CN109503116A - A kind of preparation method of aeroge compound insulating material - Google Patents
A kind of preparation method of aeroge compound insulating material Download PDFInfo
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- CN109503116A CN109503116A CN201811543009.1A CN201811543009A CN109503116A CN 109503116 A CN109503116 A CN 109503116A CN 201811543009 A CN201811543009 A CN 201811543009A CN 109503116 A CN109503116 A CN 109503116A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B30/00—Compositions for artificial stone, not containing binders
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/20—Mortars, concrete or artificial stone characterised by specific physical values for the density
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
Abstract
The present invention provides a kind of preparation methods of aeroge compound insulating material, comprising: a) mixes silicon source, hexamethyldisilazane, pH adjusting agent and solvent；B) the silica solution precursor solution being mixed to get is impregnated into magnesium silicate fiber felt, is stood, form wet gel felt body；C) wet gel felt body is dipped into 40~90 DEG C of organosiloxane, later microwave drying, obtains aeroge compound insulating material.The present invention is on the basis of improveing precursor solution formula, it is immersed in organic siloxane solution by the wet gel felt body for forming step b), the removal of impurities for realizing wet gel felt body, ageing, exchange of solvent and alkylation processing can be synchronized, to greatly shorten material manufacturing cycle.Meanwhile above-mentioned processing can also reduce the drying difficulty of material, and it is subsequent to cooperate microwave drying again, it can make material under normal pressure can rapid draing.Moreover, the method for the present invention does not introduce chloride ion during prepared by material, therefore device therefor is corroded also smaller.
Description
Technical field
The invention belongs to field of heat insulating materials more particularly to a kind of preparation methods of aeroge compound insulating material.
Background technique
Aerosil compound insulating material is a kind of heat insulating material of rising in recent years, the thermally conductive system of room temperature
Number≤0.023w/ (m.k), has a clear superiority compared with Conventional insulation, heat insulating effect more preferably, in space flight, army
Work, metallurgy, petrochemical industry, energy saving building, solar energy composite such as utilize to be widely used at the fields.
Currently, aerosil compound insulating material mostly uses alkali-free glass fibre felt greatly or alumina silicate fiber felt is
Substrate, regardless of the base using glass mat or alumina silicate fiber felt as aerosil compound insulating material
Material all not can avoid small glass fibre, alumina silicate fibre in production, work progress and escape from substrate surface, sucks human body
After can not degrade and cause healthy hidden danger, while also having certain pollution to environment.In recent years, China is in industrial circle, civil field
The Huimins policies such as " energy conservation ", " environmental protection ", " low-carbon ", " green ", " health " are all vigorously advocated, to novel heat insulation heat-barrier material field
Requirement be also continuously improved, magnesium silicate fiber has attracted much attention as a kind of material that human body is degradable, with magnesium silicate fiber felt work
Aerosil compound insulating material is prepared for substrate, it has also become the new hot spot in novel heat insulation heat-barrier material field.
201610203045.8 Chinese invention patent of application publication number discloses a kind of magnesium silicate fiber felt enhancing titanium dioxide
The preparation method of silica aerogel composite material, the composite material are combined by magnesium silicate fiber felt and aerosil,
Solvent replacement is carried out to gel felt body repeatedly with dehydrated alcohol in preparation process, finally using ethyl alcohol as supercritical drying medium
And the supercritical drying finished product under nitrogen auxiliary.Although the patented method can be used for preparing magnesium silicate fiber felt and titanium dioxide
Silica aerogel compound insulating material, but wherein used by supercritical drying equipment investment it is huge, production cost is excessively high, generally
Enterprise is difficult to bear.And in order to reduce production cost, atmosphere pressure desiccation substitution supercritical drying can be used.Atmosphere pressure desiccation is pair
Wet gel after alkylation carries out a kind of dry drying process to form aerogel structure of gradient increased temperature under ambient pressure, often
Press the equipment investment of seasoning small, production cost is relatively low.But there is also problems for constant pressure and dry: for example, normal pressure is dry
It needs to carry out repeatedly wet gel solvent replacement before dry, the manufacturing cycle of product is caused to extend；For another example, constant pressure and dry mostly uses front three
The chlorine-containing compounds such as base chlorosilane easily cause to corrode as alkylating reagent, by-product hydrochloric acid enormous amount to production equipment.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of preparation method of aeroge compound insulating material, the present invention
The method of offer can greatly shorten magnesium silicate fiber felt and aerosil is multiple while maintaining compared with low production cost
The manufacturing cycle of thermal insulation material is closed, and production equipment will not be caused to corrode.
