CN106115722A - A kind of preparation method of aerosil - Google Patents
A kind of preparation method of aerosil Download PDFInfo
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- CN106115722A CN106115722A CN201610466166.1A CN201610466166A CN106115722A CN 106115722 A CN106115722 A CN 106115722A CN 201610466166 A CN201610466166 A CN 201610466166A CN 106115722 A CN106115722 A CN 106115722A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/16—Preparation of silica xerogels
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
Abstract
The invention discloses the preparation method of aerosil, by molten for flyash acid sludge alkali, obtain sodium silicate solution；Again by resins exchange, and addition template prepares SiO2The hydrosol；Then after the hydrosol being stood aging formation hydrogel, then soak is carried out in normal hexane solvent displacement, after solvent is replaced, then template is removed；Finally use silane coupler gel surface to be modified, is dried, i.e. can get SiO2Aeroge.Replace expensive organo-silicon compound as raw material using solid waste coal ash acid sludge herein, be simultaneously introduced template, use constant pressure and dry or vacuum drying and the method for surface modification, orderly mesoporous SiO can be prepared2Aeroge, not only greatly reduces production cost and equipment cost, also improves the safety of dry run, simultaneously products obtained therefrom excellent performance.
Description
Technical field
The invention belongs to field of solid waste comprehensive utilization, prepare two with flyash acid sludge for raw material particularly to one
The method of silica aerogel.
Background technology
SiO2Aeroge is a kind of by nanometer scale particle accumulation, and the novel amorphous solid-state with air as disperse medium is received
Rice material.The special performance that this new material is had is mainly included in the high grade of transparency of visible region, has the lowest thermal conductance
Rate, the lowest velocity of sound, high-specific surface area etc..Based on these performances, SiO2Aeroge High Efficiency Thermal insulation system, acoustic impedance and
The aspects such as radioluminescence device, Liquid rocket propulsion device and catalyst carrier are widely used.
SiO2The prior synthesizing method of aeroge is using organic alkoxide as silicon source, uses sol-gel technology, and combines
Supercritical drying prepares.But, traditional handicraft does not meets the condition of large-scale production, it is difficult to realize the business metaplasia of aeroge
Producing, its reason is roughly divided into 2 points: (1) organic alkoxide includes tetraethyl orthosilicate (TEOS), methyl silicate (TMOS), silane
Deng, but these organic alkoxide costs are high, part has toxicity；(2) supercritical drying process typically uses the organic solvents such as alcohols
(such as ethanol or normal propyl alcohol) or CO2As dry medium, under high pressure-temperature or high pressure low temperature environment, form aeroge, to equipment
Requiring height, production process has certain danger, and the longest, expensive.Therefore, in recent years, how research utilizes low
The inorganic compound of cost is raw material, by constant pressure and dry process synthetic silica aeroge, has become as scholars and life
Produce unit focus of attention.
It is known that production cost can be reduced with industrial waterglass for raw material.2004, A.Venkateswara Rao etc.
With industrial waterglass as presoma, sol-gel process is still used to prepare hydrogel, and by hexamethyldisiloxane
(HMDZ) as surface modifier, under the conditions of constant pressure and dry, SiO is successfully synthesized2Aeroge.Meanwhile, A.Venkateswara
Rao etc. have studied different Na also for property2SiO3/H2O mol ratio and the gel ageing time shadow to aeroge physical property
Ring.2006, the aniso-sample of history of Dalian University of Technology, with industrial waterglass for silicon source, used sol-gel technology to be prepared into
To hydrogel, by step solvent exchange and a modification, the most successfully prepare SiO2Aeroge.
It addition, using flyash, kieselguhr and rice husk is the approach that raw material also reduces production cost, as China is special
Profit CN101244825 is using kieselguhr as preparing SiO2The raw material of aeroge, Chinese patent CN1669921, CNIO1259964,
CN1724353 is then using rice husk as preparing SiO2The raw material of aeroge.
Flyash acid sludge refer to flyash through acid molten carry aluminum after solid waste, wherein dioxide-containing silica can reach
50%～85%, if flyash acid sludge not being used, the existence of flyash acid sludge not only can take a large amount of soil, also can be tight
The most how heavily contaminated environment, process and utilize flyash acid sludge to become a highly important problem.
