarkably improved wetting spreading rate of the surface hydrophilic modification solution on aerogel powder surface, significantly slow simultaneously to the wetting extension inside aerogel powder, by the consumption for regulating and controlling modified solution, the regulation and control to aerogel powder surface hydrophilic thickness degree can accurately be realized, low surface tension solvent not only with water and surfactant there is surface to cooperate with hydrophilic modifying effect, and the capillary force into the hydrophilic modifying solution in the nano-pore of aerogel powder top layer can be greatly reduced, it is easy to that the hydrophilic modifying solution in the nano-pore of aerogel powder top layer is evaporated by drying process, without destroying its nano-porous structure, inner hydrophobic is presented in the aerogel powder of the present invention, surface hydrophilic, surface hydrophilic layer still retains the architectural feature that nano-porous structure and surface hydrophilic thickness degree are 0.1 ~ 100 μm, there is good interface cohesion between binder materials;The technique has the features such as step is simple, the cycle is short, production efficiency is high, it is adaptable to industrialized production.
In the present embodiment, in the surface hydrophilic modification step, in addition to additional physical field action step;The additional physical field action step is one kind in far infrared radiation, stirring, ultrasonication, ball milling.
In this way, additional physics field action can significantly improve the activity and the contact probability with aerogel powder of surface hydrophilic modification solution, dosage of surfactant is reduced, the surface hydrophilic modification speed of aerogel powder is improved, cost is reduced, production efficiency is improved.
In the present embodiment, the step(1)Also include drying process step;The drying process step is one kind in far-infrared ray drying, spray drying, microwave drying, constant pressure and dry, supercritical drying, subcritical drying, freeze-drying.
If in this way, aerogel powder and binder materials compound tense after hydrophilic modifying, the remaining hydrophilic modifying solution in top layer can influence interface cohesion, processing need to be pre-dried;Utilize above-mentioned drying process, on the premise of ensuring that aerogel powder top layer nano-pore structure is not destroyed, surface hydrophilic modification solution remaining in the nano-pore of aerogel powder top layer is evaporated, the interface bond strength between aerogel powder and binder materials is improved.
In the present embodiment, the preparation of the aeroge composite mortar is by step(1)Modified aerogel powder, aqueous adhesive and water mixing, stirring.
In this way, inner hydrophobic, the aerogel powder of surface hydrophilic are fully contacted into mixing with aqueous adhesive, good combination interface is formed in the liquid phase.
In the present embodiment, the curing process is the one or more in Heated by Far-Infrared Radiation, microwave heating, ultraviolet radiation, natural curing, steam curing, steam press maintenance.
So, it is ensured that the atomization mass of aeroge Surface coating aqueous adhesive completes solidification before collection vessel is fallen into, and further improves the mechanical property of aqueous adhesive clad.
Inner hydrophobic, the architectural feature of surface hydrophilic is presented in above-mentioned enhanced aerogel powder, can be on the premise of the original excellent specific property of aeroge be retained, have the advantages that high mechanical properties, particle diameter are uniform for micron order, particle diameter distribution, the fields such as coating, adhesive, insulating materials, concrete can be used for as functional stuffing;The present invention can realize it is continuous, stably, efficient industrial production.
It is specific embodiment part below.
