CN102432788B - High-efficiency furfural-acetone activator for grouting material, preparation method and application thereof - Google Patents
High-efficiency furfural-acetone activator for grouting material, preparation method and application thereof Download PDFInfo
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- CN102432788B CN102432788B CN 201110237100 CN201110237100A CN102432788B CN 102432788 B CN102432788 B CN 102432788B CN 201110237100 CN201110237100 CN 201110237100 CN 201110237100 A CN201110237100 A CN 201110237100A CN 102432788 B CN102432788 B CN 102432788B
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Abstract
The invention discloses a high-efficiency furfural-acetone activator for a grouting material, a preparation method and an application thereof. The preparation method provided by the invention comprises the following steps of: mixing polybasic amine, a phenolic compound and formaldehyde according to the mass ratio of (25-80): (15-30): (20-80), adding a catalyst, stirring, heating up to 40-70 DEG C, reacting for 5-20 hours, followed by dehydration to obtain the high-efficiency furfural-acetone activator for the grouting material. The high-efficiency furfural-acetone activator is applied in the preparation of an epoxy grouting material and can be used to prepare a high-permeability epoxy grouting material with excellent permeability and mechanical properties. The preparation method is simple. The high-permeability epoxy grouting material prepared by the adoption of the high-efficiency furfural-acetone activator has very low initial viscosity and longer operation time, and its permeability can be further raised. The mechanical properties of the grouting material are raised faster in later stages, curing period is shorter, and mechanical requirements for engineering can be reached in a shorter time, thus greatly raising work efficiency.
Description
Technical field
The present invention relates to a kind of activator, be specifically related to a kind of efficient furfural-acetone activator for injection material and preparation method thereof and application.
Background technology
Resins, epoxy have bonding force strong, can solidify at normal temperature, cure shrinkage is little, mechanical property is high and characteristics such as corrosion resistance and good, therefore is widely used in a plurality of fields such as electronics, machinery, building as tackiness agent, coating, injection material etc.The epoxy resin chemical grouting material is to use the reinforcement class injection material the most extensive, that consumption is maximum at present.Because the viscosity of Resins, epoxy own is very big, generally need to add reactive thinner when using as injection material.Furfural-acetone system reactive thinner is good with its dilution effect, can use at wet environment, advantage such as cheap becomes the most frequently used reactive thinner of epoxies injection material.If but furfural-acetone system activation efficiency is low, the mechanical property of then starching the material induration is lower, and ftractures easily.
For the low-permeability in large hydraulic engineering power station weak basic antiseepage, fixed, reinforcement, hypertonicity and the excellent mechanical property of injection material are indispensable.In addition, injection material reaches the important indicator that the needed time of mechanical property (preserving period) of engine request also is the slurry material.Because the preserving period of slurry material, directly influence the progress of engineering, and then have influence on the performance of economic benefit and the social benefit of whole engineering.Chinese invention patent 01114747.4,200610037536.6 and patent application 200910040465.9 method of series modified furfural-acetone epoxy grouting material all is provided, the injection material that is prepared by these methods is not that initial viscosity height, concrete castability are poor, be exactly that final mechanical property is low, be difficult to satisfy requirement of engineering.Chinese invention patent 87105255.5,01107590.2 and patent application 201010598220.0 etc. the epoxy resin chemical grouting material of a series of penetrating qualities, good mechanical performance is disclosed, they set forth from penetrating quality and the mechanical property of slurry material respectively, but and not mentioned listed the mechanical property temperature required and preserving period of reaching.
Summary of the invention
Primary and foremost purpose of the present invention is to overcome the shortcoming of existing epoxy grouting material furfural-acetone system activating technology with not enough, and a kind of preparation method of the efficient furfural-acetone activator for injection material is provided.
Another object of the present invention is to provide the efficient furfural-acetone activator that is used for injection material that obtains by above-mentioned preparation method.Not only initial viscosity is low, operable time is long to adopt the epoxy grouting material of this activator preparation, and penetrating quality is good, preserving period is short, and have avidity by force, characteristics such as good mechanical performance.
