CN117567062B - Concrete targeting agent and preparation method thereof - Google Patents
Concrete targeting agent and preparation method thereof Download PDFInfo
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- CN117567062B CN117567062B CN202410056399.9A CN202410056399A CN117567062B CN 117567062 B CN117567062 B CN 117567062B CN 202410056399 A CN202410056399 A CN 202410056399A CN 117567062 B CN117567062 B CN 117567062B
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- 239000004567 concrete Substances 0.000 title claims abstract description 83
- 230000008685 targeting Effects 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 48
- 239000000243 solution Substances 0.000 claims abstract description 46
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000011259 mixed solution Substances 0.000 claims abstract description 37
- 239000007788 liquid Substances 0.000 claims abstract description 30
- 239000003094 microcapsule Substances 0.000 claims abstract description 29
- PIJPYDMVFNTHIP-UHFFFAOYSA-L lead sulfate Chemical compound [PbH4+2].[O-]S([O-])(=O)=O PIJPYDMVFNTHIP-UHFFFAOYSA-L 0.000 claims abstract description 28
- 239000002775 capsule Substances 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000008367 deionised water Substances 0.000 claims abstract description 19
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 19
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims abstract description 17
- 239000004926 polymethyl methacrylate Substances 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 238000005538 encapsulation Methods 0.000 claims abstract description 16
- 239000002023 wood Substances 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 12
- 150000002191 fatty alcohols Chemical class 0.000 claims abstract description 10
- 239000002131 composite material Substances 0.000 claims abstract description 9
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 9
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 8
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract description 8
- 239000011734 sodium Substances 0.000 claims abstract description 8
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 8
- 238000001704 evaporation Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000012535 impurity Substances 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims description 25
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 19
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 12
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 12
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 12
- 235000011152 sodium sulphate Nutrition 0.000 claims description 12
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 11
- 108010010803 Gelatin Proteins 0.000 claims description 11
- 229960003638 dopamine Drugs 0.000 claims description 11
- 239000008273 gelatin Substances 0.000 claims description 11
- 229920000159 gelatin Polymers 0.000 claims description 11
- 235000019322 gelatine Nutrition 0.000 claims description 11
- 235000011852 gelatine desserts Nutrition 0.000 claims description 11
- 235000010413 sodium alginate Nutrition 0.000 claims description 11
- 239000000661 sodium alginate Substances 0.000 claims description 11
- 229940005550 sodium alginate Drugs 0.000 claims description 11
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 11
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 claims description 10
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 235000010344 sodium nitrate Nutrition 0.000 claims description 6
- 239000004317 sodium nitrate Substances 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 239000012065 filter cake Substances 0.000 claims description 5
- 238000003828 vacuum filtration Methods 0.000 claims description 5
- 230000007797 corrosion Effects 0.000 abstract description 22
- 238000005260 corrosion Methods 0.000 abstract description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract description 19
- 230000005764 inhibitory process Effects 0.000 abstract description 9
- 239000011162 core material Substances 0.000 description 19
- 239000000523 sample Substances 0.000 description 15
- 229910000831 Steel Inorganic materials 0.000 description 14
- 239000003921 oil Substances 0.000 description 14
- 235000019198 oils Nutrition 0.000 description 14
- 239000010959 steel Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 13
- 239000001993 wax Substances 0.000 description 13
- 230000000694 effects Effects 0.000 description 9
- 238000011084 recovery Methods 0.000 description 9
- 239000004568 cement Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 230000035699 permeability Effects 0.000 description 6
- 230000002195 synergetic effect Effects 0.000 description 6
- 239000000839 emulsion Substances 0.000 description 5
- 230000004907 flux Effects 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000002161 passivation Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000008439 repair process Effects 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 230000003487 anti-permeability effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000012496 blank sample Substances 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical class [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000009977 dual effect Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000003211 malignant effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002383 tung oil Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 235000004347 Perilla Nutrition 0.000 description 1
- 244000124853 Perilla frutescens Species 0.000 description 1
