CN103554842B - A kind of ungauged regions epoxy grouting material and preparation method thereof - Google Patents
A kind of ungauged regions epoxy grouting material and preparation method thereof Download PDFInfo
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- CN103554842B CN103554842B CN201310570917.0A CN201310570917A CN103554842B CN 103554842 B CN103554842 B CN 103554842B CN 201310570917 A CN201310570917 A CN 201310570917A CN 103554842 B CN103554842 B CN 103554842B
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- 239000000463 material Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000004593 Epoxy Substances 0.000 title claims abstract description 20
- 239000003822 epoxy resin Substances 0.000 claims abstract description 31
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 31
- 238000003756 stirring Methods 0.000 claims abstract description 30
- -1 butyl nitrile Chemical class 0.000 claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 20
- 239000000178 monomer Substances 0.000 claims abstract description 13
- 239000013543 active substance Substances 0.000 claims abstract description 11
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 11
- 229920001971 elastomer Polymers 0.000 claims abstract description 10
- 239000005060 rubber Substances 0.000 claims abstract description 10
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 9
- 239000006185 dispersion Substances 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 claims description 9
- 150000003839 salts Chemical class 0.000 claims description 9
- 150000001412 amines Chemical class 0.000 claims description 7
- 238000005194 fractionation Methods 0.000 claims description 6
- 230000004048 modification Effects 0.000 claims description 6
- 238000012986 modification Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 4
- 239000007795 chemical reaction product Substances 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- 238000002425 crystallisation Methods 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 2
- GBKGJMYPQZODMI-SNAWJCMRSA-N (e)-4-(furan-2-yl)but-3-en-2-one Chemical compound CC(=O)\C=C\C1=CC=CO1 GBKGJMYPQZODMI-SNAWJCMRSA-N 0.000 abstract description 8
- 239000001667 (E)-4-furan-2-ylbut-3-en-2-one Substances 0.000 abstract description 7
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000001988 toxicity Effects 0.000 abstract description 2
- 231100000419 toxicity Toxicity 0.000 abstract description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 18
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 18
- 238000000034 method Methods 0.000 description 14
- 230000008569 process Effects 0.000 description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 6
- 150000002118 epoxides Chemical class 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 230000002378 acidificating effect Effects 0.000 description 4
- 150000001299 aldehydes Chemical class 0.000 description 4
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 2
- SYBYTAAJFKOIEJ-UHFFFAOYSA-N 3-Methylbutan-2-one Chemical compound CC(C)C(C)=O SYBYTAAJFKOIEJ-UHFFFAOYSA-N 0.000 description 2
- 229930185605 Bisphenol Natural products 0.000 description 2
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 2
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 2
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 2
- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 230000008602 contraction Effects 0.000 description 2
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- GGSUCNLOZRCGPQ-UHFFFAOYSA-N diethylaniline Chemical compound CCN(CC)C1=CC=CC=C1 GGSUCNLOZRCGPQ-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- HJOVHMDZYOCNQW-UHFFFAOYSA-N isophorone Chemical compound CC1=CC(=O)CC(C)(C)C1 HJOVHMDZYOCNQW-UHFFFAOYSA-N 0.000 description 2
- 229940043265 methyl isobutyl ketone Drugs 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 description 2
