CN107513140A - The preparation method of aerogel composite based on silica - Google Patents
The preparation method of aerogel composite based on silica Download PDFInfo
- Publication number
- CN107513140A CN107513140A CN201710697383.6A CN201710697383A CN107513140A CN 107513140 A CN107513140 A CN 107513140A CN 201710697383 A CN201710697383 A CN 201710697383A CN 107513140 A CN107513140 A CN 107513140A
- Authority
- CN
- China
- Prior art keywords
- weight
- parts
- added
- dtac
- silica
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C01B33/163—Preparation of silica xerogels by hydrolysis of organosilicon compounds, e.g. ethyl orthosilicate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F292/00—Macromolecular compounds obtained by polymerising monomers on to inorganic materials
-
- 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
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/157—After-treatment of gels
- C01B33/158—Purification; Drying; Dehydrating
- C01B33/1585—Dehydration into aerogels
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The present invention discloses the preparation method of the aerogel composite based on silica, adsorbed using the negative electrical charge of aerosil wet gel surface silanol group and the electrostatic attraction effect of methylacryoyloxyethyl DTAC positive charge, unsaturated bond is recycled to be copolymerized with methyl methacrylate under bulk system, copolymer molecule chain is introduced into aeroge surface, copolymer macromolecular chain is uniformly wrapped in aeroge skeleton surface, aeroge product can be made to keep tridimensional network, possess excellent heat-insulating property.The composite material of polymethyl methacrylate of aerosil functionalization produced by the present invention has the characteristics of high boundary thermal resistance and heat-insulated height.
Description
The present patent application is the division of parent application " aerogel composite based on silica and preparation method thereof "
Application, the Application No. 2016100282257 of parent application, the applying date is on January 16th, 2016.
Technical field
The invention belongs to green construction material technical field, more particularly, is related to a kind of aerogel material and its system
Preparation Method.
Background technology
The thermal loss of transparent enclosure structure accounts for very big proportion in building energy consumption, and its reason is largely derived from building
The low thermal insulation of thing glass component.Particularly in the sternness increasingly of environment and energy problem instantly, building transparent enclosure knot is improved
The insulation of structure is horizontal, makes great efforts to promote building energy conservation, for improving building thermal environments, mitigating environmental pollution, money of preserving our planet
Source and ecological environment are respectively provided with more deep meaning.People recognize that building transparent enclosure structure heat dissipation capacity is big very early in fact
This problem, it is proposed that some improve glass component thermal insulations method, such as hollow or vacuum glass, heat-reflecting glass,
Low-E glass and pad pasting glass etc..But these methods do not solve the problems, such as the radiating of transparent enclosure structure fundamentally, or
Say be these glass components heat preservation and insulation method also reach far away we expection (Liu Nianxiong, Qin Youguo, building thermal environments,
Publishing house of Tsing-Hua University, 2005).Polymethyl methacrylate (Polymethylmethacrylate, abbreviation PMMA, English
Acrylic), acryl or lucite are also known as done, the number-average molecular weight of its cast panel polymer is generally 2.2 × 104, relatively
Density is 1.19~1.20, and refractive index is 1.482~1.521, and for wettability below 0.5%, glass transition temperature is 105 DEG C.Tool
There is the high grade of transparency, low price, be the glass alternative materials being commonly used usually the advantages that being easy to be machined.PMMA heat conduction
Coefficient is about 0.2W/m.K, is greatly differed from each other apart from building heat preservation insulation requirement, at the same time, PMMA mechanical strengths, anti-impact
Hit performance etc. still have can be lifted space (horse accounts for boomerang, methacrylate resin and its application, Chemical Industry Press,
2002；Li Lei, Yan Yue, acrylic resin and its application, Chemical Industry Press, 2012).Aerosil is a kind of new
Type low-density, transparent, structure-controllable nano-porous materials.Compared with traditional silicon dioxide particle, aerosil tool
There is continuous tridimensional network, having the design features such as low-density, high voidage, high-specific surface area, (different silica sources prepare two
The progress of silica aerogel, Wang Ni etc., material Leader A：Summarize a piece, the 1st phase of volume 28 in 2014,42-45).Simultaneously
With excellent thermal and insulating performance, thermal conductivity is extremely low under normal temperature and pressure, is the minimum solid material of the thermal conductivity being currently known,
It is with a wide range of applications in the heat-insulated field of building heat preservation.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the aerogel material with electrostatic attraction boundary, uses
Super insulating material aerosil, carries out surface chemistry conditions regulation and control to it, and by itself and PMMA bulk polymerization systems
Compound to prepare composite, obtained aerogel material has higher heat-proof quality and boundary thermal resistance.
