CN105647325A - Raw soil waterproof heat insulation coating and preparation method thereof - Google Patents
Raw soil waterproof heat insulation coating and preparation method thereof Download PDFInfo
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- CN105647325A CN105647325A CN201610028276.XA CN201610028276A CN105647325A CN 105647325 A CN105647325 A CN 105647325A CN 201610028276 A CN201610028276 A CN 201610028276A CN 105647325 A CN105647325 A CN 105647325A
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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
- 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
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/46—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with organic materials
- C04B41/48—Macromolecular compounds
- C04B41/4857—Other macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/60—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only artificial stone
- C04B41/61—Coating or impregnation
- C04B41/62—Coating or impregnation with organic materials
- C04B41/63—Macromolecular compounds
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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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- 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
- 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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- 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
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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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 invention discloses a raw soil waterproof heat insulation coating and a preparation method thereof. Methacryloyloxyethyl-dodecyl-trimethyl ammonium chloride is adsorbed to the surface of wet gel; after supercritical drying, unsaturated bonds on methacryloyloxyethyl-dodecyl-trimethyl ammonium chloride molecules adsorbed under the electrostatic attraction action of the surface of aerogel are copolymerized with methyl methacrylate under an emulsion system, and copolymer molecular chains are introduced into the surface of aerogel. According to the technical scheme, copolymer macromolecular chains wrap the surface of an aerogel skeleton uniformly, and thus the coating product can keep a three-dimensional network structure and has excellent heat insulation performance.
Description
Technical field
The invention belongs to green construction material technical field, more particularly, the preparation method relating to a kind of raw-soil waterproof heat-insulating coating.
Background technology
Earth building refers to not fired and only passes through the original state earthen materia of simple closely knit processing, builds the building body of agent structure. Earth building is building type that is a kind of the most ancient and that be also always widely adopted so far. Owing to the raw-soil is widely distributed, fetch earth conveniently, economical and practical, and it is cool in summer and warm in winter to adopt the building that the raw-soil is built to have, firm durable characteristic, so for a long time, raw soil material is a kind of construction material (" earth building field investigation " that numerous people is commonly used, the work such as Zhang Yannian, Science Press, 2014). Since being formed from human society, the raw-soil is always up topmost construction material, there is the inhabitants live of more than 1/3 in the world among earth building, China rural area so far there are that more than 100,000,000, inhabitants live is in earth building, therefore, how rapid economic development instantly with development in new countryside construction and improve traditional earth building, the improvement to China's rural residence condition, and expand raw soil material, in the application of other field, all there is very great meaning. Forming firmly chemical bond in the construction materials such as conventional concrete after cement mortar solidification, give the support force powerful with building, meanwhile, discarded concrete becomes highly stable, is difficult to reuse, and resource and environment are caused serious harm. Owing to raw soil material comes from natural original soil, strong chemical bond is rarely had so that it is there are extremely excellent reusable edible potentiality between soil particle, exactly because but raw soil material special construction, also critical defect can be brought to it, the service life of earth building in serious threat, and especially raw soil material is not water-fast, meets the shortcoming such as water softening, intensity reduction, the use making earth building is restricted (" life mechanism of earth building ", Wang Xiaohua work, China Construction Industry Press, 2010). Therefore, how raw soil material is modified, strengthens resistance to water and the durability of raw soil material, improve the service life of earth building, the problem that must first solve with regard to becoming raw soil material to study.
Summary of the invention
It is an object of the invention to overcome above-mentioned the deficiencies in the prior art, overcome the shortcoming that existing raw soil material poor water resistance, thermal and insulating performance are not good, the preparation method providing a kind of raw-soil waterproof heat-insulating coating, is conducive to significantly improving the resistance to water of raw soil material and thermal and insulating performance.
The technical purpose of the present invention is achieved by following technical proposals:
Raw-soil waterproof heat-insulating coating and preparation method thereof, carries out as steps described below:
Step 1, in 80-150 weight portion tetraethyl orthosilicate in the aqueous solution of the hydrogen chloride of addition 0.1-1 weight portion 12mol/L (i.e. hydrochloric acid), 30-180min is stood after stirring 5-30min under room temperature 20 25 degrees Celsius, it is subsequently added 0.01-0.2 parts by weight of sodium hydroxide solid, stirring is completely dissolved to it, wet gel is obtained after above-mentioned solution left standstill 2-6h, wet gel adds 0.1-1 weight portion methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride, after standing 2-6h, product is placed in CO2In supercritical high-pressure extraction device, with CO2Under temperature 30-50 DEG C and air pressure 7-10MPa, carry out supercritical drying at least 1h for medium, aerosil can be obtained.
