CN102010230A - Method for preparing curing compound - Google Patents
Method for preparing curing compound Download PDFInfo
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- CN102010230A CN102010230A CN 201010532946 CN201010532946A CN102010230A CN 102010230 A CN102010230 A CN 102010230A CN 201010532946 CN201010532946 CN 201010532946 CN 201010532946 A CN201010532946 A CN 201010532946A CN 102010230 A CN102010230 A CN 102010230A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/40—Compounds containing silicon, titanium or zirconium or other organo-metallic compounds; Organo-clays; Organo-inorganic complexes
- C04B24/42—Organo-silicon compounds
Abstract
The invention relates to a method for preparing a curing compound. The curing compound is prepared by the following steps of: performing emulsion polymerization on (methyl) acrylic ester, a styrene and organofluorine unsaturated monomer, and/or organosilicon unsaturated monomer to prepare polymer emulsion; and then compounding polymer emulsion, film forming auxiliary, plasticizer, defoamer, a flatting agent and water to obtain the curing compound. The method is easy to operate and has easily controlled reaction conditions; a hydrophobic organofluorine group and/or organosilicon group is introduced in a macromolecule chain by an emulsion polymerization method, so that hydrophobicity of macromolecules is improved; after the curing compound is sprayed on the surface of concrete, polymeric particles aggregate on the liquid level of the curing compound, so that the volatilization of moisture in the curing compound can be relieved; and after a compact polymeric membrane is formed, the speed of dissolving and diffusing the moisture on the concrete surface in the polymeric membrane is reduced due to the hydrophobicity of the polymeric membrane, so that the evaporation of moisture on the concrete surface is reduced greatly and curing effect is improved.
Description
Technical field
The present invention relates to a kind of preparation method of curing compound.
Background technology
Concrete pouring is an important step of concrete construction, and suitable maintenance can increase substantially performances such as concrete weather resistance, intensity, wear resistance, volume stability and freeze-thaw resistance.Concrete maintenance process mainly comprises spray sprinkler maintenance, wet coverture maintenance (for example sack cloth, cotton seat and blanket etc.), plastic film maintenance and the maintenance of film forming curing agent.Coverture maintenance and wet curing that the method that concrete pouring is at present often adopted is still wet, major cause is that the maintenance effect of film forming curing agent can't satisfy actual needs, promptly the relative humidity on 7 days inner concrete surfaces will remain on more than 80%.According to building material industry standard (JC-901-2002) and American Society Testing and Materials's standard (ASTM C156-03), the high-performance curing agent is under high temperature low humidity condition, and water retention will reach 90% in 72 hours, and every square metre of dehydration is less than 550 grams.Domestic emulsion-type cement concrete curing agent mainly is to prepare by benzene emulsion, after the benzene emulsion curing agent is sprayed at concrete surface, in air,, form fine and close macromolecule membrane, thereby hinder the moisture evaporation of concrete surface along with the volatilization of solvent in the curing agent.Because the high molecular hydrophobicity of phenylpropyl alcohol is poor, dissolves-spread principle according to water molecules in polymeric membrane, the water conservation effect of benzene emulsion curing agent is unsatisfactory, and product performance are difficult to satisfy above-mentioned condition, have seriously restricted promoting the use of of film forming curing agent.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of preparation method of curing compound.
Concrete scheme of the present invention is as follows:
1). make macromolecule emulsion by following monomer through letex polymerization: the organic fluorine unsaturated monomer of 1-50wt% and/organic siliceous unsaturated monomer, the vinylbenzene of 0-60wt% and the general formula of surplus are the monomer of (1);
Wherein, R
1Be H or CH
3
R
2For containing the alkyl of 1-12 carbon atom;
2). curing compound composite: the above-mentioned macromolecule emulsion of 15-50wt% and the film coalescence aid of 1-5wt%, the softening agent of 1-5wt%, the defoamer of 1-5wt%, the flow agent of 1-5wt% and the water of surplus mix, and make curing compound.
In order to increase high molecular hydrophobicity, described organic fluorine unsaturated monomer is a methacrylic acid hexafluoro butyl ester, the mixture of a kind of or two or more arbitrary proportions in trifluoroethyl methacrylate and the methacrylic acid ten difluoro heptyl esters; Described organosilicon unsaturated monomer is a vinyltrimethoxy silane, vinyltriethoxysilane, the mixture of a kind of or two or more arbitrary proportions in vinyl trichloro silane and the methyl ethylene dimethoxy silane.