Embodiment 1
Preparing inner hydrophobic, surface hydrophilic, Surface coating using following steps has the enhanced SiO of polyurethane film2Aerogel powder, polyurethane coating thickness is 8 ~ 10 μm:
(1)Pending SiO is detected using contact angle measurement2Aerogel powder surface and the contact angle of water, testing result are 55 °, are then 56 μm of SiO by particle diameter2Aerogel powder is positioned in vacuum furnace, the HMDS after weighing is positioned in vacuum furnace with container, heating and gasifying, and hydrophobically modified 1.5h obtains hydrophobic SiO2Aerogel powder, hydrophobic SiO is detected with contact angle measurement2Aerogel powder surface and the contact angle of water, testing result are 147 °;
(2)At room temperature, in mass ratio 1:1:100 weigh ethanol, n-hexane and deionized water, are well mixed, are configured to surface hydrophilic modification solution;
(3)By hydrophobic SiO2The volume ratio 1 of aerogel powder and surface hydrophilic modification solution:3, surface modification solution is weighed, and pour into corresponding container, step will be passed through(1)Hydrophobic SiO2Aerogel powder is mixed with surface hydrophilic modification solution, after ball-milling treatment 25min, takes out filtering;
(4)By step(3)Contain the SiO of hydrophilic modifying solution in obtained surface2Aerogel powder is positioned in far infrared drying stove, at a temperature of 120 DEG C, dries 0.5h, furnace cooling is to taking-up after less than 50 DEG C, to SiO2The cross section of aerogel powder is detected that testing result is shown, surface hydrophilic thickness degree is 7.9 μm;
(5)In mass ratio 1:30:100 weigh step(4)SiO2Aeroge, waterborne polyurethane resin and deionized water, stirring mixing, obtain SiO2Aeroge composite mortar;
(6)Setting ultrasonic frequency vibratory is 1GHz, opens valve so that SiO2Aeroge composite mortar flows to ultrasonic vibration table, to SiO2Aeroge composite mortar carries out atomization process, and in atomization mass dropping process, Heated by Far-Infrared Radiation is carried out to it for atomized body, solidifies, obtains enhanced SiO2Aerogel powder, polyurethane coating thickness is 8 ~ 10 μm.
Embodiment 2
Preparing inner hydrophobic, surface hydrophilic, Surface coating using following steps has the enhanced SiO of acrylate film2Aerogel powder, acrylic acid coating thickness is 8 ~ 12 μm:
(1)Pending SiO is detected using contact angle measurement2Aerogel powder surface and the contact angle of water, testing result are 45 °, then by SiO of the particle diameter for 0.1mm2Aerogel powder is positioned in vacuum furnace, the trim,ethylchlorosilane after weighing is positioned in vacuum furnace with container, heating and gasifying, and hydrophobically modified 1.5h obtains hydrophobic SiO2Aerogel powder, hydrophobic SiO is detected with contact angle measurement2Aerogel powder surface and the contact angle of water, testing result are 146 °;
(2)At room temperature, in mass ratio 1:1:100 weigh n-hexane, acetone and deionized water, are well mixed, are configured to surface hydrophilic modification solution;
(3)By hydrophobic SiO2The volume ratio 1 of aerogel powder and surface hydrophilic modification solution:3, surface modification solution is weighed, and pour into corresponding container, step will be passed through(1)Hydrophobic SiO2Aerogel powder is mixed with surface hydrophilic modification solution, after mechanical agitation 15min, and rotating speed is 2500 turns/min, filtering;
(4)By step(3)Contain the SiO of hydrophilic modifying solution in obtained surface2Aerogel powder is positioned in far infrared drying stove, at a temperature of 120 DEG C, dries 0.5h, furnace cooling is to taking-up after less than 50 DEG C, to SiO2The cross section of aerogel powder is detected that testing result is shown, surface hydrophilic thickness degree is 11.1 μm;
(5)In mass ratio 1:40:100 weigh step(4)SiO2Aeroge, water-based acrylic resin and deionized water, stirring mixing, obtain SiO2Aeroge composite mortar;
(6)Setting ultrasonic frequency vibratory is 2GHz, opens valve so that SiO2Aeroge composite mortar flows to ultrasonic vibration table, to SiO2Aeroge composite mortar carries out atomization process, and in atomization mass dropping process, Heated by Far-Infrared Radiation is carried out to it for atomized body, solidifies, obtains enhanced SiO2Aerogel powder, acrylic acid coating thickness is 8 ~ 12 μm.