In described step 1, carrying out the supercritical drying time is 2 3h.
In described step 1, with CO2Carrying out supercritical drying for medium, temperature is 35 40 DEG C, and air pressure is 8 9MPa.
In described step 1, tetraethyl orthosilicate is 100 120 weight portions, sodium hydrate solid is 0.05 0.1 weight portions, and methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride is 0.3 0.8 weight portions, and the aqueous solution of the hydrogen chloride of 12mol/L is 0.3 0.8 weight portions.
In described step 1, adding after in the aqueous solution of hydrogen chloride in tetraethyl orthosilicate, stand 60-120min after stirring 10-20min under room temperature 20 25 degrees Celsius, mixing speed is 100 150 turns per minute; Being subsequently added sodium hydrate solid, stirring is completely dissolved to it, and mixing speed is 100 150 turns per minute, obtains wet gel after above-mentioned solution left standstill 3 5h, adds methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride, stand 3 5h in wet gel.
Step 2,0.1-0.5 weight portion sodium lauryl sulphate is dissolved in 50-100 parts by weight of deionized water, aerosil 10-20 weight portion step 1 obtained is dispersed in 50 60 weight portion dehydrated alcohol, then the dehydrated alcohol being dispersed with aerosil is joined dissolved with in the deionized water of sodium lauryl sulphate and be uniformly dispersed, noble gas is used to carry out getting rid of air, so that reaction carries out under anaerobic, and it is warming up to 50-70 DEG C; Under maintaining stirring condition, dropping 80-90 parts by weight of methylmethacrylate dropwises in 15-30min, it is warming up to 70-90 DEG C, add 0.1-0.5 weight portion potassium peroxydisulfate and 0.01-0.05 pbw of potassium carbonate, cooling after reaction 5-10h, namely obtain raw-soil waterproof heat-insulating coating.
In described step 2, use noble gas is nitrogen, helium or argon.
In described step 2, sodium lauryl sulphate is 0.2 0.3 weight portions, and deionized water is 60 80 weight portions, the aerosil that step 1 obtains is 15 18 weight portions, dehydrated alcohol is 55 60 weight portions, and potassium peroxydisulfate is 0.2 0.3 weight portions, and potassium carbonate is 0.02 0.04 weight portions.
In described step 2, use noble gas to pass into reaction system at least 30min and carry out getting rid of air, so that reaction carries out under anaerobic, it is preferable that 30 40min.
In described step 2, after dropwising methyl methacrylate, using noble gas to pass into reaction system and carry out getting rid of air, so that reaction carries out under anaerobic, the time of passing into is 10 20min, then heats up.
In described step 2, reaction naturally cools to 25-40 DEG C after terminating, and namely obtains raw-soil waterproof heat-insulating coating.
The ZetaPALS type high-resolution Zeta potential and the Particle Size Analyzer that adopt U.S. Brookhaven measure Zeta potential respectively, result is as shown in Figure 1, a is the aerosil (modifying without methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride) adopting the process of step 1 of the present invention to prepare, b is that (process adopting step 2 of the present invention is prepared for the copolymer solution of methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride and methyl methacrylate, without aerosil, directly methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride and methyl methacrylate are carried out copolymerization), c is the aerosil wet gel (modifying through methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride) adopting the process of step 1 of the present invention to prepare, d is the aerosil (modifying through methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride) adopting the process of step 1 of the present invention to prepare. it can be seen that the Zeta potential of the aerosil of non-modified is negative value (-38.61mV) shown in accompanying drawing 1. its reason is owing to silicon dioxide (SA) surface without hydrophobic modification is with a large amount of silicone hydroxyl, ionizes with the water effect in air, forms electronegative ion SiO-, the Zeta potential of the copolymer solution of methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride and methyl methacrylate, for being owing to methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride is as cationic monomer on the occasion of (24.43mV), can produce positively charged quaternary ammonium group-N with water effect+(CH3)3; The Zeta potential of the aerosil wet gel modified through methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride building that boundary obtains by adelphotaxy between positive charge on the negative charge on aeroge skeleton surface and methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride molecule is-18.61mV. This is owing to building and in copolymer polymerization process at boundary, positively charged methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride molecule can attracted on electronegative gel skeleton, composite is made electrically to be neutralized, Zeta potential value is between unmodified aeroge and copolymer, and Zeta potential is negative value, illustrate that aeroge skeleton surface still has partial negative charge not to be neutralized. And when wet gel obtains after the aerosil that methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride is modified through supercritical drying process, significant change is there is not before Zeta potential is relatively dry, visible electrostatic attraction effect is sufficiently strong so that aeroge surface relies on the methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride of electrostatic interaction absorption that obvious desorption phenomenon does not occur.
