CN116283003A - Long-period hydrophilic and hydrophobic integrated concrete tube culture material and preparation method thereof - Google Patents
Long-period hydrophilic and hydrophobic integrated concrete tube culture material and preparation method thereof Download PDFInfo
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- CN116283003A CN116283003A CN202310271445.2A CN202310271445A CN116283003A CN 116283003 A CN116283003 A CN 116283003A CN 202310271445 A CN202310271445 A CN 202310271445A CN 116283003 A CN116283003 A CN 116283003A
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- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 115
- 239000000463 material Substances 0.000 title claims abstract description 95
- 238000002360 preparation method Methods 0.000 title claims abstract description 43
- 239000011248 coating agent Substances 0.000 claims abstract description 115
- 238000000576 coating method Methods 0.000 claims abstract description 115
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 99
- 239000000843 powder Substances 0.000 claims abstract description 85
- 239000004965 Silica aerogel Substances 0.000 claims abstract description 73
- 238000003756 stirring Methods 0.000 claims abstract description 69
- 239000007788 liquid Substances 0.000 claims abstract description 67
- 238000002156 mixing Methods 0.000 claims abstract description 60
- 239000002994 raw material Substances 0.000 claims abstract description 60
- 238000001035 drying Methods 0.000 claims abstract description 34
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 33
- 239000003999 initiator Substances 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 27
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 23
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000010457 zeolite Substances 0.000 claims abstract description 23
- 150000001875 compounds Chemical class 0.000 claims abstract description 22
- 239000013078 crystal Substances 0.000 claims abstract description 22
- GLOZHJZEJIXYLM-UHFFFAOYSA-N 4-hydroxy-3,3-bis(hydroxymethyl)-1-(methylamino)butane-1-sulfonic acid Chemical compound OCC(CC(S(=O)(=O)O)NC)(CO)CO GLOZHJZEJIXYLM-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001914 filtration Methods 0.000 claims abstract description 15
- 230000008569 process Effects 0.000 claims abstract description 14
- 238000010306 acid treatment Methods 0.000 claims abstract description 3
- 239000011259 mixed solution Substances 0.000 claims description 106
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 88
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 81
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 claims description 70
- 239000000725 suspension Substances 0.000 claims description 64
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims description 48
- 239000006185 dispersion Substances 0.000 claims description 40
- 229920001577 copolymer Polymers 0.000 claims description 39
- 235000019359 magnesium stearate Nutrition 0.000 claims description 35
- 239000008367 deionised water Substances 0.000 claims description 30
- 229910021641 deionized water Inorganic materials 0.000 claims description 30
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 claims description 26
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 26
- 230000007062 hydrolysis Effects 0.000 claims description 26
- 238000006460 hydrolysis reaction Methods 0.000 claims description 26
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 24
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 24
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 24
- DOOTYTYQINUNNV-UHFFFAOYSA-N Triethyl citrate Chemical compound CCOC(=O)CC(O)(C(=O)OCC)CC(=O)OCC DOOTYTYQINUNNV-UHFFFAOYSA-N 0.000 claims description 23
- 239000001069 triethyl citrate Substances 0.000 claims description 23
- VMYFZRTXGLUXMZ-UHFFFAOYSA-N triethyl citrate Natural products CCOC(=O)C(O)(C(=O)OCC)C(=O)OCC VMYFZRTXGLUXMZ-UHFFFAOYSA-N 0.000 claims description 23
- 235000013769 triethyl citrate Nutrition 0.000 claims description 23
- -1 polydiethoxysiloxane Polymers 0.000 claims description 22
- 239000000499 gel Substances 0.000 claims description 20
- 238000007873 sieving Methods 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 20
- QQIRAVWVGBTHMJ-UHFFFAOYSA-N [dimethyl-(trimethylsilylamino)silyl]methane;lithium Chemical compound [Li].C[Si](C)(C)N[Si](C)(C)C QQIRAVWVGBTHMJ-UHFFFAOYSA-N 0.000 claims description 15
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 13
- 229920002545 silicone oil Polymers 0.000 claims description 13
- FUOZJYASZOSONT-UHFFFAOYSA-N 2-propan-2-yl-1h-imidazole Chemical compound CC(C)C1=NC=CN1 FUOZJYASZOSONT-UHFFFAOYSA-N 0.000 claims description 12
- 230000032683 aging Effects 0.000 claims description 12
- YEECOJZAMZEUBB-UHFFFAOYSA-N 2,2,3,3,6,6,7,7-octamethyloctane Chemical compound CC(C)(C)C(C)(C)CCC(C)(C)C(C)(C)C YEECOJZAMZEUBB-UHFFFAOYSA-N 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 8
- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 claims description 7
- HGXJDMCMYLEZMJ-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy 2,2-dimethylpropaneperoxoate Chemical compound CC(C)(C)OOOC(=O)C(C)(C)C HGXJDMCMYLEZMJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 238000000265 homogenisation Methods 0.000 claims description 2
- 230000003301 hydrolyzing effect Effects 0.000 claims description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N methyl pentane Natural products CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims 2
- 239000004566 building material Substances 0.000 abstract description 3
- AMTWCFIAVKBGOD-UHFFFAOYSA-N dioxosilane;methoxy-dimethyl-trimethylsilyloxysilane Chemical compound O=[Si]=O.CO[Si](C)(C)O[Si](C)(C)C AMTWCFIAVKBGOD-UHFFFAOYSA-N 0.000 description 18
- 238000011056 performance test Methods 0.000 description 18
- 229940083037 simethicone Drugs 0.000 description 18
- 238000005303 weighing Methods 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 14
- 239000004568 cement Substances 0.000 description 11
- DBEDTBJGEXDPBT-UHFFFAOYSA-N 1-amino-4-hydroxy-3,3-bis(hydroxymethyl)butane-1-sulfonic acid Chemical compound OS(=O)(=O)C(N)CC(CO)(CO)CO DBEDTBJGEXDPBT-UHFFFAOYSA-N 0.000 description 9
- 239000002253 acid Substances 0.000 description 8
- 239000006260 foam Substances 0.000 description 8
- YNESATAKKCNGOF-UHFFFAOYSA-N lithium bis(trimethylsilyl)amide Chemical compound [Li+].C[Si](C)(C)[N-][Si](C)(C)C YNESATAKKCNGOF-UHFFFAOYSA-N 0.000 description 8
- 238000005336 cracking Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000007710 freezing Methods 0.000 description 5
- 230000008014 freezing Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000004964 aerogel Substances 0.000 description 4
- 230000036571 hydration Effects 0.000 description 4
- 238000006703 hydration reaction Methods 0.000 description 4
- 230000007246 mechanism Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 238000010257 thawing Methods 0.000 description 3
- 244000025254 Cannabis sativa Species 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 229920006037 cross link polymer Polymers 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 229920001477 hydrophilic polymer Polymers 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 229920000620 organic polymer Polymers 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 125000000020 sulfo group Chemical group O=S(=O)([*])O[H] 0.000 description 2
- 230000003075 superhydrophobic effect Effects 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000012669 compression test Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 238000004382 potting Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
Classifications
-
- 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
- C04B18/00—Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B18/02—Agglomerated materials, e.g. artificial aggregates
- C04B18/027—Lightweight materials
-
- 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
- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/02—Granular materials, e.g. microballoons
- C04B14/04—Silica-rich materials; Silicates
- C04B14/06—Quartz; Sand
- C04B14/064—Silica aerogel
-
- 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
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/10—Coating or impregnating
- C04B20/1051—Organo-metallic compounds; Organo-silicon compounds, e.g. bentone
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Civil Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention provides a long-period hydrophilic and hydrophobic integrated concrete curing material and a preparation method thereof, and belongs to the technical field of building materials. The material comprises the following raw materials in percentage by weight: 45-53% of hydrophobic silica aerogel powder, 11.3-13.2% of coating liquid, 32-34.6% of trimethylol methylaminopropane sulfonic acid, 2-7% of zeolite, 0.03-0.05% of cross-linking agent and 0.5-1% of initiator; wherein, the coating liquid wraps the hydrophobic silica aerogel powder. The preparation method comprises the steps of placing hydrophobic silica aerogel powder in a coating pan, controlling the temperature of the coating pan and the supply rate of coating liquid, taking out and drying after coating for a set time to obtain coated crystals G; uniformly mixing the coated crystal G and the trimethylol methylaminopropane sulfonic acid, adding zeolite subjected to acid treatment, adding a cross-linking agent and an initiator in the stirring process, and reacting for a set time to obtain a compound H; and taking out the compound H, drying and filtering to obtain the long-period hydrophilic-hydrophobic integrated concrete curing material.
Description
Technical Field
The invention belongs to the technical field of building materials, and particularly relates to a long-period hydrophilic-hydrophobic integrated concrete tube-culture material and a preparation method thereof.
Background
Concrete is one of the most widely used building materials in the civil engineering field at present, and has the advantages of wide raw material sources, low price, excellent building performance and the like, so that the concrete is widely applied to the fields of roads, bridges, hydraulic structures, house buildings and the like. And with the continuous promotion of town, the demand of cement and concrete materials on the market is still very large. However, the physical structure of concrete itself is porous, water permeates into the interior of the concrete along micropores, and the concrete cracks due to freezing and swelling in cold weather, and the concrete cracks seriously under repeated freezing and thawing cycles caused by temperature changes, so that the structural performance of the concrete is greatly reduced. And the relative humidity in the concrete is lower, and the early maintenance is insufficient and is easy to generate larger deformation due to the self-shrinkage effect, so that the crack in the concrete is generated and cracked, and the mechanical property and durability of the concrete are reduced. Therefore, certain management and maintenance measures are needed to enable the concrete to have certain hydrophobic performance, the occurrence of freezing and thawing damage and icing of the concrete is reduced, the internal humidity of the concrete is improved, the evaporation of water is controlled, and the maximum hydration of the cement is promoted.
