CN107189610A - The preparation method of raw-soil thermal insulation waterproof coating - Google Patents
The preparation method of raw-soil thermal insulation waterproof coating Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09D133/10—Homopolymers or copolymers of methacrylic acid esters
- C09D133/12—Homopolymers or copolymers of methyl methacrylate
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- 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- 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 raw-soil thermal insulation waterproof coating, silica dioxide gel is modified in the wet gel stage using methylacryoyloxyethyl dodecyl dimethyl ammonium chloride, then using emulsion polymerization by methyl methacrylate and the double bond copolymerization on the aerosil after modification, obtain being used for raw-soil waterproof heat-insulating coating.Technical scheme overcomes the not good shortcoming of existing raw soil material poor water resistance, thermal and insulating performance, is conducive to significantly improving the water resistance and thermal and insulating performance of raw soil material.
Description
The present patent application is the divisional application of parent application " being used for coating of raw-soil thermal-insulating waterproof and preparation method thereof ", female
The Application No. 2016100278213 of case application, the applying date is on January 16th, 2016.
Technical field
The invention belongs to green construction material technical field, more particularly, it is related to a kind of for raw-soil thermal-insulating waterproof
Coating and preparation method thereof.
Background technology
Earth building refers to original state earthen materia that is not fired and only passing through simple closely knit processing, builds agent structure
Building body.Earth building is building type that is a kind of most ancient and being also widely adopted always so far.Because raw-soil distribution is wide
It is general, fetch earth conveniently, it is economical and practical, and the building built using the raw-soil has cool in summer and warm in winter, firm durable characteristic, so long
Since phase, raw soil material be numerous people generally use a kind of construction material (《Earth building field investigation》, Zhang Yannian etc.
Write, Science Press, 2014).Since human society formation, the raw-soil is always topmost construction material, there is 1/3 in the world
More than inhabitants live among earth building, China rural area is so far there are inhabitants live more than 100,000,000 is in earth building, therefore,
How rapid economic development instantly with develop in new countryside construction and improve traditional earth building, to China's rural residence bar
The improvement of part, and expand application of the raw soil material in other field all with very great meaning.Conventional concrete etc. is built
Firm chemical bond can be formed by building after cement mortar solidification in material, give the powerful support force of building, at the same time, be discarded
Concrete become highly stable, be difficult to reuse, to resource and environment cause seriously endanger.Because raw soil material comes from day
Rarely have strong chemical bond between right original soil, soil particle, make it have extremely excellent reusable edible potentiality, exactly because it is but raw
Soil material special construction, can also bring critical defect to it, seriously threaten the service life of earth building, especially raw-soil material
Material is not water-fast, the shortcomings of meeting water softening, intensity decreases, the use for making earth building be restricted (《The life machine of earth building
System》, Wang Xiaohua works, China Construction Industry Press, 2010).Therefore, how raw soil material is modified, strengthens raw-soil material
The water resistance and durability of material, are improved the service life of earth building, just as asking that raw soil material research must be solved first
Topic.
The content of the invention
It is an object of the invention to overcome above-mentioned the deficiencies in the prior art, existing raw soil material poor water resistance, guarantor are overcome
The not good shortcoming of warm heat-proof quality is conducive to significantly improving there is provided a kind of preparation method for raw-soil thermal insulation waterproof coating
The water resistance and thermal and insulating performance of raw soil material.
The technical purpose of the present invention is achieved by following technical proposals：
Coating for raw-soil thermal-insulating waterproof and preparation method thereof, is carried out as steps described below：
Step 1, added in 80-150 parts by weight tetraethyl orthosilicates 0.1-1 parts by weight 12mol/L hydrogen chloride it is water-soluble
30-180min is stood after stirring 5-30min under (i.e. hydrochloric acid), 20-25 degrees Celsius of room temperature in liquid, 0.01-0.2 weights are subsequently added
Part sodium hydrate solid is measured, stirring is completely dissolved to it, will obtain wet gel after above-mentioned solution left standstill 2-6h, is added in wet gel
Enter 0.1-1 parts by weight methylacryoyloxyethyl dodecyl dimethyl ammonium chlorides, stand after 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 dodecyl dimethyl ammonium chloride be 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；It is subsequently added sodium hydrate solid,
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 dodecyl dimethyl ammonium chloride is added in wet gel, 3-5h is stood.