Adopt U.S.'s Nicolet--5DX Fourier transform infrared spectrometer to measure and obtain infrared spectrogram, wherein a is the aerosil modified without methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride, and b is the aerosil modified through methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride. It will be seen that the spectral line (a) of not modified aeroge is at 803cm from spectrogram-1And 1103cm-1There is absworption peak at place, and that corresponding is SiO respectively2The symmetry of middle Si-O and the characteristic absorption peak of asymmetrical stretching vibration, 3442cm-1That place is corresponding is SiO2The stretching vibration absworption peak of surface hydroxyl, and 1630cm-1What place was corresponding is then the absworption peak of residual water in test sample.And when aerosil is after methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride is modified, at the 1453cm of spectral line (b)-1Place occurs in that the bending vibration absworption peak corresponding to methylene adjacent with quaternary ammonium group in methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride, this further illustrates by electrostatic attraction effect, and methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride is successfully modified on aerosil.
Section after the aerosil modified through methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride and the solidification of raw-soil waterproof heat-insulating coating is observed by Nanosem430 field emission scanning electron microscope respectively that adopt Holland Philips, as shown in Figure 3, the aerosil modified through methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride has the three-dimensional net structure that Nano particles of silicon dioxide connection is formed, and nano level hole distribution is comparatively uniform. It is polymerized, with PMMA emulsion, the raw-soil waterproof heat-insulating coating obtained at the aerosil modified through methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride and does not significantly change the microstructure of material after hardening, still there is inside coating Nano particles of silicon dioxide and connect the three-dimensional net structure formed, and nano level hole distribution is comparatively uniform. Measuring through the N2 adsorption specific surface area measuring instrument of Bei Shide instrument science and technology (Beijing) company limited, utilize the porosity average out to 93 95% of the dope layer that the raw-soil waterproof heat-insulating coating of the present invention formed, pore-size distribution is comparatively uniform.
The application in the raw-soil is waterproof thermal-insulated of the raw-soil waterproof heat-insulating coating of the present invention, use coating to carry out spraying or brushing on raw-soil surface when using, to form waterproof thermal-insulated coating on raw-soil surface, waterproof thermal-insulated coating layer thickness is 0.1 1mm, it is preferable that 0.3 0.8mm. With reference to GB GB/T19250-2003, the impermeability of coating being tested, raw-soil waterproof heat-insulating coating has higher impermeability. Adopt Xi'an Xiatech Electronic Technology Co., Ltd. TC3000E type heat conductivity instrument that the heat conductivity of coating is measured, average out to 0.01 0.02Wm-1K-1, raw-soil waterproof heat-insulating coating has extremely low heat conductivility, embodies significantly high heat insulating ability.
Therefore, the preparation method of a kind of raw-soil waterproof heat-insulating coating of the present invention, in step 1, utilize the negative charge of aerosil wet gel surface silanol group and the electrostatic attraction effect of methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride positive charge, methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride is adsorbed in wet gel surface, after supercritical drying, methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride molecule is still without departing from aeroge surface, it is shown that very strong interaction. Step 2 utilizes the unsaturated bond on the methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride molecule that aeroge surface electrostatic sucking action adsorbs and methyl methacrylate copolymerization under emulsion system, copolymer molecule chain can be introduced aeroge surface, copolymer macromolecular chain is uniformly wrapped in aeroge skeleton surface, coating product can be made to keep tridimensional network, have excellent heat-insulating property.
