CN107266942B - A kind of enhanced aerogel powder and preparation method thereof - Google Patents
A kind of enhanced aerogel powder and preparation method thereof Download PDFInfo
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- CN107266942B CN107266942B CN201610214815.9A CN201610214815A CN107266942B CN 107266942 B CN107266942 B CN 107266942B CN 201610214815 A CN201610214815 A CN 201610214815A CN 107266942 B CN107266942 B CN 107266942B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT 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
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
- C09C1/30—Silicic acid
- C09C1/3045—Treatment with inorganic compounds
- C09C1/3054—Coating
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT 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
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
- C09C1/30—Silicic acid
- C09C1/3072—Treatment with macro-molecular organic compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
- C09C1/30—Silicic acid
- C09C1/309—Combinations of treatments provided for in groups C09C1/3009 - C09C1/3081
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT 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
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT 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
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
Abstract
The present invention discloses a kind of enhanced aerogel powder and preparation method thereof, which is characterized in that the enhanced aerogel powder is made of aerogel powder and covering material.The preparation method of a kind of enhanced aerogel powder provided by the invention, comprising the following steps: (1) aerogel powder is modified；(2) preparation of slurry is coated；(3) it coats；(4) solidify.A kind of enhanced aerogel powder provided by the invention and preparation method thereof has the characteristics that low cost, high efficiency, continuous production, aerogel powder is under the premise of reservation aeroge original excellent characteristics, have many advantages, such as that mechanical property is good, there is huge application prospect.
Description
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 aeroges
Powder and preparation method thereof belongs to lightweight, heat preservation, fire prevention, sound insulation, explosion-proof, damping energy-absorbing material field.
Background technique
Aeroge is a kind of light-weight inorganic solid material with three-dimensional network skeleton structure and nanoscale hole hole, has pole
High porosity, specific surface area, extremely low density and solid content, chemical inertness and noninflammability show excellent lightweight, absolutely
The characteristics such as heat, fire prevention, sound insulation, damping energy-absorbing, thermal coefficient can be down to 0.015W/mK or less.
Aerogel powder can be made with lightweight, absolutely as the Material claddings such as lightweight functional stuffing and concrete, resin
The composite material of the performances such as heat, sound insulation.However, the special structure feature of aeroge leads to the mechanics such as its fold resistance, compression strength
Performance is lower, with it is easily broken in other materials recombination process；Further, since there is a large amount of nano grade pores on aeroge surface
Siphonage easily occurs when contacting with solvent for hole, to destroy aeroge nano-pore structure, its excellent characteristics is caused to be lost.
Summary of the invention
The object of the present invention is to provide a kind of enhanced aerogel powders and preparation method thereof.
A kind of enhanced aerogel powder, is made of aerogel powder and covering material.
The covering material is aqueous adhesive in one of the embodiments,.
The aqueous adhesive is one of organic adhesion agent, inorganic adhesive or more in one of the embodiments,
Kind；The organic adhesion agent is rosin resin, alkyd resin, acrylic resin, polyurethane resin, organic siliconresin, fluorine carbon tree
Rouge, polyvinyl resin, polystyrene resin, Corvic, acrylic resin, acrylonitrile-butadiene-styrene resin etc.
One of or it is a variety of；The inorganic adhesive is one in cement, gypsum, lime stone, waterglass, copper oxide-phosphoric acid glue etc.
Kind is a variety of.
A kind of preparation method of enhanced aerogel powder of the invention, comprising the following steps:
(1) aerogel powder is modified；
(2) 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 cladding aqueous adhesive；
(4) curing process.
The step (1) includes hydrophobically modified step in one of the embodiments,；The hydrophobically modified step is close
Hydrophobically modified is carried out to aerogel powder in the hydrophobic modifier gaseous environment closed；The hydrophobic modifier is trimethylchloro-silicane
Alkane, hexamethyldisilazane, hexamethyldisiloxane, methyltrimethoxysilane, methyltriethoxysilane, dimethylformamide dimethyl
Oxysilane, dimethyl diethoxysilane, γ-aminopropyltrimethoxysilane, gamma-aminopropyl-triethoxy-silane, γ-
(the third oxygen of 2,3- epoxy) propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, N-(β-ammonia second
Base) one of-gamma-aminopropyl-triethoxy-silane or a variety of.