The hydrophobic mode and the curing mode used in most concrete engineering at present are a concrete hydrophobic coating and an external curing technology respectively. Wherein the hydrophobic coating is used for wrapping the concrete by the hydrophobic coating and isolating the concrete from water. However, the coating of the sealing package is fragile in surface microstructure, poor in durability, easy to damage through friction and collision, and poor in hydrophobic effect, and the coating is difficult to firmly adhere to the surface of concrete due to the adhesion between the hydrophobic coating and the concrete. The external curing technology refers to curing technologies such as covering a wet grass bag on the surface layer of concrete, covering a wet grass bag, a plastic film, directly spraying water and the like on the surface layer of concrete. The external curing technology from outside to inside not only consumes a great deal of manpower and financial resources, but also causes uneven curing due to the fact that external moisture is difficult to reach the inside of the concrete, can not effectively relieve self-shrinkage of the concrete, and reduces generation of internal microcracks of the concrete.
In order to effectively solve the problems of freezing resistance, icing and shrinkage cracking in the curing process in the long-term of concrete life, and improve the strength and durability of concrete, the internal mixing type concrete hydrophobic material and the internal curing technology become more and more the current research hot spot. The whole super-hydrophobic concrete is prepared by adding an organic reagent into the concrete to modify the low surface energy and constructing a rough structure on the surface of the concrete, so that the concrete has whole hydrophobicity. The action mechanism is that hydrophilic monomers on the surface of the concrete are converted into hydrophobic monomers through surface energy modification, so that the contact angle of the surface of the concrete is increased, water cannot infiltrate the concrete, water is prevented from infiltrating into the concrete, and freezing and thawing damage and surface icing phenomena are reduced. The internal curing of concrete refers to pre-impregnating light aggregate or adding a high molecular material with water absorption property as an internal curing material in the mixing process of concrete. The concrete hydration device has the advantages that the water is partially stored in the concrete, so that the humidity distribution in the concrete is adjusted, the water demand of the concrete hydration process is ensured, the hydration is promoted, the concrete is more compact, the strength of the concrete is improved, and the cracking of the concrete is reduced.
The super-hydrophobic modified materials and the internal curing materials used in the market at present can improve the hydrophobic effect and the curing effect of the concrete to a certain extent, but the strength of the concrete is reduced due to the fact that a large amount of the hydrophobic materials and the internal curing materials are added, so that the workability of the concrete is deteriorated. And as the action mechanisms of the water repellency and the internal curing of the concrete are contrary, the internal mixing material can not be ensured to have the water repellency and the internal curing simultaneously, and the effect of improving the durability of the concrete is not obvious for solving the problems of the frost resistance and the cracking of the concrete.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide the long-period hydrophilic and hydrophobic integrated concrete curing material and the preparation method thereof, which ensure that the self-shrinkage of the concrete can be reduced through internal sample protection and the hydrophobic performance can be realized through hydrophobic modification in a long period, and solve the technical problems of the reduction of the strength and the durability of the concrete.
In order to achieve the above purpose, the invention is realized by adopting the following technical scheme:
the invention provides a concrete long-period hydrophilic-hydrophobic integrated tube culture material, which comprises the following preparation raw materials in percentage by weight: 45-53% of hydrophobic silica aerogel powder, 11.3-13.2% of coating liquid, 32-34.6% of trimethylol methylaminopropane sulfonic acid, 2-7% of zeolite, 0.03-0.05% of cross-linking agent and 0.5-1% of initiator.
The invention further provides a preparation method of the hydrophobic silica aerogel powder, which comprises the following raw materials in percentage by weight:
15 to 25 percent of tetraethoxysilane, 15 to 20 percent of polydiethoxysilane, 13 to 18 percent of ethanol, 12 to 17 percent of deionized water, 0.8 to 1.2 percent of ammonia water, 8 to 15 percent of isophthalic acid, 10 to 15 percent of dimethyl dichlorosilane and 13 to 18 percent of hexamethyldisiloxane;
the coating liquid is prepared from the following raw materials:
35 to 45 percent of polylactic acid-glycolic acid copolymer, 11 to 15 percent of hexamethyldisilazane lithium, 4.5 to 8.1 percent of triethyl citrate, 37 to 43 percent of magnesium stearate and 0.5 to 0.9 percent of dimethyl silicone oil.
The invention further provides a cross-linking agent which consists of 2, 5-dimethyl-2, 5-di-tert-butyl-hexane peroxide and 2-isopropyl imidazole; wherein the mass ratio of the 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide to the 2-isopropyl imidazole is (1.7-2.2): 1, a step of;
the initiator is any one of tert-butyl peroxypivalate or tert-butyl peroxybenzoate.
The invention also provides a preparation method of the concrete long-period hydrophilic-hydrophobic integrated curing material, which comprises the following steps:
s1: placing the hydrophobic silica aerogel powder in a coating pan, coating the hydrophobic silica aerogel powder with coating liquid, taking out and drying after coating for a set time to obtain coated crystals G;
S2: uniformly mixing the coated crystal G and the trimethylol methylaminopropane sulfonic acid, adding zeolite subjected to acid treatment, adding a cross-linking agent and an initiator in the stirring process, and reacting for a set time to obtain a compound H;
s3: and taking out the compound H, drying and filtering to obtain the long-period hydrophilic-hydrophobic integrated concrete curing material.
In the invention, in the step S1, the temperature of the coating pot is 20-25 ℃, the supply rate of the coating liquid is 15-25 g/min/kg, and the coating setting time is 45-60 min; in the step S2, the reaction setting time is 0.5-1.5 h.
The preparation process of the hydrophobic silica aerogel powder is as follows:
s11: uniformly mixing tetraethoxysilane, polydiethoxysiloxane, ethanol and deionized water to obtain a mixed solution, adding isophthalic acid into the mixed solution, stirring, and hydrolyzing to obtain a hydrolyzed mixed solution A;
s12: adding ammonia water into the hydrolysis mixed solution A, mixing and stirring, and standing to obtain gel B;
mixing dimethyl dichlorosilane and hexamethyldisiloxane to obtain a mixed solution C, mixing ethanol with the mixed solution C to obtain a mixed solution D, covering the mixed solution D on the gel B, and performing surface aging to obtain hydrophobically modified silica gel E;
S13: washing and placing the hydrophobically modified silica gel E, drying, cooling, grinding and sieving to obtain the hydrophobic silica aerogel powder.
In the present invention, in S11, the concentration of isophthalic acid is 7 to 10mol/L.
In the invention, in the step S12, the concentration of the ammonia water is 15-20%;
the mass ratio of the dimethyldichlorosilane to the hexamethyldisiloxane is 1: (0.7-1.2); the mass ratio of the ethanol to the mixed solution C is (1.8-2.6): 1, a step of; the surface ageing time is 12-24 hours;
in the step S13, the washing times are more than 2 times, and ethanol is adopted for washing; the sieving adopts 500-1000 mesh sieve.
The preparation process of the coating liquid is as follows:
s21: adding polylactic acid-glycolic acid copolymer into deionized water for several times, stirring until the polylactic acid-glycolic acid copolymer is in a trickle state, and obtaining suspension A;
s22: adding a hexamethyldisilazane lithium solution into the suspension A, stirring, adding dimethyl silicone oil, and stirring to obtain a latex-like water dispersion B;
s23: filtering the latex-like aqueous dispersion B to obtain a filtered aqueous dispersion C; mixing magnesium stearate and triethyl citrate to obtain a mixed solution, adding the mixed solution into deionized water for homogenization, and then adding dimethyl silicone oil to obtain magnesium stearate suspension D;
S24: the magnesium stearate suspension D is added to the aqueous dispersion C and stirred to obtain a suspension E, and the suspension E is filtered to obtain a coating liquid.
In the step S21, the mass ratio of the polylactic acid-glycolic acid copolymer to deionized water is 1: (1.7-2.0);
in the step S22, the concentration of the hexamethyldisilazane lithium solution is 0.8-1.2 mol/L;
in the step S23, filtering is carried out by adopting a mesh sieve of 30-60 meshes; the mass ratio of magnesium stearate to triethyl citrate in the mixed solution is (1.8-2): 1, a step of; the mass ratio of the mixed solution to the deionized water is 1: (2.5-3.9); the homogenizing time is 5-10 min;
in the step S24, the solid-to-liquid ratio of the suspension E is 20-25%, and the suspension E is filtered by a mesh sieve of 30-60.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a long-period hydrophilic and hydrophobic integrated concrete curing material, wherein hydrophobic silica aerogel powder in the material has stronger hydrophobicity, the hydrophobicity of the concrete can be obviously improved, and tris (hydroxymethyl) aminopropanesulfonic acid) has extremely strong hydrophilicity due to the existence of sulfo groups, and can be easily grafted with a coating to form a space crosslinking structure, so that the prepared hydrophilic and hydrophobic integrated material has great contribution to the strength, durability and service life of cement concrete. The hydrophilic-hydrophobic integrated tube culture material is prepared by coating hydrophobic silica aerogel powder with coating liquid, and the hydrophilic long-chain space crosslinked polymer is grafted on the outer surface of the coating, so that a large amount of water can be stored. The hydrophilic-hydrophobic integrated curing material is doped into the concrete, so that the material can be used as an internal curing material to play a role in reducing self-shrinkage of the concrete, and can play a hydrophobic role after the concrete is cured so that the concrete has hydrophobicity, and the durability of the concrete is improved.