As a kind of preferred version, described organic fluorine unsaturated monomer and/or organosilicon unsaturated monomer consumption account for the 5-50wt% of monomer total amount.
The monomer of described general formula (1) is a methyl methacrylate, Jia Jibingxisuanyizhi, butyl methacrylate, methyl acrylate, ethyl propenoate, butyl acrylate, the mixture of a kind of or two or more arbitrary proportions in methacrylic dodecyl gallate and the dodecyl acrylate.
High molecular solid content is 7.5-25wt% in the described curing compound.
Described film coalescence aid is the mixture of one or more arbitrary proportions in the following composition: alcohol ester-12, phenylcarbinol, butyl glycol ether, propylene glycol monomethyl ether, propylene glycol butyl ether and propylene glycol phenylate.
Described softening agent is the mixture of one or more arbitrary proportions in the following composition: dimethyl phthalate, dibutyl phthalate, Octyl adipate, Tritolyl Phosphate and epoxyoleic acid butyl ester.
The preparation method of curing compound provided by the invention, easy control of reaction conditions, the macromolecule emulsion that makes need not to purify and separates, direct and film coalescence aid, softening agent, defoamer, flow agent and water carry out composite, and is simple to operate.Compare with the styrene-acrylate emulsion type curing compound, the present invention passes through method of emulsion polymerization, super-hydrophobic organic fluorine and/or organosilicon radical in macromolecular chain, have been introduced, reduced high molecular wetting ability, improved hydrophobicity, be sprayed at concrete surface after because hydrophobic interaction, polymeric particles is assembled at the curing agent liquid level, the volatilization that can slow down moisture in the curing agent; In air along with the volatilization of moisture in the curing agent, polymeric particles forms fine and close macromolecule membrane, in polymeric membrane, dissolve-spread principle according to water molecules, because the hydrophobic performance of this macromolecule membrane, reduced dissolving and the velocity of diffusion of concrete surface moisture in polymeric membrane, thereby reduce the moisture evaporation of concrete surface significantly, improve maintenance effect, the water retention of the curing compound that the present invention makes can be up to 95%.
Embodiment
Embodiment 1
(1) preparation of macromolecule emulsion:
The vinylbenzene of proportioning raw materials: 15wt%, the methyl methacrylate of 34.5wt%, the methacrylic acid hexafluoro butyl ester of 0.5wt%, the Potassium Persulphate initiator of 0.3wt%, the anionic emulsifier sodium lauryl sulphate of 0.3wt%, the nonionic emulsifying agent alkylphenol polyoxyethylene (op-10) of 2.7wt% and the water of surplus.
Preparation vinylbenzene, methyl methacrylate emulsion, persulfate aqueous solution and methacrylic acid hexafluoro butyl ester emulsion, wherein the emulsifying agent consumption is pressed monomer mass than distributing.Under agitation condition, temperature is 75 ℃, adds deionized water in reactor, then while drip styrene, methyl methacrylate emulsion and persulfate aqueous solution; After vinylbenzene, first class methyl acrylate emulsion dropwise, continue to drip methacrylic acid hexafluoro butyl ester emulsion.The control rate of addition adds all monomer emulsion and persulfate aqueous solution simultaneously in the 3h.After dropwising, continue reaction 4h, cooling then, discharging.
(2) even according to following ingredients and mixed, make high performance concrete curing agent: the macromolecule emulsion of 15wt%, the film coalescence aid alcohol ester-12 of 1wt%, the plasticizer phthalic acid dibutylester of 1wt%, the fluorine carbon flow agent of 2wt%, the defoamer n-Octanol of 1wt% and the water of 80wt%, testing its water retention is 60%.
Embodiment 2
(1) preparation of macromolecule emulsion:
The vinylbenzene of proportioning raw materials: 18wt%, the Jia Jibingxisuanyizhi of 24.75wt%, the methacrylic acid ten difluoro heptyl esters of 2.25wt%, the Potassium Persulphate initiator of 0.28wt%, the anionic emulsifier sodium lauryl sulphate of 0.3wt%, the nonionic emulsifying agent alkylphenol polyoxyethylene (op-10) of 2.7wt% and the water of surplus.