The technical purpose of the present invention is achieved by following technical proposals：
Aerogel composite based on silica and preparation method thereof, carry out as steps described below：
Step 1, the water-soluble of 0.1-1 parts by weight 12mol/L hydrogen chloride is added in 80-150 parts by weight tetraethyl orthosilicates
In liquid (i.e. hydrochloric acid), 30-180min is stood after stirring 5-30min under 20-25 degrees Celsius of room temperature, then adds 0.01-0.2 weights
Part sodium hydrate solid is measured, stirs to it and is completely dissolved, wet gel will be obtained after above-mentioned solution left standstill 2-6h, is added in wet gel
Enter 0.1-1 parts by weight methylacryoyloxyethyl DTACs, after standing 2-6h, product is placed in CO2It is super
In critical high-pressure extraction device, with CO2For medium supercritical drying is carried out at 30-50 DEG C of temperature and air pressure 7-10MPa at least
1h, you can obtain aerosil.
In the step 1, the progress supercritical drying time is 2-3h.
In the step 1, with CO2Supercritical drying is carried out for medium, temperature is 35-40 DEG C, and air pressure is 8-9MPa.
In the step 1, tetraethyl orthosilicate is 100-120 parts by weight, and sodium hydrate solid is 0.05-0.1 weight
Part, methylacryoyloxyethyl DTAC is 0.3-0.8 parts by weight, 12mol/L hydrogen chloride it is water-soluble
Liquid is 0.3-0.8 parts by weight.
In the step 1, after being added in tetraethyl orthosilicate in the aqueous solution of hydrogen chloride, under 20-25 degrees Celsius of room temperature
60-120min is stood after stirring 10-20min, mixing speed is 100-150 turns per minute；Sodium hydrate solid is then added,
Stirring is completely dissolved to it, and mixing speed is 100-150 turns per minute, will obtain wet gel after above-mentioned 3-5h of solution left standstill,
Methylacryoyloxyethyl DTAC is added in wet gel, stands 3-5h.
Step 2, the aerosil that 5-10 parts by weight steps 1 obtain is added to 100 weight parts of methacrylic acid
In methyl esters and it is uniformly dispersed, the dibenzoyl peroxide for adding 0.02-0.2 parts by weight is simultaneously uniformly dispersed, then heat to 75-
80 DEG C are triggered methyl methacrylate and aerosil surface methyl groups acrylyl oxy-ethyl trimethyl chlorination
The carbon-carbon double bond of ammonium carries out copolyreaction, and the copolyreaction time is at least 30h.
In the step 2, when dispersed silicon dioxide aeroge and methyl methacrylate, ultrasonic disperse, time are used
At least 1h, preferably 1-2h.
In the step 2, when carrying out scattered after addition dibenzoyl peroxide, ultrasonic disperse, time 3- are used
10min。
In the step 2, when carrying out copolyreaction, select to react 2h at 75-80 DEG C, be then cooled to 50-60
Degree Celsius lower polymerisation 24h, then at 80 DEG C, 90 DEG C and 100 DEG C react 2h successively, you can obtain having high heat-proof quality and
The aerogel material of high thermal resistance boundary.
In the step 2, water bath with thermostatic control is selected to provide corresponding temperature for reaction system.
