CN103183927B - Environment-friendly aldehyde-free epoxy injecting paste material and preparation method and application therefor - Google Patents
Environment-friendly aldehyde-free epoxy injecting paste material and preparation method and application therefor Download PDFInfo
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Abstract
The invention provides an environment-friendly aldehyde-free epoxy injecting paste material and a preparation method and application for the environment-friendly aldehyde-free epoxy injecting paste material. According to the parts by weight in the method, 20-90 parts of epoxy resin, 10-80 parts of reactive solvent and 0-5 parts of interfacial modifying agent are blended and stirred to obtain a component I; 5-80 parts of amine curing agent, 0-80 parts of curing regulating agent and 0-32 parts of curing accelerator are blended and stirred to obtain a component II; and the component I and the component II are blended according to the weight ratio of 100:3 to 100:70 to obtain the epoxy injecting paste material. The injecting paste material not only can keep the excellent mechanical property, the adhesive property, ageing resistance and corrosion resistance of the epoxy resin, but also has the advantages of low toxicity, environmental friendliness, low initial viscosity, high curing speed, light color and easiness in coloring, and can be applied to the field of traditional epoxy injecting paste materials as well as concrete surface corrosion resistance of infrastructure, cultural relic repair, geological relics protection, waterproofness and impermeability of buildings, and reinforcement compensation of the buildings.
Description
Technical field
The present invention relates to epoxy injecting paste material, particularly relate to a kind of preparation method and application of Environment-friendlyaldehyde-free aldehyde-free epoxy injecting paste material.
Background technology
Epoxide resin material is due to the mechanical property of its excellence, water tolerance, erosion resistance, anti-freezing property, antidamping performance and be widely used in various field.It is main component that epoxy injecting paste material refers to epoxy resin, is equipped with thinner, solidifying agent and other performances regulation and control auxiliary agent and the low viscosity slurries made.Because the excellent properties of its induration and the low viscosity of slurries become a most important class injecting paste material at present.Low-viscosity epoxy injecting paste material is easy to be injected in stratum or construction cement gap, is then solidified into the induration of excellent performance by home position polymerization reaction, thus reaches the object of impervious leakage-stopping reinforcement.Epoxy injecting paste material is in the past mainly using furfural acetone mixture as diluted system, and this diluted system is reactive solvents, has that initial viscosity is low, good penetrability, the features such as induration excellent in mechanical performance; But, furfural be a kind of toxicity comparatively large, be easy to the industrial chemicals that volatilizees, its use in injecting paste material is restricted in American-European countries.On the other hand, epoxy injecting paste material prepared by furfural acetone system be Vandyke brown to black material, be difficult to painted, limit its application in fields such as facility surfacecti proteons.Therefore, we are a kind of feature that both remain epoxy injecting paste material low viscosity, strong mechanical performance originally urgently, has hypotoxicity again, color is more shallow, be easy to painted novel material.Chinese invention patent 201010597831.3 reports a kind of environmental protection flexibilized epoxies injection material, replace furfural acetone system owing to make use of glycidyl ethers reactive diluents, mechanical property increases, but its initial viscosity is large, time of can filling with is relatively short, and concrete castability is restricted.
Summary of the invention
The present invention be directed to the deficiency of current material and technology, there is provided solvent can with solidifying agent generation chemical reaction, IPN cross-linked network is formed, Environment-friendlyaldehyde-free aldehyde-free epoxy injecting paste material that initial viscosity is low and preparation method thereof between reactive solvents, solidifying agent, epoxy resin.
Another object of the present invention is to provide that a kind of Environment-friendlyaldehyde-free aldehyde-free epoxy injecting paste material is anticorrosion at the concrete surface of epoxy injecting paste material field and Infrastructure, historical relic reparation, geology Ruins protection, apply in the waterproof, seepage control of buildings or the reinforcement and strengthening of buildings.