Summary of the invention
In view of this, it is an object of the invention to provide one and prepare aerosil with flyash acid sludge for raw material
Method, for the problem of current flyash acid sludge comprehensive utilization scarce capacity, give a kind of new flyash acid sludge and utilize
Thinking and technology, meanwhile, the process equipment of this method is simple, can be substantially reduced SiO2The production cost of aeroge.
Flyash acid sludge in the present invention is that flyash passes through the tailings after " a step acid pasting " produces aluminium oxide, specifically
Ground, is after flyash passes through " a step acid pasting " dissolving aluminium oxide, through the tailings that solid-liquid separation obtains." a step acid is molten for flyash
Method " extract aluminium oxide technique may refer to Chinese patent CN102145905A, it is incorporated into the application by way of reference
In.Specifically, the preparation method of the tailings after described flyash extracts aluminium oxide comprises the following steps: a) be crushed to by flyash
Below 100 mesh, such as 150 mesh or 200 mesh (Taylor standard sieve), add water and be configured to the slip that solid content is 20～40wt%, warp
Wet magnetic separation removes ferrum, makes iron content in flyash be down to below 1.0wt%, filters to obtain filter cake；B) to the filter cake of step a) gained
Middle addition hydrochloric acid reacts, and then carries out solid-liquid separation, the tailings obtained.In described step a), described wet magnetic separation removes ferrum
The equipment used is vertical-ring magnetic separator.Its concrete structure may refer to patent documentation CN102145905A.In described step b),
Concentration of hydrochloric acid is 20～37wt%；In described hydrochloric acid, HCl is 4:1～9:1 with the mol ratio of aluminium oxide in flyash；The temperature of reaction
Degree is 100～200 DEG C；The time of reaction is 0.5～4.0 hour；The pressure of reaction is 0.1～2.5MPa.Preferably, described step
In b), concentration of hydrochloric acid is 20～30wt%；In described hydrochloric acid, HCl is 4.5:1～6 with the mol ratio of aluminium oxide in flyash:
1；The temperature of reaction is 130～150 DEG C；The time of reaction is 1.5～2.5 hours；The pressure of reaction is 0.3～1.0MPa.When
So, it will be appreciated by those skilled in the art that in the present invention, obtain flyash acid sludge and can also carry out pretreatment before the reaction, such as
First it is washed to neutrality, is dried the most again.
The preparation method of the aerosil that the present invention provides includes:
1) alkali is molten
Being reacted with sodium hydroxide solution by flyash acid sludge, question response carries out solid-liquid separation after terminating, and obtains sodium silicate molten
Liquid；
2) hydrosol is prepared
By sodium silicate solution by strongly acidic styrene's cation exchange resin, obtain the first solution containing silicic acid；
Template is dissolved in alcohol, obtains the second solution；Then, under conditions of stirring, add in described first solution
Entering the second solution, obtain mixed liquor, in described mixed liquor, silicic acid is 1:1～1:2 with the mass ratio of template；Alkali liquor is utilized to regulate
The pH value of described mixed liquor is 4～7, after reaction terminates, obtains the hydrosol；
3) colloidal sol is aging
The hydrosol is stood in water aging, obtain SiO2Hydrogel；
4) solvent displacement
Being immersed in alkane solvent by gel after aging and carry out solvent displacement, be then dried to obtain after solvent displacement is solidifying
Glue；
5) removed template method
Gel after being replaced by solvent is placed in the alcoholic solution of hydrochloric acid acidifying, is heated to reflux, to remove the template in gel
Agent, then solid-liquid separation, washing, obtain the gel after removed template method；
6) modification of gel
Gel silane coupler after removed template method is modified, is then dried, obtains aerosil.
Step 1 in the present invention) in, flyash acid sludge reacts with sodium hydroxide solution, mainly produces sodium silicate and lacks
The impurity such as amount sodium metaaluminate (remaining not poor with the aluminium oxide active of hydrochloric acid reaction in acid sludge), reaction temperature is preferably 70 DEG C
～150 DEG C, more preferably 90 DEG C～100 DEG C, with the most generation sodium silicate, question response carries out solid-liquid separation after terminating,
To sodium silicate solution.
Step 2 in the present invention) in, by sodium silicate solution by strongly acidic styrene's cation exchange resin, obtain the
One solution；Wherein, described strongly acidic styrene's cation exchange resin is known in the art, preferably D001,732 or 42 trees
Fat.In this process, controlling the described sodium silicate solution flow velocity by above-mentioned resin, the pH value making effluent is 2～3, thus
Obtain the silicate solution after imurity-removal and ion exchange, the i.e. first solution, simplify preparation process, wherein Al element impurity
Content is not more than 0.1wt%.
