CN113528067A - Stone joint sealant and preparation method thereof - Google Patents
Stone joint sealant and preparation method thereof Download PDFInfo
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- CN113528067A CN113528067A CN202110906284.0A CN202110906284A CN113528067A CN 113528067 A CN113528067 A CN 113528067A CN 202110906284 A CN202110906284 A CN 202110906284A CN 113528067 A CN113528067 A CN 113528067A
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- 239000004575 stone Substances 0.000 title claims abstract description 76
- 239000000565 sealant Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 39
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 124
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 121
- 229920005989 resin Polymers 0.000 claims abstract description 97
- 239000011347 resin Substances 0.000 claims abstract description 97
- 150000001412 amines Chemical class 0.000 claims abstract description 71
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 50
- 229920000570 polyether Polymers 0.000 claims abstract description 50
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 47
- 230000001070 adhesive effect Effects 0.000 claims abstract description 46
- 239000000853 adhesive Substances 0.000 claims abstract description 43
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims abstract description 9
- -1 tungsten nitride Chemical class 0.000 claims description 74
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 70
- 239000003822 epoxy resin Substances 0.000 claims description 59
- 229920000647 polyepoxide Polymers 0.000 claims description 59
- 238000003756 stirring Methods 0.000 claims description 56
- 239000006229 carbon black Substances 0.000 claims description 44
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 claims description 42
- 238000009775 high-speed stirring Methods 0.000 claims description 40
- 238000002156 mixing Methods 0.000 claims description 39
- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 claims description 36
- 239000000463 material Substances 0.000 claims description 30
- 150000004985 diamines Chemical class 0.000 claims description 28
- 229920001451 polypropylene glycol Polymers 0.000 claims description 28
- 229910021485 fumed silica Inorganic materials 0.000 claims description 24
- 239000013008 thixotropic agent Substances 0.000 claims description 24
- 239000002245 particle Substances 0.000 claims description 23
- 229910052721 tungsten Inorganic materials 0.000 claims description 23
- 239000010937 tungsten Substances 0.000 claims description 23
- 239000003085 diluting agent Substances 0.000 claims description 20
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 19
- 239000012024 dehydrating agents Substances 0.000 claims description 18
- SYEWHONLFGZGLK-UHFFFAOYSA-N 2-[1,3-bis(oxiran-2-ylmethoxy)propan-2-yloxymethyl]oxirane Chemical compound C1OC1COCC(OCC1OC1)COCC1CO1 SYEWHONLFGZGLK-UHFFFAOYSA-N 0.000 claims description 15
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 14
- 235000019445 benzyl alcohol Nutrition 0.000 claims description 14
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 14
- 239000004359 castor oil Substances 0.000 claims description 13
- 235000019438 castor oil Nutrition 0.000 claims description 13
- GCSJLQSCSDMKTP-UHFFFAOYSA-N ethenyl(trimethyl)silane Chemical group C[Si](C)(C)C=C GCSJLQSCSDMKTP-UHFFFAOYSA-N 0.000 claims description 13
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 13
- 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 claims description 12
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 claims description 12
- CYCBPQPFMHUATH-UHFFFAOYSA-N 4-(oxiran-2-ylmethoxy)butan-1-ol Chemical compound OCCCCOCC1CO1 CYCBPQPFMHUATH-UHFFFAOYSA-N 0.000 claims description 11
- 239000003292 glue Substances 0.000 claims description 11
- 150000001875 compounds Chemical class 0.000 claims description 9
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 7
- UWFRVQVNYNPBEF-UHFFFAOYSA-N 1-(2,4-dimethylphenyl)propan-1-one Chemical compound CCC(=O)C1=CC=C(C)C=C1C UWFRVQVNYNPBEF-UHFFFAOYSA-N 0.000 claims description 7
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 7
- UXMYUFHUUYBDLL-UHFFFAOYSA-N 2,2-dimethyl-3-(oxiran-2-ylmethoxy)propan-1-ol Chemical compound OCC(C)(C)COCC1CO1 UXMYUFHUUYBDLL-UHFFFAOYSA-N 0.000 claims description 7
- YSUQLAYJZDEMOT-UHFFFAOYSA-N 2-(butoxymethyl)oxirane Chemical compound CCCCOCC1CO1 YSUQLAYJZDEMOT-UHFFFAOYSA-N 0.000 claims description 7
- QNYBOILAKBSWFG-UHFFFAOYSA-N 2-(phenylmethoxymethyl)oxirane Chemical compound C1OC1COCC1=CC=CC=C1 QNYBOILAKBSWFG-UHFFFAOYSA-N 0.000 claims description 7
- WNISWKAEAPQCJQ-UHFFFAOYSA-N 2-[(2-nonylphenoxy)methyl]oxirane Chemical compound CCCCCCCCCC1=CC=CC=C1OCC1OC1 WNISWKAEAPQCJQ-UHFFFAOYSA-N 0.000 claims description 7
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 7
- QNAYBMKLOCPYGJ-REOHCLBHSA-N L-alanine Chemical compound C[C@H](N)C(O)=O QNAYBMKLOCPYGJ-REOHCLBHSA-N 0.000 claims description 7
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 7
- FDLQZKYLHJJBHD-UHFFFAOYSA-N [3-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=CC(CN)=C1 FDLQZKYLHJJBHD-UHFFFAOYSA-N 0.000 claims description 7
- 235000004279 alanine Nutrition 0.000 claims description 7
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 claims description 7
- 229960001124 trientine Drugs 0.000 claims description 7
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical compound C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000440 bentonite Substances 0.000 claims description 6
- 229910000278 bentonite Inorganic materials 0.000 claims description 6
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 6
- 239000001913 cellulose Substances 0.000 claims description 6
- 229920002678 cellulose Polymers 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 239000007822 coupling agent Substances 0.000 claims description 5
- 230000004048 modification Effects 0.000 claims description 5
- 238000012986 modification Methods 0.000 claims description 5
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 4
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims description 3
- OBETXYAYXDNJHR-SSDOTTSWSA-M (2r)-2-ethylhexanoate Chemical class CCCC[C@@H](CC)C([O-])=O OBETXYAYXDNJHR-SSDOTTSWSA-M 0.000 claims 2
- 238000010438 heat treatment Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 8
- 238000005336 cracking Methods 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 abstract 1
- 230000007547 defect Effects 0.000 description 6
- 239000000835 fiber Substances 0.000 description 6
- 238000004513 sizing Methods 0.000 description 6
- OBETXYAYXDNJHR-UHFFFAOYSA-N 2-Ethylhexanoic acid Chemical class CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 description 5
- 230000032683 aging Effects 0.000 description 5
- 229920006332 epoxy adhesive Polymers 0.000 description 5
- 239000004579 marble Substances 0.000 description 5
- 230000035882 stress Effects 0.000 description 5
- 238000010276 construction Methods 0.000 description 4
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 4
- 239000003607 modifier Substances 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- OQILSTRGJVCFAG-UHFFFAOYSA-N 1-(oxiran-2-ylmethoxy)butan-1-ol Chemical compound CCCC(O)OCC1CO1 OQILSTRGJVCFAG-UHFFFAOYSA-N 0.000 description 3
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical group C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- 125000003700 epoxy group Chemical group 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229920002050 silicone resin Polymers 0.000 description 3
- 229920006305 unsaturated polyester Polymers 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 125000001153 fluoro group Chemical group F* 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920002647 polyamide Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 239000012945 sealing adhesive Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000009931 harmful effect Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 208000032839 leukemia Diseases 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/504—Amines containing an atom other than nitrogen belonging to the amine group, carbon and hydrogen
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Sealing Material Composition (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a stone crack-filling adhesive and a preparation method thereof, the stone crack-filling adhesive adopts a mixed curing agent consisting of a polyether amine modified curing agent and an aliphatic amine modified curing agent, has excellent adhesion and a certain stress relaxation function, and improves the dispersion effect of calcium carbonate in resin by modifying the calcium carbonate, thereby greatly improving the adhesion property of the stone crack-filling adhesive. The preparation method and operation of the stone joint sealant are relatively simple and convenient, the raw material utilization rate is high, the joint sealant has good fluidity, the bonding strength to the stone joint is high after curing, and the secondary cracking in the later period can be effectively avoided.
Description
Technical Field
The invention relates to a stone adhesive, in particular to a stone crack sealing adhesive and a preparation method thereof, and belongs to the technical field of building material adhesion.