The present invention provides a kind of preparation methods of aeroge compound insulating material, comprising the following steps:
A) silicon source, hexamethyldisilazane, pH adjusting agent and solvent are mixed, obtains silica solution precursor solution；
B) the silica solution precursor solution is impregnated into magnesium silicate fiber felt, is stood, form wet gel felt body；
C) the wet gel felt body is dipped into 40~90 DEG C of organosiloxane, it is dry that microwave heating is carried out after taking-up
It is dry, obtain aeroge compound insulating material.
Preferably, in step a), the silicon source include sodium metasilicate, acidic silicasol, alkaline silica sol, methyl orthosilicate and
One of ethyl orthosilicate is a variety of.
Preferably, in step a), content of the silicon source in silica solution precursor solution is 0.03~0.3g/mL；
Content of the hexamethyldisilazane in silica solution precursor solution is 5~15vol%.
Preferably, in step a), the solvent includes alcohols solvent and/or water.
Preferably, in step a), the mixed temperature is 2~7 DEG C.
Preferably, in step a), the pH value of the silica solution precursor solution is 5~11.
Preferably, in step b), the temperature of the standing is 15~40 DEG C；The time of the standing is 5~10min.
Preferably, in step c), the organosiloxane include methyltrimethoxysilane, methyltriethoxysilane,
Trimethylmethoxysilane, trimethylethoxysilane, hexamethyldisiloxane, dimethyldimethoxysil,ne and dimethyl two
One of Ethoxysilane is a variety of.
Preferably, in step c), the time of the immersion is 1~5h.
Preferably, in step c), the temperature of the micro-wave drying is 60~150 DEG C；The micro-wave drying
Microwave power is 80~130kW；The time of the micro-wave drying is 0.5~2.5h.
Compared with prior art, the present invention provides a kind of preparation methods of aeroge compound insulating material.The present invention mentions
The method of confession is the following steps are included: a) mix silicon source, hexamethyldisilazane, pH adjusting agent and solvent, before obtaining silica solution
Drive liquid solution；B) the silica solution precursor solution is impregnated into magnesium silicate fiber felt, is stood, form wet gel felt body；c)
The wet gel felt body is dipped into 40~90 DEG C of organosiloxane, micro-wave drying is carried out after taking-up, obtains airsetting
Glue compound insulating material.The present invention is wet by forming step b) on the basis of improveing silica solution precursor solution formula
Gel felt body impregnates in organic siloxane solution at a certain temperature, can disposably synchronize realization wet gel felt body removal of impurities,
Ageing, exchange of solvent and alkylation processing, to greatly shorten material manufacturing cycle.Meanwhile above-mentioned processing can also reduce material
Drying difficulty, it is subsequent again by cooperation micro-wave drying, material can be made to can be achieved with rapid draing under normal pressure, do not needed
Supercritical Drying Technology is reused, so as to significantly reduce the production cost of aeroge compound insulating material.Moreover, the present invention mentions
The preparation method of confession does not introduce chloride ion in its entire preparation process, therefore also smaller to the corrosion of device therefor.