The step (1) further includes surface hydrophilic modification step in one of the embodiments,；The surface hydrophilic modification
Step is to be modified using surface hydrophilic modification solution to hydrophobic aerogel powder surface；The surface hydrophilic modification solution is
The aqueous solution of the aqueous solution or low surface tension solvent of surfactant and low surface tension solvent；The surfactant is yin
One of ionic surfactant, cationic surface active agent, amphoteric surfactant, nonionic surface active agent
Or it is a variety of；The anionic surfactant is fatty alcohol phosphates, aliphatic alcohol polyoxyvinethene phosphate salt, alkyl sulfide
Hydrochlorate, fatty alcohol polyoxyethylene ether sulfate, fatty acid glyceride sulfate, sulphation ricinoleate, cycloalkanes sulfate, fat
Amidoalkyl group sulfate, alkylbenzene sulfonate, alkylsulfonate, fatty acid methyl ester ethoxylate sulfonate, fatty acid methyl ester
One of sulfonate, aliphatic alcohol polyethenoxy ether carboxylate are a variety of；The cationic surface active agent is aliphatic ammonium
Salt；The amphoteric surfactant is alkyl amino acid, carboxylic acid group's glycine betaine, sulfobetaines, phosphate glycine betaine, alkyl hydroxyl
One of base amine oxide is a variety of；The nonionic surface active agent is aliphatic polyester, alkyl phenol polyoxyethylene ether, height
Carbon fatty alcohol polyoxyethylene ether, polyoxyethylene carboxylate, fatty acid methyl ester ethoxylate, polypropylene glycol oxireme add
At one of object, sorbitan ester, sucrose fatty ester, alkyl esteramides or a variety of；The low surface tension solvent is
One of acetone, n-hexane, pentane, normal heptane, ethyl alcohol, isopropanol, the tert-butyl alcohol, propylene glycol, glycerol or a variety of mixtures.
It further include additional physical field action step in one of the embodiments, in the surface hydrophilic modification step；Institute
Stating additional physical field action step is one of far infrared radiation, stirring, ultrasonication, ball milling.
The step (1) further includes being dried step in one of the embodiments,；The drying process step is remote
One of infra-red drying, spray drying, microwave drying, constant pressure and dry, supercritical drying, subcritical drying, freeze-drying.
The preparation of the aeroge composite mortar is the airsetting rubber powder that step (1) is modified in one of the embodiments,
Body, aqueous adhesive and water mixing, stirring.
In one of the embodiments, the curing process be Heated by Far-Infrared Radiation, microwave heating, ultraviolet radiation,
One of natural curing, steam curing, steam press maintenance are a variety of.
Inner hydrophobic, the structure feature of surface hydrophilic is presented in above-mentioned enhanced aerogel powder, can retain aeroge
Under the premise of original excellent characteristics, has many advantages, such as that high mechanical properties, partial size are uniform for micron order, particle diameter distribution, can be used as function
Energy filler is for fields such as coating, adhesive, insulating materials, concrete；Continuous, stable, efficient work may be implemented in the present invention
Industry production.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, below to specific reality of the invention
The mode of applying is described in detail.In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention.But
The invention can be embodied in many other ways as described herein, and those skilled in the art can be without prejudice to this hair
Similar improvement is done in the case where bright intension, therefore the present invention is not limited to the specific embodiments disclosed below.
A kind of embodiment of enhanced aerogel powder of the invention, is made 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, for aerogel powder with other materials is compound provides precondition.
In the present embodiment, the covering material is aqueous adhesive.
In this way, the mechanical properties such as the bending strength of aqueous adhesive, compression strength are much higher than aeroge, in aerogel powder
Surface cladding cementitious material can significantly improve the mechanical property of aerogel powder under the premise of retaining aeroge excellent properties
Can, expand the engineer application of aerogel powder.
In the present embodiment, the aqueous adhesive is one of organic adhesion agent, inorganic adhesive or a variety of；It is described to have
Machine adhesive is rosin resin, alkyd resin, acrylic resin, polyurethane resin, organic siliconresin, fluorocarbon resin, polyethylene
One of resin, polystyrene resin, Corvic, acrylic resin, acrylonitrile-butadiene-styrene resin etc.
Or it is a variety of；The inorganic adhesive is one of cement, gypsum, lime stone, waterglass, copper oxide-phosphoric acid glue etc. or a variety of.
In this way, different aqueous adhesives have different mechanical property and different maintenances, curing process, usually with
Organic adhesion agent is compared, and the mechanical property of inorganic adhesive is higher, but conserve, curing process is complicated, the period is long, the present invention according to
Physical chemistry needed for mechanical property needed for aerogel powder and subsequent and other materials compound tense aerogel powder surface
Can, select suitable aqueous adhesive or a variety of aqueous adhesives to compound cladding aerogel powder.
A kind of preparation method of enhanced aerogel powder, comprising the following steps:
(1) aerogel powder is modified；
(2) 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 cladding aqueous adhesive；
(4) curing process.