- MNAHQWDCXOHBHK-UHFFFAOYSA-N 1-phenylpropane-1,1-diol Chemical compound CCC(O)(O)C1=CC=CC=C1 MNAHQWDCXOHBHK-UHFFFAOYSA-N 0.000 description 1
- HPILSDOMLLYBQF-UHFFFAOYSA-N 2-[1-(oxiran-2-ylmethoxy)butoxymethyl]oxirane Chemical compound C1OC1COC(CCC)OCC1CO1 HPILSDOMLLYBQF-UHFFFAOYSA-N 0.000 description 1
- KUAUJXBLDYVELT-UHFFFAOYSA-N 2-[[2,2-dimethyl-3-(oxiran-2-ylmethoxy)propoxy]methyl]oxirane Chemical compound C1OC1COCC(C)(C)COCC1CO1 KUAUJXBLDYVELT-UHFFFAOYSA-N 0.000 description 1
- NFVPEIKDMMISQO-UHFFFAOYSA-N 4-[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC=C(O)C=C1 NFVPEIKDMMISQO-UHFFFAOYSA-N 0.000 description 1
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical group OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 1
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 1
- 229920000459 Nitrile rubber Polymers 0.000 description 1
- 229920013649 Paracril Polymers 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- SPEUIVXLLWOEMJ-UHFFFAOYSA-N acetaldehyde dimethyl acetal Natural products COC(C)OC SPEUIVXLLWOEMJ-UHFFFAOYSA-N 0.000 description 1
- 238000005575 aldol reaction Methods 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- KCXMKQUNVWSEMD-UHFFFAOYSA-N benzyl chloride Chemical compound ClCC1=CC=CC=C1 KCXMKQUNVWSEMD-UHFFFAOYSA-N 0.000 description 1
- 229940073608 benzyl chloride Drugs 0.000 description 1
- KXHPPCXNWTUNSB-UHFFFAOYSA-M benzyl(trimethyl)azanium;chloride Chemical group [Cl-].C[N+](C)(C)CC1=CC=CC=C1 KXHPPCXNWTUNSB-UHFFFAOYSA-M 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- 239000004568 cement Substances 0.000 description 1
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- 238000004132 cross linking Methods 0.000 description 1
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 description 1
- XXBDWLFCJWSEKW-UHFFFAOYSA-N dimethylbenzylamine Chemical compound CN(C)CC1=CC=CC=C1 XXBDWLFCJWSEKW-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- FXHGMKSSBGDXIY-UHFFFAOYSA-N heptanal Chemical compound CCCCCCC=O FXHGMKSSBGDXIY-UHFFFAOYSA-N 0.000 description 1
- QEUHJZZUEFYTLK-UHFFFAOYSA-N hexanal Chemical compound [CH2]CCCCC=O QEUHJZZUEFYTLK-UHFFFAOYSA-N 0.000 description 1
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- AFEQENGXSMURHA-UHFFFAOYSA-N oxiran-2-ylmethanamine Chemical compound NCC1CO1 AFEQENGXSMURHA-UHFFFAOYSA-N 0.000 description 1
- XNLICIUVMPYHGG-UHFFFAOYSA-N pentan-2-one Chemical compound CCCC(C)=O XNLICIUVMPYHGG-UHFFFAOYSA-N 0.000 description 1
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- 229920000642 polymer Polymers 0.000 description 1
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- KUAZQDVKQLNFPE-UHFFFAOYSA-N thiram Chemical compound CN(C)C(=S)SSC(=S)N(C)C KUAZQDVKQLNFPE-UHFFFAOYSA-N 0.000 description 1
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- Epoxy Resins (AREA)
Abstract
The present invention relates to a kind of ungauged regions epoxy grouting material and preparation method thereof, described material and preparation method thereof comprises: (1), preparation low-viscosity epoxy resin and modified firming agent; (2), by low-viscosity epoxy resin, reactive thinner, low-viscosity toughner stirs in proportion until dispersion of materials is even; (3) add tensio-active agent, in the material and dispersed with stirring, then add Expanding Monomer and hydroxyl terminated butyl nitrile (HTBN) rubber and dispersed with stirring, heat gradually to 60 DEG C and disperse, after being cooled to room temperature, adding silane coupling agent and dispersed with stirring; (4) modified firming agent dispersed with stirring, is added.Beneficial effect of the present invention is: a kind of ungauged regions epoxy grouting material provided by the invention has abandoned the larger furfural-acetone system of toxicity, adopt self-control low-viscosity epoxy resin, add reactive thinner, the efficient material such as toughner and tensio-active agent reduces cure shrinkage, and ensure that lower initial viscosity, reduce harm to human body and environment etc.