Step 2,0.1-0.5 parts by weight lauryl sodium sulfate is dissolved in 50-100 parts by weight of deionized water, step 1 is obtained
To aerosil 10-20 parts by weight be dispersed in 50-60 parts by weight absolute ethyl alcohols, then will be dispersed with two
The absolute ethyl alcohol of silica aerogel is added in the deionized water dissolved with lauryl sodium sulfate and is uniformly dispersed, and uses inertia
Gas carries out exclusion air, so that reaction is carried out under anaerobic, and is warming up to 50-70 DEG C；Dripped in the case where maintaining stirring condition
Plus 80-90 parts by weight of methylmethacrylate completion of dropping in 15-30min, 70-90 DEG C is warming up to, 0.1-0.5 weight is added
Cooled down after part potassium peroxydisulfate and 0.01-0.05 pbw of potassium carbonate, reaction 5-10h, that is, obtain raw-soil waterproof heat-insulating coating.
The use of inert gas is nitrogen, helium or argon gas in the step 2.
In the step 2, lauryl sodium sulfate is 0.2-0.3 parts by weight, and deionized water is 60-80 parts by weight,
The aerosil that step 1 is obtained is 15-18 parts by weight, and absolute ethyl alcohol is 55-60 parts by weight, and potassium peroxydisulfate is
0.2-0.3 parts by weight, potassium carbonate is 0.02-0.04 parts by weight.
In the step 2, it is passed through reaction system at least 30min using inert gas and carries out exclusion air, so that reaction
Carry out under anaerobic, preferably 30-40min.
In the step 2, after completion of dropping methyl methacrylate, it is passed through reaction system using inert gas and is arranged
Except air, so that reaction is carried out under anaerobic, the time is passed through for 10-20min, then heated up.
In the step 2, reaction naturally cools to 25-40 DEG C after terminating, that is, obtains raw-soil waterproof heat-insulating coating.
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 dodecyl dimethyl ammonium chloride is modified), b is methylacryoyloxyethyl dodecyl dimethyl chlorination
The copolymer solution of ammonium and methyl methacrylate (is prepared, without titanium dioxide using the process of step 2 of the present invention
Silica aerogel, directly carries out copolymerization by methylacryoyloxyethyl dodecyl dimethyl ammonium chloride and methyl methacrylate),
C is the aerosil wet gel prepared using the process of step 1 of the present invention (through methylacryoyloxyethyl 12
Alkyl dimethyl ammonium chloride is modified), d is the aerosil prepared using the process of step 1 of the present invention (through methyl
Acrylyl oxy-ethyl dodecyl dimethyl ammonium chloride is modified).From accompanying drawing 1 Suo Shi, non-modified silica airsetting
The Zeta potential of glue is negative value (- 38.61mV), and its reason is due to that silica (SA) surface without hydrophobic modification is carried
A large amount of silicone hydroxyls, act on and ionize with the water in air, form negatively charged ion SiO-；Methylacryoyloxyethyl
The Zeta potential of the copolymer solution of dodecyl dimethyl ammonium chloride and methyl methacrylate be on the occasion of (24.43mV) be by
In methylacryoyloxyethyl dodecyl dimethyl ammonium chloride as cationic monomer, it can be produced with water effect positively charged
Quaternary ammonium group-N+(CH3)3；Pass through the negative electrical charge and methylacryoyloxyethyl dodecyl dimethyl on aeroge skeleton surface
On ammonium chloride molecule adelphotaxy between positive charge build that boundary obtains through methylacryoyloxyethyl dodecyl
The Zeta potential of the aerosil wet gel of alkyl dimethyl ammonium chloride modification is -18.61mV.This is due in boundary structure
Build and copolymer polymerization during, positively charged methylacryoyloxyethyl dodecyl dimethyl ammonium chloride molecule can
It is attracted on negatively charged gel skeleton, composite is electrically neutralized, Zeta potential value is between unmodified airsetting
Between glue and copolymer, and Zeta potential is negative value, illustrates that aeroge skeleton surface still has partial negative charge not to be neutralized.And work as
The dioxy that wet gel obtains modifying through methylacryoyloxyethyl dodecyl dimethyl ammonium chloride by supercritical drying process
After SiClx aeroge, before relatively drying significant change does not occur for Zeta potential, it is seen that electrostatic attraction effect is sufficiently strong so that airsetting
The methylacryoyloxyethyl dodecyl dimethyl ammonium chloride that glue surface is adsorbed by electrostatic interaction does not occur obvious de-
Phenomenon.