Background
The natural stone slab has elegant texture and unique and beautiful texture, and is often used as a facing material for inner and outer walls, floors, ceilings, windowsills, table tops and sanitary wares of buildings. With the development of economy, the living standard of people is improved and the culture is improved, and the quantity of the decorative materials is increased. With the wide application of stone in the construction industry, the market demand of the stone bonding adhesive is continuously expanded, which is particularly embodied in the bonding and reinforcing operation of repairing, installing and positioning the stone, and the bonding and reinforcing material for repairing, installing and positioning the stone at the present stage mainly adopts unsaturated polyester adhesive (marble adhesive); it has a lot of not enoughly when the location of stone material is consolidated, if: the volatilization is serious, the volatile matter is toxic, the unsaturated polyester adhesive contains 20-30% of styrene monomer, and is volatile at room temperature, the styrene has larger toxicity and irritation, the industrial sanitation and labor protection are influenced, and the leukemia can be caused by long-term contact; the shrinkage rate is large, and large stress is generated by curing shrinkage; high brittleness, poor ageing resistance and the like. After the epoxy adhesive is cured, the epoxy adhesive has excellent adhesiveness and mechanical strength, excellent aging resistance, environmental protection, small shrinkage rate and good toughness after modification, accelerates the curing speed on the basis of common epoxy adhesive, can completely replace unsaturated polyester adhesive (marble adhesive), and meets the requirement of quick positioning and bonding of stone dry hanging in the building industry.
The stone is difficult to be jointed strictly after being paved, the fracture condition also happens occasionally, if the gaps are not filled up, the following problems can occur in daily use: first, the gaps become locations where dust, water, and other various contaminants are retained, and the stone is eroded for a long time, which may cause contamination of the slab. Blackening and mildewing along the gap; secondly, various water and pollutants remained in the gaps can become places for breeding bacteria, and the harmful effects on the health of people can be caused for a long time; and thirdly, the structure is not integrated, and the strength is low. In daily use, the problems of loosening and warping of the plate and the like are easily caused under the action of external force. On the other hand, the adhesion of the sheet material is also rapidly reduced by the erosion of water and contaminants in the gaps. The existing gap-filling products on the market at present have two kinds: one is hard caulking glue (also called marble glue in the market) and the other is soft caulking glue (also called flexible joint mixture). However, the existing hard joint sealing glue has the defect of poor flexibility, when the stone with a large expansion coefficient is heated to linearly expand under a high-temperature condition, the hard joint sealing glue is not flexible, so that the stone is subjected to strong shearing force of an adhesive layer, the direction of the force is focused from the periphery of the plate to the central position, and the problem that the inner part of the plate is arched or even cracked can be caused. The marble glue is extruded by the stone, once the temperature is reduced, the stone shrinks, the original extruded place can be slowly restored to the original state, and the marble glue without flexibility is repeatedly extruded and stretched, so that the problems of cracking, arching and falling off can be caused. The soft crack-repairing glue has the defects of poor polishability and low strength; when the color matching and polishing treatment is required to be carried out on the joint sealing glue, the existing flexible joint sealing agent is almost completely polished and does not have luster.
The epoxy resin contains various polar groups and epoxy groups with high activity, so that the epoxy resin has high adhesive force with materials with high surface activity, and the epoxy cured material has high cohesive strength, so that the adhesive strength is high, the curing shrinkage is small, the size stability of the cured product is good, the hardness of the cured product is high, and the polishing processing is easy. Therefore, in the stone processing industry at present, the adhesive prepared by taking the epoxy resin as the raw material gradually occupies the leading position of the market.
Although the epoxy resin material is widely used, the epoxy resin material has a plurality of defects when used as a stone adhesive, and the stone adhesive has relatively small adhesive area in the repairing, installing and positioning processes, so that the adhesive is relatively large in stress, and the performance requirements on the adhesive are high, especially the adhesive strength, stability, wear resistance, stain resistance and the like of the adhesive.
Disclosure of Invention
The invention provides a stone joint sealant which is good in fluidity and low in shrinkage rate, and simultaneously adopts two modified curing agent compositions, so that the stone joint sealant has excellent adhesion and a certain stress relieving function. The stone crack filling adhesive also adopts the modified calcium carbonate, on one hand, the appearance of the cured adhesive material is as close as possible to that of the stone material, the stone material is beneficial to polishing, the bonding strength, the wear resistance, the aging resistance, the stain resistance and other properties of the stone crack filling adhesive can be enhanced, and further, the hardness and the strength of the cured adhesive material can be greatly improved by adding the tungsten nitride fiber. The preparation method and operation of the stone crack sealant are relatively simple and convenient, the material utilization rate is high, the stone crack sealant has high strength after being fixed, and secondary cracking in the later period can be effectively avoided.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
according to a first embodiment of the present invention, a stone caulking compound is provided.
The utility model provides a stone material joint sealant, this joint sealant includes A component and B component, and wherein A component includes:
the epoxy resin is 30 to 60 parts by weight, preferably 35 to 55 parts by weight, and more preferably 40 to 50 parts by weight.
The MS resin is 5 to 18 parts by weight, preferably 7 to 15 parts by weight, and more preferably 9 to 13 parts by weight.
The reactive diluent is 1 to 8 parts by weight, preferably 2 to 7 parts by weight, and more preferably 3 to 6 parts by weight.
15 to 35 parts by weight, preferably 18 to 31 parts by weight, more preferably 20 to 28 parts by weight of calcium carbonate.
The thixotropic agent is 1 to 6 parts by weight, preferably 1.5 to 5.5 parts by weight, and more preferably 2 to 5 parts by weight.
0.5 to 5 parts by weight of a dehydrating agent, preferably 0.8 to 4 parts by weight, more preferably 1 to 3.5 parts by weight.
1-8 parts of white carbon black, preferably 2-7 parts of white carbon black, and more preferably 2.5-6 parts of white carbon black.
Wherein the component B comprises:
20-45 parts by weight of MQ resin, preferably 25-40 parts by weight, more preferably 30-35 parts by weight.
The modified curing agent is 18 to 40 parts by weight, preferably 20 to 35 parts by weight, and more preferably 25 to 30 parts by weight.
1 to 7 parts by weight of accelerator, preferably 2 to 6 parts by weight, more preferably 3 to 5 parts by weight.
1 to 9 parts by weight, preferably 2 to 8 parts by weight, and more preferably 2.5 to 7 parts by weight of a silane coupling agent.
0.5-5 parts by weight of white carbon black, preferably 1-4 parts by weight, more preferably 1.5-3 parts by weight.
0.5 to 4 parts by weight, preferably 0.8 to 3.5 parts by weight, and more preferably 1 to 3 parts by weight of tungsten nitride.
Calcium carbonate 12 to 30 parts by weight, preferably 15 to 26 parts by weight, more preferably 18 to 24 parts by weight.
Wherein the modified curing agent is a mixture of polyether amine modified curing agent and fatty amine modified curing agent.
The sum of the components in the component A is 100 parts by weight. The sum of the components in the component B is 100 parts by weight.
Preferably, the epoxy resin is selected from one or more of bisphenol A type, bisphenol F type and bisphenol S type epoxy resins. E-51 epoxy resin is preferred.
Preferably, the MS resin is S203H resin and/or S227 resin, and is preferably mixed resin of S203H resin and S227 resin in a mass ratio of 1: 0.5-3.
Preferably, the polyether amine modified curing agent is a polyether amine modified curing agent obtained by modifying polyoxypropylene diamine and/or polyoxyethylene diamine and/or polyoxypropylene triamine with an epoxy resin. Preferably, the curing agent is a polyether amine modified curing agent obtained by modifying polyoxypropylene diamine and/or polyoxyethylene diamine and/or polyoxypropylene triamine with an E-51 epoxy resin and then further treating the modified curing agent with benzyl alcohol.
Preferably, the aliphatic amine modified curing agent is one or more of diethylenetriamine, triethylene tetramine, tetraethylene pentamine and m-xylene diamine modified by nonylphenol glycidyl ether.
Preferably, the amount of benzyl alcohol is 1 to 8 wt%, preferably 2 to 6 wt%, based on the total mass of the polyetheramine-modified curing agent.
Preferably, in the mixed modified curing agent consisting of the polyether amine modified curing agent and the fatty amine modified curing agent, the mass ratio of the polyether amine modified curing agent to the fatty amine modified curing agent is 1:0.5-3, and preferably 1: 0.8-2.
Preferably, the reactive diluent is one or more selected from C12-C14 alkyl glycidyl ether, benzyl glycidyl ether, butyl glycidyl ether, glycerol triglycidyl ether, 1,4 butanediol glycidyl ether, ethylene glycol diglycidyl ether and neopentyl glycol glycidyl ether. Preferably glycerol triglycidyl ether and/or 1, 4-butanediol glycidyl ether.
Preferably, the thixotropic agent is one or more of hydrogenated castor oil, cellulose and bentonite.
Preferably, the dehydrating agent is vinyltrimethylsilane.
Preferably, the calcium carbonate has a particle size composition of: 10-30% of particle size less than 100 meshes, 25-55% of particle size 100-200 meshes, 18-35% of particle size 300-500 meshes and 12-28% of particle size more than 500 meshes.