Preparation method short preparation period provided by the invention, production cost is low, small to equipment loss, is highly suitable for magnesium silicate fiber felt
It is promoted the use of with the large-scale industrial production of aerosil compound insulating material.The results showed that using this
The method that invention provides is when preparing aeroge compound insulating material, and wet gel felt body cleaned, is aged, exchange of solvent, alkyl
Change total time-consuming≤5h with constant pressure and dry；The material good heat insulating being prepared, 25 DEG C of thermal coefficient≤0.025w/ (m.k).
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
The present invention provides a kind of preparation methods of aeroge compound insulating material, comprising the following steps:
A) silicon source, hexamethyldisilazane, pH adjusting agent and solvent are mixed, obtains silica solution precursor solution；
B) the silica solution precursor solution is impregnated into magnesium silicate fiber felt, is stood, form wet gel felt body；
C) the wet gel felt body is dipped into 40~90 DEG C of organosiloxane, it is dry that microwave heating is carried out after taking-up
It is dry, obtain aeroge compound insulating material.
In method provided by the invention, silicon source, hexamethyldisilazane, pH adjusting agent and solvent are mixed first.Its
In, the silicon source includes but is not limited in sodium metasilicate, acidic silicasol, alkaline silica sol, methyl orthosilicate and ethyl orthosilicate
It is one or more；The pH adjusting agent includes acidic ph modifier and/or alkaline pH adjusting agent, the acidic ph modifier packet
Include but be not limited to one of sulfuric acid, nitric acid, hydrofluoric acid, acetic acid and oxalic acid or a variety of, the alkaline pH adjusting agent includes but not
It is limited to one of sodium hydroxide, potassium hydroxide, lithium hydroxide and ammonium hydroxide or a variety of；The solvent include alcohols solvent and/or
Water, the alcohols solvent include but is not limited to one of methanol, ethyl alcohol, propyl alcohol, ethylene glycol and glycerine or a variety of.In this hair
In bright, content of the silicon source in silica solution precursor solution is preferably 0.03~0.3g/mL, concretely 0.03g/mL,
0.035g/mL、0.04g/mL、0.042g/mL、0.045g/mL、0.048g/mL、0.05g/mL、0.055g/mL、0.06g/mL、
0.062g/mL、0.065g/mL、0.068g/mL、0.07g/mL、0.08g/mL、0.09g/mL、0.1g/mL、0.15g/mL、
0.2g/mL, 0.23g/mL, 0.24g/mL, 0.25g/mL or 0.3g/mL.In one embodiment provided by the invention, with silicic acid
Sodium preferably in the form of sodium silicate aqueous solution (also known as: waterglass) and prepares silica solution presoma as silicon source, the sodium metasilicate
Other raw material objects of solution mix, and the concentration of the waterglass is preferably 5~10wt%, concretely 5wt%, 6wt%,
7wt%, 8wt%, 9wt% or 10wt%；The volume ratio of the waterglass and the silica solution precursor solution be preferably (30~
70): (70~80), more preferably (40~60): (76~77), concretely 40:76 or 60:77.Provided by the invention another
In one embodiment, using ethyl orthosilicate as silicon source, the volume of the ethyl orthosilicate and the silica solution precursor solution
Than preferably (10~30): 78.7, concretely 20:78.7.In the present invention, the hexamethyldisilazane is before silica solution
Drive liquid solution in content be preferably 5~15vol%, concretely 5vol%, 5.5vol%, 6vol%, 6.2vol%,
6.5vol%, 6.7vol%, 7vol%, 7.2vol%, 7.5vol%, 7.9vol%, 8vol%, 8.2vol%, 8.5vol%,
8.7vol%, 9vol%, 9.2vol%, 9.5vol%, 9.7vol%, 10vol%, 10.5vol%, 11vol%,
11.5vol%, 12vol%, 12.5vol%, 13vol%, 13.5vol%, 14vol%, 14.5vol% or 15vol%.At this
In invention, the mixed temperature is preferably 2~7 DEG C, concretely 2 DEG C, 3 DEG C, 4 DEG C, 5 DEG C, 6 DEG C or 7 DEG C.In the present invention
In, in order to promote dissolving each other for silicon source and hexamethyldisilazane, a certain amount of surface is preferably also added during the mixing
Activating agent, the surfactant include but is not limited to that cetyl trimethylammonium bromide, Brij and pool Lip river are husky
One of nurse is a variety of.In the present invention, the mixed mode and time are not particularly limited, each raw material object can be mixed
It closes uniform.After mixing, silica solution precursor solution is obtained, the pH value of the silica solution precursor solution is preferably 5
~11, concretely 5,5.2,5.4,5.6,5.8,6,6.5,7,7.5,8,8.5,9,9.5,10,10.2,10.4,10.6,10.8
Or 11.