Zeta is determined using U.S. Brookhaven ZetaPALS type high-resolution Zeta potentials and Particle Size Analyzer respectively
Current potential, as a result as shown in Figure 1, a are the aerosil prepared using the process of step 1 of the present invention (without first
Base acrylyl oxy-ethyl DTAC is modified), b is methylacryoyloxyethyl trimethyl chlorination
The copolymer solution of ammonium and methyl methacrylate (is prepared using the process of step 2 of the present invention, does not add titanium dioxide
Silica aerogel, directly methylacryoyloxyethyl DTAC and methyl methacrylate are copolymerized),
C is the aerosil wet gel prepared using the process of step 1 of the present invention (through methylacryoyloxyethyl 12
Alkyl trimethyl ammonium chloride is modified), d is the aerosil prepared using the process of step 1 of the present invention (through methyl
Acrylyl oxy-ethyl DTAC is modified).From accompanying drawing 1, non-modified aerosil
Zeta potential is negative value (- 38.61mV).Its reason is due to aerosil (SA) surface band without hydrophobic modification
There are a large amount of silicone hydroxyls, act on and ionize with the water in air, form negatively charged ion SiO-；Methacryloxypropyl second
The Zeta potential of the copolymer solution of base DTAC and methyl methacrylate is to be on the occasion of (24.43mV)
Because methylacryoyloxyethyl DTAC is as cationic monomer, positively charged can be produced with water effect
Quaternary ammonium group-the N of lotus+(CH3)3；Pass through the negative electrical charge and methylacryoyloxyethyl dodecyl front three on aeroge skeleton surface
On ammonium chloride molecule between positive charge adelphotaxy structure boundary obtain through methylacryoyloxyethyl dodecane
The Zeta potential of the aerosil wet gel of base trimethyl ammonium chloride modification is -18.61mV.This is due in boundary
During structure and copolymer polymerization, positively charged methylacryoyloxyethyl DTAC molecule energy
Enough it is attracted on negatively charged gel skeleton, composite is electrically neutralized, Zeta potential value is between unmodified gas
Between gel and copolymer, and Zeta potential is negative value, illustrates that aeroge skeleton surface still has partial negative charge not to be neutralized.And
When wet gel obtains two through the modification of methylacryoyloxyethyl DTAC by supercritical drying process
After silica aerogel, before relatively drying significant change does not occur for Zeta potential, it is seen that electrostatic attraction effect is sufficiently strong so that gas
Gel surface does not occur significantly by the methylacryoyloxyethyl DTAC of electrostatic interaction absorption
It is desorbed phenomenon.
Determine to obtain infrared spectrogram using U.S.'s Nicolet--5DX FTISs, wherein a is not
The aerosil modified through methylacryoyloxyethyl DTAC, b are through methacryloxypropyl
The aerosil of ethyl DTAC modification.It can see from spectrogram, unmodified airsetting
The spectral line (a) of glue is in 803cm-1And 1103cm-1There is absworption peak at place, and corresponding respectively is SiO2The symmetrical and asymmetric of middle Si-O stretches
Contract the characteristic absorption peak vibrated, 3442cm-1It is SiO corresponding to place2The stretching vibration absworption peak of surface hydroxyl, and 1630cm-1Place
It is corresponding, it is the absworption peak of residual water in test sample.And when aerosil is through methylacryoyloxyethyl dodecane
After the modification of base trimethyl ammonium chloride, in the 1453cm of spectral line (b)-1Place occurs corresponding to methylacryoyloxyethyl dodecyl
The flexural vibrations absworption peak of the methylene adjacent with quaternary ammonium group in trimethyl ammonium chloride, this further explanation pass through electrostatic attraction
Effect, methylacryoyloxyethyl DTAC are successfully modified on aerosil.
Using Dutch Philips Nanosem430 field emission scanning electron microscopes respectively to through methacryloxypropyl second
The aerosil of base DTAC modification and the aerogel composite section of the present invention are seen
Examine, such as Fig. 3, the aerosil modified through methylacryoyloxyethyl DTAC has titanium dioxide
Silicon nano connects the three-dimensional net structure to be formed, and nano level hole distribution is more uniform.Through methacryloxypropyl second
The aerosil of base DTAC modification has high thermal resistance phase boundary with what PMMA polymerisation in bulks obtained
The silica aerogel material in face does not significantly change the microstructure of material, and material internal still has silica nanometer
Particle connects the three-dimensional net structure to be formed, and the distribution of nano level hole is more uniform.Through Bei Shide instruments science and technology (north
Capital) Co., Ltd N2 adsorption specific surface area measuring instrument measure, the porosity average out to of aerogel composite of the invention
93-94.5%, pore-size distribution is more uniform.