Object of the present invention is achieved through the following technical solutions:
The preparation method of Environment-friendlyaldehyde-free aldehyde-free epoxy injecting paste material: with a weight parts, by the epoxy resin of 20 ~ 90 parts, the reactive solvents of 10 ~ 80 parts, the interface modifier mix and blend of 0 ~ 5 part obtains first component; By 5 ~ 80 parts of amine curing agents, the solidification adjusting control agent of 0 ~ 80 part, 0 ~ 32 part of curing catalyst mix and blend obtains second component; By first, second component according to weight ratio be 100: 3 ~ 100: 70 normal temperature mixing, stir, obtain without aldehyde reaction epoxy injecting paste material; Solidification adjusting control agent is 0 time different with curing catalyst;
Described epoxy resin is bisphenol A type epoxy resin, bisphenol f type epoxy resin or nbr carboxyl terminal modified epoxy;
One or both mixture of described without aldehyde reaction solvent is ketone and Racemic glycidol ethers; Described ketone is one or more in diacetone alcohol, acetone, butanone, isophorone, methyl iso-butyl ketone (MIBK), pimelinketone, ketene dimer, dimethyl acetone, p-methyl aceto phenone and methyl ethyl diketone; Described Racemic glycidol ethers is 12 ~ tetradecyl glycidyl ether, or described Racemic glycidol ethers is butylglycidyl ether, benzyl glycidyl ether, glycidyl allyl ether and tertiary carbonic acid glycidyl ether one or more;
Described interface modifier is one or more in aluminate coupling agent, boric acid ester coupler, silane coupling agent and titanate coupling agent;
Described amine curing agent is quadrol, diethylenetriamine, triethylene tetramine, tetraethylene pentamine, N, one or more in N dimethylamine base propylamine and 3-dibutyl amino propylamine;
Described solidification adjusting control agent is one or more in modified amine curing agent, aromatic amine curing agent and Versamid class solidifying agent; Described modified amine curing agent is 591
#, 593
#, 701
#, 810
#modified amine curing agent; Described aromatic amine curing agent is mphenylenediamine, m-xylene diamine or diaminodiphenylmethane; Described Versamid class solidifying agent is 650
#or 651
#polyamide-based solidifying agent;
Described curing catalyst is trolamine, xylidine, 2,4,6-tri-(dimethylaminomethyl) phenol, 2,4, three-2-ethylhexoate of 6-tri-(dimethylaminomethyl) phenol, one or more in three oleates of 2,4,6-tri-(dimethylaminomethyl) phenol, triphenylphosphine, methyl tetrahydro phthalic anhydride and imidazoles.
Further, described bisphenol A type epoxy resin is E-51 or E-44.Described bisphenol f type epoxy resin is F-51 or F-44.With weight parts, preferably by the epoxy resin of 30 ~ 80 parts, the reactive solvents of 20 ~ 60 parts, the interface modifier mix and blend of 0 ~ 4 part obtains first component.With weight parts, preferably by 7 ~ 75 parts of amine curing agents, the solidification adjusting control agent of 0 ~ 80 part, 0 ~ 32 part of curing catalyst mix and blend obtains second component; Solidification adjusting control agent is 0 time different with curing catalyst.
A kind of Environment-friendlyaldehyde-free aldehyde-free epoxy injecting paste material, is obtained by above-mentioned preparation method; The initial viscosity of material is between 10 ~ 25mPa.s, and tensile strength is between 5.3-10.2MPa, and compression is strong between 42.3-89.9MPa, and bonding strength is between 1.8-4.6MPa.
Described Environment-friendlyaldehyde-free aldehyde-free epoxy injecting paste material is anticorrosion at the concrete surface of epoxy injecting paste material field and Infrastructure, historical relic reparation, geology Ruins protection, apply in the waterproof, seepage control of buildings or the reinforcement and strengthening of buildings.