Preferably, the calcium carbonate is modified calcium carbonate obtained after modification treatment with alanine and/or trifluoro-2-alanine.
Preferably, the ratio of M units to Q units in the MQ resin is from 0.3 to 1.8, preferably from 0.5 to 1.5.
Preferably, the accelerator is selected from one or more of 2,4, 6-tris (dimethylaminomethyl) phenol (DMP-30), tris- (2-ethylhexanoate) salt of 2,4, 6-tris (dimethylaminomethyl) phenol, triethanolamine, thiourea. 2,4, 6-tris (dimethylaminomethyl) phenol (DMP-30) is preferred.
Preferably, the white carbon black is fumed silica.
Preferably, the silane coupling agent is a dialkoxysilane or trialkoxysilane coupling agent containing an amino or hydroxyl functional group. Preferably one or more of gamma-aminopropyltriethoxysilane (KH-550), 3- (2, 3-glycidoxy) propyltrimethoxysilane (KH-560) and diethylenetriaminopropyltriethoxysilane.
According to a second embodiment of the present invention, there is provided a method for preparing a stone caulking compound or a method for preparing the stone caulking compound according to the first embodiment.
A method for preparing stone crack filling adhesive comprises the following steps:
s1: preparation of the component A: firstly, mixing epoxy resin, MS resin, reactive diluent and white carbon black. Then adding calcium carbonate, thixotropic agent and dehydrating agent, continuously mixing, and uniformly mixing to obtain the component A.
S2: preparation of the component B: firstly, mixing MQ resin, a modified curing agent and an accelerant. Then adding the thixotropic agent and the silane coupling agent and continuously mixing uniformly. And finally, adding calcium carbonate, tungsten nitride and white carbon black, and continuously mixing to obtain the component B.
S3: preparing the two-component stone joint sealant: and bottling the component A and the component B according to the proportion to obtain the two-component stone crack filling adhesive.
Wherein the modified curing agent is a mixed modified curing agent consisting of polyether amine modified curing agent and fatty amine modified curing agent according to the mass ratio of 1:0.5-3 (preferably 1: 0.8-2). The calcium carbonate is modified calcium carbonate obtained by modifying calcium carbonate by adopting alanine and/or trifluoro-2-alanine.
Preferably, the amounts of the components are as follows: wherein the component A is as follows:
the epoxy resin is 30 to 60 parts by weight, preferably 35 to 55 parts by weight, and more preferably 40 to 50 parts by weight.
The MS resin is 5 to 18 parts by weight, preferably 7 to 15 parts by weight, and more preferably 9 to 13 parts by weight.
The reactive diluent is 1 to 8 parts by weight, preferably 2 to 7 parts by weight, and more preferably 3 to 6 parts by weight.
15 to 35 parts by weight, preferably 18 to 31 parts by weight, more preferably 20 to 28 parts by weight of calcium carbonate.
The thixotropic agent is 1 to 6 parts by weight, preferably 1.5 to 5.5 parts by weight, and more preferably 2 to 5 parts by weight.
0.5 to 5 parts by weight of a dehydrating agent, preferably 0.8 to 4 parts by weight, more preferably 1 to 3.5 parts by weight.
1-8 parts of white carbon black, preferably 2-7 parts of white carbon black, and more preferably 2.5-6 parts of white carbon black.
Wherein the component B is as follows:
20-45 parts by weight of MQ resin, preferably 25-40 parts by weight, more preferably 30-35 parts by weight.
The modified curing agent is 18 to 40 parts by weight, preferably 20 to 35 parts by weight, and more preferably 25 to 30 parts by weight.
1 to 7 parts by weight of accelerator, preferably 2 to 6 parts by weight, more preferably 3 to 5 parts by weight.
1 to 9 parts by weight, preferably 2 to 8 parts by weight, and more preferably 2.5 to 7 parts by weight of a silane coupling agent.
0.5-5 parts by weight of white carbon black, preferably 1-4 parts by weight, more preferably 1.5-3 parts by weight.
0.5 to 4 parts by weight, preferably 0.8 to 3.5 parts by weight, and more preferably 1 to 3 parts by weight of tungsten nitride.
Calcium carbonate 12 to 30 parts by weight, preferably 15 to 26 parts by weight, more preferably 18 to 24 parts by weight.
Preferably, the MS resin is S203H resin and/or S227 resin, and is preferably mixed resin of S203H resin and S227 resin in a mass ratio of 1: 0.5-3.
Preferably, the epoxy resin is selected from one or more of bisphenol A type, bisphenol F type and bisphenol S type epoxy resins. E-51 epoxy resin is preferred.
Preferably, the polyether amine modified curing agent is a polyether amine modified curing agent obtained by modifying polyoxypropylene diamine and/or polyoxyethylene diamine and/or polyoxypropylene triamine with an epoxy resin. Preferably, the curing agent is a polyether amine modified curing agent obtained by modifying polyoxypropylene diamine and/or polyoxyethylene diamine and/or polyoxypropylene triamine with an E-51 epoxy resin and then further treating the modified curing agent with benzyl alcohol. The aliphatic amine modified curing agent is one or more of diethylenetriamine, triethylene tetramine, tetraethylene pentamine and m-xylene diamine which are modified by nonyl phenol glycidyl ether. Preferably, the amount of benzyl alcohol is 1 to 8 wt%, preferably 2 to 6 wt%, based on the total mass of the polyetheramine-modified curing agent.
Preferably, the reactive diluent is one or more selected from C12-C14 alkyl glycidyl ether, benzyl glycidyl ether, butyl glycidyl ether, glycerol triglycidyl ether, 1,4 butanediol glycidyl ether, ethylene glycol diglycidyl ether and neopentyl glycol glycidyl ether.
Preferably, the ratio of M units to Q units in the MQ resin is from 0.3 to 1.8, preferably from 0.5 to 1.5.
Preferably, the accelerator is selected from one or more of 2,4, 6-tris (dimethylaminomethyl) phenol (DMP-30), tris- (2-ethylhexanoate) salt of 2,4, 6-tris (dimethylaminomethyl) phenol, triethanolamine, thiourea.
Preferably, the white carbon black is fumed silica.
Preferably, the silane coupling agent is one or more of gamma-aminopropyltriethoxysilane (KH-550), 3- (2, 3-glycidoxy) propyltrimethoxysilane (KH-560), and diethylenetriaminopropyltriethoxysilane.
Preferably, the thixotropic agent is one or more of hydrogenated castor oil, cellulose and bentonite.
Preferably, the dehydrating agent is vinyltrimethylsilane.
Preferably, S1 is specifically: preparation of the component A: the epoxy resin, the MS resin, the reactive diluent and the fumed silica are uniformly mixed under the condition of raising the temperature (for example, the mixture is uniformly stirred at 50-95 ℃, preferably 60-80 ℃). Then starting high-speed stirring and vacuumizing (for example, vacuumizing to-0.01 MPa to-0.09 MPa), wherein the high-speed stirring time is 10-60 min. And finally, adding calcium carbonate, a thixotropic agent and a dehydrating agent, continuously stirring for 10-40min, cooling, stopping stirring for 30min, and then stopping vacuumizing to obtain the component A.
Preferably, S2 is specifically: preparation of the component B: firstly, mixing the MQ resin and the modified curing agent uniformly according to the proportion, then adding the accelerant and continuously mixing uniformly (for example, stirring and mixing for 10-60 min). Then adding the thixotropic agent and the silane coupling agent and mixing uniformly (for example, stirring and mixing). After a period of time, high-speed stirring is started and vacuum is pumped (for example, the vacuum pumping is from-0.01 MPa to-0.09 MPa), and the high-speed stirring time is 10-60 min. And finally, adding calcium carbonate, tungsten carbide and gas-phase white carbon black, continuously stirring (stirring for 10-40min), cooling, stopping stirring for 30min, and stopping vacuumizing to obtain the component B.
Preferably, S3 is specifically: preparing the two-component stone joint sealant: and respectively bottling the component A and the component B according to the mass ratio of 1:1.0-1.5 (preferably 1:1.1-1.3) to obtain the two-component stone crack filling adhesive.