In step 2) in, described template for it is known in the art that preferably P123, i.e. PULLRONIC F68-polyoxy
Ethylene triblock polymer；In described mixed liquor, silicic acid is preferably 1:1～1:1.5 with the mass ratio of template, such as 1:1.3,
Stirring is fully reacted；Utilize alkali liquor regulation solution pH value be 4～7, preferably 5～6, alkali liquor be preferably sodium hydroxide,
Potassium hydroxide or the one of ammonia.
Step 3 in the present invention) in, the hydrosol of preparation is stood aging in water, the most aging 12～24h, colloidal sol
Aging known in the art, repeat no more here.
Step 4 in the present invention) in, utilize alkane solution that the gel after aging is carried out solvent displacement, thus utilize alkane
Hydrocarbon solvent displaces the water in gel, to improve product follow-up pore-forming effect；Preferably, described alkane is containing 5～8 carbon atoms
Alkane, more preferably normal hexane；Described baking temperature is 60 DEG C～100 DEG C, preferably 70 DEG C～80 DEG C.
Step 5 in the present invention) in, the gel after being replaced by solvent is placed in the alcoholic solution of hydrochloric acid acidifying, carries out template
Agent removes；Wherein, the alcoholic solution of described hydrochloric acid acidifying prepares for adding a small amount of hydrochloric acid solution in alcohol, such as, and hydrochloric acid acidifying
In alcoholic solution, the content of hydrochloric acid is 0.1～1wt%, and the content of described alcohol is not less than 90wt%, such as 95wt%, with simple
Alcohol is compared, and the alcoholic solution of acidifying is more beneficial for improving template removal effect in the reaction；The described process that is heated to reflux is preferably
At 80 DEG C, backflow 10～12h, can repeat, such as, be repeated once or twice.Described solid-liquid separation and washing process are
It is known in the art that and such as separated by filtration, then utilize alcohol to wash, the gel after separating to reduce template
Residual.
Step 6 in the present invention) in, utilize silane coupler that gel is modified, described silane coupler is ability
Territory is known, preferably trim,ethylchlorosilane, dimethyldichlorosilane, methyl trichlorosilane, HMDS and hexamethyl
One or more in two silicon ethers；Modifying process obtains modified solvent for being dissolved in alcohol by described silane coupler, then utilizes
Modified solvent described in immersing hydrogels after removed template method, such as dipping 6h～12h；When gel after dipping is dried,
Can carry out constant pressure and dry or drying under reduced pressure, baking temperature can be 60 DEG C～180 DEG C, preferably 80 DEG C～120 DEG C, with removing
Alcohol.
In the present invention, alcohol used can be carbon number be the alkylol of 2～6, such as ethanol, propanol, butanol, penta
Alcohol, hexanol etc., it is preferable that described alcohol is ethanol.
Compared with conventional art, present invention have the advantage that
(1) expensive organo-silicon compound are replaced to produce SiO with cheap flyash acid sludge2Aeroge, reduces production
Cost；Simultaneously as flyash acid sludge has had the biggest specific surface area, and chemism is high, uses sodium hydroxide
It is easier to carry out to the dissolution again of the silicon oxide in flyash acid sludge；Flyash acid sludge due to through peracid treatment eliminate ferrum oxide,
The impurity such as calcium oxide, titanium oxide, as raw material production SiO2Extra removal step is need not during aeroge
To the product that purity is higher；
(2) present invention is by adding template P123 on the basis of above step, can prepare orderly mesoporous
SiO2Aeroge.
(3) through the process of above each step, the aeroge excellent performance that the present invention prepares, have low-density (0.02～
0.2g/cm3), high-specific surface area (600～1500m2/ g), the feature of high hydrophobicity (130 °～160 °), its aperture be 2～
30nm。
(4) process equipment of this method is simple, is possible not only to be substantially reduced mesoporous SiO2The production cost of aeroge, and
Effect on environment is little.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described, but the present invention is not limited to detailed description below.
The preparation embodiment of flyash acid sludge
Raw material uses certain steam power plant's output recirculating fluidized bed coal dust, and its chemical composition is as shown in table 1.