Accompanying drawing explanation
Fig. 1 is Zeta potential figure, wherein a is the aerosil adopting the process of step 1 of the present invention to prepare, b is the copolymer solution of methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride and methyl methacrylate, c is the aerosil wet gel adopting the process of step 1 of the present invention to prepare, and d is the aerosil adopting the process of step 1 of the present invention to prepare.
Fig. 2 is Fourier transform infrared spectroscopy figure, and wherein a is the aerosil modified without methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride; B is the aerosil modified through methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride.
Fig. 3 is SEM photograph, and wherein a is the aerosil modified through methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride; B is the section after raw-soil waterproof heat-insulating coating solidifies.
Detailed description of the invention
Further illustrating technical scheme below in conjunction with specific embodiment, wherein methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride is purchased from Sigma-Aldrich company; Other reagent and raw material are all purchased from Tianjin Kermel Chemical Reagent Co., Ltd., and that supercritical drying equipment adopts is Haian Oil Scientific Research Apparatus Co., Ltd. CO2Supercritical high-pressure extraction device.
Embodiment 1
80g tetraethyl orthosilicate adds 0.1g12mol/L hydrochloric acid, 35min is stood after 28min is stirred at room temperature, it is subsequently added 0.14 sodium hydroxide, stirring is completely dissolved to it, wet gel is obtained after above-mentioned solution left standstill 2h, wet gel adds 0.2g methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride, after standing 6h, product is placed in CO2In supercritical high-pressure extraction device, with CO2At temperature 33 DEG C and air pressure 7MPa, supercritical drying 3h is carried out for medium, aerosil can be obtained, 0.1g sodium lauryl sulphate is dissolved in 50g deionized water, join in sodium lauryl sulphate after 10g aerosil 50g dehydrated alcohol moistening, stir and ultrasonic 60min. Transferring it in the four-hole boiling flask equipped with agitator, reflux condensing tube, Dropping funnel and thermometer, inflated with nitrogen 30min is to get rid of air, and is progressively warmed up to 70 DEG C. Start to drip 80g methyl methacrylate, drip off in 30min, after dripping off, continue stirring, and after the about 10min of inflated with nitrogen, it is warming up to 72 DEG C, adds 0.1g potassium peroxydisulfate and 0.05g potassium carbonate, continue reaction 5h, after being cooled to 25 DEG C, namely obtain raw-soil waterproof heat-insulating coating.
Embodiment 2
110g tetraethyl orthosilicate adds 0.8g12mol/L hydrochloric acid, 150min is stood after 30min is stirred at room temperature, it is subsequently added 0.01 sodium hydroxide, stirring is completely dissolved to it, wet gel is obtained after above-mentioned solution left standstill 3h, wet gel adds 0.6g methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride, after standing 3h, product is placed in CO2In supercritical high-pressure extraction device, with CO2At temperature 46 DEG C and air pressure 8MPa, supercritical drying 3h is carried out for medium, aerosil can be obtained, 0.3g sodium lauryl sulphate is dissolved in 100g deionized water, join in sodium lauryl sulphate after 15g aerosil 54g dehydrated alcohol moistening, stir and ultrasonic 25min. Transferring it in the four-hole boiling flask equipped with agitator, reflux condensing tube, Dropping funnel and thermometer, inflated with nitrogen 30min is to get rid of air, and is progressively warmed up to 57 DEG C. Start to drip 82g methyl methacrylate, drip off in 24min, after dripping off, continue stirring, and after the about 12min of inflated with nitrogen, it is warming up to 75 DEG C, adds 0.3g potassium peroxydisulfate and 0.01g potassium carbonate, continue reaction 6h, after being cooled to 30 DEG C, namely obtain raw-soil waterproof heat-insulating coating.