In the invention, the modified curing agent is a mixture of polyether amine modified curing agent and fatty amine modified curing agent. The polyether amine modified curing agent is self-made and is prepared by modifying polyoxypropylene diamine and/or polyoxyethylene diamine and/or polyoxypropylene triamine with E-51 epoxy resin. Preferably, the polyether amine modified curing agent is a curing agent obtained by modifying polyoxypropylene diamine and/or polyoxyethylene diamine and/or polyoxypropylene triamine with E-51 epoxy resin to obtain the polyether amine modified curing agent, and then treating the polyether amine modified curing agent with benzyl alcohol. Still preferably, the amount of the benzyl alcohol is 1 to 8 wt%, preferably 2 to 6 wt%, based on the total mass of the polyetheramine-modified curing agent. The aliphatic amine modified curing agent is also self-made, and refers to the aliphatic amine modified curing agent which is prepared by modifying one or more of diethylenetriamine, triethylene tetramine, tetraethylene pentamine and m-xylene diamine by using nonyl phenol glycidyl ether. Through modification of the polyether amine, the defects of low hardness, small adhesion, poor moisture resistance, long curing time and the like of the polyether amine are overcome; the defects of high normal-temperature volatility, high toxicity and the like of aliphatic amines are overcome by modifying the aliphatic amines; meanwhile, the polyether amine modified curing agent and the fatty amine modified curing agent are compounded according to a certain proportion (for example, the mass ratio of the polyether amine modified curing agent to the fatty amine modified curing agent is 1:0.5-3, preferably 1:0.8-2), so that excellent complementation can be realized, the bonding strength, the tensile strength, the shear strength and the bending strength of the epoxy cured product are greatly improved, the high temperature resistance, the corrosion resistance, the wear resistance and the like are greatly improved, the maximum elongation is improved, the flexibility is good, and the later-stage secondary cracking and stripping can be effectively avoided.
According to the invention, the epoxy resin and the MS resin are adopted as the main bodies of the joint sealant, the deformation and deformation recovery capability of the rubber material is improved by the addition of the MS resin, and the joint sealant can be used in combination with the modified calcium carbonate, so that the modulus of the joint sealant is increased, the elongation at break is reduced, and the elastic recovery rate is reduced.
In the present invention, the reactive diluent is or includes one or more selected from C12-C14 alkyl glycidyl ether, benzyl glycidyl ether, butyl glycidyl ether, glycerol triglycidyl ether, 1,4 butanediol glycidyl ether, ethylene glycol diglycidyl ether, and neopentyl glycol glycidyl ether, and preferably one or two selected from glycerol triglycidyl ether and 1,4 butanediol glycidyl ether are used. The reactive diluent can improve the consistency and optimize the construction performance.
In the present invention, the silane coupling agent is a dialkoxysilane-based or trialkoxysilane-based coupling agent containing an amino or hydroxyl functional group. Preferably one or more of gamma-aminopropyltriethoxysilane (KH-550), 3- (2, 3-glycidoxy) propyltrimethoxysilane (KH-560) and diethylenetriaminopropyltriethoxysilane. The coupling agent can increase the adhesive property.
In the present invention, the accelerator is selected from one or more of 2,4, 6-tris (dimethylaminomethyl) phenol (DMP-30), tris- (2-ethylhexanoate) salt of 2,4, 6-tris (dimethylaminomethyl) phenol, triethanolamine, thiourea. 2,4, 6-tris (dimethylaminomethyl) phenol (DMP-30) is preferred. The accelerator can accelerate the reaction speed.
In the present invention, the calcium carbonate is modified calcium carbonate. The grain size composition is as follows: 10-30% of particle size less than 100 meshes, 25-55% of particle size 100-200 meshes, 18-35% of particle size 300-500 meshes and 12-28% of particle size more than 500 meshes. Generally, when calcium carbonate is directly used as a filler, the particle size is small, the surface energy is high, the thermodynamic property is unstable, and the particles are easy to agglomerate to influence the filling effect, so that alanine and/or trifluoro-2-alanine containing both amino and carboxyl is used as a modifier to modify the calcium carbonate to obtain modified calcium carbonate; on one hand, the modified calcium carbonate is in composite bonding with special groups (such as carboxyl) contained in the modifier, so that the van der Waals force among calcium carbonate particles can be effectively reduced, the agglomeration phenomenon among the calcium carbonate particles is avoided, and the dispersibility of the modified calcium carbonate is improved; on the other hand, the calcium carbonate is bonded on the epoxy group through the special group (such as amino group) contained in the modifier and the epoxy resin, so that the adhesive property and the adhesive strength of the epoxy adhesive are greatly improved. When the trifluoro-2-alanine is used as the modifier, the trifluoro-2-alanine is not only used as a bonding bridge between the filler and the resin, but also can be regarded as a side chain group on the main chain of the resin after being connected with an epoxy group of the resin through a chemical bond because the fluoro group is contained, and the epoxy adhesive has better weather resistance, cold resistance, high temperature resistance and corrosion resistance, higher thermal stability and surface self-cleaning performance because the carbon-fluoro bond has short length and large bond energy. The modified calcium carbonate is used as the filler, so that the mechanical strength of the colloid can be increased, the curing shrinkage is reduced, the thermal expansion coefficient of a cured material is reduced, and the sensitivity of the rubber material to high and low temperature changes is reduced, so that the internal stress is reduced, and secondary cracking is avoided.
In the present invention, MQ resins are used with a ratio of M units to Q units of 0.3 to 1.8, preferably MQ silicone resins with a ratio of M units to Q units of preferably 0.5 to 1.5 (e.g., ratios of 0.55, 0.6, 0.65, 0.7, 0.75, 0.8, 0.85, 0.9, 0.95, 1.0, 1.2, 1.4, etc.) may be selected. Therefore, the elasticity and resilience of the silica gel can be improved, and the permanent deformation can be reduced. It should be noted that, in the preferred embodiment of the present disclosure, the MQ silicone resin is preferably a vinyl MQ silicone resin, wherein the vinyl content is 2.5 to 5 wt%, if the content is too high, the hardness of the product is large, and if the content is too low, the effect of centralized crosslinking cannot be achieved, and the improvement on the product performance is not obvious. Meanwhile, the addition of the MQ resin improves the fluidity of the rubber material, and the rubber material has moderate fluidity when being matched with the hydrophobic fumed silica, so that the filling requirement of small cracks can be met, and the filling requirement of large cracks can be met. Furthermore, in order to better adapt to actual requirements, the targeted size of the crack can be matched (fine-tuned) through flexibly controlling the proportion of the component B and the component C in the field application process, and then the targeted filling and sealing operation can be carried out on the cracks with different sizes, and the overall hardness, the fatigue damage resistance, the water resistance, the wear resistance, the aging resistance, the stain resistance and other properties of the rubber compound cannot be influenced. Furthermore, the addition of the MQ resin greatly improves the fluidity of the joint sealant, and has excellent reinforcing joint sealant effects on thin joints, long joints, irregular long and thin joints and the like of the stone.
In the invention, the tungsten nitride is a tungsten nitride fiber which is mainly used for improving the tear resistance and the hardness of the silica gel, and the tungsten nitride fiber with the length of 10-50 microns is generally adopted. In the process of crosslinking and curing the sizing material, the tungsten nitride fibers are inserted into the hard framework, so that after the sizing material is cured, the hardness and strength of the cured sizing material can be greatly improved, and the curing rate and the crosslinking degree of the sizing material cannot be influenced. By adopting the tungsten nitride fiber, a multi-layer three-dimensional framework can be formed in the sizing material, and the thermal stability of the cured sizing material can be further improved. The length of the tungsten nitride fiber is not too long or too short, the too short length can cause the hardness and strength of the adhesive to be insufficient, the thermal stability is poor, and the too long length can cause the interface of the adhesive to be rough, thereby affecting the adhesive property of the adhesive.
Compared with the prior art, the invention has the following beneficial technical effects:
1. the crack sealant disclosed by the invention is prepared by compounding the epoxy resin and the MS resin, so that the deformation and deformation recovery capability of a rubber material are greatly improved, and the crack sealant is matched with modified calcium carbonate for use, so that the modulus of the crack sealant is increased, the elongation at break is reduced, and the elastic recovery rate is reduced.
2. The self-made polyether amine modified curing agent is matched with the polyamide curing agent for use, so that the defect of a single curing agent is overcome, the self-made polyether amine modified curing agent and the polyamide curing agent are complementary and mutually assisted, and the self-made polyether amine modified curing agent has high strength, high maximum elongation and good flexibility; the prepared crack-repairing glue has excellent adhesion and a certain stress relaxation function. The preparation method and operation of the joint sealant are relatively simple and convenient, the material utilization rate is high, the stone gap has higher strength after being repaired by the joint sealant, and the secondary cracking in the later period can be effectively avoided.
3. According to the invention, the modified calcium carbonate and the hydrophobic fumed silica are matched for use, so that the paste property of the joint sealant is ensured, the dispersibility of the calcium carbonate in resin is further improved, the bonding property of the joint sealant is greatly improved, and the weather resistance, the cold resistance, the high temperature resistance and the corrosion resistance of the joint sealant are further improved by introducing side chain fluorine groups, so that the joint sealant has higher thermal stability, surface self-cleaning property and the like. Further, the hardness and the strength of the joint sealant are improved by adding tungsten nitride, and the tear resistance and the thermal stability of the joint sealant are greatly enhanced.