In addition, atomising head surfacing can have hydrophobic property.
In this way, using ultrasonic atomization technique and the hydrophobic technology of ultrasonic atomization head surface, by aeroge composite mortar
It flows continuously on ultrasonic atomization head, utilizes the hole explosion effect and ultrasonic atomization head between composite mortar and air
Composite mortar around hole is ground into the atomization of micron-sized aeroge surface cladding aqueous adhesive by surface hydrophobicity characteristic
Body；The structure feature with inner hydrophobic, surface hydrophilic and surface cladding aqueous adhesive is made in the present invention through the above steps
Enhanced aerogel powder, can be under the premise of nano-porous structure be destroyed, as functional stuffing and concrete, glue
The Material claddings such as stick.
In the present embodiment, the step (1) includes hydrophobically modified step；The hydrophobically modified step is closed hydrophobic
Hydrophobically modified is carried out to aerogel powder in modifying agent gaseous environment；The hydrophobic modifier is trim,ethylchlorosilane, hexamethyl
Disilazane, hexamethyldisiloxane, methyltrimethoxysilane, methyltriethoxysilane, dimethyldimethoxysil,ne,
Dimethyl diethoxysilane, γ-aminopropyltrimethoxysilane, gamma-aminopropyl-triethoxy-silane, γ-(2,3- epoxy third
Oxygen) propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, N-(β-aminoethyl)-γ-aminopropyl
One of triethoxysilane is a variety of.
In this way, precursor, displacement solvent and drying process are to the hydrophobic of aeroge due in existing aeroge preparation method
Property have significant effect, if the contact angle of the surface of aeroge and water be greater than 90 °, hydrophobically modified can not be carried out in advance, directly
Tap into row surface hydrophilic modification；If the surface of aeroge and the contact angle of water need to carry out hydrophobic change in advance less than 90 °
Property；Hydrophobically modified is carried out to aerogel powder in closed hydrophobic modifier gaseous environment, in addition to significantly improving airsetting rubber powder
The modified effect of body, it is ensured that inside nano-porous structure is not destroyed outer when subsequent hydrophilic modifying, also significantly improves modification efficiency
And production efficiency, reduce production cost.
In the present embodiment, the step (1) further includes surface hydrophilic modification step；The surface hydrophilic modification step is to adopt
Hydrophobic aerogel powder surface is modified with surface hydrophilic modification solution；The surface hydrophilic modification solution is surface-active
The aqueous solution of the aqueous solution or low surface tension solvent of agent and low surface tension solvent；The surfactant is anionic table
One of face activating agent, cationic surface active agent, amphoteric surfactant, nonionic surface active agent are a variety of；
The anionic surfactant is fatty alcohol phosphates, aliphatic alcohol polyoxyvinethene phosphate salt, alkyl sulfate, rouge
Fat alcohol polyoxyethylene ether sulfate, fatty acid glyceride sulfate, sulphation ricinoleate, cycloalkanes sulfate, fatty acid amide alkane
Base sulfate, alkylbenzene sulfonate, alkylsulfonate, fatty acid methyl ester ethoxylate sulfonate, fatty acid methyl ester sulfonate,
One of aliphatic alcohol polyethenoxy ether carboxylate is a variety of；The cationic surface active agent is aliphatic ammonium salt；It is described
Amphoteric surfactant is alkyl amino acid, carboxylic acid group's glycine betaine, sulfobetaines, phosphate glycine betaine, alkyl hydroxy oxidation
One of amine is a variety of；The nonionic surface active agent is aliphatic polyester, alkyl phenol polyoxyethylene ether, high carbocyclic aliphatic
Alcohol polyoxyethylene ether, polyoxyethylene carboxylate, fatty acid methyl ester ethoxylate, polypropylene glycol oxireme addition product,
One of sorbitan ester, sucrose fatty ester, alkyl esteramides are a variety of；The low surface tension solvent be acetone,
One of n-hexane, pentane, normal heptane, ethyl alcohol, isopropanol, the tert-butyl alcohol, propylene glycol, glycerol are a variety of.