Embodiment 3
150g tetraethyl orthosilicate adds 0.2g12mol/L hydrochloric acid, 180min is stood after 5min is stirred at room temperature, it is subsequently added 0.16 sodium hydroxide, stirring is completely dissolved to it, wet gel is obtained after above-mentioned solution left standstill 6h, wet gel adds 0.7g methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride, after standing 5h, product is placed in CO2In supercritical high-pressure extraction device, with CO2Under temperature 50 C and air pressure 9MPa, supercritical drying 3h is carried out for medium, aerosil can be obtained, 0.5g sodium lauryl sulphate is dissolved in 65g deionized water, join in sodium lauryl sulphate after 18g aerosil 53g dehydrated alcohol moistening, stir and ultrasonic 52min.Transferring it in the four-hole boiling flask equipped with agitator, reflux condensing tube, Dropping funnel and thermometer, inflated with nitrogen 30min is to get rid of air, and is progressively warmed up to 64 DEG C. Start to drip 84g methyl methacrylate, drip off in 16min, after dripping off, continue stirring, and after the about 16min of inflated with nitrogen, it is warming up to 76 DEG C, adds 0.4g potassium peroxydisulfate and 0.02g potassium carbonate, continue reaction 7h, after being cooled to 26 DEG C, namely obtain raw-soil waterproof heat-insulating coating.
Embodiment 4
142g tetraethyl orthosilicate adds 0.5g12mol/L hydrochloric acid, 30min is stood after 21min is stirred at room temperature, it is subsequently added 0.2 sodium hydroxide, stirring is completely dissolved to it, wet gel is obtained after above-mentioned solution left standstill 5h, wet gel adds 1g methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride, after standing 2h, product is placed in CO2In supercritical high-pressure extraction device, with CO2At temperature 37 DEG C and air pressure 10MPa, supercritical drying 3h is carried out for medium, aerosil can be obtained, 0.2g sodium lauryl sulphate is dissolved in 85g deionized water, join in sodium lauryl sulphate after 17g aerosil 56g dehydrated alcohol moistening, stir and ultrasonic 45min. Transferring it in the four-hole boiling flask equipped with agitator, reflux condensing tube, Dropping funnel and thermometer, inflated with nitrogen 30min is to get rid of air, and is progressively warmed up to 53 DEG C. Start to drip 86g methyl methacrylate, drip off in 29min, after dripping off, continue stirring, and after the about 18min of inflated with nitrogen, it is warming up to 84 DEG C, adds 0.15g potassium peroxydisulfate and 0.04g potassium carbonate, continue reaction 8h, after being cooled to 40 DEG C, namely obtain raw-soil waterproof heat-insulating coating.
Embodiment 5
95g tetraethyl orthosilicate adds 1g12mol/L hydrochloric acid, 68min is stood after 13min is stirred at room temperature, it is subsequently added 0.1 sodium hydroxide, stirring is completely dissolved to it, wet gel is obtained after above-mentioned solution left standstill 4h, wet gel adds 0.3g methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride, after standing 4h, product is placed in CO2In supercritical high-pressure extraction device, with CO2Under temperature 45 C and air pressure 8.5MPa, supercritical drying 3h is carried out for medium, aerosil can be obtained, 0.4g sodium lauryl sulphate is dissolved in 96g deionized water, join in sodium lauryl sulphate after 20g aerosil 60g dehydrated alcohol moistening, stir and ultrasonic 10min. Transferring it in the four-hole boiling flask equipped with agitator, reflux condensing tube, Dropping funnel and thermometer, inflated with nitrogen 30min is to get rid of air, and is progressively warmed up to 61 DEG C. Start to drip 90g methyl methacrylate, drip off in 15min, after dripping off, continue stirring, and after the about 20min of inflated with nitrogen, it is warming up to 90 DEG C, adds 0.5g potassium peroxydisulfate and 0.03g potassium carbonate, continue reaction 10h, after being cooled to 36 DEG C, namely obtain raw-soil waterproof heat-insulating coating.
Table 1 impermeability and heat conductivity
| Embodiment | Impermeability 0.3MPa �� 30min | Heat conductivity |
| Embodiment 1 | Waterproof | 0.013Wm-1K-1 |
| Embodiment 2 | Waterproof | 0.017Wm-1K-1 |
| Embodiment 3 | Waterproof | 0.020Wm-1K-1 |
| Embodiment 4 | Waterproof | 0.011Wm-1K-1 |
| Embodiment 5 | Waterproof | 0.017Wm-1K-1 |
The technical scheme utilizing present invention carries out the adjustment of technological parameter, all can prepare raw-soil waterproof heat-insulating coating, and show essentially identical impermeability and heat conductivility.