In the present invention, after silica solution precursor solution being made, the silica solution precursor solution is impregnated into magnesium silicate
In fibrofelt.Wherein, the magnesium silicate fiber felt is preferably magnesium silicate fiber Nomex；The bulk density of the magnesium silicate fiber felt is excellent
It is selected as 70~150kg/m3, concretely 70kg/m3、75kg/m3、80kg/m3、85kg/m3、90kg/m3、96kg/m3、100kg/
m3、105kg/m3、110kg/m3、115kg/m3、120kg/m3、125kg/m3、128kg/m3、130kg/m3、135kg/m3、
140kg/m3、145kg/m3Or 150kg/m3；The fibre diameter of the magnesium silicate fiber felt is preferably 1~10 μm, concretely 1 μ
M, 2 μm, 3 μm, 4 μm, 5 μm, 6 μm, 7 μm, 8 μm, 9 μm or 10 μm.In the present invention, to the leaching of the silica solution precursor solution
Stain amount is not particularly limited, and magnesium silicate fiber felt is preferably made to reach saturation adsorbed state.After dipping, silica solution will be impregnated with
The magnesium silicate fiber felt of precursor solution is stood.Wherein, the temperature of the standing is preferably 15~40 DEG C, and concretely 15
DEG C, 16 DEG C, 17 DEG C, 18 DEG C, 19 DEG C, 20 DEG C, 21 DEG C, 22 DEG C, 23 DEG C, 24 DEG C, 25 DEG C (room temperature), 26 DEG C, 27 DEG C, 28 DEG C, 29
DEG C, 30 DEG C, 31 DEG C, 32 DEG C, 33 DEG C, 34 DEG C, 35 DEG C, 36 DEG C, 37 DEG C, 38 DEG C, 39 DEG C or 40 DEG C；The time of the standing is preferred
For 5~10min, concretely 5min, 5.5min, 6min, 6.5min, 7min, 7.5min, 8min, 8.5min, 9min,
9.5min or 10min.During standing, the silica solution precursor solution being impregnated into magnesium silicate fiber felt is gradually converted into wet solidifying
Glue.After standing, wet gel felt body is obtained.
In the present invention, after wet gel felt body being made, the wet gel felt body is dipped into 40~90 DEG C of organosilicon oxygen
In alkane.Wherein, the organosiloxane includes but is not limited to methyltrimethoxysilane, methyltriethoxysilane, trimethyl
Methoxy silane, trimethylethoxysilane, hexamethyldisiloxane, dimethyldimethoxysil,ne and dimethyl diethoxy
One of silane is a variety of, preferably hexamethyldisiloxane；The temperature of the organosiloxane concretely 40 DEG C, 45
DEG C, 50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C, 70 DEG C, 75 DEG C, 80 DEG C, 85 DEG C or 90 DEG C；The time of the immersion is preferably 1~5h, tool
Body can be 1h, 1.5h, 2h, 2.5h, 3h, 3.5h, 4h, 4.5h or 5h.In soaking process, wet gel felt body is in organosiloxane
Disposably synchronize cleaned, be aged, exchange of solvent and alkylation processing.After immersion, wet gel felt body is taken out, is carried out
Micro-wave drying.Wherein, the temperature of the micro-wave drying is preferably 60~150 DEG C, concretely 60 DEG C, 65 DEG C, 70
℃、75℃、80℃、85℃、90℃、95℃、100℃、105℃、110℃、115℃、120℃、125℃、130℃、135℃、
140 DEG C, 145 DEG C or 150 DEG C；The microwave power of the micro-wave drying is preferably 80~130kW, concretely 80kW,
85kW, 90kW, 95kW, 100kW, 105kW, 110kW, 115kW, 120kW, 125kW or 130kW；The micro-wave drying is excellent
Choosing carries out under normal pressure；The time of the micro-wave drying is preferably 0.5~2.5h, concretely 0.5h, 1h, 1.5h, 2h
Or 2.5h.After drying, magnesium silicate fiber felt and aerosil compound insulating material are obtained.