In this way, the aqueous solution of aqueous solution or low surface tension solvent using surfactant and low surface tension solvent,
It is carrying out in hydrophilic modifying treatment process there is surface to cooperate with hydrophilic modifying effect to hydrophobic aerogel powder surface, can significantly mention
High surface hydrophilic modification solution while being significantly slowed to the inside of aerogel powder in the wetting spreading rate on aerogel powder surface
Wetting extension, by regulate and control modified solution dosage, can accurately realize to aerogel powder surface hydrophilic thickness degree
Regulation, low surface tension solvent not only with water and surfactant there is surface to cooperate with hydrophilic modifying effect, but also can be big
The earth is lowered into the capillary force of the hydrophilic modifying solution in the nano-pore of aerogel powder surface layer, it is easy to pass through drying process
Hydrophilic modifying solution in the nano-pore of aerogel powder surface layer is evaporated, without destroying its nano-porous structure, the present invention
Aerogel powder inner hydrophobic is presented, surface hydrophilic, surface hydrophilic layer still retain nano-porous structure and surface hydrophilic thickness
The structure feature that degree is 0.1 ~ 100 μm has good interface cohesion between cementitious material；The technique have step it is simple,
The features such as period is short, high production efficiency is suitable for industrialized production.
It further include additional physical field action step in the surface hydrophilic modification step in the present embodiment；The additional object
Managing field action step is one of far infrared radiation, stirring, ultrasonication, ball milling.
In this way, additional physics field action can significantly improve the activity and and aerogel powder of surface hydrophilic modification solution
Contact probability, reduce dosage of surfactant, improve the surface hydrophilic modification rate of aerogel powder, reduce cost, improve
Production efficiency.
In the present embodiment, the step (1) further includes being dried step；The drying process step is dry for far infrared
One of dry, spray drying, microwave drying, constant pressure and dry, supercritical drying, subcritical drying, freeze-drying.
In this way, if aerogel powder and cementitious material compound tense, the hydrophilic modifying of surface layer remnants after hydrophilic modifying are molten
Liquid will affect interface cohesion, and processing need to be pre-dried；Using above-mentioned drying process, ensuring aerogel powder surface layer nano-pore knot
Under the premise of structure is not destroyed, surface hydrophilic modification solution remaining in the nano-pore of aerogel powder surface layer is evaporated, is mentioned
Interface bond strength between high aerogel powder and cementitious material.
In the present embodiment, the preparation of the aeroge composite mortar is by step (1) modified aerogel powder, water-base cement
Stick and water mixing, stirring.
It is mixed in this way, the aerogel powder of inner hydrophobic, surface hydrophilic is come into full contact with aqueous adhesive, in the liquid phase
Form good combination interface.
In the present embodiment, the curing process be Heated by Far-Infrared Radiation, microwave heating, ultraviolet radiation, natural curing,
One of steam curing, steam press maintenance are a variety of.
So, it is ensured that aeroge surface coats the atomization mass of aqueous adhesive before falling into collection vessel, completes solidification, and
And further increase the mechanical property of aqueous adhesive clad.
Inner hydrophobic, the structure feature of surface hydrophilic is presented in above-mentioned enhanced aerogel powder, can retain aeroge
Under the premise of original excellent characteristics, has many advantages, such as that high mechanical properties, partial size are uniform for micron order, particle diameter distribution, can be used as function
Energy filler is for fields such as coating, adhesive, insulating materials, concrete；Continuous, stable, efficient work may be implemented in the present invention
Industry production.
It is below specific embodiment part.
Embodiment 1
The enhanced SiO of polyurethane film is coated with using following steps preparation inner hydrophobic, surface hydrophilic, surface2Gas
Gel powder, polyurethane coating thickness are 8 ~ 10 μm:
(1) SiO to be processed is detected using contact angle measurement2The contact angle on aerogel powder surface and water, detection knot
Fruit is 55 °, the SiO for being then 56 μm by partial size2Aerogel powder is placed in vacuum furnace, with container by six after weighing
Methyl disilazane is placed in vacuum furnace, heating and gasifying, and hydrophobically modified 1.5h obtains hydrophobic SiO2Aerogel powder,
Hydrophobic SiO is detected with contact angle measurement2The contact angle on aerogel powder surface and water, testing result are 147 °；
(2) at room temperature, 1:1:100 in mass ratio weighs ethyl alcohol, n-hexane and deionized water, is uniformly mixed, configuration
At surface hydrophilic modification solution；
(3) hydrophobic SiO is pressed2It is molten to weigh surface modification by the volume ratio 1:3 of aerogel powder and surface hydrophilic modification solution
Liquid, and pour into corresponding container, the hydrophobic SiO of step (1) will be passed through2Aerogel powder is mixed with surface hydrophilic modification solution,
After ball-milling treatment 25min, filtering is taken out；
(4) surface that step (3) obtains is contained to the SiO of hydrophilic modifying solution2It is dry that aerogel powder is placed in far infrared
In dry furnace, at a temperature of 120 DEG C, dry 0.5h, furnace cooling is to taking-up after 50 DEG C or less, to SiO2Aerogel powder it is transversal
Face is detected, and testing result is shown, surface hydrophilic layer is with a thickness of 7.9 μm；
(5) 1:30:100 in mass ratio weighs the SiO of step (4)2Aeroge, waterborne polyurethane resin and deionized water,
It is stirred, obtains SiO2Aeroge composite mortar；
(6) setting ultrasonic frequency vibratory is 1GHz, valve is opened, so that SiO2Aeroge composite mortar flows to ultrasonic wave
Shake table, to SiO2Aeroge composite mortar carry out atomization process, atomized body, in atomization mass dropping process, to its into
Row Heated by Far-Infrared Radiation, solidification, obtains enhanced SiO2Aerogel powder, polyurethane coating thickness are 8 ~ 10 μm.