Determined using U.S.'s Nicolet--5DX FTISs and obtain infrared spectrogram, wherein a is not
The aerosil modified through methylacryoyloxyethyl dodecyl dimethyl ammonium chloride, b is through methacryloxypropyl
The aerosil of ethyl dodecyl dimethyl ammonium chloride 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-1Corresponding place is SiO2The 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 alkyl dimethyl ammonium chloride, in the 1453cm of spectral line (b)-1Place is occurred in that corresponding to methylacryoyloxyethyl dodecyl
The flexural vibrations absworption peak of the methylene adjacent with quaternary ammonium group in alkyl dimethyl ammonium chloride, this is further illustrated by electrostatic attraction
Effect, methylacryoyloxyethyl dodecyl dimethyl ammonium chloride is successfully modified on aerosil.
Using Dutch Philips Nanosem430 field emission scanning electron microscopes respectively to through methacryloxypropyl second
Section after the aerosil of base dodecyl dimethyl ammonium chloride modification and the solidification of raw-soil waterproof heat-insulating coating is carried out
Observation, such as Fig. 3, the aerosil modified through methylacryoyloxyethyl dodecyl dimethyl ammonium chloride has dioxy
SiClx nano-particle connects the three-dimensional net structure to be formed, and nano level hole distribution is more uniform.Through methacryloxypropyl
The aerosil of ethyl dodecyl dimethyl ammonium chloride modification and the raw-soil that PMMA emulsion polymerizations are obtained are waterproof thermal-insulated
Coating is not significantly changed inside the microstructure of material, coating after hardening still there is Nano particles of silicon dioxide to connect shape
Into three-dimensional net structure, and nano level hole distribution it is more uniform.Through scientific and technological (Beijing) Co., Ltd of Bei Shide instruments
N2 adsorption specific surface area measuring instrument determine, using the present invention coating formation dope layer porosity average out to 93-
95%, pore-size distribution is more uniform.
Application of the raw-soil waterproof heat-insulating coating of the present invention in the raw-soil is waterproof thermal-insulated, uses coating to exist when being used
Raw-soil surface is sprayed or brushed, to form waterproof thermal-insulated coating on raw-soil surface, and waterproof thermal-insulated coating layer thickness is 0.1-
1mm, preferably 0.3-0.8mm.The impermeability of coating is tested with reference to national standard GB/T 19250-2003,1 is the results are shown in Table,
Raw-soil waterproof heat-insulating coating has higher impermeability.Using Xi'an Xiatech Electronic Technology Co., Ltd. TC3000E type heat conduction
Coefficient instrument is measured to the thermal conductivity factor of coating, 0.01-0.025Wm of average out to-1K-1, raw-soil waterproof heat-insulating coating has pole
Low heat conductivility, embodies very high heat insulating ability.
Therefore, a kind of preparation method for raw-soil thermal insulation waterproof coating of the present invention, in step 1, utilizes titanium dioxide
The negative electrical charge of silica aerogel wet gel surface silanol group and methylacryoyloxyethyl dodecyl dimethyl ammonium chloride positive charge
Electrostatic attraction effect, methylacryoyloxyethyl dodecyl dimethyl ammonium chloride is adsorbed in wet gel surface, by super
After critical drying, methylacryoyloxyethyl dodecyl dimethyl ammonium chloride molecule is still without departing from aeroge surface, display
Go out very strong interaction.The methylacryoyloxyethyl dodecane that step 2 is adsorbed using aeroge surface electrostatic sucking action
Unsaturated bond and methyl methacrylate copolymerization under emulsion system on base alkyl dimethyl ammonium chloride molecule, can be by copolymer molecule
Chain introduces aeroge surface, and copolymer macromolecular chain is uniformly wrapped in aeroge skeleton surface, and coating product can be made to keep three-dimensional
Network structure, possesses excellent heat-insulating property.