Embodiment 3
Preparing inner hydrophobic, surface hydrophilic, Surface coating using following steps has the enhanced SiO of polyurethane film2Aerogel powder, polyurethane coating thickness is 7 ~ 11 μm:
(1)Pending SiO is detected using contact angle measurement2Aerogel powder surface and the contact angle of water, testing result are 45 °, are then 89 μm of SiO by particle diameter2Aerogel powder is positioned in vacuum furnace, the HMDS after weighing is positioned in vacuum furnace with container, heating and gasifying, and hydrophobically modified 1.5h obtains hydrophobic SiO2Aerogel powder, hydrophobic SiO is detected with contact angle measurement2Aerogel powder surface and the contact angle of water, testing result are 146 °;
(2)At room temperature, in mass ratio 1:0.8:120 weigh sodium alkyl benzene sulfonate, n-hexane and deionized water, are well mixed, are configured to surface hydrophilic modification solution;
(3)By hydrophobic SiO2The volume ratio 1 of aerogel powder and surface hydrophilic modification solution:3, surface modification solution is weighed, and pour into corresponding container, step will be passed through(1)Hydrophobic SiO2Aerogel powder is mixed with surface hydrophilic modification solution, after mechanical agitation 15min, and rotating speed is 2000 turns/min, filtering;
(4)By step(3)Contain the SiO of hydrophilic modifying solution in obtained surface2Aerogel powder is positioned in air dry oven, at a temperature of 120 DEG C, dries 0.5h, furnace cooling is to taking-up after less than 50 DEG C, to SiO2The cross section of aerogel powder is detected that testing result is shown, surface hydrophilic thickness degree is 6.0 μm;
(5)In mass ratio 1:30:100 weigh step(4)SiO2Aeroge, aqueous polyurethane UV solidified resins and deionized water, stirring mixing, obtain SiO2Aeroge composite mortar;
(6)Setting ultrasonic frequency vibratory is 1.2GHz, opens valve so that SiO2Aeroge composite mortar flows to ultrasonic vibration table, to SiO2Aeroge composite mortar carries out atomization process, and in atomization mass dropping process, treatment with UV radiation is carried out to it for atomized body, solidifies, obtains enhanced SiO2Aerogel powder, polyurethane coating thickness is 7 ~ 11 μm.
Embodiment 4
Preparing inner hydrophobic, surface hydrophilic, Surface coating using following steps has the enhanced SiO of epoxy resin thin film2Aerogel powder, epoxy resin coating thickness is 13 ~ 15 μm:
(1)Pending SiO is detected using contact angle measurement2Aerogel powder surface and the contact angle of water, testing result are 31 °, then by SiO of the particle diameter for 0.2mm2Aerogel powder is positioned in vacuum furnace, the trim,ethylchlorosilane after weighing is positioned in vacuum furnace with container, heating and gasifying, and hydrophobically modified 1.5h obtains hydrophobic SiO2Aerogel powder, hydrophobic SiO is detected with contact angle measurement2Aerogel powder surface and the contact angle of water, testing result are 150 °;
(2)At room temperature, in mass ratio 1:1:0.8:200 weigh sodium sulfate of polyethenoxy ether of fatty alcohol, sodium alkyl benzene sulfonate, isopropanol and deionized water, are well mixed, are configured to surface hydrophilic modification solution;
(3)By hydrophobic SiO2The volume ratio 1 of aerogel powder and surface hydrophilic modification solution:3, surface modification solution is weighed, and pour into corresponding container, step will be passed through(1)Hydrophobic SiO2Aerogel powder is mixed with surface hydrophilic modification solution, after mechanical agitation 15min, and rotating speed is 2500 turns/min, filtering;
(4)By step(3)Contain the SiO of hydrophilic modifying solution in obtained surface2Aerogel powder is positioned in far infrared drying stove, at a temperature of 120 DEG C, dries 0.5h, furnace cooling is to taking-up after less than 50 DEG C, to SiO2The cross section of aerogel powder is detected that testing result is shown, surface hydrophilic thickness degree is 11.1 μm;
(5)In mass ratio 1:30:100 weigh step(4)SiO2Aeroge, single-component water-based epoxy resin and deionized water, stirring mixing, obtain SiO2Aeroge composite mortar;
(6)Setting ultrasonic frequency vibratory is 3GHz, opens valve so that SiO2Aeroge composite mortar flows to ultrasonic vibration table, to SiO2Aeroge composite mortar carries out atomization process, and in atomization mass dropping process, far infrared radiation processing is carried out to it for atomized body, solidifies, obtains enhanced SiO2Aerogel powder, epoxy resin coating thickness is 13 ~ 15 μm.
