CN115925364B - Cement-based permeable crystallization type waterproofing agent and production process thereof - Google Patents
Cement-based permeable crystallization type waterproofing agent and production process thereof Download PDFInfo
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- 239000004568 cement Substances 0.000 title claims abstract description 54
- 238000002425 crystallisation Methods 0.000 title claims abstract description 27
- 230000008025 crystallization Effects 0.000 title claims abstract description 27
- 238000004078 waterproofing Methods 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 53
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- RYAGRZNBULDMBW-UHFFFAOYSA-L calcium;3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical class [Ca+2].COC1=CC=CC(CC(CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O RYAGRZNBULDMBW-UHFFFAOYSA-L 0.000 claims abstract description 24
- 229920001577 copolymer Polymers 0.000 claims abstract description 24
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 16
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims description 79
- 238000002156 mixing Methods 0.000 claims description 35
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 239000004615 ingredient Substances 0.000 claims description 22
- 238000005303 weighing Methods 0.000 claims description 22
- 238000002360 preparation method Methods 0.000 claims description 20
- 238000001291 vacuum drying Methods 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 19
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 19
- 239000000945 filler Substances 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 claims description 10
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 150000001412 amines Chemical class 0.000 claims description 10
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 10
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 10
- 239000000920 calcium hydroxide Substances 0.000 claims description 10
- 235000011116 calcium hydroxide Nutrition 0.000 claims description 10
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 229920002401 polyacrylamide Polymers 0.000 claims description 10
- 239000001509 sodium citrate Substances 0.000 claims description 10
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 10
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 10
- 239000000176 sodium gluconate Substances 0.000 claims description 10
- 235000012207 sodium gluconate Nutrition 0.000 claims description 10
- 229940005574 sodium gluconate Drugs 0.000 claims description 10
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 10
- IEDVJHCEMCRBQM-UHFFFAOYSA-N trimethoprim Chemical compound COC1=C(OC)C(OC)=CC(CC=2C(=NC(N)=NC=2)N)=C1 IEDVJHCEMCRBQM-UHFFFAOYSA-N 0.000 claims description 10
- 229960001082 trimethoprim Drugs 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 238000007710 freezing Methods 0.000 claims description 8
- 230000000149 penetrating effect Effects 0.000 claims description 8
- XYRAEZLPSATLHH-UHFFFAOYSA-N trisodium methoxy(trioxido)silane Chemical compound [Na+].[Na+].[Na+].CO[Si]([O-])([O-])[O-] XYRAEZLPSATLHH-UHFFFAOYSA-N 0.000 claims description 8
- 229920005551 calcium lignosulfonate Polymers 0.000 claims description 6
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 5
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- 239000006004 Quartz sand Substances 0.000 claims description 5
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 5
- 235000019270 ammonium chloride Nutrition 0.000 claims description 5
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- KHSLHYAUZSPBIU-UHFFFAOYSA-M benzododecinium bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 KHSLHYAUZSPBIU-UHFFFAOYSA-M 0.000 claims description 5
- JBIROUFYLSSYDX-UHFFFAOYSA-M benzododecinium chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 JBIROUFYLSSYDX-UHFFFAOYSA-M 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 claims description 5
- 239000011790 ferrous sulphate Substances 0.000 claims description 5
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 5
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 5
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 5
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 5
- -1 polysiloxane Polymers 0.000 claims description 5
- 229920001296 polysiloxane Polymers 0.000 claims description 5
- 239000012286 potassium permanganate Substances 0.000 claims description 5
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 239000004576 sand Substances 0.000 claims description 5
- 229950004959 sorbitan oleate Drugs 0.000 claims description 5
- 238000004448 titration Methods 0.000 claims description 5
- 230000002528 anti-freeze Effects 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 229920000548 poly(silane) polymer Polymers 0.000 claims description 4
- CAQWNKXTMBFBGI-UHFFFAOYSA-N C.[Na] Chemical compound C.[Na] CAQWNKXTMBFBGI-UHFFFAOYSA-N 0.000 claims description 2
- 239000011398 Portland cement Substances 0.000 claims description 2
- 239000004115 Sodium Silicate Substances 0.000 claims description 2
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 9
- 239000002253 acid Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 230000006750 UV protection Effects 0.000 abstract description 3
- 239000003242 anti bacterial agent Substances 0.000 abstract description 2
- 238000007334 copolymerization reaction Methods 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 abstract description 2
- 229920000642 polymer Polymers 0.000 abstract 2
- 230000000052 comparative effect Effects 0.000 description 9
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 230000002730 additional effect Effects 0.000 description 3
- 239000004567 concrete Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 239000003469 silicate cement Substances 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 239000003673 groundwater Substances 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920005646 polycarboxylate Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Landscapes
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to the technical field of building waterproof materials, and provides a cement-based permeable crystallization type waterproof agent and a production process thereof, wherein the compactness, impermeability and waterproof property of the waterproof agent can be improved by adding modified polysilicone ether; the modified calcium lignosulfonate and the modified high polymer polycarboxylic acid are subjected to graft copolymerization, so that the cement adaptability of the high polymer polycarboxylic acid can be improved while the water reducing performance of the modified calcium lignosulfonate is maintained, the modified calcium lignosulfonate copolymer can be better applied to cement-based waterproofing agents, antibacterial agent molecules in the antibacterial mixture are dispersed in the pore diameter of the nano titanium dioxide porous structure, and the nano titanium dioxide has stable antibacterial performance, so that the produced waterproofing agent can have mildew resistance and ultraviolet resistance, and the produced waterproofing agent has better antifreezing effect by adding antifreezing components.