The hydrophilic-hydrophobic integrated tube culture material can not only remarkably improve the cracking problem caused by self shrinkage of concrete and the hydrophobic property of concrete and improve the working performance of the concrete after mixing, but also can not reduce the strength of the concrete after mixing. The hydrophilic-hydrophobic integrated tube culture material prepared by the invention has great contribution to the strength, durability and service life of concrete.
The invention provides a preparation method of a concrete long-period hydrophilic-hydrophobic integrated tube culture material, which is used for preparing the concrete long-period hydrophilic-hydrophobic integrated tube culture material by combining a coating liquid prepared from hydrophobic silica aerogel powder and a polylactic acid-glycolic acid copolymer, wherein the hydrophobic effect of the hydrophobic silica aerogel powder can ensure that hydrophobic aerogel is uniformly distributed in the concrete to a certain extent, and the whole inside of the concrete is guaranteed to have hydrophobic performance; the polylactic acid-glycolic acid copolymer not only can well solve the problem of wrapping hydrophobic silica aerogel powder, but also can realize the timed release of an internal hydrophobic material under the alkaline condition in the concrete, and the surface of the polylactic acid-glycolic acid copolymer can be grafted with a hydrophilic polymer to form a crosslinked structure to store a certain amount of water, so that the internal sample protection of the concrete is realized.
In the invention, the hydrophobic silica aerogel powder is prepared, a large amount of hydroxyl groups are generated on the surface of the silica aerogel after raw materials of tetraethoxysilane and polydiethoxysiloxane are used as silicon sources for reaction, and dimethyl dichlorosilane and hexamethyldisiloxane react with the surface hydroxyl groups to eliminate the surface hydroxyl groups and connect with hydrophobic methyl groups, so that the hydrophobicity of the prepared hydrophobic silica aerogel powder is increased. The coating liquid prepared by the polylactic acid-glycolic acid copolymer used for coating not only can form uniform coating on the hydrophobic silicon dioxide aerogel powder, but also can be grafted with the high-hydrophilicity trimethylol methylaminopropane sulfonic acid on the surface to form a framework of a crosslinked network, and can obviously improve the hydrophilicity of the organic polymer.
Detailed Description
So that those skilled in the art can appreciate the features and effects of the present invention, a general description and definition of the terms and expressions set forth in the specification and claims follows. Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and in the event of a conflict, the present specification shall control.
The theory or mechanism described and disclosed herein, whether right or wrong, is not meant to limit the scope of the invention in any way, i.e., the present disclosure may be practiced without limitation to any particular theory or mechanism.
All features such as values, amounts, and concentrations that are defined herein in the numerical or percent ranges are for brevity and convenience only. Accordingly, the description of a numerical range or percentage range should be considered to cover and specifically disclose all possible sub-ranges and individual values (including integers and fractions) within the range.
Herein, unless otherwise indicated, "comprising," "including," "having," or similar terms encompass the meanings of "consisting of … …" and "consisting essentially of … …," e.g., "a includes a" encompasses the meanings of "a includes a and the other and" a includes a only.
In this context, not all possible combinations of the individual technical features in the individual embodiments or examples are described in order to simplify the description. Accordingly, as long as there is no contradiction between the combinations of these technical features, any combination of the technical features in the respective embodiments or examples is possible, and all possible combinations should be considered as being within the scope of the present specification.
The invention provides a long-period hydrophilic and hydrophobic integrated concrete curing material and a preparation method thereof.
The invention will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Further, it is understood that various changes and modifications may be made by those skilled in the art after reading the teachings of the present invention, and such equivalents are intended to fall within the scope of the claims appended hereto.
The following examples use instrumentation conventional in the art. The experimental methods, in which specific conditions are not noted in the following examples, are generally conducted under conventional conditions or under conditions recommended by the manufacturer. The following examples used various starting materials, unless otherwise indicated, were conventional commercial products, the specifications of which are conventional in the art. In the description of the present invention and the following examples, "%" means weight percent, and "parts" means parts by weight, and ratios means weight ratio, unless otherwise specified.
The following specific embodiments of the present invention are provided, and it should be noted that the present invention is not limited to the following specific embodiments, and all equivalent changes made on the basis of the technical solutions of the present application fall within the protection scope of the present invention.
The invention provides a concrete long-period hydrophilic-hydrophobic integrated tube culture material, which comprises the following raw materials: trimethylol methylaminopropane sulfonic acid, zeolite, cross-linking agent, initiator, coating liquid and hydrophobic silica aerogel powder;
as an alternative scheme, the concrete long-period hydrophilic-hydrophobic integrated curing material is prepared from the following raw materials in percentage by weight: 45-53% of hydrophobic silica aerogel powder, 11.3-13.2% of coating liquid, 32-34.6% of trimethylol methylaminopropane sulfonic acid, 2-7% of zeolite, 0.03-0.05% of cross-linking agent, 0.5-1% of initiator, and the sum of the weight percentages of the raw materials is 100%. The hydrophobic silica aerogel powder has stronger hydrophobicity and is used for improving the hydrophobic property of concrete; the tris (hydroxymethyl) aminopropanesulfonic acid has extremely strong hydrophilicity due to the existence of sulfo groups, and can be easily grafted with the coating to form a space crosslinking structure, so that the prepared hydrophilic-hydrophobic integrated material has great contribution to the strength, the durability and the service life of cement concrete.
The hydrophilic-hydrophobic integrated tube culture material is prepared by coating hydrophobic silica aerogel powder with coating liquid, and the hydrophilic long-chain space crosslinked polymer is grafted on the outer surface of the coating, so that a large amount of water can be stored. The hydrophilic-hydrophobic integrated curing material is doped into the concrete, so that the material can be used as an internal curing material to play a role in reducing self-shrinkage of the concrete, and can play a hydrophobic role after the concrete is cured so that the concrete has hydrophobicity, and the durability of the concrete is improved.
Wherein the cross-linking agent consists of 2, 5-dimethyl-2, 5-di-tert-butyl-hexane peroxide and 2-isopropyl imidazole according to the mass ratio of 1.7-2.2: 1, mixing;
the coating liquid comprises the following raw materials: polylactic acid-glycolic acid copolymer, lithium hexamethyldisilazide, triethyl citrate, magnesium stearate and simethicone; the initiator is one of tert-butyl peroxypivalate or tert-butyl peroxybenzoate.
As an alternative scheme, the coating liquid is prepared from the following raw materials in percentage by weight: 35 to 45 percent of polylactic acid-glycolic acid copolymer, 11 to 15 percent of hexamethyldisilazane lithium, 4.5 to 8.1 percent of triethyl citrate, 37 to 43 percent of magnesium stearate and 0.5 to 0.9 percent of dimethyl silicone oil, wherein the sum of the weight fractions of the raw materials is 100 percent.
The preparation process of the coating liquid comprises the following steps:
step one: weighing the raw materials according to the proportion for standby;
step two: adding 1.7-2.0 times of water of the polylactic acid-glycolic acid copolymer into a beaker, scattering the polylactic acid-glycolic acid copolymer into the water for multiple times, and stirring for 5-10 min to form a trickle state to obtain a suspension A, so that the powder is fully dispersed and wetted, and no lump and foam are generated;
Step three: slowly dripping 0.8-1.2 mol/L hexamethyldisilazane lithium solution into the suspension A for about 5min, stirring for 20-25 min, and dripping 2-3 drops of simethicone for stirring for 5-10 min to form a latex-like water dispersion B;
step four: the latex-like aqueous dispersion B obtained above was filtered through a 30-60 mesh sieve to obtain a filtered aqueous dispersion C.
Step five: slowly pouring the mixed solution of magnesium stearate and triethyl citrate with the mass ratio of 1.8-2:1 into water with the mass of 2.5-3.9 times of that of the mixed solution, homogenizing for 5-10 min by a high-shear homogenizer, and adding 2-3 drops of simethicone to obtain magnesium stearate suspension D;
step six: slowly adding the suspension D into the dispersion C, stirring at medium speed for 30min by using a common stirrer to obtain a suspension E with a solid-liquid ratio of 20-25%, and filtering the suspension E by using a 30-60 mesh sieve to obtain a coating liquid F.
The coating liquid prepared by the polylactic acid-glycolic acid copolymer used for coating not only can form uniform coating on the hydrophobic silicon dioxide aerogel powder, but also can be grafted with the high-hydrophilicity trimethylol methylaminopropane sulfonic acid on the surface to form a framework of a crosslinked network, and can obviously improve the hydrophilicity of the organic polymer. The polylactic acid-glycolic acid copolymer not only can well solve the problem of wrapping hydrophobic silica aerogel powder, but also can realize the timed release of the internal hydrophobic material under the alkaline condition inside the concrete. The surface of the concrete can be grafted with hydrophilic polymer to form a crosslinked structure to store a certain amount of water, so that the concrete internal sample is protected.
The hydrophobic silica aerogel powder comprises the following raw materials: ethyl orthosilicate, polydiethoxysilane, ethanol, deionized water, ammonia water, isophthalic acid, dimethyl dichlorosilane and hexamethyldisiloxane.