Table 1 circulating fluid bed coal ash chemical composition (wt%)
Take fluidization bed fly ash, be crushed to 200 mesh, add water and make the slurry that solid content is 33wt%, use vertical ring magnetic separation
Machine (sees Chinese patent CN102145905A, and entire contents is incorporated herein), magnetic separation two under field intensity is 1.5 ten thousand GS
Time, after filter press filter pressing, obtain the filter cake that solid content is 37.5wt%；Adding concentration in described filter cake is 28wt%
Technical hydrochloric acid carry out sour molten reaction, the HCl in hydrochloric acid is 5:1 with the mol ratio of the aluminium oxide in flyash, reaction temperature 150
DEG C, reaction pressure 1.0MPa, response time 2h, product separates through filter press filter pressing, obtains flyash acid sludge.
For the ease of the metering of following example, described acid sludge is washed, to obtain aluminum-extracted pulverized fuel ash further after drying residual
Slag.
Using residue of aluminum-extracted pulverized fuel ash produced above as the raw material of following example, in described residue: by weight,
SiO268wt%, Al2O312wt%, TiO23.5wt%, MgO 2wt%, CaO 4wt%, other is miscellaneous for residual charcoal etc. for surplus
Matter.
Other are commercially available conventional products, and chemical drugs used is analytical pure.
The method of testing of the present embodiment is described as follows:
Micromeritics company of the U.S. full-automatic specific surface area of ASAP2010 type is used to survey with pore analysis instrument
Fixed.The N of sample2Adsorption/desorption isotherms is to be measured from a temperature of liquid nitrogen；Then by P/P in isothermal line0Be 0.05～
The data in 0.35 interval obtain specific surface area according to BET Equation for Calculating；In conjunction with BJH method and N2De contamination isothermal line calculated hole diameters
Distribution；Pore volume presses P/P0N when 0.952Adsorbance calculates.Remaining is all measured by this area conventional method.
The sample measured need to dry 12h through 120 DEG C.
Embodiment 1
1kg residue is mixed with 5L sodium hydroxide (mass fraction is 15%) solution, is placed in reactor, sets its reaction
Temperature is 90 DEG C, and the response time is 120min；After filtering, obtain filtrate, filtrate is handed over by strongly acidic styrene's cation
Change resin, obtain the silicic acid that pH value is 2～3, then P123 is dissolved in ethanol solution, then under conditions of stirring, to silicic acid
Being slowly added to P123 solution in solution, silicic acid is 1.3 with the mass ratio of P123, stirs 3h, molten with the regulation of 1mol/l ammonia spirit
The pH value of liquid is 5, stirs 1min, after terminating to reaction, is stood by reactant, makes SiO2Hydrogel；Gained hydrogel is at water
After the aging 24h of middle standing, the gel 24h prepared with normal hexane immersion, then the gel of preparation is moved in drying baker, permanent at 70 DEG C
Temperature 4h, is then placed in the gel of preparation in the ethanol solution (content of hydrochloric acid is 1wt%) of hydrochloric acid acidifying, refluxes at 80 DEG C
12h.With trim,ethylchlorosilane solution, the gel of preparation is carried out surface modification 12h afterwards, finally modified gel is placed in
100 DEG C of freeze-day with constant temperature 6h, obtain orderly mesoporous SiO2Aeroge.
After measured, the SiO obtained2Aeroge specific surface area is 1000m2/ g, pore volume is 2.03cm3/ g, apparent density is
0.075g/cm3, contact angle is 148 °, and average pore size is 7.46nm.
Embodiment 2
1kg residue is mixed with 5L sodium hydroxide (mass fraction is 15%) solution, is placed in reactor, sets its reaction
Temperature is 90 DEG C, and the response time is 120min；After filtering, obtain filtrate, filtrate is handed over by strongly acidic styrene's cation
Change resin, obtain the silicic acid that pH value is 2～3, then P123 is dissolved in the solution of ethanol and hydrochloric acid, then in the condition of stirring
Under, in silicate solution, it being slowly added to P123 solution, silicic acid is 1.3 with the mass ratio of P123, stirs 3h, adjusts with 1mol/l ammonia
The pH value of joint solution is 5, stirs 1min, after terminating to reaction, obtains the hydrosol；Gained hydrogel obtains after standing aging 24h
Gel, the gel 24h prepared with normal hexane immersion, then the gel of preparation is moved in drying baker, and constant temperature 4h at 70 DEG C, then will
The gel of preparation is placed in the ethanol solution (content of hydrochloric acid is 0.6wt%) of hydrochloric acid acidifying, and reflux at 80 DEG C 12h.Use afterwards
Trim,ethylchlorosilane solution carries out surface modification 12h to the gel of preparation, finally modified gel is put in vacuum drying oven
Interior 4h, obtains orderly mesoporous SiO2Aeroge.