Description
Technical field
The present invention relates to a kind of preparation method of material of construction, particularly relate to a kind of ungauged regions epoxy grouting material and preparation method thereof.
Background technology
In recent years, along with expanding economy, the concrete workses such as water conservancy and hydropower, road and bridge and municipal administration get more and more, and this type of buildings generally all requires that foundation has enough intensity, overall homogeneity, good impermeability and weather resistance etc.In actual ground and batholith, be difficult to meet above-mentioned several conditions simultaneously, just must can reach requirement by based process.Grouting is the most frequently used, most effective means.The method of general employing cementation process carries out based process, and this method also can meet the requirement of most of based process.But also there is the shortcomings such as resistance to acid difference, free settling, coarse grain be thicker in cement grouting material, when there is tomography, microscopic checks, chemical mining area in ground and batholith, can because of poor permeability, the requirement and the effect that do not reach based process by reasons such as acidic substance burn into mechanical property are lower.
Existing injection material main component adopts the prepolymer adding a large amount of furfurals, acetone, furfural, acetone on E-51 epoxy resin basis mostly, then adds pnenolic aldehyde amine hardener composition.This type of injection material has that viscosity is low, operable time is long, have the advantages such as certain moist cohesive force, has been applied to some engineerings.But also exist simultaneously cure shrinkage large, be detrimental to health, the shortcoming such as contaminate environment, fragility are large.
Chinese Patent Application No. be 200910040465.9 application discloses a kind of modified furfural and furfuralacetone expoxy resin grouting material, comprising: 1, described modified furfural, is furfural and the product of the aldehyde generation aldol reaction gained containing a-H.2, described modified furfural is prepared by following methods: under catalyzer existent condition, is 1:1 ~ 1:1.4 in molar ratio by furfural and the aldehyde containing a-H, in 20 ~ 40 DEG C of reactions 1 ~ 5 hour.3, described catalyzer is basic catalyst or an acidic catalyst, and the add-on of catalyzer accounts for 0.3% ~ 1% of the aldehyde total mass of furfural and a-H; The described aldehyde containing a-H is propionic aldehyde, butyraldehyde, valeraldehyde, hexanal or enanthaldehyde.4, described basic catalyst comprises sodium hydroxide, potassium hydroxide, hydrated barta or ammoniacal liquor; Described an acidic catalyst comprises (VO)
2p
2o
7, phosphoric acid, a-VOHPO
4or niobic acid.5, a modified furfural acetone epoxide resin grouting material, comprising: thinner, epoxy resin, promotor and solidifying agent.6, the mass ratio of described thinner and epoxy resin is 1:10 ~ 4:5; Described basic catalyst comprises sodium hydroxide, potassium hydroxide, hydrated barta or ammoniacal liquor; Described an acidic catalyst comprises (VO)
2p
2o
7, phosphoric acid, a-VOHPO
4or niobic acid.7, described epoxy resin is bisphenol A-type, bisphenol-f type, dihydroxyphenyl propane D type, bisphenol type tetraglycidel ether epoxy resin, aliphatic glycidyl ether, glycidyl ester or glycidyl amine type epoxy resin.8, described letones is acetone, butanone, pentanone, pimelinketone, isophorone, methyl isopropyl Ketone or methyl iso-butyl ketone (MIBK).9, described solidifying agent is fatty amine, cycloaliphatic amines, aromatic series or polymeric amide.10, described promotor is benzyl trimethyl ammonium chloride, 2,4,6 ,-three (dimethylamino methyl) phenol, benzyl chloride, trolamine, tetramethyl-amine bromide, N, N-dimethyl benzylamine, DMA, N, N-Diethyl Aniline or tetramethyl-thiuram disulfide.