The present invention passes through the wet gel felt body for forming step b) on the basis of improveing silica solution precursor solution formula
It impregnates in organic siloxane solution at a certain temperature, can disposably synchronize removal of impurities, the ageing, solvent for realizing wet gel felt body
Exchange and alkylation processing, to greatly shorten material manufacturing cycle.Meanwhile above-mentioned processing can also reduce the dry difficult of material
Degree, it is subsequent again by cooperation micro-wave drying, material can be made to can be achieved with rapid draing under normal pressure, not need to reuse super
Critical dry technology, so as to significantly reduce the production cost of aeroge compound insulating material.Moreover, preparation provided by the invention
Method does not introduce chloride ion in its entire preparation process, therefore also smaller to the corrosion of device therefor.The present invention mentions
The preparation method short preparation period of confession, production cost is low, small to equipment loss, is highly suitable for magnesium silicate fiber felt and titanium dioxide
It is promoted the use of in the large-scale industrial production of silica aerogel compound insulating material.The results showed that being provided using the present invention
Method when preparing aeroge compound insulating material, wet gel felt body cleaned, is aged, exchange of solvent, alkylation and normal pressure
Dry total time-consuming≤5h；The material good heat insulating being prepared, 25 DEG C of thermal coefficient≤0.025w/ (m.k).
For the sake of becoming apparent from, it is described in detail below by following embodiment.
Embodiment 1
(1) match preparing silicon collosol presoma:
With the industrial waterglass solution of 5 DEG C of deionized water difference compound concentration 8wt%, the nitric acid solution of 20wt%；First
The dehydrated alcohol 10mL that 5 DEG C are injected in blender, opens stirring, sequentially adds nitre described in 6mL hexamethyldisilazane, 20mL
Acid solution persistently stirs 10min；Industrial waterglass solution described in 40mL is added thereto again, controls silica solution precursor solution
PH=5.4.
(2) choosing bulk density is 96kg/m3Magnesium silicate fiber Nomex (2~5 μm of fibre diameter) be substrate, tiled
It is placed in surrounding closed container, above-mentioned silica solution precursor solution is poured into the container, keep magnesium silicate fiber Nomex full
With absorption silica solution precursor solution.
(3) 10min will be stood by the Nomex of step (2) processing, and will form wet gel felt body.
(4) wet gel felt body is transferred in closed container, injects hexamethyldisiloxane, is totally submerged the wet gel felt
Body, 70 DEG C of heating water baths keep the temperature 3h, and wet gel felt body disposable synchronously completes removal of impurities, ageing, exchange of solvent and alkane during being somebody's turn to do
Baseization processing.
(5) it will be taken out from closed container by the wet gel felt body of step (4) processing, pair contained in the liquid phase in container
Produce ammonium hydroxide and nitric acid sodium impurity.Normal pressure microwave drying is carried out to the felt body of taking-up, drying temperature is 105 DEG C, microwave heating power
Magnesium silicate fiber felt and aerosil compound insulating material are obtained for 110kW, drying time 1h.
Thermal insulation material manufactured in the present embodiment is detected, as the result is shown: bulk density 137kg/m3, 25 DEG C of thermal coefficients
For 0.025w/ (m.k).