Application of the aerogel composite of the present invention in the raw-soil is waterproof thermal-insulated, it is when being used that aeroge is compound
Material prepares shaping, forms 0.1-1mm of thickness sheet material, preferably 0.3-0.8mm.Bibliography (Effects of
chemical bonding on heat transport across interfaces,Nature Materials,2012,
11,502) it is described, using German Linseis TF-LFA type time domain heat reflection probe assay aerogel material boundary thermal resistances,
28-32MWm of average out to-2K-1.Aeroge is answered using Xi'an Xiatech Electronic Technology Co., Ltd. TC3000E type thermal conductivity factor instruments
The thermal conductivity factor of condensation material is measured, 0.01-0.02Wm of average out to-1K-1, the aerogel composite finally prepared has
Higher boundary thermal resistance and relatively low thermal conductivity factor.
Compared with prior art, silica gas is utilized in step 1 in aerogel material of the invention and preparation method thereof
The negative electrical charge of gel wet gel surface silanol group and the electrostatic of methacryloxy DTAC positive charge
Sucking action, methacryloxy DTAC is adsorbed in wet gel surface, by supercritical drying
Afterwards, methacryloxy DTAC molecule shows very strong phase still without departing from aeroge surface
Interaction.The methacryloxy trimethyl chlorination that step 2 is adsorbed using aeroge surface electrostatic sucking action
Unsaturated bond on ammonium molecule is copolymerized with methyl methacrylate under bulk system, copolymer molecule chain can be introduced into aeroge
Surface, copolymer macromolecular chain are uniformly wrapped in aeroge skeleton surface, and aeroge product can be made to keep tridimensional network, gathered around
There is excellent heat-insulating property.
Brief description of the drawings
Fig. 1 is Zeta potential figure, and wherein a is the aerosil prepared using the process of step 1 of the present invention
(being modified without methylacryoyloxyethyl DTAC), b is methylacryoyloxyethyl dodecyl three
The copolymer solution of ammonio methacrylate and methyl methacrylate (is prepared using the process of step 2 of the present invention, not added
Add aerosil, directly enter methylacryoyloxyethyl DTAC and methyl methacrylate
Row copolymerization), c is the aerosil wet gel prepared using the process of step 1 of the present invention (through methacryloxypropyl
Ethyl DTAC is modified), d is the silica airsetting prepared using the process of step 1 of the present invention
Glue (is modified) through methylacryoyloxyethyl DTAC.
Fig. 2 is Fourier transform infrared spectroscopy figure, and wherein a is without methylacryoyloxyethyl trimethyl chlorine
Change the aerosil of ammonium modification, b is the dioxy modified through methylacryoyloxyethyl DTAC
SiClx aeroge.
Fig. 3 is SEM photograph, and wherein a is the titanium dioxide modified through methacryloxy DTAC
Silica aerogel, b are the aerogel material with high heat-proof quality and high thermal resistance boundary of the present invention.
Embodiment
Technical scheme, wherein methacryloxy dodecane are further illustrated with reference to specific embodiment
Base trimethyl ammonium chloride is purchased from Sigma-Aldrich companies；Other reagents and raw material are purchased from Tianjin Ke Miou chemical reagent
Co., Ltd, supercritical drying equipment is using Haian Oil Scientific Research Apparatus Co., Ltd. CO2Supercritical, high pressure extraction dress
Put.