But, still there is insoluble defect in above-mentioned disclosed a kind of modified furfural and furfuralacetone expoxy resin grouting material: the furfural that in conventional epoxy injection material, admixture is a large amount of, acetone or furfural acetone prepolymer, although described furfural, acetone or furfural acetone prepolymer can participate in curable epoxide, but the cure shrinkage of material can be caused very large, fragility increases, not only can cause epoxy grouting material and basement rock, concrete bonding, also the fragility of material can be made to increase, even do not have the effect of reinforcing; Secondly, furfural, acetone or furfural acetone prepolymer all belong to low-molecular(weight)polymer, have very large volatility, are detrimental to health, contaminate environment.
Summary of the invention
The technical problem to be solved in the present invention is the defect overcoming prior art, provides a kind of ungauged regions epoxy grouting material and preparation method thereof, to overcome the deficiencies in the prior art.
In order to solve the problems of the technologies described above, a kind of ungauged regions epoxy grouting material of the present invention and preparation method thereof scheme is as follows:
A kind of ungauged regions epoxy grouting material and preparation method thereof, comprising:
(1), low-viscosity epoxy resin and modified firming agent is prepared;
(2), by low-viscosity epoxy resin, reactive thinner, low-viscosity toughner stirs in proportion until dispersion of materials is even;
(3) add tensio-active agent, in the material and dispersed with stirring, then add Expanding Monomer and hydroxyl terminated butyl nitrile (HTBN) rubber and dispersed with stirring, heat gradually to 60 DEG C and disperse, after being cooled to room temperature, adding silane coupling agent and dispersed with stirring;
(4) modified firming agent dispersed with stirring, is added.
Further, described preparation low-viscosity epoxy resin comprises: take 50gBPA and join and be equipped with in the flask of agitator, take 8gNaOH 50ml distilled water to dissolve, then join in flask, be warmed up to 70 DEG C of-80 DEG C of rapid stirrings, until become amber thick liquid in flask, naturally cool to room temperature after taking out while hot thus make BPA-2Na salt out crystallization; There-necked flask being loaded onto and stirs condensation fractionation plant, get 115g epoxy chloropropane and join in there-necked flask, and add 1.5-2g catalyzer, be warming up to 110 DEG C of azeotropic and stir, when starting there is cut in fractionation plant, starting successively to add BPA-2Na salt.Each add-on 2g; Constantly by the epoxy chloropropane Returning reacting system in cut; Add BPA.2Na salt isothermal reaction half an hour, steam unreacted epoxy chloropropane; After completion of the reaction product is cooled to room temperature, washes, purify, underpressure distillation obtains light yellow clear product, can access low-viscosity epoxy resin.
Further, described preparation modified firming agent comprises: by mphenylenediamine and monocycle epoxy compounds building-up reactions, generates liquid amine affixture, carries out modification with organic acid salt liquid towards amine additives.
Further, described Expanding Monomer is bicyclic lactone class.
Beneficial effect of the present invention is:
1, a kind of ungauged regions epoxy grouting material provided by the invention and preparation method thereof has abandoned the larger furfural-acetone system of toxicity, adopt self-control low-viscosity epoxy resin, add reactive thinner, the efficient material such as toughner and tensio-active agent reduces cure shrinkage, and ensure that lower initial viscosity, reduce harm to human body and environment etc.
2, adopt self-control modified firming agent, hydroxyl terminated butyl nitrile (HTBN) rubber, extend epoxy cure time, reduce epoxy exothermic peak, reduce reaction internal stress, thus deflate cure shrinkage in solidification process, and make cured article have good snappiness.
3, in material system, add Expanding Monomer, utilize its microdilatancy in curable epoxide process to eliminate the micro-contraction in curable epoxide process, shrinkage-free object can be reached.
4, this material not only ungauged regions and environmental protection good toughness again, and meet performance index excellence simultaneously, initial viscosity is low, operable time is long, infiltering property is good, can in the advantage such as moist and solidify under having regimen condition, the groundsill and foundation process of the engineerings such as water conservancy and hydropower, highway bridge, municipal administration and covil construction can be widely used in, play the effect such as reinforcing, antiseepage.