Embodiment 5
Using following steps prepare inner hydrophobic, surface hydrophilic, Surface coating waterborne organic silicon resin film enhanced SiO2Aerogel powder, organic siliconresin coating thickness is 8 ~ 10 μm:
(1)The SiO that pending particle diameter is 77 μm is detected using contact angle measurement2Aerogel powder surface and the contact angle of water, testing result are 140 °, then the SiO2Aerogel powder has hydrophobicity;
(2)At room temperature, in mass ratio 1:0.6:150 weigh sldium lauryl sulfate, acetone and deionized water, are well mixed, are configured to surface hydrophilic modification solution;
(3)By hydrophobic SiO2The volume ratio 1 of aerogel powder and surface hydrophilic modification solution:3, surface modification solution is weighed, and pour into corresponding container, step will be passed through(1)Hydrophobic SiO2Aerogel powder is mixed with surface hydrophilic modification solution, after ball-milling treatment 25min, takes out filtering;
(4)By step(3)Contain the SiO of hydrophilic modifying solution in obtained surface2Aerogel powder is positioned in air dry oven, at a temperature of 120 DEG C, dries 0.5h, furnace cooling is to taking-up after less than 50 DEG C, to SiO2The cross section of aerogel powder is detected that testing result is shown, surface hydrophilic thickness degree is 6.9 μm;
(5)In mass ratio 1:35:100 weigh step(4)SiO2Aeroge, waterborne organic silicon resin and deionized water, stirring mixing, obtain SiO2Aeroge composite mortar;
(6)Setting ultrasonic frequency vibratory is 2GHz, opens valve so that SiO2Aeroge composite mortar flows to ultrasonic vibration table, to SiO2Aeroge composite mortar carries out atomization process, and in atomization mass dropping process, far infrared radiation processing is carried out to it for atomized body, solidifies, obtains enhanced SiO2Aerogel powder, organic siliconresin coating thickness is 8 ~ 10 μm.
Embodiment 6
Preparing inner hydrophobic, surface hydrophilic, Surface coating using following steps has the enhanced SiO of acrylate film2Aerogel powder, acrylic acid coating thickness is 9 ~ 12 μm:
(1)The SiO that pending particle diameter is 75 μm is detected using contact angle measurement2Aerogel powder surface and the contact angle of water, testing result are 141 °, then the SiO2Aerogel powder has hydrophobicity;
(2)At room temperature, in mass ratio 1:0.3:100 weigh NPE, n-hexane and deionized water, are well mixed, are configured to surface hydrophilic modification solution;
(3)By hydrophobic SiO2The volume ratio 1 of aerogel powder and surface hydrophilic modification solution:3, surface modification solution is weighed, and pour into corresponding container, step will be passed through(1)Hydrophobic SiO2Aerogel powder is mixed with surface hydrophilic modification solution, after ball milling 15min, takes out filtering;
(4)By step(3)Contain the SiO of hydrophilic modifying solution in obtained surface2Aerogel powder is positioned in far infrared drying stove, at a temperature of 120 DEG C, dries 0.5h, furnace cooling is to taking-up after less than 50 DEG C, to SiO2The cross section of aerogel powder is detected that testing result is shown, surface hydrophilic thickness degree is 11.1 μm;
(5)In mass ratio 1:40:100 weigh step(4)SiO2Aeroge, water-based acrylic resin and deionized water, stirring mixing, obtain SiO2Aeroge composite mortar;
(6)Setting ultrasonic frequency vibratory is 2GHz, opens valve so that SiO2Aeroge composite mortar flows to ultrasonic vibration table, to SiO2Aeroge composite mortar carries out atomization process, and in atomization mass dropping process, far infrared radiation processing is carried out to it for atomized body, solidifies, obtains enhanced SiO2Aerogel powder, acrylic acid coating thickness is 9 ~ 12 μm.