Embodiment 2
(1) match preparing silicon collosol presoma:
With the industrial waterglass solution of 5 DEG C of deionized water difference compound concentration 8wt%, the nitric acid solution of 20wt%；First
The dehydrated alcohol 10mL that 5 DEG C are injected in blender, opens stirring, sequentially adds nitre described in 6mL hexamethyldisilazane, 20mL
Acid solution persistently stirs 10min；Industrial waterglass solution described in 40mL is added thereto again, controls silica solution precursor solution
PH=5.4.
(2) choosing bulk density is 128kg/m3Magnesium silicate fiber Nomex (2~5 μm of fibre diameter) be substrate, put down
Laying is placed in surrounding closed container, and above-mentioned silica solution precursor solution is poured into the container, magnesium silicate fiber Nomex is made
Saturation absorption silica solution precursor solution.
(3) 10min will be stood by the Nomex of step (2) processing, and will form wet gel felt body.
(4) wet gel felt body is transferred in closed container, injects hexamethyldisiloxane, is totally submerged the wet gel felt
Body, 70 DEG C of heating water baths keep the temperature 3h, and wet gel felt body disposable synchronously completes removal of impurities, ageing, exchange of solvent and alkane during being somebody's turn to do
Baseization processing.
(5) it will be taken out from closed container by the wet gel felt body of step (4) processing, pair contained in the liquid phase in container
Produce ammonium hydroxide and nitric acid sodium impurity.Normal pressure microwave drying is carried out to the felt body of taking-up, drying temperature is 105 DEG C, microwave heating power
Magnesium silicate fiber felt and aerosil compound insulating material are obtained for 110kW, drying time 1h.
Thermal insulation material manufactured in the present embodiment is detected, as the result is shown: bulk density 183kg/m3, 25 DEG C of thermal coefficients
For 0.022w/ (m.k).
Embodiment 3
(1) match preparing silicon collosol presoma:
With the industrial waterglass solution of 5 DEG C of deionized water difference compound concentration 8wt%, the nitric acid solution of 20wt%；First
Industrial waterglass solution described in 60mL is injected in blender, stirring is opened, 0.015g cetyl trimethylammonium bromide is added,
10min is persistently stirred, 7.5mL hexamethyldisilazane is added, continues to stir 10min, it is molten to be eventually adding nitric acid described in 9.5mL
Liquid controls silica solution precursor solution pH=10.2.
(2) choosing bulk density is 96kg/m3Magnesium silicate fiber Nomex (2~5 μm of fibre diameter) be substrate, tiled
It is placed in surrounding closed container, above-mentioned silica solution precursor solution is poured into the container, keep magnesium silicate fiber Nomex full
With absorption silica solution precursor solution.
(3) 10min will be stood by the Nomex of step (2) processing, and will form wet gel felt body.
(4) wet gel felt body is transferred in closed container, injects hexamethyldisiloxane, is totally submerged the wet gel felt
Body, 70 DEG C of heating water baths keep the temperature 3h, and wet gel felt body disposable synchronously completes removal of impurities, ageing, exchange of solvent and alkane during being somebody's turn to do
Baseization processing.
(5) it will be taken out from closed container by the wet gel felt body of step (4) processing, pair contained in the liquid phase in container
Produce ammonium hydroxide and nitric acid sodium impurity.Normal pressure microwave drying is carried out to the felt body of taking-up, drying temperature is 105 DEG C, microwave heating power
Magnesium silicate fiber felt and aerosil compound insulating material are obtained for 110kW, drying time 1h.
Thermal insulation material manufactured in the present embodiment is detected, as the result is shown: bulk density 131kg/m3, 25 DEG C of thermal coefficients
For 0.024w/ (m.k).