Preparation vinylbenzene, Jia Jibingxisuanyizhi emulsion, persulfate aqueous solution and methacrylic acid ten difluoro heptyl ester emulsions, wherein the emulsifying agent consumption is pressed monomer mass than distributing.Under agitation condition, temperature is 75 ℃, adds deionized water in reactor, then while drip styrene, Jia Jibingxisuanyizhi emulsion and persulfate aqueous solution; After vinylbenzene, Jia Jibingxisuanyizhi emulsion dropwise, continue to drip methacrylic acid ten difluoro heptyl ester emulsions.The control rate of addition adds all monomer emulsion and persulfate aqueous solution simultaneously in the 3h.After dropwising, continue reaction 4h, cooling then, discharging.
(2) even according to following ingredients and mixed, make high performance concrete curing agent: the macromolecule emulsion of 20wt%, the film coalescence aid propylene glycol monomethyl ether of 2wt%, the plasticizer phthalic acid dimethyl ester of 2wt%, the fluorine carbon flow agent of 1wt%, the defoamer n-Octanol of 1wt% and the water of 74wt%, testing its water retention is 80%.
Embodiment 3
(1) preparation of macromolecule emulsion:
The methyl methacrylate of proportioning raw materials: 30wt%, the butyl methacrylate of 10wt%, the methacrylic acid ten difluoro heptyl esters of 5wt%, the vinyl trichloro silane of 5wt%, the ammonium persulfate initiator of 0.28wt%, the anionic emulsifier sodium laurylsulfonate of 0.3wt%, the nonionic emulsifying agent alkylphenol polyoxyethylene (op-10) of 3.7wt% and the water of surplus.
Preparation methyl methacrylate, butyl methacrylate emulsion, ammonium persulfate aqueous solution and methacrylic acid ten difluoro heptyl esters, vinyl trichloro silane emulsion, wherein the emulsifying agent consumption is pressed monomer mass than distributing.Under agitation condition, temperature is 80 ℃, adds deionized water in reactor, drips methyl methacrylate, butyl methacrylate emulsion and ammonium persulfate aqueous solution then simultaneously; After methyl methacrylate, butyl methacrylate emulsion droplets add to 2/3rds, begin to drip methacrylic acid ten difluoro heptyl esters, vinyl trichloro silane emulsion.The control rate of addition adds all monomer emulsion and ammonium persulfate aqueous solution simultaneously in the 3h.After dropwising, continue reaction 5h, cooling then, discharging.
(2) even according to following ingredients and mixed, make high performance concrete curing agent: the macromolecule emulsion of 40wt%, the film coalescence aid phenylcarbinol of 4wt%, the softening agent epoxyoleic acid butyl ester of 3wt%, the fluorine carbon flow agent of 4wt%, the defoamer n-Octanol of 4wt% and the water of 45wt%, testing its water retention is 89%.
Embodiment 4
(1) preparation of macromolecule emulsion:
The methyl methacrylate of proportioning raw materials: 21wt%, the butyl methacrylate of 12.6wt%, the methacrylic acid ten difluoro heptyl esters of 8.4wt%, the Potassium Persulphate initiator of 0.26wt%, the anionic emulsifier sodium laurylsulfonate of 0.6wt%, the nonionic emulsifying agent alkylphenol polyoxyethylene (op-10) of 2.4wt% and the water of surplus.
Preparation methyl methacrylate, butyl methacrylate emulsion, persulfate aqueous solution and methacrylic acid ten difluoro heptyl ester emulsions, wherein the emulsifying agent consumption is pressed monomer mass than distributing.Under agitation condition, temperature is 85 ℃, adds deionized water in reactor, drips methyl methacrylate, butyl methacrylate emulsion and persulfate aqueous solution then simultaneously; After methyl methacrylate, butyl methacrylate emulsion droplets add to 2/3rds, begin to drip methacrylic acid ten difluoro heptyl ester emulsions, the control rate of addition adds all monomer emulsion and persulfate aqueous solution simultaneously in the 3h.After dropwising, continue reaction 3h, cooling then, discharging.