As an alternative, the hydrophobic silica aerogel powder is prepared from the following raw materials in percentage by weight: 15-25% of tetraethoxysilane, 15-20% of polydiethoxysiloxane, 13-18% of ethanol, 12-17% of deionized water, 0.8-1.2% of ammonia water, 8-15% of isophthalic acid, 10-15% of dimethyl dichlorosilane and 13-18% of hexamethyldisiloxane, wherein the sum of the weight percentages of the raw materials is 100%.
The preparation process of the hydrophobic silica aerogel powder comprises the following steps:
step one: weighing the raw materials according to the proportion for standby; the hydrophobic silica aerogel powder is prepared from tetraethoxysilane, polydiethoxysilane, ethanol, deionized water, ammonia water, isophthalic acid, dimethyl dichlorosilane and hexamethyldisiloxane.
Step two: placing tetraethoxysilane, polydiethoxysiloxane, ethanol and deionized water into a container, uniformly mixing, adding isophthalic acid with the concentration of 7-10 mol/L into the mixed solution, mechanically stirring for 15-30 min, and placing the mixed solution into room temperature for hydrolysis for 0.8-1.5 h to obtain hydrolysis mixed solution A; after the tetraethoxysilane and the polydiethoxysiloxane are used as silicon sources to react, a large amount of hydroxyl groups are generated on the surface of the silicon dioxide aerogel.
Step three: adding 15-20% ammonia water into the hydrolysis mixed solution A, stirring for 20-30 min, and standing for 12-24 h to obtain gel B;
step four: the mass ratio is 1: mixing 0.7-1.2 of dimethyl dichlorosilane and hexamethyldisiloxane fully to obtain a mixed solution C, and mixing ethanol and the mixed solution C according to the mass ratio of 1.8-2.6: 1, mixing to obtain a mixed solution D, covering the mixed solution D on the surface of the gel B, and aging for 12-24 hours to obtain hydrophobically modified silica gel E; dimethyl dichlorosilane and hexamethyldisiloxane react with surface hydroxyl groups to eliminate the surface hydroxyl groups and attach hydrophobic methyl groups, so that the hydrophobicity of the prepared hydrophobic silica aerogel powder is increased.
Step five: washing the hydrophobically modified silica gel E with ethanol for more than 2 times, standing at room temperature for 2-4 h, and drying in a drying box at 60-80 ℃ for 12-24 h. And (3) after the hydrophobic silica aerogel powder is cooled, grinding and sieving with a 500-1000-mesh sieve to obtain the hydrophobic silica aerogel powder.
The invention also provides a preparation method of the concrete long-period hydrophilic-hydrophobic integrated curing material, which comprises the following specific steps:
step one: placing hydrophobic silica aerogel powder in a coating pot, controlling the temperature in the coating pot to be 20-25 ℃, adjusting the supply rate of coating liquid F to be 15-25G/min/kg, taking out the coated liquid F after coating for 45-60 min, and drying the coated liquid F in a baking oven at 40 ℃ for 2 hours to obtain coated crystals G;
Step two: uniformly mixing the coated crystal G and the trimethylol methylaminopropane sulfonic acid, putting the zeolite treated by acid into a container, adding a cross-linking agent and an initiator in the process of continuously stirring, and reacting for 0.5-1.5H to obtain a compound H;
step three: and taking out the compound H, fully drying, and sieving with a 60-100-mesh sieve to obtain the long-period hydrophilic-hydrophobic integrated concrete curing material.
The hydrophilic-hydrophobic integrated tube curing material not only can remarkably improve the cracking problem caused by self shrinkage of concrete and the hydrophobic property of the concrete and improve the working performance of the concrete after mixing, but also can not reduce the strength of the concrete after mixing.
Example 1:
the embodiment provides a concrete long-period hydrophilic-hydrophobic integrated curing material which is prepared from the following raw materials in percentage by weight: 49% of hydrophobic silica aerogel powder, 12.41% of coating liquid, 33.3% of tris (hydroxymethyl) aminopropanesulfonic acid, 4.5% of zeolite, 0.04% of cross-linking agent and 0.75% of initiator.
The hydrophobic silica aerogel powder is prepared from the following raw materials: 15% of tetraethoxysilane, 20% of polydiethoxysiloxane, 13% of ethanol, 17% of deionized water, 1.0% of ammonia water, 8% of isophthalic acid, 13% of dimethyl dichlorosilane and 13% of hexamethyldisiloxane;
The coating liquid is prepared from the following raw materials: 42.6% of polylactic acid-glycolic acid copolymer, 15% of lithium hexamethyldisilazide, 4.5% of triethyl citrate, 37% of magnesium stearate and 0.9% of simethicone.
In this embodiment:
the cross-linking agent is prepared from 2, 5-dimethyl-2, 5-di-tert-butyl-hexane peroxide and 2-isopropylimidazole according to the following 2.2:1 weight ratio.
The initiator is tert-butyl peroxypivalate.
The preparation method of the concrete long-period hydrophilic-hydrophobic integrated curing material comprises the following steps:
step one: and (3) placing the hydrophobic silica aerogel powder in a coating pot, controlling the temperature in the coating pot to be 22 ℃, adjusting the supply rate of the coating liquid F to be 20G/min/kg, coating for 50min, taking out, placing in a 40 ℃ oven, and drying for 2h to obtain coated crystals G.
Step two: uniformly mixing the coated crystal G and the trimethylol methylaminopropane sulfonic acid, putting the zeolite treated by acid into a container, adding a cross-linking agent and an initiator in the process of continuously stirring, and reacting for 1.0H to obtain a compound H;
step three: and taking out the compound H, fully drying, and sieving with a 70-mesh sieve to obtain the long-period hydrophilic-hydrophobic integrated concrete curing material.
The preparation process of the coating liquid comprises the following steps:
step one: weighing the raw materials according to the proportion for standby;
step two: adding water with the mass of 1.8 times that of the polylactic acid-glycolic acid copolymer into a beaker, scattering the polylactic acid-glycolic acid copolymer into the water for multiple times, and stirring for 7min to form a trickle state to obtain a suspension A, so that the powder is fully dispersed and wetted, and no lump and foam are generated;
step three: slowly dropwise adding 1.0mol/L hexamethyldisilazane lithium solution into the suspension A for about 5min, stirring for 22min, and dropwise adding 2 drops of simethicone to stir for 8min to form a latex-like water dispersion B;
step four: the latex-like aqueous dispersion B obtained above was filtered through a 50-mesh sieve to obtain a filtered aqueous dispersion C.
Step five: slowly pouring the mixed solution of magnesium stearate and triethyl citrate with the mass ratio of 2:1 into water with the mass of 3.0 times of that of the mixed solution, homogenizing for 5min by a high-shear homogenizer, and adding 3 drops of simethicone to obtain magnesium stearate suspension D;
step six: slowly adding the suspension D into the dispersion C, stirring at medium speed for 30min with a common stirrer to obtain a suspension E with a solid-liquid ratio of 22%, and filtering the suspension E with a 60-mesh sieve to obtain a coating solution F.
The preparation process of the hydrophobic silica aerogel powder comprises the following steps:
step one: weighing the raw materials according to the proportion for standby;
step two: placing tetraethoxysilane, polydiethoxysiloxane, ethanol and deionized water into a container, uniformly mixing, adding isophthalic acid with the concentration of 8mol/L into the mixed solution, mechanically stirring for 15min, and placing the mixed solution into room temperature for hydrolysis for 0.9h to obtain hydrolysis mixed solution A;
step three: adding 18% ammonia water into the hydrolysis mixed solution A, stirring for 20min, and standing for 24h to obtain gel B;
step four: the mass ratio is 1:0.8 dimethyl dichlorosilane and hexamethyldisiloxane are fully mixed to obtain a mixed solution C, and ethanol and the mixed solution C are mixed according to the mass ratio of 1.9:1, mixing to obtain a mixed solution D, covering the surface of the gel B with the mixed solution D, and aging for 20 hours to obtain hydrophobically modified silica gel E;
step five: the hydrophobically modified silica gel E is washed 5 times with ethanol, left at room temperature for 3 hours and then dried in a drying oven at 75 ℃ for 20 hours. And (3) after the powder is cooled, grinding and sieving with a 500-mesh sieve to obtain the hydrophobic silica aerogel powder.
Performance test: in order to verify that the hydrophilic-hydrophobic integrated tube culture material of the embodiment has good performance, the hydrophilic-hydrophobic integrated tube culture material prepared by the embodiment and cement are added into mixing equipment together for mixing, the weight mixing amount is 0.3% of the weight of the cement, and performance tests are carried out on the obtained concrete, wherein the test tests comprise a compression test, a water absorption test, a drop rolling promotion test and a self-shrinkage test. The results of the performance test of this example are shown in table 1.
Example 2:
the embodiment provides a concrete long-period hydrophilic-hydrophobic integrated curing material which is prepared from the following raw materials in percentage by weight: 48% of hydrophobic silica aerogel powder, 13.1% of coating liquid, 33% of tris (hydroxymethyl) aminopropanesulfonic acid, 5.1% of zeolite, 0.04% of cross-linking agent and 0.76% of initiator.