Accompanying drawing explanation
Accompanying drawing is depicted as a kind of ungauged regions epoxy grouting material of the present invention and preparation method thereof schema.
Reference numeral is as follows:
1-prepares low-viscosity epoxy resin and modified firming agent; Low-viscosity epoxy resin, reactive thinner, low-viscosity toughner are stirred to evenly by 2-in proportion; 3-adds tensio-active agent, adds Expanding Monomer and hydroxyl terminated butyl nitrile (HTBN) rubber disperse, adds silane coupling agent and dispersed with stirring; 4-adds modified firming agent dispersed with stirring.
Embodiment
Below in conjunction with Figure of description, the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein is only for instruction and explanation of the present invention, is not intended to limit the present invention.
As shown in the figure, a kind of ungauged regions epoxy grouting material and preparation method thereof, comprises
(1), low-viscosity epoxy resin and modified firming agent 1 is prepared;
(2), low-viscosity epoxy resin, reactive thinner, low-viscosity toughner are stirred to even 2 in proportion;
(3) add tensio-active agent, in the material and dispersed with stirring, then add Expanding Monomer and hydroxyl terminated butyl nitrile (HTBN) rubber and dispersed with stirring, heat gradually to 60 DEG C and disperse, after being cooled to room temperature, adding silane coupling agent and dispersed with stirring.
(4) modified firming agent dispersed with stirring 4, is added.
First by low-viscosity epoxy resin, reactive thinner, low-viscosity toughner adds in encloses container in proportion, 500 turns/min-800 turn/rotating speed of min under carry out dispersion 5-10min, until described low-viscosity epoxy resin, reactive thinner, low-viscosity toughner is uniformly dispersed, described ratio optimal way one is low-viscosity epoxy resin proportion is 100 weight parts, modified firming agent proportion is 45 weight parts, tensio-active agent proportion is 10 weight parts, reactive thinner proportion is 35 weight parts, low-viscosity toughner proportion is 17 weight parts, hydroxyl terminated butyl nitrile (HTBN) rubber proportion is 15 weight parts, Expanding Monomer proportion is 13 weight parts, silane coupling agent proportion is 5 weight parts.Described ratio optimal way two is that low-viscosity epoxy resin proportion is 100 weight parts, modified firming agent proportion is 50 weight parts, tensio-active agent proportion is 12 weight parts, reactive thinner proportion is 33 weight parts, low-viscosity toughner proportion is 15 weight parts, hydroxyl terminated butyl nitrile (HTBN) rubber proportion is 10 weight parts, Expanding Monomer proportion is 11 weight parts, silane coupling agent proportion is 6 weight parts.Described ratio optimal way two is that low-viscosity epoxy resin proportion is 100 weight parts, modified firming agent proportion is 55 weight parts, tensio-active agent proportion is 12 weight parts, reactive thinner proportion is 30 weight parts, low-viscosity toughner proportion is 16 weight parts, hydroxyl terminated butyl nitrile (HTBN) rubber proportion is 15 weight parts, Expanding Monomer proportion is 14 weight parts, silane coupling agent proportion is 7 weight parts.
Tensio-active agent is added with the rotating speed of 500 turns/min dispersion 3-5min in described low-viscosity epoxy resin, reactive thinner, low-viscosity toughner, add Expanding Monomer and hydroxyl terminated butyl nitrile (HTBN) rubber again, to be uniformly dispersed under the rotating speed of 800 turns/min, and heat to 60 DEG C gradually, dispersion 50-60min; Add silane coupling agent after being cooled to room temperature, and disperse 5min under the rotating speed of 500 turns/min.