After measured, the SiO obtained2Aeroge specific surface area is 1200m2/ g, pore volume is 2.26cm3/ g, apparent density is
0.064g/cm3, contact angle is 152 °, and average pore size is 7.89nm.
Embodiment 3
1kg residue is mixed with 5L sodium hydroxide (mass fraction is 15%) solution, is placed in reactor, sets its reaction
Temperature is 90 DEG C, and the response time is 120min；After filtering, obtain filtrate, filtrate is handed over by strongly acidic styrene's cation
Change resin, obtain the silicic acid that pH value is 2～3, then P123 is dissolved in the solution of ethanol and hydrochloric acid, then in the condition of stirring
Under, in silicate solution, it being slowly added to P123 solution, silicic acid is 1.4 with the mass ratio of P123, stirs 3h, adjusts with 1mol/l ammonia
The pH value of joint solution is 5, stirs 1min, after terminating to reaction, obtains the hydrosol；Gained hydrogel obtains after standing aging 24h
Gel, the gel 24h prepared with normal hexane immersion, then the gel of preparation is moved in drying baker, and constant temperature 4h at 70 DEG C, then will
The gel of preparation is placed in the ethanol solution (content of hydrochloric acid is 0.3wt%) of hydrochloric acid acidifying, and reflux at 80 DEG C 12h.Use afterwards
HMDS carries out surface modification 12h to the gel of preparation, is finally put in vacuum drying oven by modified gel
4h, obtains orderly mesoporous SiO2Aeroge.
After measured, the SiO obtained2Aeroge specific surface area is 1080m2/ g, pore volume is 2.15cm3/ g, apparent density is
0.090g/cm3, contact angle is 144 °, and average pore size is 7.35nm.
Embodiment 4
1kg residue is mixed with 5L sodium hydroxide (mass fraction is 15%) solution, is placed in reactor, sets its reaction
Temperature is 90 DEG C, and the response time is 120min；After filtering, obtain filtrate, filtrate is handed over by strongly acidic styrene's cation
Change resin, obtain the silicic acid that pH value is 2～3, then P123 is dissolved in the solution of ethanol and hydrochloric acid, then in the condition of stirring
Under, in silicate solution, it being slowly added to P123 solution, silicic acid is 1.1 with the mass ratio of P123, stirs 3h, adjusts with 1mol/l ammonia
The pH value of joint solution is 5, stirs 1min, after terminating to reaction, obtains the hydrosol；Gained hydrogel obtains after standing aging 24h
Gel, the gel 24h prepared with normal hexane immersion, then the gel of preparation is moved in drying baker, and constant temperature 4h at 70 DEG C, then will
The gel of preparation is placed in the ethanol solution (content of hydrochloric acid is 0.4wt%) of hydrochloric acid acidifying, and reflux at 80 DEG C 12h.Use afterwards
Trim,ethylchlorosilane solution carries out surface modification 3h to the gel of preparation, is finally put in vacuum drying oven by modified gel
4h, obtains orderly mesoporous SiO2Aeroge.
After measured, the SiO obtained2Aeroge specific surface area is 800m2/ g, pore volume is 1.89cm3/ g, apparent density is
0.13g/cm3, contact angle is 136 °, and average pore size is 8.54nm.
Embodiment 5
1kg residue is mixed with 5L sodium hydroxide (mass fraction is 15%) solution, is placed in reactor, sets its reaction
Temperature is 90 DEG C, and the response time is 120min；After filtering, obtain filtrate, filtrate is handed over by strongly acidic styrene's cation
Change resin, obtain the silicic acid that pH value is 2～3, then P123 is dissolved in the solution of ethanol and hydrochloric acid, then in the condition of stirring
Under, in silicate solution, it being slowly added to P123 solution, silicic acid is 1.5 with the mass ratio of P123, stirs 3h, adjusts with 1mol/l ammonia
The pH value of joint solution is 5, stirs 1min, after terminating to reaction, obtains the hydrosol；Gained hydrogel obtains after standing aging 24h
Gel, the gel 24h prepared with normal hexane immersion, then the gel of preparation is moved in drying baker, and constant temperature 4h at 70 DEG C, then will
The gel of preparation is placed in the ethanol solution (content of hydrochloric acid is 1wt%) of hydrochloric acid acidifying, and reflux at 80 DEG C 12h.Afterwards with six
Methyl disilazane carries out surface modification 3h to the gel of preparation, and modified gel is finally put in 4h in vacuum drying oven,
Obtain orderly mesoporous SiO2Aeroge.