Brief description of the drawings
Fig. 1 is Zeta potential figure, and wherein a is the aerosil prepared using step 1 process of the present invention, b
For methylacryoyloxyethyl dodecyl dimethyl ammonium chloride and the copolymer solution of methyl methacrylate, c is using this
Aerosil wet gel prepared by the process of inventive step 1, d is the process system using step 1 of the present invention
Standby aerosil.
Fig. 2 is Fourier transform infrared spectroscopy figure, and wherein a is without methylacryoyloxyethyl dodecyl dimethyl chlorine
Change the aerosil of ammonium modification；B is the dioxy modified through methylacryoyloxyethyl dodecyl dimethyl ammonium chloride
SiClx aeroge.
Fig. 3 is SEM photograph, and wherein a is the dioxy modified through methylacryoyloxyethyl dodecyl dimethyl ammonium chloride
SiClx aeroge；B is the section after raw-soil waterproof heat-insulating coating solidifies.
Embodiment
Technical scheme, wherein methylacryoyloxyethyl 12 are further illustrated with reference to specific embodiment
Alkyl dimethyl ammonium chloride is purchased from Sigma-Aldrich companies；Other reagents and raw material are purchased from close europeanized learn of Tianjin section and tried
Agent Co., Ltd, supercritical drying equipment uses Haian Oil Scientific Research Apparatus Co., Ltd. CO2Supercritical, high pressure is extracted
Device.
Embodiment 1
0.1g12mol/L hydrochloric acid is added in 80g tetraethyl orthosilicates, is stirred at room temperature after 28min and stands 35min, is then added
Enter 0.14 sodium hydroxide, stirring is completely dissolved to it, will obtain wet gel after above-mentioned solution left standstill 2h, is added in wet gel
0.2g methylacryoyloxyethyl dodecyl dimethyl ammonium chlorides, stand after 6h, product are placed in into CO2Supercritical, high pressure is extracted
In device, 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, 50g deionized waters are dissolved in by 0.1g lauryl sodium sulfate, after 10g aerosils are soaked with 50g absolute ethyl alcohols
It is added in lauryl sodium sulfate, stirs and ultrasound 60min.Transfer it to equipped with agitator, reflux condensing tube, drop
In the four-hole boiling flask of liquid funnel and thermometer, inflated with nitrogen 30min is progressively warming up to 70 DEG C to exclude air.Start to be added dropwise
Dripped off in 80g methyl methacrylates, 30min, after dripping off, continue to stir, and after inflated with nitrogen about 10min, be warming up to 72
DEG C, 0.1g potassium peroxydisulfates and 0.05g potassium carbonate are added, continues to react 5h, is cooled to after 25 DEG C, that is, obtains anti-for raw-soil insulation
Water paint.
Embodiment 2
0.8g12mol/L hydrochloric acid is added in 110g tetraethyl orthosilicates, is stirred at room temperature after 30min and stands 150min, then
0.01 sodium hydroxide is added, stirring is completely dissolved to it, will obtain wet gel after above-mentioned solution left standstill 3h, is added in wet gel
0.6g methylacryoyloxyethyl dodecyl dimethyl ammonium chlorides, stand after 3h, product are placed in into CO2Supercritical, high pressure is extracted
In device, 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, 100g deionized waters are dissolved in by 0.3g lauryl sodium sulfate, and 15g aerosils are soaked with 54g absolute ethyl alcohols
After be added in lauryl sodium sulfate, stir and ultrasound 25min.Transfer it to equipped with agitator, reflux condensing tube,
In the four-hole boiling flask of dropping funel and thermometer, inflated with nitrogen 30min is progressively warming up to 57 DEG C to exclude air.Start drop
Plus 82g methyl methacrylates, drip off in 24min, after dripping off, continue to stir, and after inflated with nitrogen about 12min, be warming up to
75 DEG C, 0.3g potassium peroxydisulfates and 0.01g potassium carbonate are added, continues to react 6h, is cooled to after 30 DEG C, that is, obtains being used for raw-soil insulation
Water-repellent paint.