4. The joint sealant disclosed by the invention is simple in preparation method, wide in raw material source, simple and convenient in construction method, greatly improves the construction efficiency, and has the advantages of low cost, good bonding performance and low curing shrinkage rate.
Detailed Description
The technical solution of the present invention is illustrated below, and the claimed scope of the present invention includes, but is not limited to, the following examples.
The utility model provides a stone material joint sealant, this joint sealant includes A component and B component, and wherein A component includes:
the epoxy resin is 30 to 60 parts by weight, preferably 35 to 55 parts by weight, and more preferably 40 to 50 parts by weight.
The MS resin is 5 to 18 parts by weight, preferably 7 to 15 parts by weight, and more preferably 9 to 13 parts by weight.
The reactive diluent is 1 to 8 parts by weight, preferably 2 to 7 parts by weight, and more preferably 3 to 6 parts by weight.
15 to 35 parts by weight, preferably 18 to 31 parts by weight, more preferably 20 to 28 parts by weight of calcium carbonate.
The thixotropic agent is 1 to 6 parts by weight, preferably 1.5 to 5.5 parts by weight, and more preferably 2 to 5 parts by weight.
0.5 to 5 parts by weight of a dehydrating agent, preferably 0.8 to 4 parts by weight, more preferably 1 to 3.5 parts by weight.
1-8 parts of white carbon black, preferably 2-7 parts of white carbon black, and more preferably 2.5-6 parts of white carbon black.
Wherein the component B comprises:
20-45 parts by weight of MQ resin, preferably 25-40 parts by weight, more preferably 30-35 parts by weight.
The modified curing agent is 18 to 40 parts by weight, preferably 20 to 35 parts by weight, and more preferably 25 to 30 parts by weight.
1 to 7 parts by weight of accelerator, preferably 2 to 6 parts by weight, more preferably 3 to 5 parts by weight.
1 to 9 parts by weight, preferably 2 to 8 parts by weight, and more preferably 2.5 to 7 parts by weight of a silane coupling agent.
0.5-5 parts by weight of white carbon black, preferably 1-4 parts by weight, more preferably 1.5-3 parts by weight.
0.5 to 4 parts by weight, preferably 0.8 to 3.5 parts by weight, and more preferably 1 to 3 parts by weight of tungsten nitride.
Calcium carbonate 12 to 30 parts by weight, preferably 15 to 26 parts by weight, more preferably 18 to 24 parts by weight.
Wherein the modified curing agent is a mixture of polyether amine modified curing agent and fatty amine modified curing agent.
Preferably, the epoxy resin is selected from one or more of bisphenol A type, bisphenol F type and bisphenol S type epoxy resins. E-51 epoxy resin is preferred.
Preferably, the MS resin is S203H resin and/or S227 resin, and is preferably mixed resin of S203H resin and S227 resin in a mass ratio of 1: 0.5-3.
Preferably, the polyether amine modified curing agent is a polyether amine modified curing agent obtained by modifying polyoxypropylene diamine and/or polyoxyethylene diamine and/or polyoxypropylene triamine with an epoxy resin. Preferably, the curing agent is a polyether amine modified curing agent obtained by modifying polyoxypropylene diamine and/or polyoxyethylene diamine and/or polyoxypropylene triamine with an E-51 epoxy resin and then further treating the modified curing agent with benzyl alcohol.
Preferably, the aliphatic amine modified curing agent is one or more of diethylenetriamine, triethylene tetramine, tetraethylene pentamine and m-xylene diamine modified by nonylphenol glycidyl ether.
Preferably, the amount of benzyl alcohol is 1 to 8 wt%, preferably 2 to 6 wt%, based on the total mass of the polyetheramine-modified curing agent.
Preferably, in the mixed modified curing agent consisting of the polyether amine modified curing agent and the fatty amine modified curing agent, the mass ratio of the polyether amine modified curing agent to the fatty amine modified curing agent is 1:0.5-3, and preferably 1: 0.8-2.
Preferably, the reactive diluent is one or more selected from C12-C14 alkyl glycidyl ether, benzyl glycidyl ether, butyl glycidyl ether, glycerol triglycidyl ether, 1,4 butanediol glycidyl ether, ethylene glycol diglycidyl ether and neopentyl glycol glycidyl ether. Preferably glycerol triglycidyl ether and/or 1, 4-butanediol glycidyl ether.
Preferably, the thixotropic agent is one or more of hydrogenated castor oil, cellulose and bentonite.
Preferably, the dehydrating agent is vinyltrimethylsilane.
Preferably, the calcium carbonate has a particle size composition of: 10-30% of particle size less than 100 meshes, 25-55% of particle size 100-200 meshes, 18-35% of particle size 300-500 meshes and 12-28% of particle size more than 500 meshes.
Preferably, the calcium carbonate is modified calcium carbonate obtained after modification treatment with alanine and/or trifluoro-2-alanine.
Preferably, the ratio of M units to Q units in the MQ resin is from 0.3 to 1.8, preferably from 0.5 to 1.5.
Preferably, the accelerator is selected from one or more of 2,4, 6-tris (dimethylaminomethyl) phenol (DMP-30), tris- (2-ethylhexanoate) salt of 2,4, 6-tris (dimethylaminomethyl) phenol, triethanolamine, thiourea. 2,4, 6-tris (dimethylaminomethyl) phenol (DMP-30) is preferred.
Preferably, the white carbon black is fumed silica.
Preferably, the silane coupling agent is a dialkoxysilane or trialkoxysilane coupling agent containing an amino or hydroxyl functional group. Preferably one or more of gamma-aminopropyltriethoxysilane (KH-550), 3- (2, 3-glycidoxy) propyltrimethoxysilane (KH-560) and diethylenetriaminopropyltriethoxysilane.
A method for preparing stone crack filling adhesive comprises the following steps:
s1: preparation of the component A: firstly, mixing epoxy resin, MS resin, reactive diluent and white carbon black. Then adding calcium carbonate, thixotropic agent and dehydrating agent, continuously mixing, and uniformly mixing to obtain the component A.
S2: preparation of the component B: firstly, mixing MQ resin, a modified curing agent and an accelerant. Then adding the thixotropic agent and the silane coupling agent and continuously mixing uniformly. And finally, adding calcium carbonate, tungsten nitride and white carbon black, and continuously mixing to obtain the component B.
S3: preparing the two-component stone joint sealant: and bottling the component A and the component B according to the proportion to obtain the two-component stone crack filling adhesive.
Wherein the modified curing agent is a mixed modified curing agent consisting of polyether amine modified curing agent and fatty amine modified curing agent according to the mass ratio of 1:0.5-3 (preferably 1: 0.8-2). The calcium carbonate is modified calcium carbonate obtained by modifying calcium carbonate by adopting alanine and/or trifluoro-2-alanine.
Preferably, the amounts of the components are as follows: wherein the component A is as follows:
the epoxy resin is 30 to 60 parts by weight, preferably 35 to 55 parts by weight, and more preferably 40 to 50 parts by weight.
The MS resin is 5 to 18 parts by weight, preferably 7 to 15 parts by weight, and more preferably 9 to 13 parts by weight.
The reactive diluent is 1 to 8 parts by weight, preferably 2 to 7 parts by weight, and more preferably 3 to 6 parts by weight.
15 to 35 parts by weight, preferably 18 to 31 parts by weight, more preferably 20 to 28 parts by weight of calcium carbonate.
The thixotropic agent is 1 to 6 parts by weight, preferably 1.5 to 5.5 parts by weight, and more preferably 2 to 5 parts by weight.
0.5 to 5 parts by weight of a dehydrating agent, preferably 0.8 to 4 parts by weight, more preferably 1 to 3.5 parts by weight.
1-8 parts of white carbon black, preferably 2-7 parts of white carbon black, and more preferably 2.5-6 parts of white carbon black.
Wherein the component B is as follows:
20-45 parts by weight of MQ resin, preferably 25-40 parts by weight, more preferably 30-35 parts by weight.
The modified curing agent is 18 to 40 parts by weight, preferably 20 to 35 parts by weight, and more preferably 25 to 30 parts by weight.
1 to 7 parts by weight of accelerator, preferably 2 to 6 parts by weight, more preferably 3 to 5 parts by weight.
1 to 9 parts by weight, preferably 2 to 8 parts by weight, and more preferably 2.5 to 7 parts by weight of a silane coupling agent.
0.5-5 parts by weight of white carbon black, preferably 1-4 parts by weight, more preferably 1.5-3 parts by weight.
0.5 to 4 parts by weight, preferably 0.8 to 3.5 parts by weight, and more preferably 1 to 3 parts by weight of tungsten nitride.
Calcium carbonate 12 to 30 parts by weight, preferably 15 to 26 parts by weight, more preferably 18 to 24 parts by weight.