Embodiment 1
0.1g12mol/L hydrochloric acid is added in 80g tetraethyl orthosilicates, 35min is stood after 28min is stirred at room temperature, is then added
Enter 0.14 sodium hydroxide, stir to it and be completely dissolved, wet gel will be obtained after above-mentioned solution left standstill 2h, added in wet gel
0.2g methacryloxy DTACs, after standing 6h, product is placed in CO2Supercritical, high pressure extraction dress
In putting, with CO2Supercritical drying 3h is carried out at 33 DEG C of temperature and air pressure 7MPa for medium, you can obtain silica airsetting
Glue, 10g aerosils are added in 100g methyl methacrylates, then carry out ultrasonic disperse 1h, then add
0.2g dibenzoyl peroxide, ultrasonic disperse 10min, then dispersion liquid is successively placed in 75 DEG C of water-bath and triggers methyl-prop
E pioic acid methyl ester and aerosil surface methyl groups acryloxy DTAC carry out combined polymerization, after 2h
Taken out from water-bath and be put into 50 DEG C of water bath with thermostatic control and polymerize 24h, then by it successively at 80 DEG C, 90 DEG C, 100 DEG C of thermostatted water
2h is respectively placed in bath, you can obtain the aerogel material with high heat-proof quality and high thermal resistance boundary.
Embodiment 2
0.8g12mol/L hydrochloric acid is added in 110g tetraethyl orthosilicates, stands 150min after 30min is stirred at room temperature, then
0.01 sodium hydroxide is added, stirs to it and is completely dissolved, wet gel will be obtained after above-mentioned solution left standstill 3h, added in wet gel
0.6g methacryloxy DTACs, after standing 3h, product is placed in CO2Supercritical, high pressure extraction dress
In putting, with CO2Supercritical drying 3h is carried out at 46 DEG C of temperature and air pressure 8MPa for medium, you can obtain silica airsetting
Glue, 5g aerosils are added in 100g methyl methacrylates, then carry out ultrasonic disperse 1h, then add
0.02g dibenzoyl peroxide, ultrasonic disperse 3min, then dispersion liquid is successively placed in 75 DEG C of water-bath and triggers methyl-prop
E pioic acid methyl ester and aerosil surface methyl groups acryloxy DTAC carry out combined polymerization, after 2h
Taken out from water-bath and be put into 50 DEG C of water bath with thermostatic control and polymerize 24h, then by it successively at 80 DEG C, 90 DEG C, 100 DEG C of thermostatted water
2h is respectively placed in bath, you can obtain the aerogel material with high heat-proof quality and high thermal resistance boundary.
Embodiment 3
0.2g12mol/L hydrochloric acid is added in 150g tetraethyl orthosilicates, 180min is stood after 5min is stirred at room temperature, is then added
Enter 0.16 sodium hydroxide, stir to it and be completely dissolved, wet gel will be obtained after above-mentioned solution left standstill 6h, added in wet gel
0.7g methacryloxy DTACs, after standing 5h, product is placed in CO2Supercritical, high pressure extraction dress
In putting, with CO2Supercritical drying 3h is carried out under temperature 50 C and air pressure 9MPa for medium, you can obtain silica airsetting
Glue, 7g aerosils are added in 100g methyl methacrylates, then carry out ultrasonic disperse 1h, then add
0.14g dibenzoyl peroxide, ultrasonic disperse 4.8min, then dispersion liquid is successively placed in 75 DEG C of water-bath and triggers methyl
Methyl acrylate carries out combined polymerization, 2h with aerosil surface methyl groups acryloxy DTAC
Taken out afterwards from water-bath and be put into 50 DEG C of water bath with thermostatic control and polymerize 24h, then by it successively at 80 DEG C, 90 DEG C, 100 DEG C of constant temperature
2h is respectively placed in water-bath, you can obtain the aerogel material with high heat-proof quality and high thermal resistance boundary.
Embodiment 4
0.5g12mol/L hydrochloric acid is added in 142g tetraethyl orthosilicates, 30min is stood after 21min is stirred at room temperature, is then added
Enter 0.2 sodium hydroxide, stir to it and be completely dissolved, wet gel will be obtained after above-mentioned solution left standstill 5h, 1g is added in wet gel
Methacryloxy DTAC, after standing 2h, product is placed in CO2Supercritical high-pressure extraction device
In, with CO2Supercritical drying 3h is carried out at 37 DEG C of temperature and air pressure 10MPa for medium, you can aerosil is obtained,
9g aerosils are added in 100g methyl methacrylates, ultrasonic disperse 1h is then carried out, then adds 0.14g
Dibenzoyl peroxide, ultrasonic disperse 9min, then dispersion liquid is successively placed in 75 DEG C of water-bath and triggers methacrylic acid
Methyl esters and aerosil surface methyl groups acryloxy DTAC carry out combined polymerization, from water after 2h
Take out to be put into 50 DEG C of water bath with thermostatic control in bath and polymerize 24h, then by it successively at 80 DEG C, 90 DEG C, in 100 DEG C of water bath with thermostatic control
It is each to place 2h, you can to obtain the aerogel material with high heat-proof quality and high thermal resistance boundary.