- 244000137852 Petrea volubilis Species 0.000 description 1
- 239000011398 Portland cement Substances 0.000 description 1
- 229910001294 Reinforcing steel Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 235000013871 bee wax Nutrition 0.000 description 1
- 239000012166 beeswax Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000004203 carnauba wax Substances 0.000 description 1
- 239000004359 castor oil Substances 0.000 description 1
- 235000019438 castor oil Nutrition 0.000 description 1
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical group OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 239000011365 complex material Substances 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000001453 impedance spectrum Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000009545 invasion Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 230000010220 ion permeability Effects 0.000 description 1
- 239000000944 linseed oil Substances 0.000 description 1
- 235000021388 linseed oil Nutrition 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- -1 nitrite ions Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910021487 silica fume Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 235000020238 sunflower seed Nutrition 0.000 description 1
- 239000010496 thistle oil Substances 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
- 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
- C04B20/1055—Coating or impregnating with inorganic materials
- C04B20/107—Acids or salts thereof
-
- 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
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/04—Portland cements
-
- 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/24—Sea water resistance
-
- 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/34—Non-shrinking or non-cracking materials
- C04B2111/343—Crack resistant materials
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The application relates to the technical field of concrete, and particularly discloses a concrete targeting agent and a preparation method thereof. The preparation method of the concrete targeting agent comprises the steps of firstly preparing an emulsified core mixed solution: dissolving sodium fatty alcohol ether sulfate in the G-M solution to form a composite emulsifier, and then adding wood wax oil to obtain an emulsified core mixed solution; adding the modified Ca-Al-LDH and lead sulfate into methylene dichloride solution of polymethyl methacrylate, and stirring for 30-60min at 30-40 ℃ to obtain a capsule wall mixed solution; then adding the capsule wall mixed solution into the emulsified core mixed solution, and continuously stirring for 6-8 hours at 30-40 ℃ to complete microcapsule encapsulation, thus obtaining encapsulated capsule liquid; finally, heating the encapsulation liquid to 42-45 ℃, evaporating dichloromethane to obtain microcapsule mixed liquid, removing broken microcapsules and impurities suspended on the liquid surface, filtering the microcapsule mixed liquid, and washing with deionized water. The concrete targeting agent prepared by the method has the advantages of self-repairing, chloride ion curing and corrosion inhibition.
Description
Technical Field
The application relates to the technical field of concrete, in particular to a concrete targeting agent and a preparation method thereof.
Background
One of the greatest threats to cement-based concrete structures in deicing salt applications in marine environments and northern areas is corrosion and disease of steel bars induced by chloride ion attack in the environment. The high alkaline pore solution formed by the muddy water product in the concrete can form a compact passivation film on the surface of the steel bar so as to protect the steel bar in the concrete from being corroded by corrosive substances such as chloride. However, concrete is inevitably prone to microcracks in the natural environment, which enhance the permeability of the concrete and provide a more direct penetration transmission path for the accelerated invasion of chloride ions. When chloride ions diffuse to the surface of the steel bar and exceed a concentration threshold, the passivation film becomes unstable, and then the steel bar corrosion is induced under the synergistic effect of water and oxygen, so that the durability of the cement-based material is reduced and even the cement-based material is damaged and fails in advance.
The self-healing microcapsule can actively repair microcracks of the cement-based concrete, so that the chloride ion permeability resistance of the cement-based concrete is improved. However, most of the capsule cores of the current self-healing microcapsules must be contacted with a curing agent to produce a curing reaction to form a repair product, which enables self-healing of the microcracks. The complex material characteristics and the environment of the cement-based concrete lead to difficult contact of the curing agent and the repairing agent, and the repairing effect of microcracks is reduced. In addition, chloride ions cannot be consumed or converted into other substances in the corrosion reaction, so that the steel bars are continuously eroded by free chloride ions existing in the cement matrix in the use process, and the service life of the steel bars is greatly reduced by the free chloride ions.
Disclosure of Invention
In order to further improve the service life of the reinforcing steel bars in the concrete, the application provides a multifunctional synergistic corrosion-resistant concrete targeting agent and a preparation method thereof.