The present invention possesses following outstanding advantages and effect relative to prior art:
1) traditional epoxy injecting paste material is different from, conventional epoxy injecting paste material diluted system is aldehyde ketone mixed solvent, by there is aldol reaction between aldehyde and ketone, then under the interaction of the group such as epoxy group(ing), amido, the final entirety forming IPN cross-linked network.The reactive solvents that the present invention adopts not containing aldehyde material, solvent can with solidifying agent generation chemical reaction, by the bridge joint of solidifying agent, between reactive solvents, solidifying agent, epoxy resin, form IPN cross-linked network, thus form unified entirety; It maintains the feature of the low initial viscosity of epoxy injecting paste material, its initial viscosity can be low to moderate 10 ~ 23mPa.s;
2) owing to not using aldehydes solvent in diluted system, the epoxy injecting paste material more environmental friendliness of preparation, higher to environmental protection requirement for majority, higher to the requirement of workmen's healthy protect engineering is suitable for;
3) epoxide resin material provided by the invention, also has of light color, and material tinctorial property is excellent, solves the problem that epoxy material color variety is few;
4) be different from epoxy chemical slip casting in the past, provided by the present invention is a kind of epoxy material infiltrating consolidation type.It has lower initial viscosity, fast curing speed than traditional furfural acetone system epoxy injecting paste material, and the present invention also maintains the mechanical property of the excellence of epoxy resin, adhesiveproperties, ageing-resistant, corrosion resistance nature, not only can be more widely used in traditional epoxy slip casting field; But also the concrete surface that can be applied to Infrastructure is anticorrosion, historical relic reparation, geology Ruins protection, in the waterproof, seepage control of buildings or the reinforcement and strengthening of buildings.
Embodiment
Below in conjunction with embodiment, further detailed description is done to the present invention, but embodiments of the present invention are not limited thereto.
Embodiment 1
In mass fraction, by 65 parts of epoxy resin E-51,33 parts of dimethyl acetone, 2 parts of silane coupling agent KH590 normal temperature mixing and stirring obtain first component; By 30 parts of amine curing agent 3-dibutyl amino propylamine, 50 parts of solidification adjusting control agent modified amine 701
#, 10 parts of curing catalyst trolamines, 10 parts of curing catalyst 2-ethyl-4-methylimidazole mix and blends obtain second component.During use, the ratio mixing and stirring of first, second component by weight 100: 20 is obtained oyster white epoxy injecting paste material.
Embodiment 2
In mass fraction, by 20 parts of epoxy resin E-51,15 parts of nbr carboxyl terminal modified epoxy KR-100 (Korea S's national capital chemical industry), 32 parts of acetone, 32 parts of diacetone alcohols, 0.5 part of silane coupling agent KH602,0.5 part of boric acid ester coupler DN931 normal temperature mixing and stirring obtain first component; By 15 parts of amine curing agent diethylenetriamines, 53 parts of solidification adjusting control agent modified amine 810
#, 32 parts of curing catalyst 2,4,6-tri-(dimethylaminomethyl) phenol mix and blends obtain second component.During use, the ratio mixing and stirring of the first and second components by weight 100: 23 is obtained pale red brown epoxy injecting paste material.
Embodiment 3
In mass fraction, by 47 parts of epoxy resin E-44s, 23 parts of isophorones, 23.5 parts of ketene dimers, 5 parts of benzyl glycidyl ethers, 0.5 part of silane coupling agent KH560,1 part of aluminate coupling agent SG-AI821, normal temperature mixing and stirring obtains first component; By 70 parts of amine curing agent quadrols, 16 parts of solidification adjusting control agent modified amine 591
#, 7 parts of mphenylenediamines, three-2-ethylhexoate mix and blend of 7 parts of curing catalyst 2,4,6-tri-(dimethylaminomethyl) phenol obtains second component.During use, the ratio mixing and stirring of the first and second components by weight 100: 9 is obtained faint yellow epoxy injecting paste material.
Embodiment 4
In mass fraction, by 40 parts of epoxy resin E-44s, 40 parts of nbr carboxyl terminals are epoxy resin toughened, and 20 parts of 1,2-PD diglycidylether normal temperature mixing and stirring obtain first component; By 65 parts of amine curing agent triethylene tetramines, 18 parts of solidification adjusting control agent modified amine 593
#, 7 parts of solidification adjusting control agent aromatic amine curing agent m-xylene diamines, three oleate mix and blends of 10 parts of curing catalyst 2,4,6-tri-(dimethylaminomethyl) phenol obtain second component.During use, the ratio mixing and stirring of the first and second components by weight 100: 15 is obtained light yellow epoxy injecting paste material.