Preferably, the MS resin is S203H resin and/or S227 resin, and is preferably mixed resin of S203H resin and S227 resin in a mass ratio of 1: 0.5-3.
Preferably, the epoxy resin is selected from one or more of bisphenol A type, bisphenol F type and bisphenol S type epoxy resins. E-51 epoxy resin is preferred.
Preferably, the polyether amine modified curing agent is a polyether amine modified curing agent obtained by modifying polyoxypropylene diamine and/or polyoxyethylene diamine and/or polyoxypropylene triamine with an epoxy resin. Preferably, the curing agent is a polyether amine modified curing agent obtained by modifying polyoxypropylene diamine and/or polyoxyethylene diamine and/or polyoxypropylene triamine with an E-51 epoxy resin and then further treating the modified curing agent with benzyl alcohol. The aliphatic amine modified curing agent is one or more of diethylenetriamine, triethylene tetramine, tetraethylene pentamine and m-xylene diamine which are modified by nonyl phenol glycidyl ether. Preferably, the amount of benzyl alcohol is 1 to 8 wt%, preferably 2 to 6 wt%, based on the total mass of the polyetheramine-modified curing agent.
Preferably, the reactive diluent is one or more selected from C12-C14 alkyl glycidyl ether, benzyl glycidyl ether, butyl glycidyl ether, glycerol triglycidyl ether, 1,4 butanediol glycidyl ether, ethylene glycol diglycidyl ether and neopentyl glycol glycidyl ether.
Preferably, the ratio of M units to Q units in the MQ resin is from 0.3 to 1.8, preferably from 0.5 to 1.5.
Preferably, the accelerator is selected from one or more of 2,4, 6-tris (dimethylaminomethyl) phenol (DMP-30), tris- (2-ethylhexanoate) salt of 2,4, 6-tris (dimethylaminomethyl) phenol, triethanolamine, thiourea.
Preferably, the white carbon black is fumed silica.
Preferably, the silane coupling agent is one or more of gamma-aminopropyltriethoxysilane (KH-550), 3- (2, 3-glycidoxy) propyltrimethoxysilane (KH-560), and diethylenetriaminopropyltriethoxysilane.
Preferably, the thixotropic agent is one or more of hydrogenated castor oil, cellulose and bentonite.
Preferably, the dehydrating agent is vinyltrimethylsilane.
Preferably, S1 is specifically: preparation of the component A: the epoxy resin, the MS resin, the reactive diluent and the fumed silica are uniformly mixed under the condition of raising the temperature (for example, the mixture is uniformly stirred at 50-95 ℃, preferably 60-80 ℃). Then starting high-speed stirring and vacuumizing (for example, vacuumizing to-0.01 MPa to-0.09 MPa), wherein the high-speed stirring time is 10-60 min. And finally, adding calcium carbonate, a thixotropic agent and a dehydrating agent, continuously stirring for 10-40min, cooling, stopping stirring for 30min, and then stopping vacuumizing to obtain the component A.
Preferably, S2 is specifically: preparation of the component B: firstly, mixing the MQ resin and the modified curing agent uniformly according to the proportion, then adding the accelerant and continuously mixing uniformly (for example, stirring and mixing for 10-60 min). Then adding the thixotropic agent and the silane coupling agent and mixing uniformly (for example, stirring and mixing). After a period of time, high-speed stirring is started and vacuum is pumped (for example, the vacuum pumping is from-0.01 MPa to-0.09 MPa), and the high-speed stirring time is 10-60 min. And finally, adding calcium carbonate, tungsten carbide and gas-phase white carbon black, continuously stirring (stirring for 10-40min), cooling, stopping stirring for 30min, and stopping vacuumizing to obtain the component B.
Preferably, S3 is specifically: preparing the two-component stone joint sealant: and respectively bottling the component A and the component B according to the mass ratio of 1:1.0-1.5 (preferably 1:1.1-1.3) to obtain the two-component stone crack filling adhesive.
Example 1
Preparation of the component A: 48.0g of E-51 epoxy resin, 4.0g of S203H resin, 8.0g of S227 resin, 5.0g of glycerol triglycidyl ether and 4.0g of fumed silica are stirred and mixed uniformly under the condition of raising the temperature to 70 ℃. After 25min, starting high-speed stirring and vacuumizing to-0.08 MPa, wherein the high-speed stirring time is 40 min. Then 25.2g of modified calcium carbonate, 3.0g of hydrogenated castor oil and 2.8g of vinyltrimethylsilane were added and stirred for another 30min, the temperature was reduced to room temperature and the stirring was stopped. Stopping stirring for 30min, and stopping vacuumizing to obtain component A.
Preparation of the component B: 32.5gMQ resin, 12.0g of polyether amine modified curing agent and 17.5g of fatty amine modified curing agent are mixed uniformly, and then 4.2g of DMP-30 is added to continue stirring and mixing for 30 min. Then 5.5gKH-550 is added to be stirred and mixed evenly. After 25min, starting high-speed stirring and vacuumizing to-0.08 MPa, wherein the high-speed stirring time is 30 min. Then adding 23.6g of modified calcium carbonate, 2.5g of tungsten nitride and 2.2g of fumed silica, continuing stirring for 25min, cooling to room temperature, stopping stirring for 30min, and then stopping vacuumizing to obtain the component B.
Preparation of stone joint sealant I: and filling the component A and the component B into a double tube according to the mass ratio of 1:1.1 to obtain the stone crack filling adhesive I.
Example 2
Preparation of the component A: 48.0g of E-51 epoxy resin, 4.0g of S203H resin, 8.0g of S227 resin, 5.0g of 1,4 g of butanediol glycidyl ether and 4.0g of fumed silica are stirred and mixed uniformly under the condition of raising the temperature to 70 ℃. After 25min, starting high-speed stirring and vacuumizing to-0.08 MPa, wherein the high-speed stirring time is 40 min. Then 25.2g of modified calcium carbonate, 3.0g of hydrogenated castor oil and 2.8g of vinyltrimethylsilane were added and stirred for another 30min, the temperature was reduced to room temperature and the stirring was stopped. Stopping stirring for 30min, and stopping vacuumizing to obtain component A.
Preparation of the component B: 32.5gMQ resin, 12.0g of polyether amine modified curing agent and 17.5g of fatty amine modified curing agent are mixed uniformly, and then 4.2g of DMP-30 is added to continue stirring and mixing for 30 min. Then 5.5gKH-550 is added to be stirred and mixed evenly. After 25min, starting high-speed stirring and vacuumizing to-0.08 MPa, wherein the high-speed stirring time is 30 min. Then adding 26.1g of modified calcium carbonate and 2.2g of fumed silica, continuing stirring for 25min, cooling to room temperature, stopping stirring for 30min, and then stopping vacuumizing to obtain the component B.
Preparation of stone joint sealant II: and filling the component A and the component B into a double tube according to the mass ratio of 1:1.1 to obtain the stone crack filling adhesive II.
Example 3
Preparation of the component A: 48.0g of E-51 epoxy resin, 4.0g of S203H resin, 8.0g of S227 resin, 5.0g of glycerol triglycidyl ether and 4.0g of fumed silica are stirred and mixed uniformly under the condition of raising the temperature to 70 ℃. After 25min, starting high-speed stirring and vacuumizing to-0.08 MPa, wherein the high-speed stirring time is 40 min. Then 25.2g of modified calcium carbonate, 3.0g of hydrogenated castor oil and 2.8g of vinyltrimethylsilane were added and stirred for another 30min, the temperature was reduced to room temperature and the stirring was stopped. Stopping stirring for 30min, and stopping vacuumizing to obtain component A.
Preparation of the component B: 32.5gMQ resin, 12.0g of polyether amine curing agent and 17.5g of fatty amine curing agent are mixed uniformly, and then 4.2g of DMP-30 is added to be stirred and mixed for 30 min. Then 5.5gKH-550 is added to be stirred and mixed evenly. After 25min, starting high-speed stirring and vacuumizing to-0.08 MPa, wherein the high-speed stirring time is 30 min. Then adding 23.6g of modified calcium carbonate, 2.5g of tungsten nitride and 2.2g of fumed silica, continuing stirring for 25min, cooling to room temperature, stopping stirring for 30min, and then stopping vacuumizing to obtain the component B.
Preparing stone joint sealant III: and filling the component A and the component B into a double tube according to the mass ratio of 1:1.1 to obtain the stone crack filling adhesive III.
Example 4
Preparation of the component A: 48.0g of E-51 epoxy resin, 4.0g of S203H resin, 8.0g of S227 resin, 5.0g of 1,4 g of butanediol glycidyl ether and 4.0g of fumed silica are stirred and mixed uniformly under the condition of raising the temperature to 70 ℃. After 25min, starting high-speed stirring and vacuumizing to-0.08 MPa, wherein the high-speed stirring time is 40 min. Then 25.2g of calcium carbonate, 3.0g of hydrogenated castor oil and 2.8g of vinyltrimethylsilane were added and stirring was continued for 30min, the temperature was lowered to room temperature and the stirring was stopped. Stopping stirring for 30min, and stopping vacuumizing to obtain component A.