In a first aspect, the present application provides a preparation method of a concrete targeting agent, which adopts the following technical scheme:
the preparation method of the concrete targeting agent comprises the following steps: s1, preparing an emulsified core mixed solution: dissolving sodium fatty alcohol ether sulfate in the G-M solution to form a composite emulsifier, and then adding wood wax oil to obtain an emulsified core mixed solution; s2, adding the modified Ca-Al-LDH and lead sulfate into a methylene dichloride solution of polymethyl methacrylate, and stirring for 30-60min at 30-40 ℃ to obtain a capsule wall mixed solution; s3, adding the capsule wall mixed solution into the emulsified core mixed solution, and continuously stirring for 6-8 hours at the temperature of 30-40 ℃ to complete microcapsule encapsulation, thus obtaining encapsulated capsule liquid; s4, heating the encapsulation liquid to 42-45 ℃, evaporating dichloromethane to obtain microcapsule mixed liquid, removing broken microcapsules and impurities suspended on the liquid surface, filtering the microcapsule mixed liquid, and washing with deionized water to obtain the microcapsule-state concrete targeting agent.
According to the technical scheme, wood wax oil is used as a core material, the repairing effect of concrete cracks is improved, sodium fatty alcohol ether sulfate and G-M solution are used as composite emulsifying agents, polymethyl methacrylate is doped with modified Ca-Al-LDH and lead sulfate to serve as capsule walls, and then mixed encapsulation is carried out, so that the microcapsule-state concrete targeting agent is prepared, curing exchange of chloride ions is realized through lead sulfate and modified Ca-Al-LDH targeting, the impermeability and corrosion resistance are improved, an ion triggering and mechanical triggering dual triggering mechanism is provided, the self-repairing and chloride ion curing synergistic corrosion resisting effect is achieved, and the malignant cycle caused by concrete cracking and steel bar corrosion is effectively solved.
Preferably, the sodium fatty alcohol ether sulfate in S1 is 3EO-AES.
By adopting the technical scheme, the 3EO-AES and G-M solution of the fatty alcohol ether sodium sulfate is used as the composite emulsifier, so that the emulsification dispersion stability of the wood wax oil is facilitated, and the subsequent microcapsule encapsulation effect is improved.
Preferably, the G-M solution is a mixed aqueous solution of gelatin and sodium alginate, the mass concentration of the gelatin is 1-3%, and the mass concentration of the sodium alginate is 2-4%.
By adopting the technical scheme, the gelatin and the sodium alginate in the proportion have strong interaction and good compatibility, show better synergistic effect and are beneficial to the stability of emulsion.
Preferably, the mass volume ratio of the sodium fatty alcohol ether sulfate, the G-M solution and the wood wax oil in the S1 is (0.2-0.3G): (800-1000 mL): (30-50G).
By adopting the technical scheme, the emulsion core mixed solution in the proportion is stable, and emulsion droplets formed subsequently are not easy to aggregate.
Preferably, the mass volume ratio of the polymethyl methacrylate to the methylene dichloride in the methylene dichloride solution of the polymethyl methacrylate in the step S2 is (50-80 g) (400-800 mL); the mass ratio of the modified Ca-Al-LDH to the lead sulfate to the polymethyl methacrylate in the S2 is (3-5) (0.8-1.2) (50-80).
By adopting the technical scheme, in the capsule wall mixed solution in the proportion, the modified Ca-Al-LDH and the lead sulfate are doped with a proper amount, and the triggering efficiency is high.
Preferably, the preparation method of the modified Ca-Al-LDH in the S2 comprises the following steps: (1) Mixing 100mL of a 1mol/L calcium nitrate solution with 100mL of a 1mol/L aluminum nitrate solution; (2) Adding 17g of sodium nitrate and 12g of sodium hydroxide into 100mL of deionized water, then adding 1g of zwitterionic dopamine sulfonate, and uniformly mixing; (3) Mixing the two solutions obtained in (1) and (2), stirring at 65 ℃ for 30min, transferring to a hydrothermal reaction kettle, reacting at 120 ℃ for 24h, pouring out supernatant to obtain precipitate, washing with deionized water and absolute ethyl alcohol to neutrality, vacuum-drying after suction filtration, grinding into powder, and sieving with 300-mesh sieve.