The hydrophobic silica aerogel powder is prepared from the following raw materials: 25% of tetraethoxysilane, 15% of polydiethoxysiloxane, 16.2% of ethanol, 12% of deionized water, 0.8% of ammonia water, 8% of isophthalic acid, 10% of dimethyl dichlorosilane and 13% of hexamethyldisiloxane;
the coating liquid is prepared from the following raw materials: 45% of polylactic acid-glycolic acid copolymer, 13% of lithium hexamethyldisilazide, 4.5% of triethyl citrate, 37% of magnesium stearate and 0.5% of dimethyl silicone oil.
In this embodiment:
the cross-linking agent is prepared from 2, 5-dimethyl-2, 5-di-tert-butylperoxyhexane and 2-isopropylimidazole according to the following ratio of 1.7:1 weight ratio.
The initiator is tert-butyl peroxypivalate.
The preparation method of the concrete long-period hydrophilic-hydrophobic integrated curing material comprises the following steps:
step one: and (3) placing the hydrophobic silica aerogel powder in a coating pot, controlling the temperature in the coating pot to be 25 ℃, adjusting the supply rate of the coating liquid F to be 20G/min/kg, coating for 55min, taking out, and placing in a baking oven at 40 ℃ for drying for 2h to obtain coated crystals G.
Step two: uniformly mixing the coated crystal G and the trimethylol methylaminopropane sulfonic acid, putting the zeolite treated by acid into a container, adding a cross-linking agent and an initiator in the process of continuously stirring, and reacting for 1.5 hours to obtain a compound H;
step three: and taking out the compound H, fully drying, and sieving with a 90-mesh sieve to obtain the long-period hydrophilic-hydrophobic integrated concrete curing material.
The preparation process of the coating liquid comprises the following steps:
step one: weighing the raw materials according to the proportion for standby;
step two: adding water with the mass of 1.9 times that of the polylactic acid-glycolic acid copolymer into a beaker, scattering the polylactic acid-glycolic acid copolymer into the water for multiple times, and stirring for 8min to form a trickle state to obtain a suspension A, so that the powder is fully dispersed and wetted, and no lump and foam are generated;
step three: slowly dropwise adding 1.0mol/L hexamethyldisilazane lithium solution into the suspension A for about 5min, stirring for 20min, and dropwise adding 2 drops of simethicone to stir for 8min to form a latex-like water dispersion B;
step four: the latex-like aqueous dispersion B obtained above was filtered through a 60-mesh sieve to obtain a filtered aqueous dispersion C.
Step five: slowly pouring the mixed solution of magnesium stearate and triethyl citrate with the mass ratio of 2:1 into water with the mass of 3.9 times of that of the mixed solution, homogenizing for 10min by a high-shear homogenizer, and adding 3 drops of simethicone to obtain magnesium stearate suspension D;
Step six: slowly adding the suspension D into the dispersion C, stirring at medium speed for 30min with a common stirrer to obtain a suspension E with a solid-liquid ratio of 24%, and filtering the suspension E with a 30-mesh sieve to obtain a coating solution F.
The preparation process of the hydrophobic silica aerogel powder comprises the following steps:
step one: weighing the raw materials according to the proportion for standby;
step two: placing tetraethoxysilane, polydiethoxysiloxane, ethanol and deionized water into a container, uniformly mixing, adding isophthalic acid with the concentration of 8mol/L into the mixed solution, mechanically stirring for 15min, and placing the mixed solution into room temperature for hydrolysis for 0.8h to obtain hydrolysis mixed solution A;
step three: adding 19% ammonia water into the hydrolysis mixed solution A, stirring for 25min, and standing for 12h to obtain gel B;
step four: the mass ratio is 1:0.7 dimethyl dichlorosilane and hexamethyldisiloxane are fully mixed to obtain a mixed solution C, and ethanol and the mixed solution C are mixed according to the mass ratio of 1.8:1, mixing to obtain a mixed solution D, covering the surface of the gel B with the mixed solution D, and aging for 12 hours to obtain hydrophobically modified silica gel E;
step five: the hydrophobically modified silica gel E is washed 2 times with ethanol, left at room temperature for 3 hours and then dried in a drying oven at 75 ℃ for 20 hours. And (3) after the powder is cooled, grinding and sieving with a 500-mesh sieve to obtain the hydrophobic silica aerogel powder.
The performance test procedure of this example is basically the same as that of example 1, and the mixing amount of the concrete long-period hydrophilic-hydrophobic integrated curing material is 0.3% of that of cement, and the performance test result of this example is shown in table 1.
Example 3:
the embodiment provides a concrete long-period hydrophilic-hydrophobic integrated curing material which is prepared from the following raw materials in percentage by weight: 53% of hydrophobic silica aerogel powder, 11.3% of coating liquid, 33.15% of tris (hydroxymethyl) aminopropanesulfonic acid, 2% of zeolite, 0.05% of cross-linking agent and 0.5% of initiator.
The hydrophobic silica aerogel powder is prepared from the following raw materials: 20% of tetraethoxysilane, 15% of polydiethoxysiloxane, 18% of ethanol, 12% of deionized water, 1.2% of ammonia water, 10.8% of isophthalic acid, 10% of dimethyl dichlorosilane and 13% of hexamethyldisiloxane;
the coating liquid is prepared from the following raw materials: 35% of polylactic acid-glycolic acid copolymer, 13% of lithium hexamethyldisilazide, 8.1% of triethyl citrate, 43% of magnesium stearate and 0.9% of dimethyl silicone oil.
In this embodiment:
the cross-linking agent is prepared from 2, 5-dimethyl-2, 5-di-tert-butyl-hexane peroxide and 2-isopropylimidazole according to the following 2.2:1 weight ratio.
The initiator is tert-butyl peroxybenzoate.
The preparation method of the concrete long-period hydrophilic-hydrophobic integrated curing material comprises the following steps:
step one: placing the hydrophobic silica aerogel powder in a coating pot, controlling the temperature in the coating pot to be 25 ℃, adjusting the supply rate of the coating liquid F to be 15G/min/kg, coating for 45min, taking out, placing in a 40 ℃ oven, and drying for 2h to obtain coated crystals G.
Step two: uniformly mixing the coated crystal G and the trimethylol methylaminopropane sulfonic acid, putting the zeolite treated by acid into a container, adding a cross-linking agent and an initiator in the process of continuously stirring, and reacting for 1.0H to obtain a compound H;
step three: and taking out the compound H, fully drying, and sieving with an 80-mesh sieve to obtain the long-period hydrophilic-hydrophobic integrated concrete curing material.
The preparation process of the coating liquid comprises the following steps:
step one: weighing the raw materials according to the proportion for standby;
step two: adding water with the mass of 1.85 times that of the polylactic acid-glycolic acid copolymer into a beaker, scattering the polylactic acid-glycolic acid copolymer into the water for multiple times, and stirring for 5min to form a trickle state to obtain a suspension A, so that the powder is fully dispersed and wetted, and no lump and foam are generated;
Step three: slowly dropwise adding 0.8mol/L hexamethyldisilazane lithium solution into the suspension A for about 5min, stirring for 25min, and dropwise adding 2 drops of simethicone to stir for 10min to form a latex-like water dispersion B;
step four: the latex-like aqueous dispersion B obtained above was filtered through a 60-mesh sieve to obtain a filtered aqueous dispersion C.
Step five: slowly pouring the mixed solution of magnesium stearate and triethyl citrate with the mass ratio of 2:1 into water with the mass of 3.9 times of that of the mixed solution, homogenizing for 10min by a high-shear homogenizer, and adding 2 drops of simethicone to obtain magnesium stearate suspension D;
step six: slowly adding the suspension D into the dispersion C, stirring at medium speed for 30min with a common stirrer to obtain a suspension E with a solid-liquid ratio of 20%, and filtering the suspension E with a 30-mesh sieve to obtain a coating solution F.
The preparation process of the hydrophobic silica aerogel powder comprises the following steps:
step one: weighing the raw materials according to the proportion for standby;
step two: placing tetraethoxysilane, polydiethoxysiloxane, ethanol and deionized water into a container, uniformly mixing, adding isophthalic acid with the concentration of 10mol/L into the mixed solution, mechanically stirring for 15min, and placing the mixed solution into room temperature for hydrolysis for 1.5h to obtain hydrolysis mixed solution A;
Step three: adding ammonia water with the concentration of 20% into the hydrolysis mixed solution A, stirring for 30min, and standing for 12h to obtain gel B;
step four: the mass ratio is 1:0.7 dimethyl dichlorosilane and hexamethyldisiloxane are fully mixed to obtain a mixed solution C, and ethanol and the mixed solution C are mixed according to the mass ratio of 2.6:1, mixing to obtain a mixed solution D, covering the mixed solution D on the surface of the gel B, and aging for 24 hours to obtain hydrophobically modified silica gel E;
step five: the hydrophobically modified silica gel E is washed 2 times with ethanol, left at room temperature for 3 hours and then dried in a drying oven at 80 ℃ for 12 hours. And (3) after the powder is cooled, grinding and sieving with a 500-mesh sieve to obtain the hydrophobic silica aerogel powder.
The performance test procedure of this example is basically the same as that of example 1, and the mixing amount of the concrete long-period hydrophilic-hydrophobic integrated curing material is 0.3% of that of cement, and the performance test result of this example is shown in table 1.
Example 4:
the embodiment provides a concrete long-period hydrophilic-hydrophobic integrated curing material which is prepared from the following raw materials in percentage by weight: 45% of hydrophobic silica aerogel powder, 13.2% of coating liquid, 33.77% of tris (hydroxymethyl) aminopropanesulfonic acid, 7% of zeolite, 0.03% of cross-linking agent and 1% of initiator.