Embodiment 3
0.2g12mol/L hydrochloric acid is added in 150g tetraethyl orthosilicates, is stirred at room temperature after 5min and stands 180min, is then added
Enter 0.16 sodium hydroxide, stirring is completely dissolved to it, will obtain wet gel after above-mentioned solution left standstill 6h, is added in wet gel
0.7g methylacryoyloxyethyl dodecyl dimethyl ammonium chlorides, stand after 5h, product are placed in into CO2Supercritical, high pressure is extracted
In device, with CO2Supercritical drying 3h is carried out under temperature 50 C and air pressure 9MPa for medium, you can obtain silica airsetting
Glue, 65g deionized waters are dissolved in by 0.5g lauryl sodium sulfate, after 18g aerosils are soaked with 53g absolute ethyl alcohols
It is added in lauryl sodium sulfate, stirs and ultrasound 52min.Transfer it to equipped with agitator, reflux condensing tube, drop
In the four-hole boiling flask of liquid funnel and thermometer, inflated with nitrogen 30min is progressively warming up to 64 DEG C to exclude air.Start to be added dropwise
Dripped off in 84g methyl methacrylates, 16min, after dripping off, continue to stir, and after inflated with nitrogen about 16min, be warming up to 76
DEG C, 0.4g potassium peroxydisulfates and 0.02g potassium carbonate are added, continues to react 7h, is cooled to after 26 DEG C, that is, obtains anti-for raw-soil insulation
Water paint.
Embodiment 4
0.5g12mol/L hydrochloric acid is added in 142g tetraethyl orthosilicates, is stirred at room temperature after 21min and stands 30min, is then added
Enter 0.2 sodium hydroxide, stirring is completely dissolved to it, will obtain wet gel after above-mentioned solution left standstill 5h, 1g is added in wet gel
Methylacryoyloxyethyl dodecyl dimethyl ammonium chloride, stands after 2h, product is placed in into 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 obtain aerosil,
0.2g lauryl sodium sulfate is dissolved in 85g deionized waters, added after 17g aerosils are soaked with 56g absolute ethyl alcohols
Enter into lauryl sodium sulfate, stir and ultrasound 45min.Transfer it to equipped with agitator, reflux condensing tube, dropping liquid
In the four-hole boiling flask of funnel and thermometer, inflated with nitrogen 30min is progressively warming up to 53 DEG C to exclude air.Start that 86g is added dropwise
Dripped off in methyl methacrylate, 29min, after dripping off, continue to stir, and after inflated with nitrogen about 18min, be warming up to 84 DEG C,
0.15g potassium peroxydisulfates and 0.04g potassium carbonate are added, continues to react 8h, is cooled to after 40 DEG C, that is, obtains being used for raw-soil thermal-insulating waterproof
Coating.
Embodiment 5
1g12mol/L hydrochloric acid is added in 95g tetraethyl orthosilicates, is stirred at room temperature after 13min and stands 68min, be subsequently added
0.1 sodium hydroxide, stirring is completely dissolved to it, will obtain wet gel after above-mentioned solution left standstill 4h, 0.3g is added in wet gel
Methylacryoyloxyethyl dodecyl dimethyl ammonium chloride, stands after 4h, product is placed in into 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, 96g deionized waters are dissolved in by 0.4g lauryl sodium sulfate, after 20g aerosils are soaked with 60g absolute ethyl alcohols
It is added in lauryl sodium sulfate, stirs and ultrasound 10min.Transfer it to equipped with agitator, reflux condensing tube, drop
In the four-hole boiling flask of liquid funnel and thermometer, inflated with nitrogen 30min is progressively warming up to 61 DEG C to exclude air.Start to be added dropwise
Dripped off in 90g methyl methacrylates, 15min, after dripping off, continue to stir, and after inflated with nitrogen about 20min, be warming up to 90
DEG C, 0.5g potassium peroxydisulfates and 0.03g potassium carbonate are added, continues to react 10h, is cooled to after 36 DEG C, that is, obtains being used for raw-soil insulation
Water-repellent paint.