By adopting the technical scheme, the Ca-Al-LDH is modified by the zwitterionic dopamine sulfonate, so that the dispersity of the Ca-Al-LDH can be increased, the specific surface area of the Ca-Al-LDH is increased, and the agglomeration is reduced, thereby improving the triggering efficiency.
Preferably, the preparation method of the lead sulfate in the step S2 comprises the following steps: 100mL of 0.8mol/L sodium sulfate aqueous solution and 0.8mol/L lead nitrate aqueous solution are respectively measured, then the lead nitrate aqueous solution is slowly dripped into the sodium sulfate aqueous solution, and stirred at the speed of 800r/min, vacuum filtration is carried out after 4 hours, a filter cake is taken, and the lead sulfate powder is obtained after drying.
By adopting the technical scheme, the prepared lead sulfate powder has the size as small as 0.8 mu m and is not easy to agglomerate.
Preferably, the volume ratio of the capsule wall mixed solution to the emulsified core mixed solution in the step S3 is (3-5) (9-12).
By adopting the technical scheme, the prepared microcapsule has moderate wall thickness, uniform microcapsule particles and high encapsulation efficiency.
In a second aspect, the present application provides a concrete targeting agent prepared by the method described above.
In summary, the present application has the following beneficial effects:
1. according to the method, wood wax oil is used as a core material, the repairing effect of concrete cracks is improved, sodium fatty alcohol ether sulfate and a G-M solution are used as composite emulsifying agents, polymethyl methacrylate is doped to modify Ca-Al-LDH and lead sulfate to serve as capsule walls, then mixed encapsulation is carried out, the microcapsule-state concrete targeting agent is prepared, curing exchange of chloride ions is achieved through lead sulfate and modified Ca-Al-LDH targeting, the impermeability and corrosion resistance are improved, the dual triggering mechanism of ion triggering and mechanical triggering is achieved, the synergistic corrosion resistance effect of self-repairing and chloride ion curing is achieved, and the malignant circulation caused by concrete cracking and steel bar corrosion is effectively solved.
2. In the application, the zwitterionic dopamine sulfonate is preferably adopted to modify Ca-Al-LDH, and the zwitterionic dopamine sulfonate is self-assembled to hydroxyl on the surface of the Ca-Al-LDH through chemical bonds between catechol groups of the zwitterionic dopamine sulfonate, so that Ca-Al-LDH is promoted to be dispersed, and agglomeration is reduced.
3. The concrete targeting agent prepared by the preparation method has the multifunctional synergistic corrosion resistance effects of self-repairing, curing chloride ions and inhibiting corrosion.
Detailed Description
The present application is described in further detail below with reference to examples.
The raw materials of the examples and comparative examples herein are commercially available in general unless otherwise specified.
The wood wax oil comprises, by mass, 35% of linseed oil, 25% of castor oil, 10% of perilla oil, 5% of natural beeswax, 10% of palm wax, 7% of soybean oil, 5% of thistle oil and 3% of sunflower seed oil.
Examples
Example 1
The preparation method of the concrete targeting agent comprises the following steps: s1, preparing an emulsified core mixed solution: dissolving 0.2G of 3EO-AES in 800G-M solution (the G-M solution is a mixed aqueous solution of gelatin and sodium alginate, the mass concentration of gelatin is 1% and the mass concentration of sodium alginate is 2%) to form a composite emulsifier, and then adding 30G of wood wax oil to obtain an emulsified core mixed solution; s2, adding 3g of modified Ca-Al-LDH and 0.8g of lead sulfate into a methylene dichloride solution of polymethyl methacrylate (containing 50g of polymethyl methacrylate and 400mL of methylene dichloride), and stirring for 30min at 30 ℃ to obtain a capsule wall mixed solution; s3, adding 300mL of the capsule wall mixed solution into 900mL of the emulsion core mixed solution, and continuously stirring for 6h at 30 ℃ to complete microcapsule encapsulation to obtain encapsulated capsule liquid; and S4, heating the encapsulation liquid to 42 ℃, evaporating dichloromethane to obtain microcapsule mixed liquid, removing broken microcapsules and impurities suspended on the liquid surface, filtering the microcapsule mixed liquid, and washing with deionized water to obtain the microcapsule-state concrete targeting agent.