(2) even according to following ingredients and mixed, make high performance concrete curing agent: the macromolecule emulsion of 35wt%, the film coalescence aid phenylcarbinol of 4wt%, the softening agent epoxyoleic acid butyl ester of 3wt%, the fluorine carbon flow agent of 4wt%, the defoamer n-Octanol of 4wt% and the water of 50wt%, testing its water retention is 90%.
Embodiment 5
(1) preparation of macromolecule emulsion:
The vinylbenzene of proportioning raw materials: 20wt%, the butyl methacrylate of 18wt%, the vinyltriethoxysilane of 2wt%, the ammonium persulfate initiator of 0.25wt%, the anionic emulsifier sodium lauryl sulphate of 0.6wt%, the nonionic emulsifying agent alkylphenol polyoxyethylene (op-10) of 2.4wt% and the water of surplus.
Preparation vinylbenzene, butyl methacrylate emulsion, ammonium persulfate aqueous solution and vinyltriethoxysilane emulsion, wherein the emulsifying agent consumption is pressed monomer mass than distributing.Under agitation condition, temperature is 75 ℃, adds deionized water in reactor, then while drip styrene, butyl methacrylate emulsion and ammonium persulfate aqueous solution; After vinylbenzene, butyl methacrylate emulsion dropwise, continue to drip the vinyltriethoxysilane emulsion.The control rate of addition adds all monomer emulsion and ammonium persulfate aqueous solution simultaneously in the 3h.After dropwising, continue reaction 5h, cooling then, discharging.
(2) even according to following ingredients and mixed, make high performance concrete curing agent: the macromolecule emulsion of 30wt%, the film coalescence aid butyl glycol ether of 4wt%, the plasticizer phthalic acid dibutylester of 3wt%, the fluorine carbon flow agent of 3wt%, the defoamer n-Octanol of 3wt% and the water of 57wt%, testing its water retention is 85%.
Embodiment 6
(1) preparation of macromolecule emulsion:
The vinylbenzene of proportioning raw materials: 19.2wt%, the ethyl propenoate of 19.2wt%, the vinyltrimethoxy silane of 9.6wt%, the ammonium persulfate initiator of 0.3wt%, the anionic emulsifier sodium lauryl sulphate of 0.4wt%, the nonionic emulsifying agent alkylphenol polyoxyethylene (op-10) of 2.6wt% and the water of surplus.
Preparation vinylbenzene, ethyl propenoate emulsion, ammonium persulfate aqueous solution and vinyltrimethoxy silane emulsion, wherein the emulsifying agent consumption is pressed monomer mass than distributing.Under agitation condition, temperature is 70 ℃, adds deionized water in reactor, then while drip styrene, ethyl propenoate emulsion and ammonium persulfate aqueous solution; After vinylbenzene, ethyl propenoate emulsion droplets add to 2/3rds, begin to drip the vinyltrimethoxy silane emulsion.The control rate of addition adds all monomer emulsion and ammonium persulfate aqueous solution simultaneously in the 3h.After dropwising, continue reaction 3h, cooling then, discharging.
(2) even according to following ingredients and mixed, make high performance concrete curing agent: the macromolecule emulsion of 45wt%, the film coalescence aid alcohol ester-12 of 5wt%, the softening agent Tritolyl Phosphate of 5wt%, the fluorine carbon flow agent of 3wt%, the defoamer n-Octanol of 2wt% and the water of 40wt%, testing its water retention is 87%.
Embodiment 7
(1) preparation of macromolecule emulsion:
The vinylbenzene of proportioning raw materials: 14wt%, the butyl methacrylate of 6wt%, the vinyltriethoxysilane of 20wt%, the Potassium Persulphate initiator of 0.3wt%, the anionic emulsifier sodium lauryl sulphate of 0.6wt%, the nonionic emulsifying agent alkylphenol polyoxyethylene (op-10) of 3.4wt% and the water of surplus.
Preparation vinylbenzene, butyl methacrylate emulsion, persulfate aqueous solution and vinyltriethoxysilane emulsion, wherein the emulsifying agent consumption is pressed monomer mass than distributing.Under agitation condition, temperature is 80 ℃, adds deionized water in reactor, then while drip styrene, butyl methacrylate emulsion and persulfate aqueous solution; After vinylbenzene, butyl methacrylate emulsion droplets add to 2/3rds, begin to drip the vinyltriethoxysilane emulsion.The control rate of addition adds all monomer emulsion and persulfate aqueous solution simultaneously in the 3h.After dropwising, continue reaction 3h, cooling then, discharging.