Embodiment 5
1g12mol/L hydrochloric acid is added in 95g tetraethyl orthosilicates, 68min is stood after 13min is stirred at room temperature, is then added
0.1 sodium hydroxide, stirs to it and is completely dissolved, and will obtain wet gel after above-mentioned solution left standstill 4h, 0.3g is added in wet gel
Methacryloxy DTAC, after standing 4h, product is placed in CO2Supercritical high-pressure extraction device
In, with CO2Supercritical drying 3h is carried out under temperature 45 C and air pressure 8.5MPa for medium, you can obtain silica airsetting
Glue, 9.1g aerosils are added in 100g methyl methacrylates, then carry out ultrasonic disperse 1h, then add
0.19g dibenzoyl peroxide, ultrasonic disperse 6min, then dispersion liquid is successively placed in 75 DEG C of water-bath and triggers methyl-prop
E pioic acid methyl ester and aerosil surface methyl groups acryloxy DTAC carry out combined polymerization, after 2h
Taken out from water-bath and be put into 50 DEG C of water bath with thermostatic control and polymerize 24h, then by it successively at 80 DEG C, 90 DEG C, 100 DEG C of thermostatted water
2h is respectively placed in bath, you can obtain the aerogel material with high heat-proof quality and high thermal resistance boundary.
The impermeability of table 1 and thermal conductivity factor
The adjustment of technological parameter is carried out using the technical scheme of present invention, can prepare raw-soil water-proof heat-insulation material,
And showing essentially identical impermeability and heat conductivility.
Exemplary description has been done to the present invention above, it should explanation, in the situation for the core for not departing from the present invention
Under, any simple deformation, modification or other skilled in the art can not spend the equivalent substitution of creative work equal
Fall into protection scope of the present invention.
Claims (5)
1. the preparation method of the aerogel composite based on silica, it is characterised in that carry out as steps described below：
Step 1, added in 80-150 parts by weight tetraethyl orthosilicates in the 0.1-1 parts by weight 12mol/L aqueous solution of hydrogen chloride,
30-180min is stood after stirring 5-30min under 20-25 degrees Celsius of room temperature, 0.01-0.2 parts by weight of sodium hydroxide is then added and consolidates
Body, stir to it and be completely dissolved, wet gel will be obtained after above-mentioned solution left standstill 2-6h, 0.1-1 parts by weight are added in wet gel
Methylacryoyloxyethyl DTAC, after standing 2-6h, product is placed in CO2Supercritical, high pressure extraction dress
In putting, with CO2Supercritical drying at least 1h is carried out at 30-50 DEG C of temperature and air pressure 7-10MPa for medium, you can obtain dioxy
SiClx aeroge；
Step 2, the aerosil that 5-10 parts by weight steps 1 obtain is added to 100 parts by weight of methylmethacrylate
In and be uniformly dispersed, add 0.02-0.2 parts by weight dibenzoyl peroxide simultaneously be uniformly dispersed, then heat to 75-80 DEG C
Trigger methyl methacrylate and aerosil surface methyl groups acrylyl oxy-ethyl DTAC
Carbon-carbon double bond carries out copolyreaction, and the copolyreaction time is at least 30h.
2. the preparation method of the aerogel composite according to claim 1 based on silica, it is characterised in that
In the step 1, the progress supercritical drying time is 2-3h；With CO2Supercritical drying is carried out for medium, temperature is 35-40
DEG C, air pressure is 8-9MPa.