Embodiment 2
The enhanced SiO of acrylate film is coated with using following steps preparation inner hydrophobic, surface hydrophilic, surface2Gas
Gel powder, acrylic acid coating thickness are 8 ~ 12 μm:
(1) SiO to be processed is detected using contact angle measurement2The contact angle on aerogel powder surface and water, detection knot
Fruit is 45 °, the SiO for being then 0.1mm by partial size2Aerogel powder is placed in vacuum furnace, will be after weighing with container
Trim,ethylchlorosilane is placed in vacuum furnace, heating and gasifying, and hydrophobically modified 1.5h obtains hydrophobic SiO2Aerogel powder,
Hydrophobic SiO is detected with contact angle measurement2The contact angle on aerogel powder surface and water, testing result are 146 °；
(2) at room temperature, 1:1:100 in mass ratio weighs n-hexane, acetone and deionized water, is uniformly mixed, is configured to
Surface hydrophilic modification solution；
(3) hydrophobic SiO is pressed2It is molten to weigh surface modification by the volume ratio 1:3 of aerogel powder and surface hydrophilic modification solution
Liquid, and pour into corresponding container, the hydrophobic SiO of step (1) will be passed through2Aerogel powder is mixed with surface hydrophilic modification solution,
After mechanical stirring 15min, revolving speed is 2500 turns/min, filtering；
(4) surface that step (3) obtains is contained to the SiO of hydrophilic modifying solution2It is dry that aerogel powder is placed in far infrared
In dry furnace, at a temperature of 120 DEG C, dry 0.5h, furnace cooling is to taking-up after 50 DEG C or less, to SiO2Aerogel powder it is transversal
Face is detected, and testing result is shown, surface hydrophilic layer is with a thickness of 11.1 μm；
(5) 1:40:100 in mass ratio weighs the SiO of step (4)2Aeroge, water-based acrylic resin and deionized water,
It is stirred, obtains SiO2Aeroge composite mortar；
(6) setting ultrasonic frequency vibratory is 2GHz, valve is opened, so that SiO2Aeroge composite mortar flows to ultrasonic wave
Shake table, to SiO2Aeroge composite mortar carry out atomization process, atomized body, in atomization mass dropping process, to its into
Row Heated by Far-Infrared Radiation, solidification, obtains enhanced SiO2Aerogel powder, acrylic acid coating thickness are 8 ~ 12 μm.
Embodiment 3
The enhanced SiO of polyurethane film is coated with using following steps preparation inner hydrophobic, surface hydrophilic, surface2Gas
Gel powder, polyurethane coating thickness are 7 ~ 11 μm:
(1) SiO to be processed is detected using contact angle measurement2The contact angle on aerogel powder surface and water, detection knot
Fruit is 45 °, the SiO for being then 89 μm by partial size2Aerogel powder is placed in vacuum furnace, with container by six after weighing
Methyl disilazane is placed in vacuum furnace, heating and gasifying, and hydrophobically modified 1.5h obtains hydrophobic SiO2Aerogel powder,
Hydrophobic SiO is detected with contact angle measurement2The contact angle on aerogel powder surface and water, testing result are 146 °；
(2) at room temperature, 1:0.8:120 in mass ratio weighs sodium alkyl benzene sulfonate, n-hexane and deionized water, and mixing is equal
It is even, it is configured to surface hydrophilic modification solution；
(3) hydrophobic SiO is pressed2It is molten to weigh surface modification by the volume ratio 1:3 of aerogel powder and surface hydrophilic modification solution
Liquid, and pour into corresponding container, the hydrophobic SiO of step (1) will be passed through2Aerogel powder is mixed with surface hydrophilic modification solution,
After mechanical stirring 15min, revolving speed is 2000 turns/min, filtering；
(4) surface that step (3) obtains is contained to the SiO of hydrophilic modifying solution2Aerogel powder is placed in forced air drying
In case, at a temperature of 120 DEG C, dry 0.5h, furnace cooling is to taking-up after 50 DEG C or less, to SiO2The cross section of aerogel powder
It is detected, testing result is shown, surface hydrophilic layer is with a thickness of 6.0 μm；
(5) 1:30:100 in mass ratio weighs the SiO of step (4)2Aeroge, aqueous polyurethane UV solidified resin and go from
Sub- water, is stirred, and obtains SiO2Aeroge composite mortar；
(6) setting ultrasonic frequency vibratory is 1.2GHz, valve is opened, so that SiO2Aeroge composite mortar flow direction ultrasound
Wave shake table, to SiO2Aeroge composite mortar carries out atomization process, atomized body, in atomization mass dropping process, to it
Treatment with UV radiation is carried out, solidification obtains enhanced SiO2Aerogel powder, polyurethane coating thickness are 7 ~ 11 μm.