The preparation method of the modified Ca-Al-LDH in the S2 comprises the following steps: (1) Mixing 100mL of a 1mol/L calcium nitrate solution with 100mL of a 1mol/L aluminum nitrate solution; (2) Adding 17g of sodium nitrate and 12g of sodium hydroxide into 100mL of deionized water, then adding 1g of zwitterionic dopamine sulfonate, and uniformly mixing; (3) Mixing the two solutions obtained in (1) and (2), stirring at 65 ℃ for 30min, transferring to a hydrothermal reaction kettle, reacting at 120 ℃ for 24h, pouring out supernatant to obtain precipitate, washing with deionized water and absolute ethyl alcohol to neutrality, vacuum-drying after suction filtration, grinding into powder, and sieving with 300-mesh sieve.
The preparation method of the lead sulfate in the S2 comprises the following steps: 100mL of 0.8mol/L sodium sulfate aqueous solution and 0.8mol/L lead nitrate aqueous solution are respectively measured, then the lead nitrate aqueous solution is slowly dripped into the sodium sulfate aqueous solution, and stirred at the speed of 800r/min, vacuum filtration is carried out after 4 hours, a filter cake is taken, and the lead sulfate powder is obtained after drying.
Example 2
The preparation method of the concrete targeting agent comprises the following steps: s1, preparing an emulsified core mixed solution: dissolving 0.25G of 3EO-AES in 900mL of G-M solution (the G-M solution is a mixed aqueous solution of gelatin and sodium alginate, the mass concentration of the gelatin is 2%, and the mass concentration of the sodium alginate is 3%) to form a composite emulsifier, and then adding 40G of wood wax oil to obtain an emulsified core mixed solution; s2, adding 4g of modified Ca-Al-LDH and 1.0g of lead sulfate into a methylene dichloride solution of polymethyl methacrylate (containing 65g of polymethyl methacrylate and 600mL of methylene dichloride), and stirring for 45min at 35 ℃ to obtain a capsule wall mixed solution; s3, 400mL of the capsule wall mixed solution is added into 1000mL of the emulsion core mixed solution, and the mixture is continuously stirred for 7 hours at 35 ℃ to complete the microcapsule encapsulation, so as to obtain encapsulated capsule liquid; and S4, heating the encapsulation liquid to 44 ℃, evaporating dichloromethane to obtain microcapsule mixed liquid, removing broken microcapsules and impurities suspended on the liquid surface, filtering the microcapsule mixed liquid, and washing with deionized water to obtain the microcapsule-state concrete targeting agent.
The preparation method of the modified Ca-Al-LDH in the S2 comprises the following steps: (1) Mixing 100mL of a 1mol/L calcium nitrate solution with 100mL of a 1mol/L aluminum nitrate solution; (2) Adding 17g of sodium nitrate and 12g of sodium hydroxide into 100mL of deionized water, then adding 1g of zwitterionic dopamine sulfonate, and uniformly mixing; (3) Mixing the two solutions obtained in (1) and (2), stirring at 65 ℃ for 30min, transferring to a hydrothermal reaction kettle, reacting at 120 ℃ for 24h, pouring out supernatant to obtain precipitate, washing with deionized water and absolute ethyl alcohol to neutrality, vacuum-drying after suction filtration, grinding into powder, and sieving with 300-mesh sieve.
The preparation method of the lead sulfate in the S2 comprises the following steps: 100mL of 0.8mol/L sodium sulfate aqueous solution and 0.8mol/L lead nitrate aqueous solution are respectively measured, then the lead nitrate aqueous solution is slowly dripped into the sodium sulfate aqueous solution, and stirred at the speed of 800r/min, vacuum filtration is carried out after 4 hours, a filter cake is taken, and the lead sulfate powder is obtained after drying.