The hydrophobic silica aerogel powder is prepared from the following raw materials: 15% of tetraethoxysilane, 15% of polydiethoxysiloxane, 13% of ethanol, 12% of deionized water, 1.2% of ammonia water, 10.8% of isophthalic acid, 15% of dimethyl dichlorosilane and 18% of hexamethyldisiloxane;
the coating liquid is prepared from the following raw materials: 40% of polylactic acid-glycolic acid copolymer, 11% of lithium hexamethyldisilazide, 6.5% of triethyl citrate, 42% of magnesium stearate and 0.5% of dimethyl silicone oil.
In this embodiment:
the cross-linking agent is prepared from 2, 5-dimethyl-2, 5-di-tert-butyl-hexane peroxide and 2-isopropylimidazole according to a ratio of 1.8:1 weight ratio.
The initiator is tert-butyl peroxybenzoate.
The preparation method of the concrete long-period hydrophilic-hydrophobic integrated curing material comprises the following steps:
step one: and (3) placing the hydrophobic silica aerogel powder in a coating pot, controlling the temperature in the coating pot to be 20 ℃, adjusting the supply rate of the coating liquid F to be 25G/min/kg, coating for 45min, taking out, and placing in a 40 ℃ oven for drying for 2h to obtain coated crystals G.
Step two: uniformly mixing the coated crystal G and the trimethylol methylaminopropane sulfonic acid, putting the zeolite treated by acid into a container, adding a cross-linking agent and an initiator in the process of continuously stirring, and reacting for 1.0H to obtain a compound H;
Step three: and taking out the compound H, fully drying, and sieving with a 90-mesh sieve to obtain the long-period hydrophilic-hydrophobic integrated concrete curing material.
The preparation process of the coating liquid comprises the following steps:
step one: weighing the raw materials according to the proportion for standby;
step two: adding water with the mass of 2.0 times of that of the polylactic acid-glycolic acid copolymer into a beaker, scattering the polylactic acid-glycolic acid copolymer into the water for multiple times, and stirring for 5min to form a trickle state to obtain a suspension A, so that the powder is fully dispersed and wetted, and no lump and foam are generated;
step three: slowly dropwise adding 1.2mol/L hexamethyldisilazane lithium solution into the suspension A for about 5min, stirring for 25min, and dropwise adding 3 drops of simethicone to stir for 5min to form a latex-like water dispersion B;
step four: the latex-like aqueous dispersion B obtained above was filtered through a 50-mesh sieve to obtain a filtered aqueous dispersion C.
Step five: slowly pouring the mixed solution of magnesium stearate and triethyl citrate with the mass ratio of 2:1 into water with the mass of 2.5 times of that of the mixed solution, homogenizing for 5min by a high-shear homogenizer, and adding 2 drops of simethicone to obtain magnesium stearate suspension D;
step six: slowly adding the suspension D into the dispersion C, stirring at medium speed for 30min with a common stirrer to obtain a suspension E with a solid-liquid ratio of 20%, and filtering the suspension E with a 40-mesh sieve to obtain a coating solution F.
The preparation process of the hydrophobic silica aerogel powder comprises the following steps:
step one: weighing the raw materials according to the proportion for standby;
step two: placing tetraethoxysilane, polydiethoxysiloxane, ethanol and deionized water into a container, uniformly mixing, adding isophthalic acid with the concentration of 10mol/L into the mixed solution, mechanically stirring for 15min, and placing the mixed solution into room temperature for hydrolysis for 1.5h to obtain hydrolysis mixed solution A;
step three: adding ammonia water with the concentration of 20% into the hydrolysis mixed solution A, stirring for 20min, and standing for 24h to obtain gel B;
step four: the mass ratio is 1:1.2, fully mixing dimethyl dichlorosilane and hexamethyldisiloxane to obtain a mixed solution C, and mixing ethanol and the mixed solution C according to a mass ratio of 2.6:1, mixing to obtain a mixed solution D, covering the mixed solution D on the surface of the gel B, and aging for 24 hours to obtain hydrophobically modified silica gel E;
step five: washing the hydrophobically modified silica gel E with ethanol for more than 2 times, standing at room temperature for 4 hours, and drying in a drying box at 80 ℃ for 24 hours. And after the silica aerogel is cooled, grinding and sieving with a 1000-mesh sieve to obtain the hydrophobic silica aerogel powder.
The performance test procedure of this example is basically the same as that of example 1, and the mixing amount of the concrete long-period hydrophilic-hydrophobic integrated curing material is 1.2% of that of cement, and the performance test result of this example is shown in table 1.
Example 5:
the embodiment provides a concrete long-period hydrophilic-hydrophobic integrated curing material which is prepared from the following raw materials in percentage by weight: 49.15% of hydrophobic silica aerogel powder, 12.5% of coating liquid, 32% of tris (hydroxymethyl) aminopropanesulfonic acid, 5.6% of zeolite, 0.05% of cross-linking agent and 0.7% of initiator.
The hydrophobic silica aerogel powder is prepared from the following raw materials: 15% of tetraethoxysilane, 15% of polydiethoxysiloxane, 13% of ethanol, 17% of deionized water, 1.2% of ammonia water, 10.8% of isophthalic acid, 10% of dimethyl dichlorosilane and 18% of hexamethyldisiloxane;
the coating liquid is prepared from the following raw materials: 45% of polylactic acid-glycolic acid copolymer, 11% of lithium hexamethyldisilazide, 4.5% of triethyl citrate, 39% of magnesium stearate and 0.5% of dimethyl silicone oil.
In this embodiment:
the cross-linking agent is prepared from 2, 5-dimethyl-2, 5-di-tert-butyl-hexane peroxide and 2-isopropylimidazole according to the following ratio of 2.0:1 weight ratio.
The initiator is tert-butyl peroxybenzoate.
The preparation method of the concrete long-period hydrophilic-hydrophobic integrated curing material comprises the following steps:
step one: and (3) placing the hydrophobic silica aerogel powder in a coating pot, controlling the temperature in the coating pot to be 20 ℃, adjusting the supply rate of the coating liquid F to be 25G/min/kg, coating for 45min, taking out, and placing in a 40 ℃ oven for drying for 2h to obtain coated crystals G.
Step two: uniformly mixing the coated crystal G and the trimethylol methylaminopropane sulfonic acid, putting the zeolite treated by acid into a container, adding a cross-linking agent and an initiator in the process of continuously stirring, and reacting for 1.5 hours to obtain a compound H;
step three: and taking out the compound H, fully drying, and sieving with a 60-mesh sieve to obtain the long-period hydrophilic-hydrophobic integrated concrete curing material.
The preparation process of the coating liquid comprises the following steps:
step one: weighing the raw materials according to the proportion for standby;
step two: adding water with the mass of 2.0 times of that of the polylactic acid-glycolic acid copolymer into a beaker, scattering the polylactic acid-glycolic acid copolymer into the water for multiple times, and stirring for 5min to form a trickle state to obtain a suspension A, so that the powder is fully dispersed and wetted, and no lump and foam are generated;
step three: slowly dropwise adding 1.2mol/L hexamethyldisilazane lithium solution into the suspension A for about 5min, stirring for 20min, and dropwise adding 3 drops of simethicone to stir for 5min to form a latex-like water dispersion B;
step four: the latex-like aqueous dispersion B obtained above was filtered through a 60-mesh sieve to obtain a filtered aqueous dispersion C.
Step five: slowly pouring the mixed solution of magnesium stearate and triethyl citrate with the mass ratio of 1.8:1 into water with the mass of 3.9 times of that of the mixed solution, homogenizing for 5min by a high-shear homogenizer, and adding 3 drops of simethicone to obtain magnesium stearate suspension D;
Step six: slowly adding the suspension D into the dispersion C, stirring at medium speed for 30min with a common stirrer to obtain a suspension E with a solid-liquid ratio of 20%, and filtering the suspension E with a 60-mesh sieve to obtain a coating solution F.
The preparation process of the hydrophobic silica aerogel powder comprises the following steps:
step one: weighing the raw materials according to the proportion for standby;
step two: placing tetraethoxysilane, polydiethoxysiloxane, ethanol and deionized water into a container, uniformly mixing, adding isophthalic acid with the concentration of 7mol/L into the mixed solution, mechanically stirring for 30min, and placing the mixed solution into room temperature for hydrolysis for 0.8h to obtain hydrolysis mixed solution A;
step three: adding ammonia water with the concentration of 20% into the hydrolysis mixed solution A, stirring for 20min, and standing for 24h to obtain gel B;
step four: the mass ratio is 1:0.7 dimethyl dichlorosilane and hexamethyldisiloxane are fully mixed to obtain a mixed solution C, and ethanol and the mixed solution C are mixed according to the mass ratio of 2.6:1, mixing to obtain a mixed solution D, covering the surface of the gel B with the mixed solution D, and aging for 12 hours to obtain hydrophobically modified silica gel E;
step five: the hydrophobically modified silica gel E is washed 2 times with ethanol, left at room temperature for 4 hours and then dried in a drying oven at 60 ℃ for 24 hours. And (3) after the powder is cooled, grinding and sieving with a 500-mesh sieve to obtain the hydrophobic silica aerogel powder.
The performance test procedure of this example is basically the same as that of example 1, and the mixing amount of the concrete long-period hydrophilic-hydrophobic integrated curing material is 1.2% of that of cement, and the performance test result of this example is shown in table 1.