Embodiment 5
In mass fraction, by 37 parts of epoxy resin F-44,20 parts of butylglycidyl ethers, 39 parts of methyl iso-butyl ketone (MIBK), 4 parts of titanate coupling agent TMC-102, normal temperature mixing and stirring obtains first component; By 27 parts of amine curing agent N, N dimethylamine base propylamine, 44 parts of amine curing agent diethylenetriamines, 13 parts of curing catalyst triphenylphosphines, 16 part 2,4,6-tri-(dimethylaminomethyl) phenol mix and blend obtains second component.During use, the ratio mixing and stirring of first, second component by weight 100: 62 is obtained yellow epoxy injecting paste material.
Embodiment 6
In mass fraction, by 24 parts of epoxy resin F-51,24 parts of nbr carboxyl terminal modified epoxies, 27.5 parts of pimelinketone, 24 parts of methyl iso-butyl ketone (MIBK), 0.5 part of Silane coupling agent KH550 normal temperature mixing and stirring obtains first component; By 7 parts of amine curing agent diethylenetriamines, 80 parts of solidification adjusting control agent Versamid class solidifying agent 650
#, 13 parts of curing catalyst xylidine mix and blends obtain second component.During use, the ratio mixing and stirring of the first and second components by weight 100: 34 is obtained oyster white epoxy injecting paste material.
Embodiment 7
In mass fraction, by 46.5 parts of epoxy resin F-51,38 parts of 12 ~ tetradecyl glycidyl ethers, 15 parts of glycidyl allyl ethers, 0.3 part of titanate coupling agent TMC-102,0.2 part of silane coupling agent DL602, normal temperature mixing and stirring obtains first component; By 18.5 parts of amine curing agent tetraethylene pentamine, 19 parts of amine curing agent N, N dimethylamine base propylamine, 56 parts of solidification adjusting control agent Versamid class solidifying agent 651
#, 6.5 parts of curing catalyst methyl tetrahydro phthalic anhydride mix and blends obtain second component.During use, the ratio mixing and stirring of the first and second components by weight 100: 9.5 is obtained oyster white epoxy injecting paste material.
Embodiment 8
In mass fraction, by 52.6 parts of epoxy resin F-51,31 parts of butanone, 16 parts of tertiary carbonic acid glycidyl ethers, 0.4 part of titanate coupling agent TMC-201, normal temperature mixing and stirring obtains first component; By 37.5 parts of amine curing agent quadrols, 62.5 parts of solidification adjusting control agent modified amine curing agents 810
#mix and blend obtains second component.During use, the ratio mixing and stirring of the first and second components by weight 100: 29 is obtained oyster white epoxy injecting paste material.
Embodiment 9
In mass fraction, by 32.8 parts of epoxy resin E-51,16 parts of p-methyl aceto phenone, 16 parts of methyl ethyl diketones, 16 parts of propanetriol-diglycidyl-ethers, 16 ethylene glycol diglycidylethers, 3.2 parts of silane coupling agent KH590 normal temperature mixing and stirring obtain first component; By 66 parts of amine curing agent diethylenetriamines, 16.5 parts of solidification adjusting control agent Versamid class solidifying agent 651
#, three-2-ethylhexoate mix and blend of 17.5 parts of curing catalyst 2,4,6-tri-(dimethylaminomethyl) phenol obtains second component.During use, the ratio mixing and stirring of first, second component by weight 100: 43 is obtained oyster white epoxy injecting paste material.
The performance test situation of embodiment 1-9 gained epoxy injecting paste material is as shown in table 1.