A further object of the present invention is to provide the application of described efficient furfural-acetone activator for injection material.
Purpose of the present invention is achieved through the following technical solutions: a kind of preparation method of the efficient furfural-acetone activator for injection material, may further comprise the steps: polyamine, phenolic compound and formaldehyde are pressed mass ratio (25～80): (15～30): (20～80) proportioning is mixed, add catalyzer, stirring is warming up to 40～70 ℃ of reactions 5～20 hours, and dehydration obtains the efficient furfural-acetone activator for injection material then;
Described polyamine is preferably one or both in aliphatic amide or the aliphatic cyclic amine;
Described polyamine is a kind of in diethylenetriamine, triethylene tetramine or the isophorone diamine more preferably;
Described phenolic compound refers to the phenol derivmives blend biology, is preferably the mixture of a kind of or at least two kinds of formation in phenol, p-aminophenol, p-methyl phenol, 4-methylphenol, 4-methoxyphenol or the 4-amino-phenol;
Described formaldehyde is the formalin of mass percent 37%;
Described catalyzer is alkali metal hydroxide, is preferably in sodium hydroxide or the potassium hydroxide one or both;
Catalyst consumption is used by those skilled in the art's general knowledge and is got final product, and is generally 0.1%～2% of reaction raw materials total mass;
A kind of efficient furfural-acetone activator for injection material prepares by above-mentioned preparation method;
Described efficient furfural-acetone activator for injection material is applied to the preparation of epoxies injection material, can make the height infiltration epoxy grouting material of penetrating quality and good mechanical performance.
The present invention has following advantage and effect with respect to prior art:
The preparation method is simple for efficient furfural-acetone activator for injection material of the present invention.The height infiltration epoxy grouting material of the furfural of the present invention that use obtains by formulation optimization-acetone activator preparation except having extremely low initial viscosity, also has longer operable time, and penetrating quality is further enhanced.And the mechanical property of high infiltration epoxy grouting material induration is faster in the later stage rising, and preserving period is shorter, can reach the required mechanics requirement of engineering in the shorter time, thereby has greatly improved working efficiency.
Embodiment
The present invention is described in further detail below in conjunction with embodiment, but embodiments of the present invention are not limited thereto.
Embodiment 1
With 25 mass parts diethylenetriamines, 20 mass parts to methoxyl group phenol and 20 mass parts formaldehyde (mass percents 37%, mix down together), add catalyst n aOH (aforementioned used material total mass 1%), be warming up to 40 ℃ of reactions 20 hours under stirring, by decompression, fully dehydration obtains the efficient furfural-acetone activator for injection material then.
Embodiment 2
40 mass parts triethylene tetramines, 13 mass parts phenol, 2 mass parts p-aminophenol and 50 mass parts formaldehyde are mixed, add catalyzer sodium hydroxide (aforementioned used material total mass 1%), be warming up to 60 ℃ of reactions 15 hours under stirring, by decompression, fully dehydration obtains the efficient furfural-acetone activator for injection material then.
Embodiment 3
45 mass parts diethylenetriamines, 25 mass parts are mixed sylvan, 5 mass parts p-aminophenol and 80 mass parts formaldehyde, add catalyzer potassium hydroxide (aforementioned used material total mass 1%), be warming up to 50 ℃ of reactions 18 hours under stirring, by decompression, fully dehydration obtains the efficient furfural-acetone activator for injection material then.
Embodiment 4
80 mass parts isophorone diamines, 22 mass parts phenol, 3 mass parts p-methyl phenols and 60 mass parts formaldehyde are mixed, add catalyzer potassium hydroxide (aforementioned used material total mass 1%), be warming up to 70 ℃ of reactions 5 hours under stirring, by decompression, fully dehydration obtains the efficient furfural-acetone activator for injection material then.