Example 3
The preparation method of the concrete targeting agent comprises the following steps: s1, preparing an emulsified core mixed solution: dissolving 0.3G of 3EO-AES in 1000mL of G-M solution (the G-M solution is a mixed aqueous solution of gelatin and sodium alginate, the mass concentration of the gelatin is 3%, and the mass concentration of the sodium alginate is 4%) to form a composite emulsifier, and then adding 50G of wood wax oil to obtain an emulsified core mixed solution; s2, adding 5g of modified Ca-Al-LDH and 1.2g of lead sulfate into a methylene dichloride solution of polymethyl methacrylate (containing 80g of polymethyl methacrylate and 800mL of methylene dichloride), and stirring at 40 ℃ for 60min to obtain a capsule wall mixed solution; s3, adding 500mL of the capsule wall mixed solution into 1200mL of the emulsified core mixed solution, and continuously stirring for 8 hours at 40 ℃ to complete microcapsule encapsulation, thus obtaining encapsulated capsule liquid; and S4, heating the encapsulation liquid to 45 ℃, evaporating dichloromethane to obtain microcapsule mixed liquid, removing broken microcapsules and impurities suspended on the liquid surface, filtering the microcapsule mixed liquid, and washing with deionized water to obtain the microcapsule-state concrete targeting agent.
The preparation method of the modified Ca-Al-LDH in the S2 comprises the following steps: (1) Mixing 100mL of a 1mol/L calcium nitrate solution with 100mL of a 1mol/L aluminum nitrate solution; (2) Adding 17g of sodium nitrate and 12g of sodium hydroxide into 100mL of deionized water, then adding 1g of zwitterionic dopamine sulfonate, and uniformly mixing; (3) Mixing the two solutions obtained in (1) and (2), stirring at 65 ℃ for 30min, transferring to a hydrothermal reaction kettle, reacting at 120 ℃ for 24h, pouring out supernatant to obtain precipitate, washing with deionized water and absolute ethyl alcohol to neutrality, vacuum-drying after suction filtration, grinding into powder, and sieving with 300-mesh sieve.
The preparation method of the lead sulfate in the S2 comprises the following steps: 100mL of 0.8mol/L sodium sulfate aqueous solution and 0.8mol/L lead nitrate aqueous solution are respectively measured, then the lead nitrate aqueous solution is slowly dripped into the sodium sulfate aqueous solution, and stirred at the speed of 800r/min, vacuum filtration is carried out after 4 hours, a filter cake is taken, and the lead sulfate powder is obtained after drying.
Comparative example
Comparative example 1
The same as in example 2, except that the "wood wax oil" in S1 was replaced with an equal amount of "tung oil".
Comparative example 2
The same as in example 2, except that "modified Ca-Al-LDH" in S2 was replaced with an equal amount of "Ca-Al-LDH", the specific preparation method was: (1) Mixing 100mL of a 1mol/L calcium nitrate solution with 100mL of a 1mol/L aluminum nitrate solution; (2) Adding 17g of sodium nitrate and 12g of sodium hydroxide into 100mL of deionized water, and uniformly mixing; (3) Mixing the two solutions obtained in (1) and (2), stirring at 65 ℃ for 30min, transferring to a hydrothermal reaction kettle, reacting at 120 ℃ for 24h, pouring out supernatant to obtain precipitate, washing with deionized water and absolute ethyl alcohol to neutrality, vacuum-drying after suction filtration, grinding into powder, and sieving with 300-mesh sieve.
Comparative example 3
The same as in example 2, except that no "lead sulfate" component was added to S2.
Performance test
TABLE 1 mixing ratio of raw materials of concrete
The concrete targeting agents prepared in examples 1-3 and comparative examples 1-3 were doped into the remaining raw materials of the concrete in the proportions described in table 1: firstly placing coarse aggregate, fine aggregate, ordinary Portland cement and silica fume into a stirrer to be stirred for 60s, then adding all water to be stirred for 90s, finally adding a concrete targeting agent to be stirred for 30s, thus obtaining a self-repairing concrete mixture, then preparing a sample, removing a mould after 1d, and carrying out standard curing until the age of 7d to obtain a concrete sample. For the following tests:
self-healing performance test:
a pre-damage stress of 60% of the maximum compressive strength was applied to generate micro cracks in the concrete samples doped with the concrete targeting agent prepared in examples 1 to 3 and comparative examples 1 to 3. The pre-damaged concrete samples were then placed in standard curing boxes for continuous hydration to 28d and a concrete blank without doped concrete targeting agent was set. The cured hardened slurry concrete sample after repair was subjected to a compressive strength (MPa) test, and the self-healing property thereof was evaluated from the compressive strength (MPa) of the hardened slurry concrete sample cured to 28d with the concrete sample not subjected to the pre-damage treatment: self-healing recovery%o = compressive strength of pre-damaged concrete sample cured to 28 d/compressive strength of concrete sample cured without pre-damage treatment to 28 d;
test of permeation resistance:
coulombic fluxes of concrete samples doped with the concrete targeting agent prepared in examples 1 to 3 and comparative examples 1 to 3 were tested according to the national standard GB/T50082-2009: when the concrete sample was cured to 28d age, 50% of f was applied to the concrete sample c0 Pre-damaging stress, transferring the concrete sample to a standard curing box for 7d self-repairing, testing the electric flux of the concrete sample, and simultaneously setting undoped concrete targetingAnd (5) calculating the permeability resistance recovery rate of a blank concrete sample of the agent: permeability recovery = initial electric flux/electric flux after self-repair of the concrete targeting agent.