Preparation low-viscosity epoxy resin comprises: take 50gBPA and join and be equipped with in the flask of agitator, take 8gNaOH 50ml distilled water to dissolve, then join in flask, be warmed up to 70 DEG C of-80 DEG C of rapid stirrings, until become amber thick liquid in flask, naturally cool to room temperature after taking out while hot thus make BPA-2Na salt out crystallization.There-necked flask being loaded onto and stirs condensation fractionation plant, get 115g epoxy chloropropane and join in there-necked flask, and add 1.5-2g catalyzer, be warming up to 110 DEG C of azeotropic and stir, when starting there is cut in fractionation plant, starting successively to add BPA-2Na salt.Each add-on 2g.Constantly by the epoxy chloropropane Returning reacting system in cut; Add BPA.2Na salt isothermal reaction half an hour, steam unreacted epoxy chloropropane; After completion of the reaction product is cooled to room temperature, washes, purify, underpressure distillation obtains light yellow clear product, can access low-viscosity epoxy resin.
Described solidifying agent is modification mphenylenediamine solidifying agent.The method of modifying of modification mphenylenediamine is: by mphenylenediamine and monocycle epoxy compounds building-up reactions, generates liquid amine affixture; Carry out modification with organic acid salt again, make it between macromole, form metal ion-chelant key bridge crosslinking structure, and introduce benzyl alcohol group on main chain, these modifications to reduce curable epoxide contraction, improve cured article toughness there is unusual effect.And its reaction times is longer, curing reaction is hot low, injection material can be mixed and stirred in a large number and do not occur sudden and violent poly-.
Described Expanding Monomer is bicyclic lactone class.In curable epoxide process, bicyclic lactone can participate in reaction, and generates linear structure by ring texture, produces volumetric expansion, offsets the contraction of material further.
Described reactive thinner is specially Isosorbide-5-Nitrae butanediol diglycidyl ether, neopentylglycol diglycidyl ether or butyl and shrinks certain oily ether.
Described liquid acrylonitrile butadiene rubber is specially terminal hydroxy group low-molecular-weight liquid paracril.
The present invention is not limited to above-mentioned embodiment, and when not deviating from flesh and blood of the present invention, any distortion that it may occur to persons skilled in the art that, improvement, replacement all fall into the protection domain that claim of the present invention is recorded.
Claims (2)
1. a preparation method for ungauged regions epoxy grouting material, is characterized in that, described material and preparation method thereof comprises:
(1), low-viscosity epoxy resin and modified firming agent is prepared;
(2), by low-viscosity epoxy resin, reactive thinner, low-viscosity toughner stirs in proportion until dispersion of materials is even;
(3) add tensio-active agent, in the material and dispersed with stirring, then add Expanding Monomer and hydroxyl terminated butyl nitrile (HTBN) rubber and dispersed with stirring, heat gradually to 60 DEG C and disperse, after being cooled to room temperature, adding silane coupling agent and dispersed with stirring;
(4) modified firming agent dispersed with stirring, is added;
Described preparation low-viscosity epoxy resin comprises: take 50gBPA and join and be equipped with in the flask of agitator, take 8gNaOH 50ml distilled water to dissolve, then join in flask, be warmed up to 70 DEG C of-80 DEG C of rapid stirrings, until become amber thick liquid in flask, naturally cool to room temperature after taking out while hot thus make BPA-2Na salt out crystallization; There-necked flask being loaded onto and stirs condensation fractionation plant, get 115g epoxy chloropropane and join in there-necked flask, and add 1.5-2g catalyzer, be warming up to 110 DEG C of azeotropic and stir, when starting there is cut in fractionation plant, starting successively to add BPA-2Na salt; Each add-on 2g, constantly by the epoxy chloropropane Returning reacting system in cut; Add BPA-2Na salt isothermal reaction half an hour, steam unreacted epoxy chloropropane; After completion of the reaction product is cooled to room temperature, washes, purify, underpressure distillation obtains light yellow clear product, can access low-viscosity epoxy resin;
Described preparation modified firming agent comprises: by mphenylenediamine and monocycle epoxy compounds building-up reactions, generates liquid amine affixture, carries out modification with organic acid salt liquid towards amine additives.
2. the preparation method of a kind of ungauged regions epoxy grouting material according to claim 1, is characterized in that, described Expanding Monomer is bicyclic lactone class.
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