The performance perameter of the Light epoxy injecting paste material that table 1 embodiment provides
In table 1, initial viscosity is tested according to GB/T 2794-1995 sizing agent viscosity determining procedure (rotational viscosimeter method); Gel time is tested according to JC/T 1041-2007 distress in concrete epoxide resin grouting material; Tensile strength is tested according to GB/T2568-1995 casting resin stretching test method; Compressive strength is tested according to GB/T2569-1995 casting resin compression testing method; Bonding strength is tested according to JC/T 1041-2007 distress in concrete epoxide resin grouting material.
Known by the analysis of these embodiment results: 1) material initial viscosity provided by the invention is lower, in normal temperature between 10 ~ 25mPa.s, material inside can be infiltrated well; 2) color is more shallow, is easy to painted; 3) excellent in mechanical performance, wherein tensile strength is at 5.3-10.2MPa, and compression is strong at 42.3-89.9MPa, and bonding strength is at 1.8-4.6MPa; 4) to compare conventional epoxy injecting paste material toxicity lower for material therefor toxicity.The Environment-friendlyaldehyde-free aldehyde-free epoxy injecting paste material initial viscosity prepared due to the present invention is lower, excellent in mechanical performance, color is more shallow, be easy to painted, especially solvent is not containing aldehyde material, solvent can with solidifying agent generation chemical reaction, by the bridge joint of solidifying agent, form IPN cross-linked network between reactive solvents, solidifying agent, epoxy resin, thus form unified entirety; This injecting paste material can, historical relic reparation anticorrosion at the concrete surface of epoxy injecting paste material field and Infrastructure, geology Ruins protection, apply in the waterproof, seepage control of buildings or the reinforcement and strengthening of buildings, its application method is identical with general injecting paste material.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (7)
1. a preparation method for Environment-friendlyaldehyde-free aldehyde-free epoxy injecting paste material, is characterized in that: with weight parts, by the epoxy resin of 20 ~ 90 parts, 10 ~ 80 parts without aldehyde reaction solvent, the interface modifier mix and blend of 0 ~ 5 part obtains first component; By 5 ~ 80 parts of amine curing agents, the solidification adjusting control agent of 0 ~ 80 part, 0 ~ 32 part of curing catalyst mix and blend obtains second component; By first, second component according to weight ratio be 100:3 ~ 100:70 normal temperature mixing, stir, obtain without aldehyde reaction epoxy injecting paste material; Solidification adjusting control agent is 0 time different with curing catalyst;
Described epoxy resin is bisphenol A type epoxy resin, bisphenol f type epoxy resin or nbr carboxyl terminal modified epoxy;
One or both mixture of described without aldehyde reaction solvent is ketone and Racemic glycidol ethers; Described ketone is one or more in diacetone alcohol, acetone, butanone, isophorone, methyl iso-butyl ketone (MIBK), pimelinketone, ketene dimer, dimethyl acetone, p-methyl aceto phenone and methyl ethyl diketone; Described Racemic glycidol ethers is 12 ~ tetradecyl glycidyl ether, or described Racemic glycidol ethers is butylglycidyl ether, benzyl glycidyl ether, glycidyl allyl ether and tertiary carbonic acid glycidyl ether one or more;
Described interface modifier is one or more in aluminate coupling agent, boric acid ester coupler, silane coupling agent and titanate coupling agent;
Described amine curing agent be quadrol, diethylenetriamine, triethylene tetramine, tetraethylene pentamine, N, N ?diethyl amino propylamine and 3 ?one or more in dibutyl amino propylamine;
Described solidification adjusting control agent is one or more in modified amine curing agent, aromatic amine curing agent and Versamid class solidifying agent; Described modified amine curing agent is 591
#, 593
#, 701
#, 810
#modified amine curing agent; Described aromatic amine curing agent is mphenylenediamine, m-xylene diamine or diaminodiphenylmethane; Described Versamid class solidifying agent is 650
#or 651
#polyamide-based solidifying agent;
Described curing catalyst is trolamine, xylidine, 2,4,6 ?three (dimethylaminomethyl) phenol, 2,4, three ?2 ?ethyl hexyl hydrochlorates of 6 ?tri-(dimethylaminomethyl) phenol, 2,4,6 ?one or more in three oleates of three (dimethylaminomethyl) phenol, triphenylphosphine, methyl tetrahydro phthalic anhydride and imidazoles.