(2) even according to following ingredients and mixed, make high performance concrete curing agent: the macromolecule emulsion of 30wt%, the film coalescence aid propylene glycol butyl ether of 4wt%, the plasticizer phthalic acid dibutylester of 3wt%, the fluorine carbon flow agent of 5wt%, the defoamer n-Octanol of 3wt% and the water of 55wt%, testing its water retention is 90%.
Embodiment 8
(1) preparation of macromolecule emulsion:
The vinylbenzene of proportioning raw materials: 15wt%, the butyl methacrylate of 15wt%, the methacrylic acid hexafluoro butyl ester of 10wt%, the vinyltriethoxysilane of 10wt%, the Potassium Persulphate initiator of 0.3wt%, the anionic emulsifier sodium lauryl sulphate of 0.3wt%, the nonionic emulsifying agent alkylphenol polyoxyethylene (op-10) of 2.7wt% and the water of surplus.
Preparation vinylbenzene, butyl methacrylate emulsion, persulfate aqueous solution and methacrylic acid hexafluoro butyl ester, vinyltriethoxysilane emulsion, wherein the emulsifying agent consumption is pressed monomer mass than distributing.Under agitation condition, temperature is 80 ℃, adds deionized water in reactor, then while drip styrene, butyl methacrylate emulsion and persulfate aqueous solution; After vinylbenzene, butyl methacrylate emulsion droplets add to 2/3rds, begin to drip methacrylic acid hexafluoro butyl ester, vinyltriethoxysilane emulsion.The control rate of addition adds all monomer emulsion and persulfate aqueous solution simultaneously in the 3h.After dropwising, continue reaction 4h, cooling then, discharging.
(2) even according to following ingredients and mixed, make high performance concrete curing agent: the macromolecule emulsion of 50wt%, the film coalescence aid alcohol ester-12 of 4wt%, the plasticizer phthalic acid dibutylester of 2wt%, the fluorine carbon flow agent of 3wt%, the defoamer n-Octanol of 1wt% and the water of 40wt%, testing its water retention is 95%.
Embodiment 9
(1) preparation of macromolecule emulsion:
The vinylbenzene of proportioning raw materials: 27wt%, the butyl methacrylate of 9wt%, the trifluoroethyl methacrylate of 4.5wt%, the vinyl trichloro silane of 4.5wt%, the ammonium persulfate initiator of 0.4wt%, the anionic emulsifier Sodium dodecylbenzene sulfonate of 0.3wt%, the nonionic emulsifying agent alkylphenol polyoxyethylene (op-10) of 3.2wt% and the water of surplus.
Preparation vinylbenzene, butyl methacrylate emulsion, ammonium persulfate aqueous solution and trifluoroethyl methacrylate, vinyl trichloro silane emulsion, wherein the emulsifying agent consumption is pressed monomer mass than distributing.Under agitation condition, temperature is 70 ℃, adds deionized water in reactor, then while drip styrene, butyl methacrylate emulsion and ammonium persulfate aqueous solution; After vinylbenzene, butyl methacrylate emulsion droplets add to 2/3rds, begin to drip trifluoroethyl methacrylate, vinyl trichloro silane emulsion.The control rate of addition adds all monomer emulsion and ammonium persulfate aqueous solution simultaneously in the 3h.After dropwising, continue reaction 5h, cooling then, discharging.
(2) even according to following ingredients and mixed, make high performance concrete curing agent: the macromolecule emulsion of 30wt%, the film coalescence aid phenylcarbinol of 4wt%, the softening agent epoxyoleic acid butyl ester of 3wt%, the fluorine carbon flow agent of 3wt%, the defoamer n-Octanol of 5wt% and the water of 55wt%, testing its water retention is 86%.