Description
Technical Field
The invention relates to the technical field of building waterproof materials, in particular to a cement-based permeable crystallization type waterproof agent and a production process thereof.
Background
Along with the sustainable development of the economy of China, the cities are continuously enlarged, the requirements for building quality are gradually increased, and the problems of house water leakage, ground water seepage and the like are improved by using waterproof materials. The waterproof materials commonly used at present are divided into three categories, namely flexible waterproof materials, rigid waterproof materials and rigid-flexible combined waterproof materials; the flexible waterproof material can be well attached to the building surface layer, but is easy to age, poor in durability, high in maintenance cost and not suitable for popularization and use. Cement-based penetrating crystalline waterproofing agents have been rapidly developed in recent years, and the materials have been widely used because of their permanent water repellency.
The cement-based permeable crystallization type waterproof agent disclosed in Chinese patent No. CN200910227545.5 has the characteristics of low cost, good impermeability, good self-healing property, strong binding power, steel bar corrosion resistance, no toxicity and harm, and easy construction; however, the invention does not improve other properties of the waterproof agent, such as mildew resistance, antifreezing performance and ultraviolet resistance, and in order to make the waterproof agent have better application prospect, the additional properties of the waterproof agent need to be improved on the basis of having better impermeability, so how to produce the waterproof agent with good impermeability and additional properties such as mildew resistance becomes a technical problem to be solved urgently by those skilled in the art.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a cement-based permeable crystallization type waterproof agent and a production process thereof, which aim to improve the permeability resistance of the waterproof agent, and further have the additional properties of mildew resistance and the like, so that the cement-based permeable crystallization type waterproof agent has better application prospect.
Technical proposal
In order to achieve the above purpose, the invention is realized by the following technical scheme:
the cement-based permeable crystallization type waterproof agent comprises the following ingredients in parts by weight: 35-38 parts of modified polysilicone ether, 45-50 parts of modified calcium lignosulfonate copolymer, 6-8 parts of mildew-proof component, 5-6 parts of antifreezing component, 1-2 parts of amine trimethoprim, 1-2 parts of polyacrylamide, 0.5-0.8 part of sodium citrate, 1-2 parts of hydrated lime, 2-3 parts of sodium methyl silicate and 900-1000 parts of cement-based filler.
Further, the preparation method of the modified polysilicone ether comprises the following steps: firstly, 2 parts by weight of sodium dodecyl benzene sulfonate and 25 parts by weight of deionized water are weighed and poured into a container to be stirred and dispersed, 12 parts by weight of methyl methacrylate is added after stirring for 10min, and stirring is carried out again for 5min; and secondly, adding 2 parts by weight of sodium dodecyl benzene sulfonate into the system again, stirring for 5min, adding 58 parts by weight of polysilicone ether, stirring for 2.5h at 78 ℃, adding 0.5 part by weight of potassium persulfate after stirring, mixing, and uniformly mixing to obtain the modified polysilicone ether.
Still further, the stirring speed is 400-500r/min.