Preparation of the component B: 32.5gMQ resin, 12.0g of polyether amine modified curing agent and 17.5g of fatty amine modified curing agent are mixed uniformly, and then 4.2g of DMP-30 is added to continue stirring and mixing for 30 min. Then 5.5gKH-550 is added to be stirred and mixed evenly. After 25min, starting high-speed stirring and vacuumizing to-0.08 MPa, wherein the high-speed stirring time is 30 min. Then 23.6g of calcium carbonate, 2.5g of tungsten nitride and 2.2g of fumed silica are added and stirred for 25min, the temperature is reduced to room temperature, the stirring is stopped, and the component B is obtained after the stirring is stopped for 30min and the vacuumizing is stopped.
Preparation of stone joint sealant IV: and filling the component A and the component B into a double tube according to the mass ratio of 1:1.1 to obtain the stone crack filling adhesive IV.
Example 5
Preparation of the component A: 48.0g of E-51 epoxy resin, 4.0g of S203H resin, 8.0g of S227 resin, 5.0g of glycerol triglycidyl ether and 4.0g of fumed silica are stirred and mixed uniformly under the condition of raising the temperature to 70 ℃. After 25min, starting high-speed stirring and vacuumizing to-0.08 MPa, wherein the high-speed stirring time is 40 min. Then 25.2g of modified calcium carbonate, 3.0g of hydrogenated castor oil and 2.8g of vinyltrimethylsilane were added and stirred for another 30min, the temperature was reduced to room temperature and the stirring was stopped. Stopping stirring for 30min, and stopping vacuumizing to obtain component A.
Preparation of the component B: 32.5gMQ resin and 29.5g of polyether amine modified curing agent are mixed evenly, and then 4.2g of DMP-30 is added and stirred for 30 min. Then 5.5gKH-560 is added to be stirred and mixed evenly. After 25min, starting high-speed stirring and vacuumizing to-0.08 MPa, wherein the high-speed stirring time is 30 min. Then adding 23.6g of modified calcium carbonate, 2.5g of tungsten nitride and 2.2g of fumed silica, continuing stirring for 25min, cooling to room temperature, stopping stirring for 30min, and then stopping vacuumizing to obtain the component B.
Preparing stone joint sealant V: and filling the component A and the component B into a double tube according to the mass ratio of 1:1.1 to obtain the stone crack filling adhesive V.
Example 6
Preparation of the component A: 48.0g of E-51 epoxy resin, 4.0g of S203H resin, 8.0g of S227 resin, 5.0g of glycerol triglycidyl ether and 4.0g of fumed silica are stirred and mixed uniformly under the condition of raising the temperature to 70 ℃. After 25min, starting high-speed stirring and vacuumizing to-0.08 MPa, wherein the high-speed stirring time is 40 min. Then 25.2g of modified calcium carbonate, 3.0g of hydrogenated castor oil and 2.8g of vinyltrimethylsilane were added and stirred for another 30min, the temperature was reduced to room temperature and the stirring was stopped. Stopping stirring for 30min, and stopping vacuumizing to obtain component A.
Preparation of the component B: 32.5gMQ resin and 29.5g fatty amine modified curing agent are mixed evenly, and then 4.2g DMP-30 is added to continue stirring and mixing for 30 min. Then 5.5gKH-560 is added to be stirred and mixed evenly. After 25min, starting high-speed stirring and vacuumizing to-0.08 MPa, wherein the high-speed stirring time is 30 min. Then adding 23.6g of modified calcium carbonate, 2.5g of tungsten nitride and 2.2g of fumed silica, continuing stirring for 25min, cooling to room temperature, stopping stirring for 30min, and then stopping vacuumizing to obtain the component B.
Preparation of stone joint sealant VI: and filling the component A and the component B into a double tube according to the mass ratio of 1:1.1 to obtain the stone crack filling adhesive VI.
Example 7
Preparation of the component A: 48.0g of E-51 epoxy resin, 4.0g of S203H resin, 8.0g of S227 resin, 5.0g of 1,4 g of butanediol glycidyl ether and 4.0g of fumed silica are stirred and mixed uniformly under the condition of raising the temperature to 70 ℃. After 25min, starting high-speed stirring and vacuumizing to-0.08 MPa, wherein the high-speed stirring time is 40 min. Then 25.2g of modified calcium carbonate, 3.0g of hydrogenated castor oil and 2.8g of vinyltrimethylsilane were added and stirred for another 30min, the temperature was reduced to room temperature and the stirring was stopped. Stopping stirring for 30min, and stopping vacuumizing to obtain component A.
Preparation of the component B: 12.0g of polyether amine modified curing agent and 17.5g of fatty amine modified curing agent are uniformly mixed, and then 4.2g of DMP-30 is added to continue stirring and mixing for 30 min. Then 5.5gKH-560 is added to be stirred and mixed evenly. After 25min, starting high-speed stirring and vacuumizing to-0.08 MPa, wherein the high-speed stirring time is 30 min. Then adding 23.6g of modified calcium carbonate, 2.5g of tungsten nitride and 2.2g of fumed silica, continuing stirring for 25min, cooling to room temperature, stopping stirring for 30min, and then stopping vacuumizing to obtain the component B.
Preparation of stone joint sealant VII: and filling the component A and the component B into a double tube according to the mass ratio of 1:1.1 to obtain the stone crack filling adhesive VII.
And (3) effect testing: the stone joint sealing adhesives I-VII prepared in examples 1-7 were subjected to aging and strength tests, and the results were as follows:
TABLE 1 Performance test one
TABLE 2 Performance test two
Claims (10)
1. The utility model provides a stone material mending crack is glued which characterized in that: the joint sealant comprises a component A and a component B, wherein the component A comprises:
30-60 parts by weight of epoxy resin, preferably 35-55 parts by weight, more preferably 40-50 parts by weight;
5-18 parts by weight of MS resin, preferably 7-15 parts by weight, more preferably 9-13 parts by weight;
1-8 parts by weight of reactive diluent, preferably 2-7 parts by weight, more preferably 3-6 parts by weight;
15-35 parts by weight of calcium carbonate, preferably 18-31 parts by weight, more preferably 20-28 parts by weight;
1 to 6 parts by weight of a thixotropic agent, preferably 1.5 to 5.5 parts by weight, more preferably 2 to 5 parts by weight;
0.5 to 5 parts by weight of a dehydrating agent, preferably 0.8 to 4 parts by weight, more preferably 1 to 3.5 parts by weight;
1-8 parts of white carbon black, preferably 2-7 parts of white carbon black, and more preferably 2.5-6 parts of white carbon black;
wherein the component B comprises:
20-45 parts by weight of MQ resin, preferably 25-40 parts by weight, more preferably 30-35 parts by weight;
18-40 parts of modified curing agent, preferably 20-35 parts, more preferably 25-30 parts;
1-7 parts by weight of accelerator, preferably 2-6 parts by weight, more preferably 3-5 parts by weight;
1-9 parts by weight of silane coupling agent, preferably 2-8 parts by weight, more preferably 2.5-7 parts by weight;
0.5-5 parts of white carbon black, preferably 1-4 parts of white carbon black, more preferably 1.5-3 parts of white carbon black;
0.5 to 4 parts by weight, preferably 0.8 to 3.5 parts by weight, more preferably 1 to 3 parts by weight of tungsten nitride;
12-30 parts by weight of calcium carbonate, preferably 15-26 parts by weight, more preferably 18-24 parts by weight;
wherein the modified curing agent is a mixture of polyether amine modified curing agent and fatty amine modified curing agent.
2. The stone material joint sealing glue of claim 1, characterized in that: the epoxy resin is selected from one or more of bisphenol A type, bisphenol F type and bisphenol S type epoxy resin; preferably E-51 epoxy resin; and/or
The MS resin is S203H resin and/or S227 resin, preferably mixed resin of S203H resin and S227 resin in a mass ratio of 1: 0.5-3; and/or
The polyether amine modified curing agent is a polyether amine modified curing agent obtained by modifying polyoxypropylene diamine and/or polyoxyethylene diamine and/or polyoxypropylene triamine by epoxy resin; preferably a polyether amine modified curing agent which is modified by polyoxypropylene diamine and/or polyoxyethylene diamine and/or polyoxypropylene triamine by E-51 epoxy resin and then is further treated by benzyl alcohol;
the aliphatic amine modified curing agent is one or more of diethylenetriamine, triethylene tetramine, tetraethylene pentamine and m-xylene diamine which are modified by nonyl phenol glycidyl ether;
preferably, the amount of the benzyl alcohol is 1 to 8 wt%, preferably 2 to 6 wt%, based on the total mass of the polyether amine modified curing agent; and/or
In the mixed modified curing agent consisting of the polyether amine modified curing agent and the fatty amine modified curing agent, the mass ratio of the polyether amine modified curing agent to the fatty amine modified curing agent is 1:0.5-3, preferably 1: 0.8-2.