Embodiment 10
(1) preparation of macromolecule emulsion:
The vinylbenzene of proportioning raw materials: 20wt%, the methyl methacrylate of 12wt%, the methacrylic acid ten difluoro heptyl esters of 4wt%, the vinyl trichloro silane of 4wt%, the Potassium Persulphate initiator of 0.25wt%, the anionic emulsifier sodium laurylsulfonate of 0.4wt%, the nonionic emulsifying agent alkylphenol polyoxyethylene (op-10) of 3.6wt% and the water of surplus.
Preparation vinylbenzene, methyl methacrylate emulsion, persulfate aqueous solution and methacrylic acid ten difluoro heptyl esters, vinyl trichloro silane emulsion, wherein the emulsifying agent consumption is pressed monomer mass than distributing.Under agitation condition, temperature is 75 ℃, adds deionized water in reactor, then while drip styrene, methyl methacrylate emulsion and persulfate aqueous solution; After vinylbenzene, methyl methacrylate emulsion droplets add to 2/3rds, begin to drip methacrylic acid ten difluoro heptyl esters, vinyl trichloro silane emulsion.The control rate of addition adds all monomer emulsion and persulfate aqueous solution simultaneously in the 3h.After dropwising, continue reaction 4h, cooling then, discharging.
(2) even according to following ingredients and mixed, make high performance concrete curing agent: the macromolecule emulsion of 40wt%, the film coalescence aid phenylcarbinol of 4wt%, the softening agent epoxyoleic acid butyl ester of 3wt%, the fluorine carbon flow agent of 4wt%, the defoamer n-Octanol of 4wt% and the water of 45wt%, testing its water retention is 90%.
Embodiment 11
(1) preparation of macromolecule emulsion:
The vinylbenzene of proportioning raw materials: 14.4wt%, the butyl methacrylate of 9.6wt%, the methacrylic dodecyl gallate of 4.8wt%, the methacrylic acid hexafluoro butyl ester of 9.6wt%, the vinyltriethoxysilane of 9.6wt%, the Potassium Persulphate initiator of 0.3wt%, the anionic emulsifier sodium lauryl sulphate of 0.6wt%, the nonionic emulsifying agent alkylphenol polyoxyethylene (op-10) of 3.4wt% and the water of surplus.
Preparation vinylbenzene, butyl methacrylate, methacrylic dodecyl gallate emulsion, persulfate aqueous solution and methacrylic acid hexafluoro butyl ester, vinyltriethoxysilane emulsion, wherein the emulsifying agent consumption is pressed monomer mass than distributing.Under agitation condition, temperature is 80 ℃, adds deionized water in reactor, then while drip styrene, butyl methacrylate, methacrylic dodecyl gallate emulsion and persulfate aqueous solution; After vinylbenzene, butyl methacrylate, methacrylic dodecyl gallate emulsion droplets add to 2/3rds, begin to drip methacrylic acid hexafluoro butyl ester, vinyltriethoxysilane emulsion, the control rate of addition adds all monomer emulsion and persulfate aqueous solution simultaneously in the 3h.After dropwising, continue reaction 3h, cooling then, discharging.
(2) even according to following ingredients and mixed, make high performance concrete curing agent: the macromolecule emulsion of 50wt%, the film coalescence aid alcohol ester-12 of 4wt%, the plasticizer phthalic acid dibutylester of 2wt%, the fluorine carbon flow agent of 3wt%, the defoamer n-Octanol of 1wt% and the water of 40wt%, testing its water retention is 93%.
Embodiment 12
(1) preparation of macromolecule emulsion:
The vinylbenzene of proportioning raw materials: 16.8wt%, the butyl methacrylate of 7.2wt%, the dodecyl acrylate of 9.6wt%, the vinyltriethoxysilane of 14.4wt%, the Potassium Persulphate initiator of 0.3wt%, the anionic emulsifier sodium lauryl sulphate of 0.4wt%, the nonionic emulsifying agent alkylphenol polyoxyethylene (op-10) of 2.6wt% and the water of surplus.
Preparation vinylbenzene, butyl methacrylate, dodecyl acrylate emulsion, persulfate aqueous solution and vinyltriethoxysilane emulsion, wherein the emulsifying agent consumption is pressed monomer mass than distributing.Under agitation condition, temperature is 75 ℃, adds deionized water in reactor, then while drip styrene, butyl methacrylate, dodecyl acrylate emulsion and persulfate aqueous solution; After vinylbenzene, butyl methacrylate, dodecyl acrylate emulsion droplets add to 2/3rds, begin to drip the vinyltriethoxysilane emulsion.The control rate of addition adds all monomer emulsion and persulfate aqueous solution simultaneously in the 3h.After dropwising, continue reaction 4h, cooling then, discharging.