Embodiment 7
Using following steps prepare inner hydrophobic, surface hydrophilic, Surface coating epoxy resin thin film enhanced TiO2Aerogel powder, epoxy resin coating thickness is 13 ~ 15 μm:
(1)Pending TiO is detected using contact angle measurement2Aerogel powder surface and the contact angle of water, testing result are 145 °, then the TiO2Aerogel powder has hydrophobicity;
(2)At room temperature, in mass ratio 1:0.8:120 weigh sodium alkyl benzene sulfonate, n-hexane and deionized water, are well mixed, are configured to surface hydrophilic modification solution;
(3)By hydrophobic TiO2The volume ratio 1 of aerogel powder and surface hydrophilic modification solution:3, surface modification solution is weighed, and pour into corresponding container, step will be passed through(1)Hydrophobic TiO2Aerogel powder is mixed with surface hydrophilic modification solution, after mechanical agitation 15min, and rotating speed is 2000 turns/min, filtering;
(4)By step(3)Contain the TiO of hydrophilic modifying solution in obtained surface2Aerogel powder is positioned in air dry oven, at a temperature of 120 DEG C, dries 0.5h, furnace cooling is to taking-up after less than 50 DEG C, to TiO2The cross section of aerogel powder is detected that testing result is shown, surface hydrophilic thickness degree is 6.0 μm;
(5)In mass ratio 1:40:100 weigh step(4)TiO2Aeroge, aqueous epoxy resins and deionized water, stirring mixing, obtain TiO2Aeroge composite mortar;
(6)Setting ultrasonic frequency vibratory is 2GHz, opens valve so that TiO2Aeroge composite mortar flows to ultrasonic vibration table, to TiO2Aeroge composite mortar carries out atomization process, and in atomization mass dropping process, far infrared radiation processing is carried out to it for atomized body, solidifies, obtains enhanced TiO2Aerogel powder, epoxy resin coating thickness is 13 ~ 15 μm.
Embodiment 8
Preparing inner hydrophobic, surface hydrophilic, Surface coating using following steps has the enhanced SiO of acrylate film2Aerogel powder, acrylic acid coating thickness is 9 ~ 13 μm:
(1)The SiO that pending particle diameter is 0.3mm is detected using contact angle measurement2Aerogel powder surface and the contact angle of water, testing result are 148 °, then the SiO2Aerogel powder has hydrophobicity;
(2)At room temperature, in mass ratio 1:0.4:0.3:130 weigh AESA, n-hexane, ethanol and deionized water, are well mixed, are configured to surface hydrophilic modification solution;
(3)By hydrophobic SiO2The volume ratio 1 of aerogel powder and surface hydrophilic modification solution:3, surface modification solution is weighed, and pour into corresponding container, step will be passed through(1)Hydrophobic SiO2Aerogel powder is mixed with surface hydrophilic modification solution, after mechanical agitation 15min, and rotating speed is 2500 turns/min, filtering;
(4)By step(3)Contain the SiO of hydrophilic modifying solution in obtained surface2Aerogel powder is positioned in far infrared drying stove, at a temperature of 120 DEG C, dries 0.5h, furnace cooling is to taking-up after less than 50 DEG C, to SiO2The cross section of aerogel powder is detected that testing result is shown, surface hydrophilic thickness degree is 11.1 μm;
(5)In mass ratio 1:40:100 weigh step(4)SiO2Aeroge, water-based acrylic resin and deionized water, stirring mixing, obtain SiO2Aeroge composite mortar;
(6)Setting ultrasonic frequency vibratory is 2.5GHz, opens valve so that SiO2Aeroge composite mortar flows to ultrasonic vibration table, to SiO2Aeroge composite mortar carries out atomization process, and in atomization mass dropping process, microwave heating treatment is carried out to it for atomized body, solidifies, obtains enhanced SiO2Aerogel powder, acrylic acid coating thickness is 9 ~ 13 μm.
Above-described embodiment is the present invention preferably embodiment; but embodiments of the present invention are simultaneously not restricted to the described embodiments; other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, combine, simplification; equivalent substitute mode is should be, is included within protection scope of the present invention.

Claims (10)

1. a kind of enhanced aerogel powder, it is characterised in that the enhanced aerogel powder is made up of aerogel powder and covering material.
2. a kind of enhanced aerogel powder according to claim 1, it is characterised in that the covering material is aqueous adhesive.