The impermeability of table 1 and thermal conductivity factor
| Embodiment | Impermeability 0.3MPa × 30min | Thermal conductivity factor |
| Embodiment 1 | It is waterproof | 0.012Wm-1K-1 |
| Embodiment 2 | It is waterproof | 0.016Wm-1K-1 |
| Embodiment 3 | It is waterproof | 0.019Wm-1K-1 |
| Embodiment 4 | It is waterproof | 0.022Wm-1K-1 |
| Embodiment 5 | It is waterproof | 0.020Wm-1K-1 |
The adjustment of technological parameter is carried out using the technical scheme of present invention, raw-soil waterproof heat-insulating coating can be prepared,
And showing essentially identical impermeability and heat conductivility.
Exemplary description is 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 raw-soil thermal insulation waterproof coating, it is characterised in that carry out as steps described below：
Step 1, in the aqueous solution of hydrogen chloride that 0.1-1 parts by weight 12mol/L is added in 80-150 parts by weight tetraethyl orthosilicates,
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 subsequently added and consolidates
Body, stirring is completely dissolved to it, will obtain wet gel after above-mentioned solution left standstill 2-6h, and 0.1-1 parts by weight are added in wet gel
Methylacryoyloxyethyl dodecyl dimethyl ammonium chloride, stands after 2-6h, product is placed in into 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 2,0.1-0.5 parts by weight lauryl sodium sulfate is dissolved in 50-100 parts by weight of deionized water, step 1 is obtained
Aerosil 10-20 parts by weight are dispersed in 50-60 parts by weight absolute ethyl alcohols, then will be dispersed with titanium dioxide
The absolute ethyl alcohol of silica aerogel is added in the deionized water dissolved with lauryl sodium sulfate and is uniformly dispersed, and uses inert gas
Exclusion air is carried out, so that reaction is carried out under anaerobic, and 50-70 DEG C is warming up to；80- is added dropwise in the case where maintaining stirring condition
90 parts by weight of methylmethacrylate completion of dropping in 15-30min, is warming up to 70-90 DEG C, adds 0.1-0.5 parts by weight mistakes
Cooled down after potassium sulfate and 0.01-0.05 pbw of potassium carbonate, reaction 5-10h, that is, obtain raw-soil waterproof heat-insulating coating.
2. the preparation method of raw-soil thermal insulation waterproof coating according to claim 1, it is characterised in that in the step 1,
The progress supercritical drying time is 2-3h, with CO2For medium carry out supercritical drying, temperature be 35-40 DEG C, air pressure be 8-
9MPa。
3. the preparation method of raw-soil thermal insulation waterproof coating according to claim 1, 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, methylacryoyloxyethyl 12
Alkyl dimethyl ammonium chloride is 0.3-0.8 parts by weight, and the aqueous solution of 12mol/L hydrogen chloride is 0.3-0.8 parts by weight；Just
After being added in silester in the aqueous solution of hydrogen chloride, 60- is stood after stirring 10-20min under 20-25 degrees Celsius of room temperature
120min, mixing speed is 100-150 turns per minute；Sodium hydrate solid is subsequently added, stirring is completely dissolved to it, stirred
Speed is 100-150 turns per minute, will obtain wet gel after above-mentioned 3-5h of solution left standstill, metering system is added in wet gel
Acyloxyethyl dodecyl dimethyl ammonium chloride, stands 3-5h.
4. the preparation method of raw-soil thermal insulation waterproof coating according to claim 1, it is characterised in that in the step 2,
The use of inert gas is nitrogen, helium or argon gas；Reaction system at least 30min is passed through using inert gas to carry out excluding sky
Gas, so that reaction is carried out under anaerobic, preferably 30-40min；After completion of dropping methyl methacrylate, indifferent gas is used
Body is passed through reaction system and carries out exclusion air, so that reaction is carried out under anaerobic, is passed through the time for 10-20min, then enter
Row heating；Reaction naturally cools to 25-40 DEG C after terminating, that is, obtains raw-soil waterproof heat-insulating coating.