(2) even according to following ingredients and mixed, make high performance concrete curing agent: the macromolecule emulsion of 30wt%, the film coalescence aid propylene glycol butyl ether of 4wt%, the plasticizer phthalic acid dibutylester of 3wt%, the fluorine carbon flow agent of 5wt%, the defoamer n-Octanol of 3wt% and the water of 55wt%, testing its water retention is 92%.
Embodiment 13
(1) preparation of macromolecule emulsion:
The vinylbenzene of proportioning raw materials: 21wt%, the butyl methacrylate of 14.7wt%, the vinyl trichloro silane of 6.3wt%, the Potassium Persulphate initiator of 0.3wt%, the anionic emulsifier sodium lauryl sulphate of 0.3wt%, the nonionic emulsifying agent alkylphenol polyoxyethylene (op-10) of 2.7wt% and the water of surplus.
Preparation vinylbenzene, butyl methacrylate emulsion, persulfate aqueous solution and vinyl trichloro silane emulsion, wherein the emulsifying agent consumption is pressed monomer mass than distributing.Under agitation condition, temperature is 75 ℃, adds deionized water in reactor, then while drip styrene, butyl methacrylate emulsion and persulfate aqueous solution; After vinylbenzene, butyl methacrylate emulsion droplets add to 2/3rds, begin to drip the vinyl trichloro silane emulsion.The control rate of addition adds all monomer emulsion and persulfate aqueous solution simultaneously in the 3h.After dropwising, continue reaction 5h, cooling then, discharging.
(2) even according to following ingredients and mixed, make high performance concrete curing agent: the macromolecule emulsion of 40wt%, the film coalescence aid phenylcarbinol of 4wt%, the softening agent epoxyoleic acid butyl ester of 3wt%, the fluorine carbon flow agent of 3wt%, the defoamer n-Octanol of 5wt% and the water of 45wt%, testing its water retention is 88%.
The water retention of curing compound is tested according to building material industry standard (JC-901-2002) in the foregoing description.
Claims (7)
1. the preparation method of a curing compound is characterized in that may further comprise the steps:
1). make macromolecule emulsion by following monomer through letex polymerization: the organic fluorine unsaturated monomer of 1-50wt% and/or organosilicon unsaturated monomer, the vinylbenzene of 0-60wt% and the general formula of surplus are the monomer of (1);
Wherein, R
1Be H or CH
3
R
2For containing the alkyl of 1-12 carbon atom;
2). curing compound composite: the above-mentioned macromolecule emulsion of 15-50wt% and the film coalescence aid of 1-5wt%, the softening agent of 1-5wt%, the defoamer of 1-5wt%, the flow agent of 1-5wt% and the water of surplus mix, and make curing compound.
2. by the preparation method of the described curing compound of claim 1, it is characterized in that: high molecular solid content is 7.5-25wt% in the described curing compound.
3. press the preparation method of claim 1 or 2 described curing compounds, it is characterized in that described organic fluorine unsaturated monomer is a methacrylic acid hexafluoro butyl ester, the mixture of a kind of or two or more arbitrary proportions in trifluoroethyl methacrylate and the methacrylic acid ten difluoro heptyl esters; Described organosilicon unsaturated monomer is a vinyltrimethoxy silane, vinyltriethoxysilane, the mixture of a kind of or two or more arbitrary proportions in vinyl trichloro silane and the methyl ethylene dimethoxy silane.
4. by the preparation method of claim 1 or 2 described curing compounds, it is characterized in that: described organic fluorine unsaturated monomer and/or organosilicon unsaturated monomer consumption account for the 5-50wt% of monomer total amount.
5. press the preparation method of claim 1 or 2 described curing compounds, the monomer that it is characterized in that described general formula (1) is a methyl methacrylate, Jia Jibingxisuanyizhi, butyl methacrylate, methyl acrylate, ethyl propenoate, butyl acrylate, the mixture of a kind of or two or more arbitrary proportions in methacrylic dodecyl gallate and the dodecyl acrylate.