Example 6:
the embodiment provides a concrete long-period hydrophilic-hydrophobic integrated curing material which is prepared from the following raw materials in percentage by weight: 49% of hydrophobic silica aerogel powder, 12.9% of coating liquid, 33.5% of tris (hydroxymethyl) aminopropanesulfonic acid, 4.07% of zeolite, 0.03% of cross-linking agent and 0.5% of initiator.
The hydrophobic silica aerogel powder is prepared from the following raw materials: 21.8% of tetraethoxysilane, 15% of polydiethoxysiloxane, 16.2% of ethanol, 12% of deionized water, 1.2% of ammonia water, 10.8% of isophthalic acid, 10% of dimethyl dichlorosilane and 13% of hexamethyldisiloxane;
the coating liquid is prepared from the following raw materials: 41% of polylactic acid-glycolic acid copolymer, 13% of lithium hexamethyldisilazide, 8.1% of triethyl citrate, 37% of magnesium stearate and 0.9% of dimethyl silicone oil.
In this embodiment:
the cross-linking agent is prepared from 2, 5-dimethyl-2, 5-di-tert-butyl-hexane peroxide and 2-isopropylimidazole according to the following ratio of 2.0:1 weight ratio.
The initiator is tert-butyl peroxybenzoate.
The preparation method of the concrete long-period hydrophilic-hydrophobic integrated curing material comprises the following steps:
step one: and (3) placing the hydrophobic silica aerogel powder in a coating pot, controlling the temperature in the coating pot to be 25 ℃, adjusting the supply rate of the coating liquid F to be 25G/min/kg, coating for 60min, taking out, and placing in a 40 ℃ oven for drying for 2h to obtain coated crystals G.
Step two: uniformly mixing the coated crystal G and the trimethylol methylaminopropane sulfonic acid, putting the zeolite treated by acid into a container, adding a cross-linking agent and an initiator in the process of continuously stirring, and reacting for 1.5 hours to obtain a compound H;
step three: and taking out the compound H, fully drying, and sieving with a 100-mesh sieve to obtain the long-period hydrophilic-hydrophobic integrated concrete curing material.
The preparation process of the coating liquid comprises the following steps:
step one: weighing the raw materials according to the proportion for standby;
step two: adding water with the mass of 2.0 times of that of the polylactic acid-glycolic acid copolymer into a beaker, scattering the polylactic acid-glycolic acid copolymer into the water for multiple times, and stirring for 10min to form a trickle state to obtain a suspension A, so that the powder is fully dispersed and wetted, and no lump and foam are generated;
Step three: slowly dropwise adding 1.2mol/L hexamethyldisilazane lithium solution into the suspension A for about 5min, stirring for 25min, and dropwise adding 3 drops of simethicone to stir for 10min to form a latex-like water dispersion B;
step four: the latex-like aqueous dispersion B obtained above was filtered through a 60-mesh sieve to obtain a filtered aqueous dispersion C.
Step five: slowly pouring the mixed solution of magnesium stearate and triethyl citrate with the mass ratio of 2:1 into water with the mass of 3.9 times of that of the mixed solution, homogenizing for 10min by a high-shear homogenizer, and adding 3 drops of simethicone to obtain magnesium stearate suspension D;
step six: slowly adding the suspension D into the dispersion C, stirring at medium speed for 30min with a common stirrer to obtain a suspension E with a solid-liquid ratio of 25%, and filtering the suspension E with a 60-mesh sieve to obtain a coating solution F.
The preparation process of the hydrophobic silica aerogel powder comprises the following steps:
step one: weighing the raw materials according to the proportion for standby;
step two: placing tetraethoxysilane, polydiethoxysiloxane, ethanol and deionized water into a container, uniformly mixing, adding isophthalic acid with the concentration of 10mol/L into the mixed solution, mechanically stirring for 30min, and placing the mixed solution into room temperature for hydrolysis for 1.5h to obtain hydrolysis mixed solution A;
Step three: adding ammonia water with the concentration of 20% into the hydrolysis mixed solution A, stirring for 30min, and standing for 24h to obtain gel B;
step four: the mass ratio is 1:1.2, fully mixing dimethyl dichlorosilane and hexamethyldisiloxane to obtain a mixed solution C, and mixing ethanol and the mixed solution C according to a mass ratio of 2.6:1, mixing to obtain a mixed solution D, covering the mixed solution D on the surface of the gel B, and aging for 24 hours to obtain hydrophobically modified silica gel E;
step five: the hydrophobically modified silica gel E is washed 4 times with ethanol, left at room temperature for 4 hours and then dried in a drying oven at 80 ℃ for 24 hours. And after the silica aerogel is cooled, grinding and sieving with a 1000-mesh sieve to obtain the hydrophobic silica aerogel powder.
The performance test procedure of this example is basically the same as that of example 1, and the mixing amount of the concrete long-period hydrophilic-hydrophobic integrated curing material is 1.2% of that of cement, and the performance test result of this example is shown in table 1.
Example 7
The embodiment provides a concrete long-period hydrophilic-hydrophobic integrated curing material which is prepared from the following raw materials in percentage by weight: 49% of hydrophobic silica aerogel powder, 12.9% of coating liquid, 34.6% of tris (hydroxymethyl) aminopropanesulfonic acid, 2.97% of zeolite, 0.03% of cross-linking agent and 0.5% of initiator.
The hydrophobic silica aerogel powder is prepared from the following raw materials: 23.2% of tetraethoxysilane, 15% of polydiethoxysiloxane, 13% of ethanol, 17% of deionized water, 0.8% of ammonia water, 8% of isophthalic acid, 10% of dimethyl dichlorosilane and 13% of hexamethyldisiloxane;
the coating liquid is prepared from the following raw materials: 37% of polylactic acid-glycolic acid copolymer, 13% of lithium hexamethyldisilazide, 7.5% of triethyl citrate, 42% of magnesium stearate and 0.5% of dimethyl silicone oil.
In this embodiment:
the cross-linking agent is prepared from 2, 5-dimethyl-2, 5-di-tert-butyl-hexane peroxide and 2-isopropyl imidazole according to the following ratio of 2.1:1 weight ratio.
The initiator is tert-butyl peroxypivalate.
The preparation method of the concrete long-period hydrophilic-hydrophobic integrated curing material comprises the following steps:
step one: and (3) placing the hydrophobic silica aerogel powder in a coating pot, controlling the temperature in the coating pot to be 20 ℃, adjusting the supply rate of the coating liquid F to be 15G/min/kg, coating for 45min, taking out, and placing in a 40 ℃ oven for drying for 2h to obtain coated crystals G.
Step two: uniformly mixing the coated crystal G and the trimethylol methylaminopropane sulfonic acid, putting the zeolite treated by acid into a container, adding a cross-linking agent and an initiator in the process of continuously stirring, and reacting for 0.5H to obtain a compound H;
Step three: and taking out the compound H, fully drying, and sieving with a 60-mesh sieve to obtain the long-period hydrophilic-hydrophobic integrated concrete curing material.
The preparation process of the coating liquid comprises the following steps:
step one: weighing the raw materials according to the proportion for standby;
step two: adding water with the mass of 1.7 times of that of the polylactic acid-glycolic acid copolymer into a beaker, scattering the polylactic acid-glycolic acid copolymer into the water for multiple times, and stirring for 5min to form a trickle state to obtain a suspension A, so that the powder is fully dispersed and wetted, and no lump and foam are generated;
step three: slowly dropwise adding 0.8mol/L hexamethyldisilazane lithium solution into the suspension A for about 5min, stirring for 20min, and dropwise adding 2 drops of simethicone to stir for 5min to form a latex-like water dispersion B;
step four: the latex-like aqueous dispersion B obtained above was filtered through a 30-mesh sieve to obtain a filtered aqueous dispersion C.
Step five: slowly pouring the mixed solution of magnesium stearate and triethyl citrate with the mass ratio of 1.8:1 into water with the mass of 2.5 times of that of the mixed solution, homogenizing for 5min by a high-shear homogenizer, and adding 2 drops of simethicone to obtain magnesium stearate suspension D;
step six: slowly adding the suspension D into the dispersion C, stirring at medium speed for 30min with a common stirrer to obtain a suspension E with a solid-liquid ratio of 20%, and filtering the suspension E with a 30-mesh sieve to obtain a coating solution F.
The preparation process of the hydrophobic silica aerogel powder comprises the following steps:
step one: weighing the raw materials according to the proportion for standby;
step two: placing tetraethoxysilane, polydiethoxysiloxane, ethanol and deionized water into a container, uniformly mixing, adding isophthalic acid with the concentration of 7mol/L into the mixed solution, mechanically stirring for 15min, and placing the mixed solution into room temperature for hydrolysis for 0.8h to obtain hydrolysis mixed solution A;
step three: adding 15% ammonia water into the hydrolysis mixed solution A, stirring for 20min, and standing for 12h to obtain gel B;
step four: the mass ratio is 1:0.7 dimethyl dichlorosilane and hexamethyldisiloxane are fully mixed to obtain a mixed solution C, and ethanol and the mixed solution C are mixed according to the mass ratio of 1.8:1, mixing to obtain a mixed solution D, covering the surface of the gel B with the mixed solution D, and aging for 12 hours to obtain hydrophobically modified silica gel E;
step five: the hydrophobically modified silica gel E is washed 3 times with ethanol, placed at 25℃for 2 hours and then dried in a drying oven at 60℃for 12 hours. And (3) after the powder is cooled, grinding and sieving with a 500-mesh sieve to obtain the hydrophobic silica aerogel powder.