After measured, the SiO obtained2Aeroge specific surface area is 730m2/ g, pore volume is 1.65cm3/ g, apparent density is
0.18g/cm3, contact angle is 132 °, and average pore size is 8.97nm.
Claims (10)
1. a preparation method for aerosil, comprises the following steps:
1) alkali is molten
Being reacted with sodium hydroxide solution by flyash acid sludge, question response carries out solid-liquid separation after terminating, and obtains sodium silicate solution；
2) hydrosol is prepared
By sodium silicate solution by strongly acidic styrene's cation exchange resin, obtain the first solution containing silicic acid；
Template is dissolved in alcohol, obtains the second solution；Then, under conditions of stirring, in described first solution, the is added
Two solution, obtain mixed liquor, and in described mixed liquor, silicic acid is 1:1～1:2 with the mass ratio of template；Utilize alkali liquor regulation described
The pH value of mixed liquor is 4～7, after reaction terminates, obtains the hydrosol；
3) colloidal sol is aging
The hydrosol is stood in water aging, obtain SiO2Hydrogel；
4) solvent displacement
Gel after aging is immersed in alkane solvent and carries out solvent displacement, be then dried to obtain the gel after solvent displacement；
5) removed template method
Gel after being replaced by solvent is placed in the alcoholic solution of hydrochloric acid acidifying, is heated to reflux, to remove the template in gel, so
Rear solid-liquid separation, washing, obtain the gel after removed template method；
6) modification of gel
Gel silane coupler after removed template method is modified, is then dried, obtains aerosil.
Preparation method the most according to claim 1, it is characterised in that step 2) in, described template is P123, silicic acid with
The mass ratio of template P123 is 1～1.5.
Preparation method the most according to claim 1 and 2, it is characterised in that step 4) in, described alkane is containing 5～8 carbon
The alkane of atom, preferably normal hexane；Described baking temperature is 60 DEG C～100 DEG C, preferably 70 DEG C～80 DEG C.
4. according to the preparation method according to any one of claims 1 to 3, it is characterised in that step 5) in, described hydrochloric acid is acidified
Alcoholic solution in, the content of hydrochloric acid is 0.1～1wt%, the content of described alcohol be not less than 90wt%.
5. according to the preparation method according to any one of Claims 1 to 4, it is characterised in that step 5) in, in solid-liquid separation
After, utilize alcohol that isolated gel is washed.
6. according to the preparation method according to any one of Claims 1 to 5, it is characterised in that step 6) in, described silane coupled
Agent is in trim,ethylchlorosilane, dimethyldichlorosilane, methyl trichlorosilane, HMDS and hexamethyldisiloxane
One or more；Modifying process obtains modified solvent for being dissolved in alcohol by described silane coupler, then utilizes removed template method
After immersing hydrogels described in modified solvent.
7. according to the preparation method according to any one of claim 1～6, it is characterised in that step 6) in, described being dried is
Constant pressure and dry or vacuum drying, baking temperature is 60 DEG C～180 DEG C.
8. according to the preparation method according to any one of claim 1～7, it is characterised in that step 1) in, the acid of described flyash
Slag is the tailings formed after flyash produces aluminium oxide by a step acid pasting.