6. press the preparation method of claim 1 or 2 described curing compounds, it is characterized in that described film coalescence aid is the mixture of one or more arbitrary proportions in the following composition: alcohol ester-12, phenylcarbinol, butyl glycol ether, propylene glycol monomethyl ether, propylene glycol butyl ether and propylene glycol phenylate.
7. press the preparation method of claim 1 or 2 described curing compounds, it is characterized in that described softening agent is the mixture of one or more arbitrary proportions in the following composition: dimethyl phthalate, dibutyl phthalate, Octyl adipate, Tritolyl Phosphate and epoxyoleic acid butyl ester.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102936443A (en) * | 2012-11-22 | 2013-02-20 | 江苏博特新材料有限公司 | Concrete protection paint and preparation method thereof |
| CN102976653A (en) * | 2012-11-01 | 2013-03-20 | 江苏博特新材料有限公司 | High-performance concrete maintenance agent and its preparation method |
| CN102976652A (en) * | 2012-11-01 | 2013-03-20 | 江苏博特新材料有限公司 | Concrete maintenance agent having high water retention rate, and its preparation method |
| CN103073220A (en) * | 2013-01-16 | 2013-05-01 | 江苏博特新材料有限公司 | Emulsion type concrete curing agent |
| CN105085792A (en) * | 2015-09-17 | 2015-11-25 | 安徽森普新型材料发展有限公司 | Preparation method of organic fluorine monomer modified acrylic emulsion |
| CN105294161A (en) * | 2015-12-07 | 2016-02-03 | 江西洪屏抽水蓄能有限公司 | Unsaturated siloxane group phosphate emulsion concrete curing agent and preparation method thereof |
| CN108558441A (en) * | 2018-04-20 | 2018-09-21 | 万玉梅 | A kind of preparation method of compound concrete curing agent |
| CN115304873A (en) * | 2022-08-12 | 2022-11-08 | 湖南新湘路交通科技有限公司 | Semi-flexible composite pavement interface reinforcing agent and composite pavement material |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102976653A (en) * | 2012-11-01 | 2013-03-20 | 江苏博特新材料有限公司 | High-performance concrete maintenance agent and its preparation method |
| CN102976652A (en) * | 2012-11-01 | 2013-03-20 | 江苏博特新材料有限公司 | Concrete maintenance agent having high water retention rate, and its preparation method |
| CN102976653B (en) * | 2012-11-01 | 2014-08-06 | 江苏苏博特新材料股份有限公司 | High-performance concrete maintenance agent and its preparation method |
| CN102936443A (en) * | 2012-11-22 | 2013-02-20 | 江苏博特新材料有限公司 | Concrete protection paint and preparation method thereof |
| CN102936443B (en) * | 2012-11-22 | 2015-05-20 | 江苏苏博特新材料股份有限公司 | Concrete protection paint and preparation method thereof |
| CN103073220A (en) * | 2013-01-16 | 2013-05-01 | 江苏博特新材料有限公司 | Emulsion type concrete curing agent |
| CN105085792A (en) * | 2015-09-17 | 2015-11-25 | 安徽森普新型材料发展有限公司 | Preparation method of organic fluorine monomer modified acrylic emulsion |
| CN105085792B (en) * | 2015-09-17 | 2018-06-19 | 安徽森普新型材料发展有限公司 | A kind of preparation method of the monomer modified acrylic emulsion of Organic fluoride |
| CN105294161A (en) * | 2015-12-07 | 2016-02-03 | 江西洪屏抽水蓄能有限公司 | Unsaturated siloxane group phosphate emulsion concrete curing agent and preparation method thereof |
| CN105294161B (en) * | 2015-12-07 | 2018-10-16 | 江西洪屏抽水蓄能有限公司 | A kind of unsaturated siloxane base phosphate lotion curing compound and preparation method thereof |
| CN108558441A (en) * | 2018-04-20 | 2018-09-21 | 万玉梅 | A kind of preparation method of compound concrete curing agent |
| CN115304873A (en) * | 2022-08-12 | 2022-11-08 | 湖南新湘路交通科技有限公司 | Semi-flexible composite pavement interface reinforcing agent and composite pavement material |
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