Further, the preparation method of the modified calcium lignosulfonate copolymer comprises the following steps:
Step 1, weighing 200 parts of calcium lignosulfonate and 12-15 parts of sodium hydroxide solution according to parts by weight, mixing uniformly, adjusting the pH value to 9-10, and heating the system under continuous stirring until the temperature of the system is 55-60 ℃;
step 2, adding 0.4-0.6 weight part of ferrous sulfate and 8-12 weight parts of potassium permanganate into the system in the step 1, uniformly stirring, standing for 3-5 hours, adding 3-5 weight parts of polysiloxane, stirring for 50-60 minutes at the temperature of 58-60 ℃, standing for 1 hour, cooling, vacuum drying in a vacuum drying oven at the temperature of 55-58 ℃, grinding into powder by using a ball mill after drying, and obtaining the modified calcium lignosulfonate;
Step 3, adding 50 parts by weight of polyethylene glycol into a three-neck flask with a dropping funnel, a condenser pipe and a water separator, heating the three-neck flask in a water bath kettle until the temperature of the three-neck flask is maintained at 80-82 ℃, slowly dropping 1-2 parts by weight of p-toluenesulfonic acid and 5-6 parts by weight of maleic anhydride into the three-neck flask through the dropping funnel, and reacting for 1h at 80 ℃ after the titration is finished;
and 4, weighing 4-5 parts by weight of acrylamide, 22-25 parts by weight of the modified calcium lignosulfonate obtained in the step 2, 2-3 parts by weight of ammonium persulfate and 150-160 parts by weight of deionized water, adding into the three-neck flask, uniformly stirring, standing for 4 hours for reaction, and placing into a vacuum drying oven at 56-58 ℃ for vacuum drying after the reaction is finished, thus obtaining the modified calcium lignosulfonate copolymer.
Further, the concentration of the sodium hydroxide solution in the step 1 is 30-40%.
Further, the preparation method of the mildew-proof component comprises the following steps: first, according to 4:3:2:3, weighing and mixing trilauryl ammonium chloride, dodecyl trimethyl ammonium chloride, dodecyl dimethyl benzyl ammonium chloride and dodecyl dimethyl benzyl ammonium bromide according to the weight ratio, and uniformly mixing to obtain an antibacterial mixture; and secondly, weighing 8-10 parts by weight of nano titanium dioxide, dissolving the nano titanium dioxide in 60 parts by weight of ethanol aqueous solution, adding 12-15 parts by weight of antibacterial mixture and 1-2 parts by weight of sorbitan oleate polyoxyethylene ether, stirring and mixing, uniformly dispersing by ultrasonic waves, and filtering and drying to obtain the mildew-proof component.
Further, the concentration of the ethanol water solution is 50-60%, the ultrasonic dispersion frequency is 26-28kHz, and the ultrasonic dispersion time is 25-30min.
Further, the preparation method of the antifreezing component comprises the following steps: weighing sodium gluconate and methanol according to the weight ratio of 1:18, pouring the sodium gluconate and the methanol into a specified container, adding 5-6 times of ionized water, uniformly mixing, and performing ultrasonic dispersion to obtain the antifreezing component.
Still further, the cement-based filler is Portland cement, quartz sand, and natural sand according to 3:2:1 weight ratio.
A process for producing a cement-based penetrating crystallization type waterproofing agent, comprising the steps of:
Pouring the cement-based filler in the ingredients into a stirring tank, stirring for 3-5min, and then adding the modified polysilicone ether, the modified calcium lignosulfonate copolymer, the amine trimethoprim, the polyacrylamide, the sodium citrate, the slaked lime and the methyl sodium silicate in the ingredients for stirring again for 8-10min;
and step two, adding the mildew-proof component and the anti-freezing component in the ingredients into the stirring tank in the step one, stirring for 12-15min, and obtaining the cement-based permeable crystallization type waterproof agent.
Advantageous effects
The invention provides a cement-based permeable crystallization type waterproofing agent and a production process thereof, and compared with the prior art, the cement-based permeable crystallization type waterproofing agent has the following beneficial effects:
1. according to the invention, the polysilicone ether is modified, so that a silicon oxygen tetrahedral structure is formed among chemical bonds in the modified polysilicone ether, the infiltration crystallization of the modified polysilicone ether can be promoted to react with a mortar system in cement filler, so that the arrangement structure of the mortar system is changed, hydration products can be closely and orderly arranged together to form a compact waterproof structure, and the compactness, the permeability and the water resistance of the waterproof agent can be improved by adding the modified polysilicone ether.
2. According to the invention, the modified calcium lignosulfonate is modified in the preparation of the modified calcium lignosulfonate copolymer, and hydrophobic groups in the modified calcium lignosulfonate can be increased on the basis of weakening the hydrophilic groups in the modified calcium lignosulfonate, so that the water reducing performance of the modified calcium lignosulfonate is improved; secondly, the modified calcium lignosulfonate and the modified high molecular polycarboxylic acid are subjected to graft copolymerization, so that the cement adaptability of the high molecular polycarboxylic acid can be improved while the water reducing performance of the modified calcium lignosulfonate is maintained, and the modified calcium lignosulfonate copolymer can be better applied to cement-based waterproof agents.