Preparation method the most according to claim 8, it is characterised in that described flyash extracts the system of the tailings after aluminium oxide
Preparation Method comprises the following steps: flyash a) is crushed to below 100 mesh, adds water and is configured to the material that solid content is 20～40wt%
Slurry, through wet magnetic separation except ferrum, makes iron content in flyash be down to below 1.0wt%, filters to obtain filter cake；B) to step a) gained
Filter cake adds hydrochloric acid react, then carry out solid-liquid separation, the tailings obtained；
In described step b), concentration of hydrochloric acid is 20～37wt%；In described hydrochloric acid, HCl with the mol ratio of aluminium oxide in flyash is
4:1～9:1；The temperature of reaction is 100～200 DEG C；The time of reaction is 0.5～4.0 hour；Reaction pressure be 0.1～
2.5MPa。
10. according to the preparation method according to any one of claim 1～9, it is characterised in that described alcohol is ethanol.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106745000A (en) * | 2016-12-23 | 2017-05-31 | 伊科纳诺（北京）科技发展有限公司 | A kind of preparation method of waterglass base aerosil |
| CN106745005A (en) * | 2017-02-17 | 2017-05-31 | 中国神华能源股份有限公司 | A kind of method for preparing hydrophobic silicon dioxide aerogel |
| CN109012517A (en) * | 2018-08-28 | 2018-12-18 | 浙江工业大学 | A method of compound silica-based aerogel is prepared by raw material of iron tailings |
| CN111960425A (en) * | 2020-09-03 | 2020-11-20 | 河南兴安新型建筑材料有限公司 | Low-cost preparation process of aerogel |
| CN112408401A (en) * | 2020-10-29 | 2021-02-26 | 中国建筑材料科学研究总院有限公司 | Method for preparing silicon dioxide aerogel by utilizing industrial solid waste fly ash and silicon dioxide aerogel prepared by method |
| CN112574504A (en) * | 2020-11-20 | 2021-03-30 | 应急管理部沈阳消防研究所 | Aerogel prepared by boron mud waste, flame retardant and modification application of aerogel |
| CN113336231A (en) * | 2021-06-30 | 2021-09-03 | 同济大学 | Method for preparing aerogel by taking municipal incineration waste ash as raw material through normal pressure drying |
| CN114621739A (en) * | 2020-12-09 | 2022-06-14 | 中国石油化工股份有限公司 | Temperature-resistant salt-resistant super-hydrophobic particle plugging agent and preparation method thereof |
| WO2024060328A1 (en) * | 2022-09-20 | 2024-03-28 | 江西联锴科技有限公司 | Silicon dioxide-rare earth composite photocatalytic material, preparation method therefor, and application thereof |
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| CN104071797B (en) * | 2014-05-21 | 2015-12-09 | 合肥科斯孚安全科技有限公司 | A kind of method preparing low density bigger serface aerosil coating with water glass atmospheric pressure at room |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106745000A (en) * | 2016-12-23 | 2017-05-31 | 伊科纳诺（北京）科技发展有限公司 | A kind of preparation method of waterglass base aerosil |
| CN106745005A (en) * | 2017-02-17 | 2017-05-31 | 中国神华能源股份有限公司 | A kind of method for preparing hydrophobic silicon dioxide aerogel |
| CN106745005B (en) * | 2017-02-17 | 2019-05-24 | 中国神华能源股份有限公司 | A method of preparing hydrophobic silicon dioxide aerogel |
| CN109012517A (en) * | 2018-08-28 | 2018-12-18 | 浙江工业大学 | A method of compound silica-based aerogel is prepared by raw material of iron tailings |
| CN109012517B (en) * | 2018-08-28 | 2020-09-29 | 浙江工业大学 | Method for preparing composite silicon-based aerogel by taking iron tailings as raw materials |
| CN111960425A (en) * | 2020-09-03 | 2020-11-20 | 河南兴安新型建筑材料有限公司 | Low-cost preparation process of aerogel |
| CN112408401A (en) * | 2020-10-29 | 2021-02-26 | 中国建筑材料科学研究总院有限公司 | Method for preparing silicon dioxide aerogel by utilizing industrial solid waste fly ash and silicon dioxide aerogel prepared by method |
| CN112574504A (en) * | 2020-11-20 | 2021-03-30 | 应急管理部沈阳消防研究所 | Aerogel prepared by boron mud waste, flame retardant and modification application of aerogel |
| CN114621739A (en) * | 2020-12-09 | 2022-06-14 | 中国石油化工股份有限公司 | Temperature-resistant salt-resistant super-hydrophobic particle plugging agent and preparation method thereof |
| CN114621739B (en) * | 2020-12-09 | 2023-08-04 | 中国石油化工股份有限公司 | Temperature-resistant salt-resistant super-hydrophobic particle plugging agent and preparation method thereof |
| CN113336231A (en) * | 2021-06-30 | 2021-09-03 | 同济大学 | Method for preparing aerogel by taking municipal incineration waste ash as raw material through normal pressure drying |
| WO2024060328A1 (en) * | 2022-09-20 | 2024-03-28 | 江西联锴科技有限公司 | Silicon dioxide-rare earth composite photocatalytic material, preparation method therefor, and application thereof |
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