3. a kind of enhanced aerogel powder according to claim 2, it is characterised in that the aqueous adhesive is the one or more in organic adhesion agent, inorganic adhesive;The organic adhesion agent is the one or more in rosin resin, alkyd resin, acrylic resin, polyurethane resin, organic siliconresin, fluorocarbon resin, polyvinyl resin, polystyrene resin, Corvic, acrylic resin, acrylonitrile-butadiene-styrene resin etc.;The inorganic adhesive is the one or more in cement, gypsum, lime stone, waterglass, cupric oxide-phosphoric acid glue etc..
4. a kind of preparation method of enhanced aerogel powder, it is characterised in that comprise the following steps:
(1)Aerogel powder is modified;
(2)The preparation of aeroge composite mortar;
(3)Aeroge composite mortar is flowed continuously on ultrasonic atomization head so that aeroge composite mortar is dispersed into the atomization mass of aerogel powder Surface coating aqueous adhesive;
(4)Curing process.
5. a kind of preparation method of enhanced aerogel powder according to claim 4, it is characterised in that the step(1)Including hydrophobically modified step;The hydrophobically modified step is to carry out hydrophobically modified to aerogel powder in closed hydrophobic modifier gaseous environment;The hydrophobic modifier be trim,ethylchlorosilane, HMDS, HMDO, MTMS, MTES, dimethyldimethoxysil,ne, dimethyldiethoxysilane, γ-aminopropyltrimethoxysilane, gamma-aminopropyl-triethoxy-silane, γ-(The oxygen of 2,3- epoxies third)Propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, N-(β-aminoethyl)One or more in-gamma-aminopropyl-triethoxy-silane.
6. a kind of preparation method of enhanced aerogel powder according to claim 4, it is characterised in that the step(1)Also include surface hydrophilic modification step;The surface hydrophilic modification step is that hydrophobic aerogel powder top layer is modified using surface hydrophilic modification solution;The surface hydrophilic modification solution is surfactant and the aqueous solution or the aqueous solution of low surface tension solvent of low surface tension solvent;The surfactant is the one or more in anionic surfactant, cationic surface active agent, amphoteric surfactant, nonionic surface active agent;The anionic surfactant is the one or more in fatty alcohol phosphates, aliphatic alcohol polyoxyvinethene phosphate salt, alkyl sulfate, fatty alcohol polyoxyethylene ether sulfate, fatty acid glyceride sulfate, sulphation ricinoleate, cycloalkanes sulfate, fatty acid amide alkyl sulfate, alkylbenzenesulfonate, alkylsulfonate, fatty acid methyl ester ethoxylate sulfonate, MES, aliphatic alcohol polyethenoxy ether carboxylate;The cationic surface active agent is aliphatic ammonium salt;The amphoteric surfactant is the one or more in alkyl amino acid, carboxylic acid group's glycine betaine, sulfobetaines, phosphate glycine betaine, alkyl hydroxy amine oxide;The nonionic surface active agent is the one or more in aliphatic polyester, APES, high-carbon fatty alcohol polyoxyethylene ether, polyoxyethylene carboxylate, fatty acid methyl ester ethoxylate, the oxireme addition product of polypropylene glycol, sorbitan ester, sucrose fatty ester, alkyl esteramides;The low surface tension solvent is one or more mixtures in acetone, n-hexane, pentane, normal heptane, ethanol, isopropanol, the tert-butyl alcohol, propane diols, glycerine.
7. a kind of preparation method of enhanced aerogel powder according to claim 6, it is characterised in that in the surface hydrophilic modification step, in addition to additional physical field action step;The additional physical field action step is one kind in far infrared radiation, stirring, ultrasonication, ball milling.
8. a kind of preparation method of enhanced aerogel powder according to claim 4, it is characterised in that the step(1)Also include drying process step;The drying process step is one kind in far-infrared ray drying, spray drying, microwave drying, constant pressure and dry, supercritical drying, subcritical drying, freeze-drying.
9. a kind of preparation method of enhanced aerogel powder according to claim 4, it is characterised in that the preparation of the aeroge composite mortar is by step(1)Modified aerogel powder, aqueous adhesive and water mixing, stirring.
10. a kind of preparation method of enhanced aerogel powder according to claim 4, it is characterised in that the curing process is the one or more in Heated by Far-Infrared Radiation, microwave heating, ultraviolet radiation, natural curing, steam curing, steam press maintenance.
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