Embodiment 5
Adopt the height infiltration epoxy grouting material of activator of the present invention (embodiment 1 preparation) preparation, preparation process is as follows:
A liquid: 50 mass parts Resins, epoxy E44,40 mass parts furfurals, 30 mass parts acetone, 15 mass parts octyl glycidyl ether and 3 mass parts two (octyl group phosphorus acyloxy) metatitanic acid second diester mixing obtains;
B liquid: 15 mass parts diethylenetriamines, 6 mass parts activators (embodiment 1), 3 mass parts γ-An Bingjisanjiayangjiguiwans and 2 mass parts 2,4,6-three (dimethylamino) phenol mixing obtains;
During use A liquid and B liquid are mixed, obtain the high-intensity epoxy grouting material of hypertonicity.
Embodiment 6
Adopt the height infiltration epoxy grouting material of activator of the present invention (embodiment 2 preparations) preparation, preparation process is as follows:
A liquid: 50 mass parts Resins, epoxy E51,30 mass parts furfurals, 30 mass parts acetone, 8 mass parts 1,4-butanediol diglycidyl ether and 3 mass parts two (octyl group phosphorus acyloxy) metatitanic acid second diester mixing obtains;
B liquid: 12 mass parts diethylenetriamines, 8 mass parts activators (embodiment 2), 3 mass parts γ-An Bingjisanjiayangjiguiwans and 2 mass parts 2,4,6-three (dimethylamino) phenol mixing obtains;
During use A liquid and B liquid are mixed, obtain the high-intensity epoxy grouting material of hypertonicity.
Embodiment 7
Adopt the height infiltration epoxy grouting material of activator of the present invention (embodiment 3 preparations) preparation, preparation process is as follows:
A liquid: 40 mass parts Resins, epoxy E44,30 mass parts furfurals, 30 mass parts acetone, 6 mass parts 1,4-butanediol diglycidyl ether and 2 mass parts two (octyl group phosphorus acyloxy) metatitanic acid second diester mixing obtains;
B liquid: 12 mass parts triethylene tetramines, 6 mass parts activators (embodiment 3), 3 mass parts γ-An Bingjisanjiayangjiguiwans and 2 mass parts 2,4,6-three (dimethylamino) phenol mixing obtains;
During use A liquid and B liquid are mixed, obtain the high-intensity epoxy grouting material of hypertonicity.
Embodiment 8
Adopt the height infiltration epoxy grouting material of activator of the present invention (embodiment 4 preparations) preparation, preparation process is as follows:
A liquid: 45 mass parts Resins, epoxy E51,25 mass parts furfurals, 25 mass parts acetone, 12 mass parts benzyl glycidyl ethers and 3 mass parts isopropyl tri (dioctylpyrophosphato)titanate mixings obtain;
B liquid: 15 mass parts diethylenetriamines, 5 mass parts activators (embodiment 4), 3 mass parts γ-An Bingjisanyiyangjiguiwans and 4 mass parts 2,4,6-three (dimethylamino) phenol mixing obtains;
During use A liquid and B liquid are mixed, obtain the high-intensity epoxy grouting material of hypertonicity.
Embodiment 9
Adopt the height infiltration epoxy grouting material of activator of the present invention (embodiment 4 preparations) preparation, preparation process is as follows:
A liquid: 35 mass parts Resins, epoxy E44,25 mass parts furfurals, 25 mass parts acetone, 10 mass parts benzyl glycidyl ethers and 3 mass parts isopropyl tri (dioctylpyrophosphato)titanate mixings obtain;
B liquid: 5 parts of diethylenetriamines of 1 quality, 6 mass parts activators (embodiment 4), 3 mass parts γ-An Bingjisanjiayangjiguiwans and 6 mass parts trolamine mixings obtain;
During use A liquid and B liquid are mixed, obtain the high-intensity epoxy grouting material of hypertonicity.
The comparative example 1:
The high infiltration of preparation epoxy grouting material, the composition ratio is consistent with embodiment 5, and the linear intermediate of only distinguishing state's patent of invention 01107590.2 embodiment 1 preparation in use substitutes the activator of the embodiment of the invention 1.
The comparative example 2:
The high infiltration of preparation epoxy grouting material, the composition ratio is consistent with embodiment 9, and the linear intermediate of only distinguishing state's patent of invention 01107590.2 embodiment 2 preparations in use substitutes the activator of the embodiment of the invention 1.