Corrosion resistance test: HPB400 grade steel bars are cut into cylinders with the diameter of 12mm multiplied by 12mm, the cylinders are polished step by using 200# to 1500# metallographic sand paper, the steel bars are sequentially washed by deionized water, dilute hydrochloric acid and acetone, and then the steel bars are soaked in saturated calcium hydroxide solution for 7d to form a passivation film. One end of the steel bar is welded with a copper wire and then placed in a cylindrical die with the bottom surface poured with 0.2mm epoxy resin, the self-repairing concrete mixture doped with the concrete targeting agent prepared in the examples 1-3 and the comparative examples 1-3 is used for sealing the steel bar electrode, and a blank sample without the concrete targeting agent is arranged. Two cracks with the width of 0.3mm are orthogonally cut on the lower bottom surface along the diameter direction through a scratch tester, the cracks are repaired by a concrete targeting agent for 7d and then are placed in an etching solution, the etching solution consists of saturated calcium hydroxide, saturated sodium chloride and 0.24wt% of sodium hydroxide, sodium chloride is gradually added into the etching solution in a mode of 0.005 mol/(L.d), the time is 3d, an electrochemical impedance spectrum experiment is carried out under the open circuit potential condition, and a charge transfer resistor is obtained according to an equivalent circuit fitting EIS test result, and corrosion inhibition efficiency is calculated: corrosion inhibition efficiency = (charge transfer resistance of sample doped with concrete targeting agent-charge transfer resistance of blank sample)/charge transfer resistance of sample doped with concrete targeting agent.
The above test results are shown in Table 2:
TABLE 2 concrete performance test results of doped concrete targeting agent
As can be seen from Table 2, the concrete targeting agents prepared in examples 1-3 of the present application have excellent self-healing properties, anti-permeability properties and corrosion inhibition properties, wherein the self-healing recovery rate is as high as 105.6%, the anti-permeability recovery rate is as high as 113.5%, and the corrosion inhibition efficiency is as high as 97.2%. Compared with a blank group, the self-healing recovery rate, the permeability resistance recovery rate and the corrosion inhibition performance of the comparative examples 1-3 are improved, but the three properties are different from those of the concrete targeting agent prepared in the examples 1-3. As can be seen from the combination of example 2 and comparative example 1, the application of wood wax oil as a core material is better than tung oil, probably due to the effect of the wood wax oil containing a small amount of wax; as can be seen from the combination of example 2 and comparative example 2, the Ca-Al-LDH modified by the zwitterionic dopamine sulfonate has better impermeability and corrosion inhibition effect, which is probably due to the fact that the zwitterionic dopamine sulfonate and the Ca-Al-LDH increase the dispersion uniformity of the Ca-Al-LDH, reduce the Ca-Al-LDH agglomeration, and make the Ca-Al-LDH better capture chloride ions in the external environment and release nitrite ions for exchanging with chloride ions, thereby having excellent impermeability and corrosion inhibition performance; it can be seen from the combination of example 2 and comparative example 3 that the addition of lead sulfate to the mixed solution of the wall can improve the permeability recovery rate of the concrete targeting agent, probably because the lead sulfate can be better complexed with chloride ions, thereby fixing the chloride ions and improving the permeability recovery rate.