Embodiment 4
The enhanced SiO of epoxy resin thin film is coated with using following steps preparation inner hydrophobic, surface hydrophilic, surface2
Aerogel powder, epoxy resin coating thickness are 13 ~ 15 μm:
(1) SiO to be processed is detected using contact angle measurement2The contact angle on aerogel powder surface and water, detection knot
Fruit is 31 °, the SiO for being then 0.2mm by partial size2Aerogel powder is placed in vacuum furnace, will be after weighing with container
Trim,ethylchlorosilane is placed in vacuum furnace, heating and gasifying, and hydrophobically modified 1.5h obtains hydrophobic SiO2Aerogel powder,
Hydrophobic SiO is detected with contact angle measurement2The contact angle on aerogel powder surface and water, testing result are 150 °；
(2) at room temperature, 1:1:0.8:200 in mass ratio weighs sodium sulfate of polyethenoxy ether of fatty alcohol, alkyl benzene sulphonate
Sodium, isopropanol and deionized water are uniformly mixed, are configured to surface hydrophilic modification solution；
(3) hydrophobic SiO is pressed2It is molten to weigh surface modification by the volume ratio 1:3 of aerogel powder and surface hydrophilic modification solution
Liquid, and pour into corresponding container, the hydrophobic SiO of step (1) will be passed through2Aerogel powder is mixed with surface hydrophilic modification solution,
After mechanical stirring 15min, revolving speed is 2500 turns/min, filtering；
(4) surface that step (3) obtains is contained to the SiO of hydrophilic modifying solution2It is dry that aerogel powder is placed in far infrared
In dry furnace, at a temperature of 120 DEG C, dry 0.5h, furnace cooling is to taking-up after 50 DEG C or less, to SiO2Aerogel powder it is transversal
Face is detected, and testing result is shown, surface hydrophilic layer is with a thickness of 11.1 μm；
(5) 1:30:100 in mass ratio weighs the SiO of step (4)2Aeroge, single-component water-based epoxy resin and deionization
Water is stirred, and obtains SiO2Aeroge composite mortar；
(6) setting ultrasonic frequency vibratory is 3GHz, valve is opened, so that SiO2Aeroge composite mortar flows to ultrasonic wave
Shake table, to SiO2Aeroge composite mortar carry out atomization process, atomized body, in atomization mass dropping process, to its into
The processing of row far infrared radiation, solidification obtain enhanced SiO2Aerogel powder, epoxy resin coating thickness are 13 ~ 15 μm.
Embodiment 5
The enhanced of waterborne organic silicon resin film is coated using following steps preparation inner hydrophobic, surface hydrophilic, surface
SiO2Aerogel powder, organic siliconresin coating thickness are 8 ~ 10 μm:
(1) SiO that partial size to be processed is 77 μm is detected using contact angle measurement2Aerogel powder surface and water
Contact angle, testing result are 140 °, then the SiO2Aerogel powder has hydrophobicity；
(2) at room temperature, 1:0.6:150 in mass ratio weighs sldium lauryl sulfate, acetone and deionized water, and mixing is equal
It is even, it is configured to surface hydrophilic modification solution；
(3) hydrophobic SiO is pressed2It is molten to weigh surface modification by the volume ratio 1:3 of aerogel powder and surface hydrophilic modification solution
Liquid, and pour into corresponding container, the hydrophobic SiO of step (1) will be passed through2Aerogel powder is mixed with surface hydrophilic modification solution,
After ball-milling treatment 25min, filtering is taken out；
(4) surface that step (3) obtains is contained to the SiO of hydrophilic modifying solution2Aerogel powder is placed in forced air drying
In case, at a temperature of 120 DEG C, dry 0.5h, furnace cooling is to taking-up after 50 DEG C or less, to SiO2The cross section of aerogel powder
It is detected, testing result is shown, surface hydrophilic layer is with a thickness of 6.9 μm；
(5) 1:35:100 in mass ratio weighs the SiO of step (4)2Aeroge, waterborne organic silicon resin and deionized water,
It is stirred, obtains SiO2Aeroge composite mortar；
(6) setting ultrasonic frequency vibratory is 2GHz, valve is opened, so that SiO2Aeroge composite mortar flows to ultrasonic wave
Shake table, to SiO2Aeroge composite mortar carry out atomization process, atomized body, in atomization mass dropping process, to its into
The processing of row far infrared radiation, solidification obtain enhanced SiO2Aerogel powder, organic siliconresin coating thickness are 8 ~ 10 μm.