2. the preparation method of Environment-friendlyaldehyde-free aldehyde-free epoxy injecting paste material according to claim 1, is characterized in that: described bisphenol A type epoxy resin be E ?51 or E ?44.
3. the preparation method of Environment-friendlyaldehyde-free aldehyde-free epoxy injecting paste material according to claim 1, is characterized in that: described bisphenol f type epoxy resin be F ?51 or F ?44.
4. the preparation method of Environment-friendlyaldehyde-free aldehyde-free epoxy injecting paste material according to claim 1, it is characterized in that: with weight parts, by the epoxy resin of 30 ~ 80 parts, the reactive solvents of 20 ~ 60 parts, the interface modifier mix and blend of 0 ~ 4 part obtains first component.
5. the preparation method of Environment-friendlyaldehyde-free aldehyde-free epoxy injecting paste material according to claim 1, it is characterized in that: with weight parts, by 7 ~ 75 parts of amine curing agents, the solidification adjusting control agent of 0 ~ 80 part, 0 ~ 32 part of curing catalyst mix and blend obtains second component; Solidification adjusting control agent is 0 time different with curing catalyst.
6. an Environment-friendlyaldehyde-free aldehyde-free epoxy injecting paste material, is characterized in that it is obtained by preparation method described in any one of claim 1 ?5; The initial viscosity of material between 10 ~ 25mPa.s, tensile strength 5.3 ?between 10.2MPa, compression by force 42.3 ?between 89.9MPa, bonding strength 1.8 ?between 4.6MPa.
7. Environment-friendlyaldehyde-free aldehyde-free epoxy injecting paste material according to claim 6, historical relic reparation anticorrosion at the concrete surface of epoxy injecting paste material field and Infrastructure, geology Ruins protection, apply in the waterproof, seepage control of buildings or the reinforcement and strengthening of buildings.
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| CN105238217B (en) * | 2015-10-30 | 2018-05-15 | 华南理工大学 | One kind penetrates into consolidation type solventless epoxy anti-corrosive coating and preparation method and application |
| CN105273361B (en) * | 2015-10-30 | 2017-10-20 | 华南理工大学 | A kind of filler response type epoxy composite material and preparation method and application |
| CN105237960B (en) * | 2015-10-30 | 2018-04-13 | 华南理工大学 | A kind of material for road repair with high spreadability and preparation method and application |
| CN105419241A (en) * | 2015-12-29 | 2016-03-23 | 广州盈天建材科技有限公司 | Transparent and environment-friendly underwater consolidated solvent-free epoxy grouting material and preparation method and application thereof |
| TWI647265B (en) * | 2018-02-05 | 2019-01-11 | Taiwan Union Technology Corporation | Resin composition, and prepreg, metal foil laminate, and printed circuit board prepared using the same |
| CN112408879B (en) * | 2020-11-18 | 2022-07-12 | 临沂大学 | High-strength fast-curing epoxy/styrene-acrylic resin composite grouting repair material and preparation method and application thereof |
| CN112480648B (en) * | 2020-11-26 | 2022-05-03 | 湖南科技大学 | Slurry foam material for blocking air leakage and generating heat through oxidation of shallow coal seam and preparation method thereof |
| CN113061323A (en) * | 2021-04-13 | 2021-07-02 | 广州大学 | Grouting material, preparation method and application |
| CN113512389B (en) * | 2021-08-03 | 2022-09-20 | 威盛亚（上海）有限公司 | Water-based environment-friendly binder for producing fire-resistant decorative material and preparation method thereof |
| CN114524655B (en) * | 2022-01-28 | 2022-09-09 | 广东铁科灌浆科技有限公司 | High-strength epoxy polymer modified cement mortar and preparation method thereof |
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| CN102585441B (en) * | 2012-02-28 | 2014-06-11 | 华南理工大学 | Performance-controllable epoxy-polyketone grouting material as well as preparation method and application thereof |
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