3. the preparation method of the aerogel composite according to claim 1 based on silica, it is characterised in that
In the step 1, tetraethyl orthosilicate is 100-120 parts by weight, and sodium hydrate solid is 0.05-0.1 parts by weight, metering system
Acyloxyethyl DTAC is 0.3-0.8 parts by weight, the aqueous solution of 12mol/L hydrogen chloride for 0.3-
0.8 parts by weight；After being added in tetraethyl orthosilicate in the aqueous solution of hydrogen chloride, 10-20min is stirred under 20-25 degrees Celsius of room temperature
After stand 60-120min, mixing speed is 100-150 turns per minute；Sodium hydrate solid is then added, is stirred complete to its
Dissolving, mixing speed are 100-150 turns per minute, will obtain wet gel after above-mentioned 3-5h of solution left standstill, are added in wet gel
Enter methylacryoyloxyethyl DTAC, stand 3-5h.
4. the preparation method of the aerogel composite according to claim 1 based on silica, it is characterised in that
In the step 2, when dispersed silicon dioxide aeroge and methyl methacrylate, using ultrasonic disperse, time at least 1h, preferably
1—2h；When carrying out scattered after addition dibenzoyl peroxide, ultrasonic disperse, time 3-10min are used.
5. the preparation method of the aerogel composite according to claim 1 based on silica, it is characterised in that
In the step 2, when carrying out copolyreaction, select to react 2h at 75-80 DEG C, be then cooled under 50-60 degrees Celsius and gather
Reaction 24h is closed, then at 80 DEG C, 90 DEG C and 100 DEG C reacts 2h successively, you can obtains that there is high heat-proof quality and high thermal resistance phase boundary
The aerogel material in face.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710697383.6A CN107513140A (en) | 2016-01-16 | 2016-01-16 | The preparation method of aerogel composite based on silica |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710697383.6A CN107513140A (en) | 2016-01-16 | 2016-01-16 | The preparation method of aerogel composite based on silica |
| CN201610028225.7A CN105600795A (en) | 2016-01-16 | 2016-01-16 | SiO2 based composite aerogel material and preparation method thereof |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610028225.7A Division CN105600795A (en) | 2016-01-16 | 2016-01-16 | SiO2 based composite aerogel material and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107513140A true CN107513140A (en) | 2017-12-26 |
Family
ID=55981225
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710697383.6A Pending CN107513140A (en) | 2016-01-16 | 2016-01-16 | The preparation method of aerogel composite based on silica |
| CN201610028225.7A Pending CN105600795A (en) | 2016-01-16 | 2016-01-16 | SiO2 based composite aerogel material and preparation method thereof |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610028225.7A Pending CN105600795A (en) | 2016-01-16 | 2016-01-16 | SiO2 based composite aerogel material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (2) | CN107513140A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109651529A (en) * | 2018-11-14 | 2019-04-19 | 宁波绿之健药业有限公司 | A kind of chondroitin sulfate preparation method of high bioavilability |
| CN111777952A (en) * | 2020-06-12 | 2020-10-16 | 上海嗣高新材料科技有限公司 | Aerogel and nano hydrotalcite synergistic fireproof sealant and preparation method thereof |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105693958A (en) * | 2016-01-16 | 2016-06-22 | 天津城建大学 | Silicon dioxide-methyl methacrylate composite aerogel material based on surface modification and preparation method thereof |
| CN106084274B (en) * | 2016-06-12 | 2019-05-24 | 武汉理工大学 | A kind of preparation method of light high-strength heat preservation foamed composite |
| CN107868190A (en) * | 2016-09-27 | 2018-04-03 | 天津城建大学 | A kind of silica polymethyl methacrylate compound insulating material and preparation method thereof |
| CN109081675A (en) * | 2017-06-14 | 2018-12-25 | 天津城建大学 | Multiple dimensioned galapectite-silicon dioxide composite aerogel material and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101787171B (en) * | 2010-01-11 | 2011-11-23 | 西北师范大学 | Silicon oxide (SiOX)/polymethyl methacrylate (PMMA) nano composite resin and preparation and application thereof |