In addition, in the corrosion inhibition performance test, the cracks of the concrete are further reduced in the concrete targeting agent doped sample prepared in the examples 1-3, which is probably due to the fact that the Ca-Al-LDH ion exchange and the lead sulfate are further coordinated and dissolved with chloride ions, so that more capsule shells of the concrete targeting agent are broken, the core material flows out, and the repairing function is further generated.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, but is protected by patent laws within the scope of the claims of the present application.
Claims (7)
1. The preparation method of the concrete targeting agent is characterized by comprising the following steps of: s1, preparing an emulsified core mixed solution: dissolving sodium fatty alcohol ether sulfate in the G-M solution to form a composite emulsifier, and then adding wood wax oil to obtain an emulsified core mixed solution; s2, adding the modified Ca-Al-LDH and lead sulfate into a methylene dichloride solution of polymethyl methacrylate, and stirring for 30-60min at 30-40 ℃ to obtain a capsule wall mixed solution; s3, adding the capsule wall mixed solution into the emulsified core mixed solution, and continuously stirring for 6-8 hours at the temperature of 30-40 ℃ to complete microcapsule encapsulation, thus obtaining encapsulated capsule liquid; s4, heating the encapsulation liquid to 42-45 ℃, evaporating dichloromethane to obtain microcapsule mixed liquid, removing broken microcapsules and impurities suspended on the liquid surface, filtering the microcapsule mixed liquid, and washing with deionized water to obtain microcapsule-state concrete targeting agent; the G-M solution is a mixed aqueous solution of gelatin and sodium alginate, wherein the mass concentration of the gelatin is 1-3%, and the mass concentration of the sodium alginate is 2-4%; the preparation method of the modified Ca-Al-LDH in the S2 comprises the following steps: (1) Mixing 100mL of a 1mol/L calcium nitrate solution with 100mL of a 1mol/L aluminum nitrate solution; (2) Adding 17g of sodium nitrate and 12g of sodium hydroxide into 100mL of deionized water, then adding 1g of zwitterionic dopamine sulfonate, and uniformly mixing; (3) Mixing the two solutions obtained in (1) and (2), stirring at 65 ℃ for 30min, transferring to a hydrothermal reaction kettle, reacting at 120 ℃ for 24h, pouring out supernatant to obtain precipitate, washing with deionized water and absolute ethyl alcohol to neutrality, vacuum-drying after suction filtration, grinding into powder, and sieving with 300-mesh sieve.
2. The method for preparing a concrete targeting agent according to claim 1, wherein the sodium fatty alcohol ether sulfate in the S1 is 3EO-AES.
3. The preparation method of the concrete targeting agent according to claim 2, wherein the mass volume ratio of the fatty alcohol ether sodium sulfate, the G-M solution and the wood wax oil in the S1 is (0.2-0.3G): (800-1000 mL): (30-50G).
4. The method for preparing a concrete targeting agent according to claim 3, wherein the mass-to-volume ratio of polymethyl methacrylate to methylene dichloride in the methylene dichloride solution of polymethyl methacrylate in the step S2 is (50-80 g) (400-800 mL); the mass ratio of the modified Ca-Al-LDH to the lead sulfate to the polymethyl methacrylate in the S2 is (3-5) (0.8-1.2) (50-80).
5. The method for preparing the concrete targeting agent according to claim 4, wherein the method for preparing the lead sulfate in the step S2 is as follows: 100mL of 0.8mol/L sodium sulfate aqueous solution and 0.8mol/L lead nitrate aqueous solution are respectively measured, then the lead nitrate aqueous solution is slowly dripped into the sodium sulfate aqueous solution, and stirred at the speed of 800r/min, vacuum filtration is carried out after 4 hours, a filter cake is taken, and the lead sulfate powder is obtained after drying.
6. The method for preparing a concrete targeting agent according to claim 5, wherein the volume ratio of the capsule wall mixed solution to the emulsified core mixed solution in the step S3 is (3-5) (9-12).
7. A concrete targeting agent, characterized in that it is prepared by the preparation method of the concrete targeting agent according to any one of claims 1 to 6.
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