3. According to the invention, the antibacterial mixture and the nano titanium dioxide are subjected to ultrasonic dispersion, so that antibacterial agent molecules in the antibacterial mixture are dispersed in the pore diameter of the nano titanium dioxide porous structure, and the nano titanium dioxide has stable antibacterial property, so that the produced waterproof agent has mildew-proof performance; furthermore, the nano titanium dioxide has a certain ultraviolet adsorption effect, and the nano titanium dioxide is added into the production raw materials of the waterproof agent, so that the waterproof agent has good ultraviolet resistance; finally, the produced waterproofing agent has better anti-freezing and anti-freezing effects by adding the anti-freezing component, so that the cement-based permeable crystallization type waterproofing agent produced by the method has better application prospect.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1:
The cement-based permeable crystallization type waterproofing agent comprises the following ingredients in parts by weight: 35 parts of modified polysilicone ether, 45 parts of modified calcium lignosulfonate copolymer, 6 parts of mildew-proof component, 5 parts of antifreeze component, 1 part of amine trimethoprim, 1 part of polyacrylamide, 0.5 part of sodium citrate, 1 part of hydrated lime, 2 parts of sodium methyl silicate and 900 parts of cement-based filler.
The preparation method of the modified polysilane comprises the following steps: firstly, 2 parts by weight of sodium dodecyl benzene sulfonate and 25 parts by weight of deionized water are weighed and poured into a container to be stirred and dispersed, 12 parts by weight of methyl methacrylate is added after stirring for 10min, and stirring is carried out again for 5min; and secondly, adding 2 parts by weight of sodium dodecyl benzene sulfonate into the system again, stirring for 5min, adding 58 parts by weight of polysilicone ether, stirring for 2.5h at 78 ℃, adding 0.5 part by weight of potassium persulfate after stirring, mixing, and uniformly mixing to obtain the modified polysilicone ether.
The stirring speed was 400r/min.
The preparation method of the modified calcium lignosulfonate copolymer comprises the following steps:
Step 1, weighing 200 parts of calcium lignosulfonate and 12 parts of sodium hydroxide solution according to parts by weight, mixing uniformly, adjusting the pH value to 9, and heating the system under continuous stirring until the temperature of the system is 55 ℃;
Step 2, adding 0.4 part by weight of ferrous sulfate and 8 parts by weight of potassium permanganate into the system in the step 1, uniformly stirring, standing for 3 hours, adding 3 parts by weight of polysiloxane, stirring for 50 minutes at 58 ℃, standing for 1 hour, cooling, vacuum drying in a vacuum drying oven at 55 ℃, grinding into powder by using a ball mill after drying, and obtaining the modified calcium lignosulfonate;
Step 3, adding 50 parts by weight of polyethylene glycol into a three-neck flask with a dropping funnel, a condenser pipe and a water separator, heating the three-neck flask in a water bath kettle until the temperature of the three-neck flask is maintained at 80 ℃, slowly dropping 1 part by weight of p-toluenesulfonic acid and 5 parts by weight of maleic anhydride into the three-neck flask through the dropping funnel, and reacting for 1h at 80 ℃ after the titration is finished;
and 4, weighing 4 parts by weight of acrylamide, 22 parts by weight of the modified calcium lignosulfonate obtained in the step 2,2 parts by weight of ammonium persulfate and 150 parts by weight of deionized water, adding into the three-neck flask, uniformly stirring, standing for 4 hours for reaction, and placing into a vacuum drying oven at 56 ℃ for vacuum drying after the reaction is finished, thus obtaining the modified calcium lignosulfonate copolymer.
The concentration of sodium hydroxide solution in step 1 was 30%.
The preparation method of the mildew-proof component comprises the following steps: first, according to 4:3:2:3, weighing and mixing trilauryl ammonium chloride, dodecyl trimethyl ammonium chloride, dodecyl dimethyl benzyl ammonium chloride and dodecyl dimethyl benzyl ammonium bromide according to the weight ratio, and uniformly mixing to obtain an antibacterial mixture; secondly, 8 parts by weight of nano titanium dioxide is weighed and dissolved in 60 parts by weight of ethanol water solution, then 12 parts by weight of antibacterial mixture and 1 part by weight of sorbitan oleate polyoxyethylene ether are added for stirring and mixing, and after uniform ultrasonic dispersion, filtration and drying are carried out, thus obtaining the mildew-proof component.
The concentration of the ethanol aqueous solution was 50%, and the frequency of ultrasonic dispersion was 26kHz and the ultrasonic dispersion time was 25min.
The preparation method of the antifreezing component comprises the following steps: weighing sodium gluconate and methanol according to the weight ratio of 1:18, pouring the sodium gluconate and the methanol into a specified container, adding ionized water with the weight being 5 times of that of the container, uniformly mixing, and performing ultrasonic dispersion to obtain the antifreezing component.