Effect embodiment
The epoxy grouting material of embodiment 5～9, comparative example's 1～2 preparation is detected, and wherein: initial viscosity is with reference to the GB/T10247-2008 standard testing; Surface tension is with reference to GB/T 18396-2008 standard detection; Ultimate compression strength is with reference to GB/T 2569-1981 standard testing; Tensile strength is tested with reference to the GB16777-2008 testing standard with reference to GB/T 2568-1995 standard testing and bonding strength.
Test result is as shown in table 1:
Physics, the mechanical property of table 1 hypertonicity high-strength epoxy injection material
Table 1 has provided the hypertonicity high-strength epoxy injection material embodiment 5～8 of employing furfural activator preparation of the present invention and comparative example 1 physics and mechanical property test result.Test-results shows: the initial viscosity of the hypertonicity high-strength epoxy injection material of the present invention's preparation is at 10～14mPas, and surface tension is in (33～35) * 10
-5Between the N/cm, this has just given slurry material excellent permeation performance; Back 28 days ultimate compression strength of slurry 20 ℃ of maintenances of material reaches 66～86MPa, tensile strength reaches 20～25MPa and solidify, and bonding strength also between 3.9～5.5MPa, shows that the slurry material has excellent mechanical property.And comparative example 1 and 2 maintenance after 28 days mechanical property just far short of what is expected.Certainly As time goes on, the curing reaction of Resins, epoxy is also being proceeded, and in following considerable time, mechanical property such as ultimate compression strength, the tensile strength etc. of slurry material induration also can constantly rise.
Above-described embodiment is preferred implementation of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (5)
1. preparation method who is used for the efficient furfural-acetone activator of injection material, it is characterized in that may further comprise the steps: polyamine, phenolic compound and formaldehyde are pressed mass ratio (25～80): (15～30): (20～80) proportioning is mixed, add catalyzer, stirring is warming up to 40～70 ℃ of reactions 5～20 hours, and dehydration obtains the efficient furfural-acetone activator for injection material then;
Described phenolic compound is the phenol or derivatives thereof;
Described catalyzer is alkali metal hydroxide;
Described polyamine is a kind of in diethylenetriamine, triethylene tetramine or the isophorone diamine.
2. the preparation method of the efficient furfural-acetone activator for injection material according to claim 1, it is characterized in that: described phenolic compound is the mixture of a kind of or at least two kinds of formation in phenol, p-methyl phenol, 4-methoxyphenol or the 4-amino-phenol.
3. the preparation method of the efficient furfural-acetone activator for injection material according to claim 1, it is characterized in that: described catalyzer is one or both in sodium hydroxide or the potassium hydroxide.
4. efficient furfural-acetone activator that is used for injection material, each described preparation method prepares by claim 1～3.
5. the described efficient furfural-acetone activator for injection material of claim 4 is in the application of epoxies injection material.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201110237100 CN102432788B (en) | 2011-08-18 | 2011-08-18 | High-efficiency furfural-acetone activator for grouting material, preparation method and application thereof |
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| CN 201110237100 CN102432788B (en) | 2011-08-18 | 2011-08-18 | High-efficiency furfural-acetone activator for grouting material, preparation method and application thereof |
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| CN102432788B true CN102432788B (en) | 2013-08-07 |
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| CN110903598A (en) * | 2018-09-17 | 2020-03-24 | 张艳萍 | High-strength 3D printing chemical ink material for buildings and preparation method thereof |
| JP2021004270A (en) * | 2019-06-25 | 2021-01-14 | 住友ベークライト株式会社 | Phenol resin |
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| CN1151204C (en) * | 2001-02-28 | 2004-05-26 | 中国科学院广州化学研究所 | High-penetrability water-proof reinforcing carbonyl epoxy material and process for preparing its component |
| CN1211451C (en) * | 2003-02-28 | 2005-07-20 | 长江水利委员会长江科学院 | Underwater epoxy resin grouting material |
| CN101880134B (en) * | 2010-06-13 | 2012-11-21 | 成都威邦科技有限公司 | Grouting material for water conservancy and hydropower project and grouting method thereof |
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