Above the present invention has been done exemplary description; should be noted that; when without departing from the core of the present invention, any simple deformation, amendment or other those skilled in the art can not spend the equivalent replacement of creative work to each fall within protection scope of the present invention.
Claims (10)
1. raw-soil waterproof heat-insulating coating, it is characterised in that carry out as steps described below:
Step 1,80-150 weight portion tetraethyl orthosilicate add in the aqueous solution of hydrogen chloride of 0.1-1 weight portion 12mol/L, 30-180min is stood after stirring 5-30min under room temperature 20 25 degrees Celsius, it is subsequently added 0.01-0.2 parts by weight of sodium hydroxide solid, stirring is completely dissolved to it, obtains wet gel after above-mentioned solution left standstill 2-6h, adds 0.1-1 weight portion methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride in wet gel, after standing 2-6h, product is placed in CO2In supercritical high-pressure extraction device, with CO2Under temperature 30-50 DEG C and air pressure 7-10MPa, carry out supercritical drying at least 1h for medium, aerosil can be obtained;
Step 2,0.1-0.5 weight portion sodium lauryl sulphate is dissolved in 50-100 parts by weight of deionized water, aerosil 10-20 weight portion step 1 obtained is dispersed in 50 60 weight portion dehydrated alcohol, then the dehydrated alcohol being dispersed with aerosil is joined dissolved with in the deionized water of sodium lauryl sulphate and be uniformly dispersed, noble gas is used to carry out getting rid of air, so that reaction carries out under anaerobic, and it is warming up to 50-70 DEG C; Under maintaining stirring condition, dropping 80-90 parts by weight of methylmethacrylate dropwises in 15-30min, it is warming up to 70-90 DEG C, add 0.1-0.5 weight portion potassium peroxydisulfate and 0.01-0.05 pbw of potassium carbonate, cooling after reaction 5-10h, namely obtain raw-soil waterproof heat-insulating coating.
2. raw-soil waterproof heat-insulating coating according to claim 1, it is characterised in that in described step 1, carrying out the supercritical drying time is 2 3h, with CO2Carrying out supercritical drying for medium, temperature is 35 40 DEG C, and air pressure is 8 9MPa.
3. raw-soil waterproof heat-insulating coating according to claim 1, it is characterized in that, in described step 1, tetraethyl orthosilicate is 100 120 weight portions, sodium hydrate solid is 0.05 0.1 weight portions, methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride is 0.3 0.8 weight portions, and the aqueous solution of the hydrogen chloride of 12mol/L is 0.3 0.8 weight portions; Adding in tetraethyl orthosilicate after in the aqueous solution of hydrogen chloride, stand 60-120min after stirring 10-20min under room temperature 20 25 degrees Celsius, mixing speed is 100 150 turns per minute; Being subsequently added sodium hydrate solid, stirring is completely dissolved to it, and mixing speed is 100 150 turns per minute, obtains wet gel after above-mentioned solution left standstill 3 5h, adds methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride, stand 3 5h in wet gel.
4. raw-soil waterproof heat-insulating coating according to claim 1, it is characterised in that in described step 2, use noble gas is nitrogen, helium or argon; Use noble gas to pass into reaction system at least 30min to carry out getting rid of air, so that reaction carries out under anaerobic, it is preferable that 30 40min; After dropwising methyl methacrylate, using noble gas to pass into reaction system and carry out getting rid of air, so that reaction carries out under anaerobic, the time of passing into is 10 20min, then heats up; Reaction naturally cools to 25-40 DEG C after terminating, and namely obtains raw-soil waterproof heat-insulating coating.
5. raw-soil waterproof heat-insulating coating according to claim 1, it is characterized in that, in described step 2, sodium lauryl sulphate is 0.2 0.3 weight portions, deionized water is 60 80 weight portions, and the aerosil that step 1 obtains is 15 18 weight portions, and dehydrated alcohol is 55 60 weight portions, potassium peroxydisulfate is 0.2 0.3 weight portions, and potassium carbonate is 0.02 0.04 weight portions.