The cement-based filler is silicate cement, quartz sand and natural sand according to the following weight ratio of 3:2:1 weight ratio.
The production process of the cement-based permeable crystallization type waterproof agent comprises the following steps:
Pouring the cement-based filler in the ingredients into a stirring tank for stirring for 3min, and then adding the modified polysilicone ether, the modified calcium lignosulfonate copolymer, the amine trimethoprim, the polyacrylamide, the sodium citrate, the slaked lime and the sodium methyl silicate in the ingredients for stirring again for 8min;
and step two, adding the mildew-proof component and the anti-freezing component in the ingredients into the stirring tank in the step one, stirring for 12min, and obtaining the cement-based permeable crystallization type waterproof agent.
Example 2:
The cement-based permeable crystallization type waterproofing agent comprises the following ingredients in parts by weight: 38 parts of modified polysilicone ether, 50 parts of modified calcium lignosulfonate copolymer, 8 parts of mildew-proof component, 6 parts of antifreeze component, 2 parts of amine trimethoprim, 2 parts of polyacrylamide, 0.8 part of sodium citrate, 2 parts of hydrated lime, 3 parts of sodium methyl silicate and 1000 parts of cement-based filler.
The preparation method of the modified polysilane comprises the following steps: firstly, 2 parts by weight of sodium dodecyl benzene sulfonate and 25 parts by weight of deionized water are weighed and poured into a container to be stirred and dispersed, 12 parts by weight of methyl methacrylate is added after stirring for 10min, and stirring is carried out again for 5min; and secondly, adding 2 parts by weight of sodium dodecyl benzene sulfonate into the system again, stirring for 5min, adding 58 parts by weight of polysilicone ether, stirring for 2.5h at 78 ℃, adding 0.5 part by weight of potassium persulfate after stirring, mixing, and uniformly mixing to obtain the modified polysilicone ether.
The stirring speed was 500r/min.
The preparation method of the modified calcium lignosulfonate copolymer comprises the following steps:
Step 1, weighing 200 parts of calcium lignosulfonate and 15 parts of sodium hydroxide solution according to parts by weight, mixing uniformly, adjusting the pH value to 10, and heating the system under continuous stirring until the temperature of the system is 60 ℃;
Step 2, adding 0.6 part by weight of ferrous sulfate and 12 parts by weight of potassium permanganate into the system in the step 1, uniformly stirring, standing for 5 hours, adding 5 parts by weight of polysiloxane, stirring at 60 ℃ for 60 minutes, standing for 1 hour, cooling, vacuum drying in a vacuum drying oven at 58 ℃, grinding into powder by using a ball mill after drying, and obtaining the modified calcium lignosulfonate;
step 3, adding 50 parts by weight of polyethylene glycol into a three-neck flask with a dropping funnel, a condenser pipe and a water separator, heating the three-neck flask in a water bath kettle until the temperature of the three-neck flask is maintained at 82 ℃, slowly dropping 2 parts by weight of p-toluenesulfonic acid and 6 parts by weight of maleic anhydride into the three-neck flask through the dropping funnel, and reacting for 1h at 80 ℃ after the titration is finished;
And 4, weighing 5 parts by weight of acrylamide, 25 parts by weight of the modified calcium lignosulfonate obtained in the step 2,3 parts by weight of ammonium persulfate and 160 parts by weight of deionized water, adding into the three-neck flask, uniformly stirring, standing for 4 hours for reaction, and placing into a vacuum drying oven at 58 ℃ for vacuum drying after the reaction is finished, thus obtaining the modified calcium lignosulfonate copolymer.
The concentration of sodium hydroxide solution in step 1 was 40%.
The preparation method of the mildew-proof component comprises the following steps: first, according to 4:3:2:3, weighing and mixing trilauryl ammonium chloride, dodecyl trimethyl ammonium chloride, dodecyl dimethyl benzyl ammonium chloride and dodecyl dimethyl benzyl ammonium bromide according to the weight ratio, and uniformly mixing to obtain an antibacterial mixture; secondly, 10 parts by weight of nano titanium dioxide is weighed and dissolved in 60 parts by weight of ethanol water solution, then 15 parts by weight of antibacterial mixture and 2 parts by weight of sorbitan oleate polyoxyethylene ether are added for stirring and mixing, and after uniform ultrasonic dispersion, filtration and drying are carried out, thus obtaining the mildew-proof component.
The concentration of the ethanol aqueous solution was 60%, and the frequency of ultrasonic dispersion was 28kHz, and the ultrasonic dispersion time was 30min.