| CN102766241A (en) * | 2011-05-06 | 2012-11-07 | 北京化工大学 | Core-shell structured nano-silica/polyacrylate emulsion and its preparation method |
-
2016
- 2016-01-16 CN CN201710697383.6A patent/CN107513140A/en active Pending
- 2016-01-16 CN CN201610028225.7A patent/CN105600795A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109651529A (en) * | 2018-11-14 | 2019-04-19 | 宁波绿之健药业有限公司 | A kind of chondroitin sulfate preparation method of high bioavilability |
| CN109651529B (en) * | 2018-11-14 | 2020-10-30 | 宁波绿之健药业有限公司 | Preparation method of chondroitin sulfate with high bioavailability |
| CN111777952A (en) * | 2020-06-12 | 2020-10-16 | 上海嗣高新材料科技有限公司 | Aerogel and nano hydrotalcite synergistic fireproof sealant and preparation method thereof |
| CN111777952B (en) * | 2020-06-12 | 2022-03-15 | 上海嗣高新材料科技有限公司 | Aerogel and nano hydrotalcite synergistic fireproof sealant and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105600795A (en) | 2016-05-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107513140A (en) | The preparation method of aerogel composite based on silica | |
| CN104558447B (en) | Inorganic nano composite anti-doodling resin and preparation method thereof | |
| Zhou et al. | Synthesis and Characterization of nano-SiO2 modified fluorine-containing polyacrylate emulsifier-free emulsion | |
| Yao et al. | Synthesis and characterization of poly (fluorinated acrylate)/silica hybrid nanocomposites | |
| CN102702419B (en) | Preparation method of montmorillonite-modified crosslinked acrylate-hybridized core-shell emulsion | |
| CN105418820B (en) | Cinepazid polymer/SiO of hydroxyl2Hybridisation emulsion and the preparation method and application thereof | |
| CN108641050A (en) | A kind of preparation method of aqueous super hydrophobic material | |
| CN109705692A (en) | A kind of elastic compounded emulsion and preparation method thereof with super contaminated resistance | |
| CN108329417A (en) | Nano-meter SiO_22/ organic-silicon-modified core-shell acrylic-resin emulsion and preparation method | |
| CN109666111A (en) | A kind of Nano-meter SiO_22/ organosilicon-modified acrylate emulsion | |
| CN103387645A (en) | Fluorine-containing copolymer grafted modified nano TiO2 compound particle and preparation method thereof | |
| CN108359047A (en) | A kind of waterborne acrylic paint and preparation method thereof that graphene is modified | |
| CN108641049A (en) | A kind of preparation method of the aqueous super hydrophobic material of fluorine-free monomer | |
| CN114230723B (en) | Graphene oxide modified styrene-acrylic pickering emulsion, composite emulsion, and preparation method and application thereof | |
| Zhang et al. | Fluorinated acrylic monomer modified core-shell polyacrylate latex particles: Preparation, properties and characterizations | |
| CN105038533B (en) | A kind of special-purpose aqueous baking varnish coating of antitheft door and preparation method thereof | |
| CN106699955A (en) | Application for methacryloyloxyethylhexyldimethyl ammonium bromide in disperse silicon dioxide, composite material of methacryloyloxyethylhexyldimethyl ammonium bromide, and preparation method of composite material | |
| Zhou et al. | Synthesis and characterization of organic fluorine and nano-SiO2 modified polyacrylate emulsifier-free latex | |
| CN105693958A (en) | Silicon dioxide-methyl methacrylate composite aerogel material based on surface modification and preparation method thereof | |
| Zhang et al. | Synthesis of ambient temperature self-crosslinking VTES-based core–shell polyacrylate emulsion via modified micro-emulsion polymerization process | |
| Zhang et al. | Preparation and properties of multilayer assembled polymer gel microsphere profile control agents | |
| CN105566583A (en) | Highly-impact-resistant highly-light-transmitting highly-heat-insulating polymethylmethacrylate composite material and preparation method thereof | |
| Wang et al. | The surface modification of extruded polystyrene foams through UV curing and its stable adhesion to mortar | |
| CN111500018A (en) | SiO2 modified fluorinated epoxy resin super-hydrophobic material and preparation method thereof | |
| CN106496604A (en) | The preparation method of polymer Janus nanometer sheets PtBMA/PAM |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171226 |