Embodiment 4
(1) match preparing silicon collosol presoma:
With the industrial waterglass solution of 5 DEG C of deionized water difference compound concentration 8wt%, the nitric acid solution of 20wt%；First
Industrial waterglass solution described in 60mL is injected in blender, stirring is opened, 0.015g cetyl trimethylammonium bromide is added,
10min is persistently stirred, 7.5mL hexamethyldisilazane is added, continues to stir 10min, it is molten to be eventually adding nitric acid described in 9.5mL
Liquid controls silica solution precursor solution pH=10.2.
(2) choosing bulk density is 128kg/m3Magnesium silicate fiber Nomex (2~5 μm of fibre diameter) be substrate, put down
Laying is placed in surrounding closed container, and above-mentioned silica solution precursor solution is poured into the container, magnesium silicate fiber Nomex is made
Saturation absorption silica solution precursor solution.
(3) 10min will be stood by the Nomex of step (2) processing, and will form wet gel felt body.
(4) wet gel felt body is transferred in closed container, injects hexamethyldisiloxane, is totally submerged the wet gel felt
Body, 70 DEG C of heating water baths keep the temperature 3h, and wet gel felt body disposable synchronously completes removal of impurities, ageing, exchange of solvent and alkane during being somebody's turn to do
Baseization processing
(5) it will be taken out from closed container by the wet gel felt body of step (4) processing, pair contained in the liquid phase in container
Produce ammonium hydroxide and nitric acid sodium impurity.Normal pressure microwave drying is carried out to the felt body of taking-up, drying temperature is 105 DEG C, microwave heating power
Magnesium silicate fiber and aerosil compound insulating material are obtained for 110kW, drying time 1h.
Thermal insulation material manufactured in the present embodiment is detected, as the result is shown: bulk density 173kg/m3, 25 DEG C of thermal coefficients
For 0.021w/ (m.k).
Embodiment 5
(1) match preparing silicon collosol presoma:
With 5 DEG C of the deionized waters oxalic acid solution that compound concentration is 0.1mol/L respectively, the ammonia spirit of 0.2mol/L；First
The ethanol solution 30mL that 5 DEG C are injected in blender, opens stirring, is subsequently added into 20mL ethyl orthosilicate, adds 5 DEG C
Deionized water 15mL, persistently stir 10min, be subsequently added into oxalic acid solution described in 6mL, persistently stir 40min, add
5.5mL hexamethyldisilazane is eventually adding ammonia spirit described in 2.2mL, controls silica solution precursor solution pH=5.6.
(2) choosing bulk density is 96kg/m3Magnesium silicate fiber Nomex (2~5 μm of fibre diameter) be substrate, tiled
It is placed in surrounding closed container, above-mentioned silica solution precursor solution is poured into the container, keep magnesium silicate fiber Nomex full
With absorption silica solution precursor solution.
(3) 5min will be stood by the Nomex of step (2) processing, and will form wet gel felt body.
(4) wet gel felt body is transferred in closed container, injects hexamethyldisiloxane, is totally submerged the wet gel felt
Body, 70 DEG C of heating water baths keep the temperature 3h, and wet gel felt body disposable synchronously completes ageing, exchange of solvent and alkylation during being somebody's turn to do
Processing.
(5) it will be taken out from closed container by the wet gel felt body of step (4) processing, pair contained in the liquid phase in container
Produce ammonium hydroxide, ammonium oxalate and ethyl alcohol.Normal pressure microwave drying is carried out to the felt body of taking-up, drying temperature is 105 DEG C, microwave heating power
Magnesium silicate fiber and aerosil compound insulating material are obtained for 110kW, drying time 1h.
Thermal insulation material manufactured in the present embodiment is detected, as the result is shown: bulk density 142kg/m3, 25 DEG C of thermal coefficients
For 0.023w/ (m.k).