The preparation method of the antifreezing component comprises the following steps: weighing sodium gluconate and methanol according to the weight ratio of 1:18, pouring the sodium gluconate and the methanol into a specified container, adding ionized water with the weight being 6 times of that of the container, uniformly mixing, and performing ultrasonic dispersion to obtain the antifreezing component.
The cement-based filler is silicate cement, quartz sand and natural sand according to the following weight ratio of 3:2:1 weight ratio.
The production process of the cement-based permeable crystallization type waterproof agent comprises the following steps:
Pouring the cement-based filler in the ingredients into a stirring tank for stirring for 5min, and then adding the modified polysilicone ether, the modified calcium lignosulfonate copolymer, the amine trimethoprim, the polyacrylamide, the sodium citrate, the slaked lime and the sodium methyl silicate in the ingredients for stirring again for 10min;
And step two, adding the mildew-proof component and the anti-freezing component in the ingredients into the stirring tank in the step one, stirring for 15min, and obtaining the cement-based permeable crystallization type waterproof agent.
Example 3:
The cement-based permeable crystallization type waterproofing agent comprises the following ingredients in parts by weight: 37 parts of modified polysilicone ether, 48 parts of modified calcium lignosulfonate copolymer, 7 parts of mildew-proof component, 6 parts of antifreeze component, 2 parts of amine trimethoprim, 1 part of polyacrylamide, 0.7 part of sodium citrate, 2 parts of hydrated lime, 2 parts of sodium methyl silicate and 950 parts of cement-based filler.
The preparation method of the modified polysilane comprises the following steps: firstly, 2 parts by weight of sodium dodecyl benzene sulfonate and 25 parts by weight of deionized water are weighed and poured into a container to be stirred and dispersed, 12 parts by weight of methyl methacrylate is added after stirring for 10min, and stirring is carried out again for 5min; and secondly, adding 2 parts by weight of sodium dodecyl benzene sulfonate into the system again, stirring for 5min, adding 58 parts by weight of polysilicone ether, stirring for 2.5h at 78 ℃, adding 0.5 part by weight of potassium persulfate after stirring, mixing, and uniformly mixing to obtain the modified polysilicone ether.
The stirring speed was 500r/min.
The preparation method of the modified calcium lignosulfonate copolymer comprises the following steps:
Step 1, weighing 200 parts of calcium lignosulfonate and 13 parts of sodium hydroxide solution according to parts by weight, mixing uniformly, adjusting the pH value to 10, and heating the system under continuous stirring until the temperature of the system is 57 ℃;
step 2, adding 0.5 part by weight of ferrous sulfate and 10 parts by weight of potassium permanganate into the system in the step 1, uniformly stirring, standing for 4 hours, adding 4 parts by weight of polysiloxane, stirring for 55 minutes at a temperature of 59 ℃, standing for 1 hour, cooling, vacuum drying in a vacuum drying oven at a temperature of 56 ℃, and grinding into powder by using a ball mill after drying, thus obtaining the modified calcium lignosulfonate;
Step 3, adding 50 parts by weight of polyethylene glycol into a three-neck flask with a dropping funnel, a condenser pipe and a water separator, heating the three-neck flask in a water bath kettle until the temperature of the three-neck flask is maintained at 81 ℃, slowly dropping 2 parts by weight of p-toluenesulfonic acid and 6 parts by weight of maleic anhydride into the three-neck flask through the dropping funnel, and reacting for 1h at 80 ℃ after the titration is finished;
And 4, weighing 4 parts by weight of acrylamide, 24 parts by weight of the modified calcium lignosulfonate obtained in the step 2,3 parts by weight of ammonium persulfate and 155 parts by weight of deionized water, adding into the three-neck flask, uniformly stirring, standing for 4 hours for reaction, and placing into a vacuum drying oven at 57 ℃ for vacuum drying after the reaction is finished, thus obtaining the modified calcium lignosulfonate copolymer.
The concentration of sodium hydroxide solution in step 1 was 30%.
The preparation method of the mildew-proof component comprises the following steps: first, according to 4:3:2:3, weighing and mixing trilauryl ammonium chloride, dodecyl trimethyl ammonium chloride, dodecyl dimethyl benzyl ammonium chloride and dodecyl dimethyl benzyl ammonium bromide according to the weight ratio, and uniformly mixing to obtain an antibacterial mixture; secondly, 9 parts by weight of nano titanium dioxide is weighed and dissolved in 60 parts by weight of ethanol water solution, then 14 parts by weight of antibacterial mixture and 2 parts by weight of sorbitan oleate polyoxyethylene ether are added for stirring and mixing, and after uniform ultrasonic dispersion, the mixture is filtered and dried, thus obtaining the mildew-proof component.