6. the preparation method of raw-soil waterproof heat-insulating coating, it is characterised in that carry out as steps described below:
Step 1,80-150 weight portion tetraethyl orthosilicate add in the aqueous solution of hydrogen chloride of 0.1-1 weight portion 12mol/L, 30-180min is stood after stirring 5-30min under room temperature 20 25 degrees Celsius, it is subsequently added 0.01-0.2 parts by weight of sodium hydroxide solid, stirring is completely dissolved to it, obtains wet gel after above-mentioned solution left standstill 2-6h, adds 0.1-1 weight portion methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride in wet gel, after standing 2-6h, product is placed in CO2In supercritical high-pressure extraction device, with CO2Under temperature 30-50 DEG C and air pressure 7-10MPa, carry out supercritical drying at least 1h for medium, aerosil can be obtained;
Step 2,0.1-0.5 weight portion sodium lauryl sulphate is dissolved in 50-100 parts by weight of deionized water, aerosil 10-20 weight portion step 1 obtained is dispersed in 50 60 weight portion dehydrated alcohol, then the dehydrated alcohol being dispersed with aerosil is joined dissolved with in the deionized water of sodium lauryl sulphate and be uniformly dispersed, noble gas is used to carry out getting rid of air, so that reaction carries out under anaerobic, and it is warming up to 50-70 DEG C; Under maintaining stirring condition, dropping 80-90 parts by weight of methylmethacrylate dropwises in 15-30min, it is warming up to 70-90 DEG C, add 0.1-0.5 weight portion potassium peroxydisulfate and 0.01-0.05 pbw of potassium carbonate, cooling after reaction 5-10h, namely obtain raw-soil waterproof heat-insulating coating.
7. the preparation method of raw-soil waterproof heat-insulating coating according to claim 6, it is characterised in that in described step 1, carrying out the supercritical drying time is 2 3h, with CO2Carrying out supercritical drying for medium, temperature is 35 40 DEG C, and air pressure is 8 9MPa.
8. the preparation method of raw-soil waterproof heat-insulating coating according to claim 6, it is characterized in that, in described step 1, tetraethyl orthosilicate is 100 120 weight portions, sodium hydrate solid is 0.05 0.1 weight portions, methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride is 0.3 0.8 weight portions, and the aqueous solution of the hydrogen chloride of 12mol/L is 0.3 0.8 weight portions; Adding in tetraethyl orthosilicate after in the aqueous solution of hydrogen chloride, stand 60-120min after stirring 10-20min under room temperature 20 25 degrees Celsius, mixing speed is 100 150 turns per minute; Being subsequently added sodium hydrate solid, stirring is completely dissolved to it, and mixing speed is 100 150 turns per minute, obtains wet gel after above-mentioned solution left standstill 3 5h, adds methylacryoyloxyethyl Dodecyl trimethyl ammonium chloride, stand 3 5h in wet gel.
9. the preparation method of raw-soil waterproof heat-insulating coating according to claim 6, it is characterised in that in described step 2, use noble gas is nitrogen, helium or argon; Use noble gas to pass into reaction system at least 30min to carry out getting rid of air, so that reaction carries out under anaerobic, it is preferable that 30 40min; After dropwising methyl methacrylate, using noble gas to pass into reaction system and carry out getting rid of air, so that reaction carries out under anaerobic, the time of passing into is 10 20min, then heats up; Reaction naturally cools to 25-40 DEG C after terminating, and namely obtains raw-soil waterproof heat-insulating coating.
10. the preparation method of raw-soil waterproof heat-insulating coating according to claim 6, it is characterized in that, in described step 2, sodium lauryl sulphate is 0.2 0.3 weight portions, deionized water is 60 80 weight portions, and the aerosil that step 1 obtains is 15 18 weight portions, and dehydrated alcohol is 55 60 weight portions, potassium peroxydisulfate is 0.2 0.3 weight portions, and potassium carbonate is 0.02 0.04 weight portions.
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| CN201710412923.1A CN107177265A (en) | 2016-01-16 | 2016-01-16 | Application of the waterproof heat-insulating coating in the raw-soil is waterproof thermal-insulated |
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