5. the preparation method of raw-soil thermal insulation waterproof coating according to claim 1, it is characterised in that in the step 2,
Lauryl sodium sulfate is 0.2-0.3 parts by weight, and deionized water is 60-80 parts by weight, the silica airsetting that step 1 is obtained
Glue is 15-18 parts by weight, and absolute ethyl alcohol is 55-60 parts by weight, and potassium peroxydisulfate is 0.2-0.3 parts by weight, and potassium carbonate is
0.02-0.04 parts by weight.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2778195A1 (en) * | 2013-03-15 | 2014-09-17 | Rohm and Haas Company | Redox polymers for improved dirt and water resistance for elastomeric wall and roof coatings |
| CN104327659A (en) * | 2014-11-19 | 2015-02-04 | 井冈山大学 | Raw soil building wall reinforcing protective agent and preparation method of raw soil building wall reinforcing protective agent |
| US20150038644A1 (en) * | 2013-07-30 | 2015-02-05 | Rohm And Haas Company | Ureido-functionalized aqueous polymeric dispersion |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2546216B2 (en) * | 1991-11-18 | 1996-10-23 | 株式会社日本触媒 | High weather resistance one-pack cross-linking emulsion |
| CN100537673C (en) * | 2005-11-08 | 2009-09-09 | 财团法人工业技术研究院 | Thermal-isolating coating |
| KR20110042267A (en) * | 2008-06-30 | 2011-04-26 | 에스티씨. 유엔엠 | Durable polymer-aerogel based superhydrophobic coatings: a composite material |
| KR101137657B1 (en) * | 2009-11-04 | 2012-04-20 | 이재환 | Emulsion aerogel composition |
| CN101973558B (en) * | 2010-09-30 | 2012-02-29 | 南京工业大学 | Amino modified SiO2 aerogel material and application thereof |
| JP2016506432A (en) * | 2012-12-13 | 2016-03-03 | アンガス ケミカル カンパニー | Nitro-functional acrylate copolymers for binder compositions |
| CN104087047A (en) * | 2014-07-25 | 2014-10-08 | 徐子航 | Thermal-insulation paint and preparation method thereof |
| CN104609825B (en) * | 2015-02-05 | 2016-09-28 | 泉州三欣新材料科技有限公司 | A kind of heat-insulation and heat-preservation inorganic coating and preparation method thereof |
| CN105038452A (en) * | 2015-07-08 | 2015-11-11 | 当涂县科辉商贸有限公司 | Anti-cracking nanoporous super thermal-insulation heat-preserving paint and preparation method thereof |
-
2016
- 2016-01-16 CN CN201610027821.3A patent/CN105694643B/en not_active Expired - Fee Related
- 2016-01-16 CN CN201710552632.2A patent/CN107236403A/en active Pending
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2778195A1 (en) * | 2013-03-15 | 2014-09-17 | Rohm and Haas Company | Redox polymers for improved dirt and water resistance for elastomeric wall and roof coatings |
| US20150038644A1 (en) * | 2013-07-30 | 2015-02-05 | Rohm And Haas Company | Ureido-functionalized aqueous polymeric dispersion |
| CN104327659A (en) * | 2014-11-19 | 2015-02-04 | 井冈山大学 | Raw soil building wall reinforcing protective agent and preparation method of raw soil building wall reinforcing protective agent |
Non-Patent Citations (2)
| Title |
|---|
| 刘国强: "介孔氧化硅气凝胶和微孔活性炭的制备、织构及氢气吸附性能", 《中国博士学位论文全文数据库 工程科技I辑》 * |
| 汪慧: "SiO2气凝胶/苯丙原位复合乳液的制备及其在隔热涂料中的应用", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107502184A (en) * | 2017-09-28 | 2017-12-22 | 马鞍山松鹤信息科技有限公司 | One kind building waterproof paint specially and preparation method thereof |
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Application publication date: 20170922 |