Embodiment 6
The enhanced SiO of acrylate film is coated with using following steps preparation inner hydrophobic, surface hydrophilic, surface2Gas
Gel powder, acrylic acid coating thickness are 9 ~ 12 μm:
(1) SiO that partial size to be processed is 75 μm is detected using contact angle measurement2Aerogel powder surface and water
Contact angle, testing result are 141 °, then the SiO2Aerogel powder has hydrophobicity；
(2) at room temperature, 1:0.3:100 in mass ratio weighs nonylphenol polyoxyethylene ether, n-hexane and deionized water, mixes
It closes uniformly, is configured to surface hydrophilic modification solution；
(3) hydrophobic SiO is pressed2It is molten to weigh surface modification by the volume ratio 1:3 of aerogel powder and surface hydrophilic modification solution
Liquid, and pour into corresponding container, the hydrophobic SiO of step (1) will be passed through2Aerogel powder is mixed with surface hydrophilic modification solution,
After ball milling 15min, filtering is taken out；
(4) surface that step (3) obtains is contained to the SiO of hydrophilic modifying solution2It is dry that aerogel powder is placed in far infrared
In dry furnace, at a temperature of 120 DEG C, dry 0.5h, furnace cooling is to taking-up after 50 DEG C or less, to SiO2Aerogel powder it is transversal
Face is detected, and testing result is shown, surface hydrophilic layer is with a thickness of 11.1 μm；
(5) 1:40:100 in mass ratio weighs the SiO of step (4)2Aeroge, water-based acrylic resin and deionized water,
It is stirred, obtains SiO2Aeroge composite mortar；
(6) setting ultrasonic frequency vibratory is 2GHz, valve is opened, so that SiO2Aeroge composite mortar flows to ultrasonic wave
Shake table, to SiO2Aeroge composite mortar carry out atomization process, atomized body, in atomization mass dropping process, to its into
The processing of row far infrared radiation, solidification obtain enhanced SiO2Aerogel powder, acrylic acid coating thickness are 9 ~ 12 μm.
Embodiment 7
Using following steps preparation inner hydrophobic, surface hydrophilic, surface coated epoxy resin film enhanced TiO2Gas
Gel powder, epoxy resin coating thickness are 13 ~ 15 μm:
(1) TiO to be processed is detected using contact angle measurement2The contact angle on aerogel powder surface and water, detection knot
Fruit is 145 °, then the TiO2Aerogel powder has hydrophobicity；
(2) at room temperature, 1:0.8:120 in mass ratio weighs sodium alkyl benzene sulfonate, n-hexane and deionized water, and mixing is equal
It is even, it is configured to surface hydrophilic modification solution；
(3) hydrophobic TiO is pressed2It is molten to weigh surface modification by the volume ratio 1:3 of aerogel powder and surface hydrophilic modification solution
Liquid, and pour into corresponding container, the hydrophobic TiO of step (1) will be passed through2Aerogel powder is mixed with surface hydrophilic modification solution,
After mechanical stirring 15min, revolving speed is 2000 turns/min, filtering；
(4) surface that step (3) obtains is contained to the TiO of hydrophilic modifying solution2Aerogel powder is placed in forced air drying
In case, at a temperature of 120 DEG C, dry 0.5h, furnace cooling is to taking-up after 50 DEG C or less, to TiO2The cross section of aerogel powder
It is detected, testing result is shown, surface hydrophilic layer is with a thickness of 6.0 μm；
(5) 1:40:100 in mass ratio weighs the TiO of step (4)2Aeroge, aqueous epoxy resins and deionized water, are stirred
Mixing is mixed, TiO is obtained2Aeroge composite mortar；
(6) setting ultrasonic frequency vibratory is 2GHz, valve is opened, so that TiO2Aeroge composite mortar flows to ultrasonic wave
Shake table, to TiO2Aeroge composite mortar carry out atomization process, atomized body, in atomization mass dropping process, to its into
The processing of row far infrared radiation, solidification obtain enhanced TiO2Aerogel powder, epoxy resin coating thickness are 13 ~ 15 μm.