The concentration of the aqueous ethanol solution was 55%, and the frequency of ultrasonic dispersion was 27kHz, and the ultrasonic dispersion time was 27min.
The preparation method of the antifreezing component comprises the following steps: weighing sodium gluconate and methanol according to the weight ratio of 1:18, pouring the sodium gluconate and the methanol into a specified container, adding ionized water with the weight being 6 times of that of the container, uniformly mixing, and performing ultrasonic dispersion to obtain the antifreezing component.
The cement-based filler is silicate cement, quartz sand and natural sand according to the following weight ratio of 3:2:1 weight ratio.
The production process of the cement-based permeable crystallization type waterproof agent comprises the following steps:
Pouring the cement-based filler in the ingredients into a stirring tank, stirring for 4min, and then adding the modified polysilicone ether, the modified calcium lignosulfonate copolymer, the amine trimethoprim, the polyacrylamide, the sodium citrate, the slaked lime and the sodium methyl silicate in the ingredients for stirring again for 9min;
And step two, adding the mildew-proof component and the anti-freezing component in the ingredients into the stirring tank in the step one, stirring for 13min, and obtaining the cement-based permeable crystallization type waterproof agent.
Comparative example 1:
The ingredients and the production method of the waterproof agent provided in this example are substantially the same as those in example 1, and the main differences are that: the formulation of comparative example 1 replaced the modified polysilicone ether and modified calcium lignosulfonate copolymer of the formulation of example 1 with glycerin, calcium lignosulfonate and a polycarboxylate water reducer.
Comparative example 2:
the ingredients and the production method of the waterproof agent provided in this example are substantially the same as those in example 2, and the main differences are that: the formulation of comparative example 2 was not added with the mildew-proof and freeze-proof components.
Performance detection
The cement-based penetrating crystalline waterproofing agents prepared by examples 1 to 3 in the present invention were respectively described as examples 1 to 3; the waterproofing agents prepared by comparative examples 1-2 were recorded as comparative examples 1-2, and then the correlation performance tests were performed on examples 1-3 and comparative examples 1-2, and the obtained data are recorded in the following table:
Wherein, the detection standard of the compressive strength and the flexural strength refers to GB/T17671; the detection method of the impervious pressure comprises the following steps: concrete blocks are prepared according to GB/T1346-2011 in examples 1-3 and comparative examples 1-2 respectively, and then the concrete blocks are put into water with the temperature of 20+/-2 ℃ to be cured for 14 days to test the first permeation resistance pressure, and the concrete blocks are continuously cured for 28 days to test the second permeation resistance pressure after being broken down by water.
As shown by the data of the table, the impermeability pressure of the cement-based permeable crystalline waterproofing agent produced in the examples 1-3 is obviously better than that of the comparative example, and the cement-based permeable crystalline waterproofing agent produced in the examples 1-3 has higher comprehensive antibacterial rate and is not easy to mildew. Therefore, the cement-based permeable crystallization type waterproof agent prepared by the invention has better application prospect and market popularization value.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (8)
1. The cement-based permeable crystallization type waterproof agent is characterized by comprising the following ingredients in parts by weight: 35-38 parts of modified polysilicate, 45-50 parts of modified calcium lignosulfonate copolymer, 6-8 parts of mildew-proof component, 5-6 parts of antifreezing component, 1-2 parts of amine trimethoprim, 1-2 parts of polyacrylamide, 0.5-0.8 part of sodium citrate, 1-2 parts of slaked lime, 2-3 parts of sodium methyl silicate and 900-1000 parts of cement-based filler;
The preparation method of the modified polysilane comprises the following steps: firstly, 2 parts by weight of sodium dodecyl benzene sulfonate and 25 parts by weight of deionized water are weighed and poured into a container to be stirred and dispersed, 12 parts by weight of methyl methacrylate is added after stirring for 10min, and stirring is carried out again for 5min; secondly, adding 2 parts by weight of sodium dodecyl benzene sulfonate into the system again, stirring for 5min, adding 58 parts by weight of polysilicone ether, stirring for 2.5h at 78 ℃, adding 0.5 part by weight of potassium persulfate after stirring is finished, mixing, and uniformly mixing to obtain the modified polysilicone ether;
the preparation method of the modified calcium lignosulfonate copolymer comprises the following steps:
Step 1, weighing 200 parts of calcium lignosulfonate and 12-15 parts of sodium hydroxide solution according to parts by weight, mixing uniformly, adjusting the pH value to 9-10, and heating the system under continuous stirring until the temperature of the system is 55-60 ℃;
step 2, adding 0.4-0.6 weight part of ferrous sulfate and 8-12 weight parts of potassium permanganate into the system in the step 1, uniformly stirring, standing for 3-5 hours, adding 3-5 weight parts of polysiloxane, stirring for 50-60 minutes at the temperature of 58-60 ℃, standing for 1 hour, cooling, vacuum drying in a vacuum drying oven at the temperature of 55-58 ℃, grinding into powder by using a ball mill after drying, and obtaining the modified calcium lignosulfonate;
Step 3, adding 50 parts by weight of polyethylene glycol into a three-neck flask with a dropping funnel, a condenser pipe and a water separator, heating the three-neck flask in a water bath kettle until the temperature of the three-neck flask is maintained at 80-82 ℃, slowly dropping 1-2 parts by weight of p-toluenesulfonic acid and 5-6 parts by weight of maleic anhydride into the three-neck flask through the dropping funnel, and reacting for 1h at 80 ℃ after the titration is finished;
and 4, weighing 4-5 parts by weight of acrylamide, 22-25 parts by weight of the modified calcium lignosulfonate obtained in the step 2, 2-3 parts by weight of ammonium persulfate and 150-160 parts by weight of deionized water, adding into the three-neck flask, uniformly stirring, standing for 4 hours for reaction, and placing into a vacuum drying oven at 56-58 ℃ for vacuum drying after the reaction is finished, thus obtaining the modified calcium lignosulfonate copolymer.
2. A cementitious capillary crystalline waterproofing agent according to claim 1, wherein the agitation speed is 400-500r/min.
3. A cementitious capillary crystalline waterproofing agent according to claim 1, wherein the concentration of sodium hydroxide solution in step 1 is 30-40%.
4. The cement-based penetrating and crystallizing waterproofing agent as claimed in claim 1, wherein the preparation method of the mildew-proof component comprises the following steps: first, according to 4:3:2:3, weighing and mixing trilauryl ammonium chloride, dodecyl trimethyl ammonium chloride, dodecyl dimethyl benzyl ammonium chloride and dodecyl dimethyl benzyl ammonium bromide according to the weight ratio, and uniformly mixing to obtain an antibacterial mixture; and secondly, weighing 8-10 parts by weight of nano titanium dioxide, dissolving the nano titanium dioxide in 60 parts by weight of ethanol aqueous solution, adding 12-15 parts by weight of antibacterial mixture and 1-2 parts by weight of sorbitan oleate polyoxyethylene ether, stirring and mixing, uniformly dispersing by ultrasonic waves, and filtering and drying to obtain the mildew-proof component.
5. The cement-based penetrating crystallization type waterproof agent according to claim 4, wherein the concentration of the ethanol aqueous solution is 50-60%, the frequency of ultrasonic dispersion is 26-28kHz, and the ultrasonic dispersion time is 25-30min.
6. The cement-based penetrating crystalline waterproofing agent according to claim 1, wherein the antifreeze component is prepared by the following method: weighing sodium gluconate and methanol according to the weight ratio of 1:18, pouring the sodium gluconate and the methanol into a specified container, adding 5-6 times of ionized water, uniformly mixing, and performing ultrasonic dispersion to obtain the antifreezing component.
7. A cement-based penetrating crystalline waterproofing agent according to claim 1, wherein the cement-based filler is portland cement, quartz sand, and natural sand according to 3:2:1 weight ratio.
8. A process for producing a cement-based penetrating crystalline waterproofing agent according to any one of claims 1to 7, characterized in that the production process comprises the steps of:
Pouring the cement-based filler in the ingredients into a stirring tank, stirring for 3-5min, and then adding the modified polysilicone ether, the modified calcium lignosulfonate copolymer, the amine trimethoprim, the polyacrylamide, the sodium citrate, the slaked lime and the methyl sodium silicate in the ingredients for stirring again for 8-10min;
and step two, adding the mildew-proof component and the anti-freezing component in the ingredients into the stirring tank in the step one, stirring for 12-15min, and obtaining the cement-based permeable crystallization type waterproof agent.
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| CN106928612A (en) * | 2017-03-10 | 2017-07-07 | 呼伦贝尔辰研化工新科技有限公司 | Emulsion polymerization and preparation method thereof and the water-repellent paint prepared with it |
| CN112358226A (en) * | 2020-10-27 | 2021-02-12 | 桂林理工大学 | Stainless steel slag curing agent and preparation method thereof |
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| CN106928612A (en) * | 2017-03-10 | 2017-07-07 | 呼伦贝尔辰研化工新科技有限公司 | Emulsion polymerization and preparation method thereof and the water-repellent paint prepared with it |
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