Embodiment 6
(1) match preparing silicon collosol presoma:
With 5 DEG C of the deionized waters oxalic acid solution that compound concentration is 0.1mol/L respectively, the ammonia spirit of 0.2mol/L；First
The ethanol solution 30mL that 5 DEG C are injected in blender, opens stirring, is subsequently added into 20mL ethyl orthosilicate, adds 5 DEG C
Deionized water 15mL, persistently stir 10min, be subsequently added into oxalic acid solution described in 6mL, persistently stir 40min, add
5.5mL hexamethyldisilazane is eventually adding ammonia spirit described in 2.2mL, controls silica solution precursor solution pH=5.6.
(2) choosing bulk density is 128kg/m3Magnesium silicate fiber Nomex (2~5 μm of fibre diameter) be substrate, put down
Laying is placed in surrounding closed container, and above-mentioned silica solution precursor solution is poured into the container, magnesium silicate fiber Nomex is made
Saturation absorption silica solution precursor solution.
(3) 5min will be stood by the Nomex of step (2) processing, and will form wet gel felt body.
(4) wet gel felt body is transferred in closed container, injects hexamethyldisiloxane, is totally submerged the gel felt
Body, 70 DEG C of heating water baths keep the temperature 3h, and wet gel felt body disposable synchronously completes ageing, exchange of solvent and alkylation during being somebody's turn to do
Processing.
(5) it will be taken out from closed container by the wet gel felt body of step (4) processing, pair contained in the liquid phase in container
Produce ammonium hydroxide, ammonium oxalate and ethyl alcohol.Normal pressure microwave drying is carried out to the felt body of taking-up, drying temperature is 105 DEG C, microwave heating power
Magnesium silicate fiber and aerosil compound insulating material are obtained for 110kW, drying time 1h.
Thermal insulation material manufactured in the present embodiment is detected, as the result is shown: bulk density 188kg/m3, 25 DEG C of thermal coefficients
For 0.019w/ (m.k).
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of aeroge compound insulating material, comprising the following steps:
A) silicon source, hexamethyldisilazane, pH adjusting agent and solvent are mixed, obtains silica solution precursor solution；
B) the silica solution precursor solution is impregnated into magnesium silicate fiber felt, is stood, form wet gel felt body；
C) the wet gel felt body is dipped into 40~90 DEG C of organosiloxane, micro-wave drying is carried out after taking-up, is obtained
To aeroge compound insulating material.
2. preparation method according to claim 1, which is characterized in that in step a), the silicon source includes sodium metasilicate, acidity
One of silica solution, alkaline silica sol, methyl orthosilicate and ethyl orthosilicate are a variety of.
3. preparation method according to claim 1, which is characterized in that in step a), the silicon source is in silica solution presoma
Content in solution is 0.03~0.3g/mL；
Content of the hexamethyldisilazane in silica solution precursor solution is 5~15vol%.
4. preparation method according to claim 1, which is characterized in that in step a), the solvent include alcohols solvent and/
Or water.
5. preparation method according to claim 1, which is characterized in that in step a), the mixed temperature is 2~7 DEG C.
6. preparation method according to claim 1, which is characterized in that in step a), the silica solution precursor solution
PH value is 5~11.
7. preparation method according to claim 1, which is characterized in that in step b), the temperature of the standing is 15~40
℃；The time of the standing is 5~10min.
8. preparation method according to claim 1, which is characterized in that in step c), the organosiloxane includes methyl
Trimethoxy silane, methyltriethoxysilane, trimethylmethoxysilane, trimethylethoxysilane, two silicon oxygen of hexamethyl
One of alkane, dimethyldimethoxysil,ne and dimethyl diethoxysilane are a variety of.
9. preparation method according to claim 1, which is characterized in that in step c), the time of the immersion is 1~5h.
10. preparation method according to claim 1, which is characterized in that in step c), the temperature of the micro-wave drying
It is 60~150 DEG C；The microwave power of the micro-wave drying is 80~130kW；The time of the micro-wave drying is 0.5
~2.5h.
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| CN112062538A (en) * | 2019-05-23 | 2020-12-11 | 李振声 | Preparation method of silicon dioxide aerogel heat-insulating material by normal-pressure microwave plasma method |
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