Embodiment 8
The enhanced SiO of acrylate film is coated with using following steps preparation inner hydrophobic, surface hydrophilic, surface2Gas
Gel powder, acrylic acid coating thickness are 9 ~ 13 μm:
(1) SiO that partial size to be processed is 0.3mm is detected using contact angle measurement2Aerogel powder surface and water
Contact angle, testing result are 148 °, then the SiO2Aerogel powder has hydrophobicity；
(2) at room temperature, 1:0.4:0.3:130 in mass ratio weighs fatty alcohol polyoxyethylene ether ammonium sulfate, n-hexane, second
Pure and mild deionized water is uniformly mixed, is configured to surface hydrophilic modification solution；
(3) hydrophobic SiO is pressed2It is molten to weigh surface modification by the volume ratio 1:3 of aerogel powder and surface hydrophilic modification solution
Liquid, and pour into corresponding container, the hydrophobic SiO of step (1) will be passed through2Aerogel powder is mixed with surface hydrophilic modification solution,
After mechanical stirring 15min, revolving speed is 2500 turns/min, filtering；
(4) surface that step (3) obtains is contained to the SiO of hydrophilic modifying solution2It is dry that aerogel powder is placed in far infrared
In dry furnace, at a temperature of 120 DEG C, dry 0.5h, furnace cooling is to taking-up after 50 DEG C or less, to SiO2Aerogel powder it is transversal
Face is detected, and testing result is shown, surface hydrophilic layer is with a thickness of 11.1 μm；
(5) 1:40:100 in mass ratio weighs the SiO of step (4)2Aeroge, water-based acrylic resin and deionized water,
It is stirred, obtains SiO2Aeroge composite mortar；
(6) setting ultrasonic frequency vibratory is 2.5GHz, valve is opened, so that SiO2Aeroge composite mortar flow direction ultrasound
Wave shake table, to SiO2Aeroge composite mortar carries out atomization process, atomized body, in atomization mass dropping process, to it
Microwave heating treatment is carried out, solidification obtains enhanced SiO2Aerogel powder, acrylic acid coating thickness are 9 ~ 13 μm.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (1)
1. a kind of preparation method of enhanced aerogel powder is wrapped using following steps preparation inner hydrophobic, surface hydrophilic, surface
It is covered with the enhanced SiO of polyurethane film2Aerogel powder, polyurethane coating thickness are 8-10 μm:
(1) SiO to be processed is detected using contact angle measurement2The contact angle on aerogel powder surface and water, testing result are
55 °, the SiO for being then 56 μm by partial size2Aerogel powder is placed in vacuum furnace, with container by the hexamethyl after weighing
Disilazane is placed in vacuum furnace, heating and gasifying, and hydrophobically modified 1.5h obtains hydrophobic SiO2Aerogel powder, with connecing
Feeler measuring instrument detects hydrophobic SiO2The contact angle on aerogel powder surface and water, testing result are 147 °；
(2) at room temperature, 1:1:100 in mass ratio weighs ethyl alcohol, n-hexane and deionized water, is uniformly mixed, is configured to table
Face hydrophilic modifying solution；
(3) hydrophobic SiO is pressed2The volume ratio 1:3 of aerogel powder and surface hydrophilic modification solution weighs surface modification solution, and falls
Enter in corresponding container, the hydrophobic SiO of step (1) will be passed through2Aerogel powder is mixed with surface hydrophilic modification solution, ball-milling treatment
After 25min, filtering is taken out；
(4) surface that step (3) obtains is contained to the SiO of hydrophilic modifying solution2Aerogel powder is placed in far infrared drying stove
In, at a temperature of 120 DEG C, dry 0.5h, furnace cooling is to taking-up after 50 DEG C or less, to SiO2The cross section of aerogel powder into
Row detection, testing result show that surface hydrophilic layer is with a thickness of 7.9 μm；
(5) 1:30:100 in mass ratio weighs the SiO of step (4)2Aeroge, waterborne polyurethane resin and deionized water, stirring are mixed
It closes, obtains SiO2Aeroge composite mortar；
(6) setting ultrasonic frequency vibratory is 1GHz, valve is opened, so that SiO2Aeroge composite mortar flows to ultrasonic activation
Platform, to SiO2Aeroge composite mortar carries out atomization process, and atomized body carries out it far in atomization mass dropping process
Infrared radiation heating, solidification, obtains enhanced SiO2Aerogel powder, polyurethane coating thickness are 8-10 μm.
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