The preparation method of the concrete long-period hydrophilic-hydrophobic integrated curing material of the embodiment is basically the same as that of the embodiment 1.
Comparative example 1:
the comparative example shows a general concrete of the same proportion as in example 1, and the component contents of the raw materials are proportionally enlarged according to the proportion relation in example 1 so that the sum of the weight parts of the raw materials is 100%.
The amounts of the concrete components in this comparative example were the same as in example 1.
The performance test procedure of this comparative example was substantially the same as in example 1, and the results of the performance test of this comparative example are shown in table 1.
Comparative example 2:
the comparative example shows that the internal curing material of concrete is used by being mixed with the hydrophobic soil layer, and the internal curing material is basically the same as that of the example 1, except that the hydrophobic material in the comparative example is a common acrylic paint, and the component contents of other raw materials are expanded in the same proportion according to the proportioning relation in the example 1, so that the sum of the weight parts of the raw materials is 100%.
The kinds and amounts of the respective raw materials in this comparative example were the same as those in example 1.
The preparation method of the concrete long-period hydrophilic-hydrophobic integrated tube culture material of the comparative example is basically the same as that of example 1.
The performance test procedure of this comparative example was substantially the same as in example 1, and the results of the performance test of this comparative example are shown in table 1.
Table 1 shows the results of the performance test of the cured materials (all changes relative to the reference concrete)
As can be seen from table 1:
from the comparison of examples 1 to 6, it is clear that: the hydrophilic and hydrophobic integrated curing materials in examples 1-6 can obviously improve the compressive strength of concrete, and the 28d compressive strength in four groups of examples is more than 115% of the standard concrete strength. The average water absorption of the 72h concrete is also improved obviously, and the drop rolling rate in the examples 1-6 also shows higher performance at 5 ℃. In addition, the internal curing materials of examples 1 to 6 can reduce the self-shrinkage of concrete to a large extent. Among them, the hydrophilic-hydrophobic integrated potting material of example 2 had the best overall performance.
From the comparison of examples 1 to 3 and examples 4 to 6, it is clear that: as the mixing amount of the hydrophilic and hydrophobic integrated concrete curing material is increased, the hydrophobic effect and the internal curing effect of the concrete are gradually improved, but the 7d and 28d compressive strength of the concrete are reduced. However, the strength, the hydrophobic effect and the hydrophilic effect are still remarkably improved as compared with those of comparative examples 1 and 2.
From the comparison of examples 1 to 6 and comparative examples 1 and 2, it is clear that: compared with common concrete, the concrete long-period hydrophilic-hydrophobic integrated curing material provided by the examples 1-6 has obvious hydrophobic effect when being used as the internal curing and hydrophobic material of the concrete, and the 7d and 28d compressive strength of the concrete is improved.
In conclusion, the invention obviously improves the compressive strength and the hydrophobic effect of the concrete, the compressive strength of the concrete 28d is more than 120% of the standard concrete strength, and the hydrophobic effect of the concrete is also obviously improved. In addition, the self-shrinkage of the concrete is reduced to a great extent, the problem that the hydrophilic performance and the hydrophobic performance of the existing material cannot coexist is effectively solved, the shrinkage cracking and frost resistance problems of the concrete are effectively controlled, and the durability of the concrete is improved.
The above is only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited by this, and any modification made on the basis of the technical scheme according to the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (10)
1. The long-period hydrophilic-hydrophobic integrated concrete tube culture material is characterized by comprising the following preparation raw materials in percentage by weight: 45-53% of hydrophobic silica aerogel powder, 11.3-13.2% of coating liquid, 32-34.6% of trimethylol methylaminopropane sulfonic acid, 2-7% of zeolite, 0.03-0.05% of cross-linking agent and 0.5-1% of initiator.
2. The concrete long-period hydrophilic-hydrophobic integrated curing material according to claim 1, wherein the preparation raw materials of the hydrophobic silica aerogel powder comprise, by weight:
15 to 25 percent of tetraethoxysilane, 15 to 20 percent of polydiethoxysilane, 13 to 18 percent of ethanol, 12 to 17 percent of deionized water, 0.8 to 1.2 percent of ammonia water, 8 to 15 percent of isophthalic acid, 10 to 15 percent of dimethyl dichlorosilane and 13 to 18 percent of hexamethyldisiloxane;
the coating liquid is prepared from the following raw materials:
35 to 45 percent of polylactic acid-glycolic acid copolymer, 11 to 15 percent of hexamethyldisilazane lithium, 4.5 to 8.1 percent of triethyl citrate, 37 to 43 percent of magnesium stearate and 0.5 to 0.9 percent of dimethyl silicone oil.
3. The long-period hydrophilic-hydrophobic integrated concrete curing material according to claim 1, wherein the cross-linking agent consists of 2, 5-dimethyl-2, 5-di-tert-butylperoxy hexane and 2-isopropylimidazole; wherein the mass ratio of the 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide to the 2-isopropyl imidazole is (1.7-2.2): 1, a step of;
the initiator is any one of tert-butyl peroxypivalate or tert-butyl peroxybenzoate.
4. A method for preparing the long-period hydrophilic-hydrophobic integrated concrete curing material according to any one of claims 1 to 3, comprising the following steps:
s1: placing the hydrophobic silica aerogel powder in a coating pan, coating the hydrophobic silica aerogel powder with coating liquid, taking out and drying after coating for a set time to obtain coated crystals G;
S2: uniformly mixing the coated crystal G and the trimethylol methylaminopropane sulfonic acid, adding zeolite subjected to acid treatment, adding a cross-linking agent and an initiator in the stirring process, and reacting for a set time to obtain a compound H;
s3: and taking out the compound H, drying and filtering to obtain the long-period hydrophilic-hydrophobic integrated concrete curing material.
5. The method for preparing a concrete long-period hydrophilic-hydrophobic integrated tube culture material according to claim 4, wherein in the step S1, the temperature of the coating pot is 20-25 ℃, the supply rate of the coating liquid is 15-25 g/min/kg, and the coating setting time is 45-60 min; in the step S2, the reaction setting time is 0.5-1.5 h.
6. The method for preparing the long-period hydrophilic-hydrophobic integrated concrete curing material according to claim 4, wherein the preparation process of the hydrophobic silica aerogel powder is as follows:
s11: uniformly mixing tetraethoxysilane, polydiethoxysiloxane, ethanol and deionized water to obtain a mixed solution, adding isophthalic acid into the mixed solution, stirring, and hydrolyzing to obtain a hydrolyzed mixed solution A;
s12: adding ammonia water into the hydrolysis mixed solution A, mixing and stirring, and standing to obtain gel B;
Mixing dimethyl dichlorosilane and hexamethyldisiloxane to obtain a mixed solution C, mixing ethanol with the mixed solution C to obtain a mixed solution D, covering the mixed solution D on the gel B, and performing surface aging to obtain hydrophobically modified silica gel E;
s13: washing and placing the hydrophobically modified silica gel E, drying, cooling, grinding and sieving to obtain the hydrophobic silica aerogel powder.
7. The method for preparing a long-period hydrophilic-hydrophobic integrated concrete curing material according to claim 6, wherein in S11, the concentration of isophthalic acid is 7-10 mol/L.
8. The method for preparing the long-period hydrophilic-hydrophobic integrated concrete curing material according to claim 6, wherein in the step S12, the concentration of the ammonia water is 15-20%;
the mass ratio of the dimethyldichlorosilane to the hexamethyldisiloxane is 1: (0.7-1.2); the mass ratio of the ethanol to the mixed solution C is (1.8-2.6): 1, a step of; the surface ageing time is 12-24 hours;
in the step S13, the washing times are more than 2 times, and ethanol is adopted for washing; the sieving adopts 500-1000 mesh sieve.
9. The method for preparing the concrete long-period hydrophilic-hydrophobic integrated tube culture material according to claim 4, wherein the preparation process of the coating liquid is as follows:
S21: adding polylactic acid-glycolic acid copolymer into deionized water for several times, stirring until the polylactic acid-glycolic acid copolymer is in a trickle state, and obtaining suspension A;
s22: adding a hexamethyldisilazane lithium solution into the suspension A, stirring, adding dimethyl silicone oil, and stirring to obtain a latex-like water dispersion B;
s23: filtering the latex-like aqueous dispersion B to obtain a filtered aqueous dispersion C; mixing magnesium stearate and triethyl citrate to obtain a mixed solution, adding the mixed solution into deionized water for homogenization, and then adding dimethyl silicone oil to obtain magnesium stearate suspension D;
s24: the magnesium stearate suspension D is added to the aqueous dispersion C and stirred to obtain a suspension E, and the suspension E is filtered to obtain a coating liquid.
10. The concrete long-period hydrophilic-hydrophobic integrated curing material according to claim 9, wherein in S21, the mass ratio of the polylactic acid-glycolic acid copolymer to deionized water is 1: (1.7-2.0);
in the step S22, the concentration of the hexamethyldisilazane lithium solution is 0.8-1.2 mol/L;
in the step S23, filtering is carried out by adopting a mesh sieve of 30-60 meshes; the mass ratio of magnesium stearate to triethyl citrate in the mixed solution is (1.8-2): 1, a step of; the mass ratio of the mixed solution to the deionized water is 1: (2.5-3.9); the homogenizing time is 5-10 min;
In the step S24, the solid-to-liquid ratio of the suspension E is 20-25%, and the suspension E is filtered by a mesh sieve of 30-60.
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