3. The stone caulking compound according to claim 1 or 2, wherein: the reactive diluent is one or more selected from C12-C14 alkyl glycidyl ether, benzyl glycidyl ether, butyl glycidyl ether, glycerol triglycidyl ether, 1,4 butanediol glycidyl ether, ethylene glycol diglycidyl ether and neopentyl glycol glycidyl ether; preferably glycerol triglycidyl ether and/or 1, 4-butanediol glycidyl ether; and/or
The thixotropic agent is one or more of hydrogenated castor oil, cellulose and bentonite; and/or
The dehydrating agent is vinyl trimethylsilane.
4. The stone caulking compound according to any one of claims 1 to 3, wherein: the particle size composition of the calcium carbonate is as follows: 10-30% of particle size less than 100 meshes, 25-55% of particle size 100-200 meshes, 18-35% of particle size 300-500 meshes and 12-28% of particle size more than 500 meshes;
preferably, the calcium carbonate is modified calcium carbonate obtained after modification treatment with alanine and/or trifluoro-2-alanine.
5. The stone caulking compound according to any one of claims 1 to 4, wherein: the ratio of M unit to Q unit in the MQ resin is 0.3-1.8, preferably 0.5-1.5; and/or
The promoter is selected from one or more of 2,4, 6-tri (dimethylaminomethyl) phenol (DMP-30), tri- (2-ethylhexanoic acid) salt of 2,4, 6-tri (dimethylaminomethyl) phenol, triethanolamine and thiourea; preferably 2,4, 6-tris (dimethylaminomethyl) phenol (DMP-30); and/or
The white carbon black is fumed silica.
6. The stone caulking compound according to any one of claims 1 to 5, wherein: the silane coupling agent is dialkoxysilane or trialkoxysilane coupling agent containing amino or hydroxyl functional groups; preferably one or more of gamma-aminopropyltriethoxysilane (KH-550), 3- (2, 3-glycidoxy) propyltrimethoxysilane (KH-560) and diethylenetriaminopropyltriethoxysilane.
7. Method for preparing a stone caulking compound according to any one of claims 1 to 6, characterized in that: the method comprises the following steps:
s1: preparation of the component A: firstly, mixing epoxy resin, MS resin, reactive diluent and white carbon black; then adding calcium carbonate, a thixotropic agent and a dehydrating agent, and continuously mixing to obtain a component A after uniform mixing;
s2: preparation of the component B: firstly, mixing MQ resin, a modified curing agent and an accelerant; then adding a thixotropic agent and a silane coupling agent and continuously mixing uniformly; finally, adding calcium carbonate, tungsten nitride and white carbon black, and continuously mixing to obtain a component B;
s3: preparing the two-component stone joint sealant: bottling the component A and the component B according to a proportion to obtain the two-component stone crack filling adhesive;
wherein the modified curing agent is a mixed modified curing agent consisting of a polyether amine modified curing agent and a fatty amine modified curing agent according to the mass ratio of 1:0.5-3 (preferably 1: 0.8-2); the calcium carbonate is modified calcium carbonate obtained by modifying calcium carbonate by adopting alanine and/or trifluoro-2-alanine.
8. The method of claim 7, wherein: the dosage of each component is as follows: wherein the component A is as follows:
30-60 parts by weight of epoxy resin, preferably 35-55 parts by weight, more preferably 40-50 parts by weight;
5-18 parts by weight of MS resin, preferably 7-15 parts by weight, more preferably 9-13 parts by weight;
1-8 parts by weight of reactive diluent, preferably 2-7 parts by weight, more preferably 3-6 parts by weight;
15-35 parts by weight of calcium carbonate, preferably 18-31 parts by weight, more preferably 20-28 parts by weight;
1 to 6 parts by weight of a thixotropic agent, preferably 1.5 to 5.5 parts by weight, more preferably 2 to 5 parts by weight;
0.5 to 5 parts by weight of a dehydrating agent, preferably 0.8 to 4 parts by weight, more preferably 1 to 3.5 parts by weight;
1-8 parts of white carbon black, preferably 2-7 parts of white carbon black, and more preferably 2.5-6 parts of white carbon black;
wherein the component B is as follows:
20-45 parts by weight of MQ resin, preferably 25-40 parts by weight, more preferably 30-35 parts by weight;
18-40 parts of modified curing agent, preferably 20-35 parts, more preferably 25-30 parts;
1-7 parts by weight of accelerator, preferably 2-6 parts by weight, more preferably 3-5 parts by weight;
1-9 parts by weight of silane coupling agent, preferably 2-8 parts by weight, more preferably 2.5-7 parts by weight;
0.5-5 parts of white carbon black, preferably 1-4 parts of white carbon black, more preferably 1.5-3 parts of white carbon black;
0.5 to 4 parts by weight, preferably 0.8 to 3.5 parts by weight, more preferably 1 to 3 parts by weight of tungsten nitride;
calcium carbonate 12 to 30 parts by weight, preferably 15 to 26 parts by weight, more preferably 18 to 24 parts by weight.
9. The method according to claim 7 or 8, characterized in that: the MS resin is S203H resin and/or S227 resin, preferably mixed resin of S203H resin and S227 resin in a mass ratio of 1: 0.5-3; and/or
The epoxy resin is selected from one or more of bisphenol A type, bisphenol F type and bisphenol S type epoxy resin; preferably E-51 epoxy resin; and/or
The polyether amine modified curing agent is a polyether amine modified curing agent obtained by modifying polyoxypropylene diamine and/or polyoxyethylene diamine and/or polyoxypropylene triamine by epoxy resin; preferably a polyether amine modified curing agent which is modified by polyoxypropylene diamine and/or polyoxyethylene diamine and/or polyoxypropylene triamine by E-51 epoxy resin and then is further treated by benzyl alcohol; the aliphatic amine modified curing agent is one or more of diethylenetriamine, triethylene tetramine, tetraethylene pentamine and m-xylene diamine which are modified by nonyl phenol glycidyl ether; preferably, the amount of benzyl alcohol is 1 to 8 wt%, preferably 2 to 6 wt%, based on the total mass of the polyetheramine modified curing agent; and/or
The reactive diluent is one or more selected from C12-C14 alkyl glycidyl ether, benzyl glycidyl ether, butyl glycidyl ether, glycerol triglycidyl ether, 1,4 butanediol glycidyl ether, ethylene glycol diglycidyl ether and neopentyl glycol glycidyl ether; and/or
The ratio of M unit to Q unit in the MQ resin is 0.3-1.8, preferably 0.5-1.5; and/or
The promoter is selected from one or more of 2,4, 6-tri (dimethylaminomethyl) phenol (DMP-30), tri- (2-ethylhexanoic acid) salt of 2,4, 6-tri (dimethylaminomethyl) phenol, triethanolamine and thiourea; and/or
The white carbon black is fumed silica; and/or
The silane coupling agent is one or more of gamma-aminopropyltriethoxysilane (KH-550), 3- (2, 3-glycidoxy) propyltrimethoxysilane (KH-560) and diethylenetriaminopropyltriethoxysilane; and/or
The thixotropic agent is one or more of hydrogenated castor oil, cellulose and bentonite; and/or
The dehydrating agent is vinyl trimethylsilane.
10. The method of claim 9, wherein: s1 specifically includes: preparation of the component A: firstly, uniformly mixing the epoxy resin, the MS resin, the reactive diluent and the gas-phase white carbon black under the condition of heating (for example, uniformly stirring and mixing at 50-95 ℃, preferably 60-80 ℃); then starting high-speed stirring and vacuumizing (for example, vacuumizing to-0.01 MPa to-0.09 MPa), wherein the high-speed stirring time is 10-60 min; finally, adding calcium carbonate, a thixotropic agent and a dehydrating agent, continuously stirring for 10-40min, cooling, stopping stirring for 30min, and then stopping vacuumizing to obtain a component A; and/or
S2 specifically includes: preparation of the component B: firstly, uniformly mixing the MQ resin and the modified curing agent in proportion, and then adding the accelerant to continuously and uniformly mix (for example, stirring and mixing for 10-60 min); then adding the thixotropic agent and the silane coupling agent and uniformly mixing (for example, stirring and mixing); after a period of time, starting high-speed stirring and vacuumizing (for example, vacuumizing to-0.01 MPa to-0.09 MPa), wherein the high-speed stirring time is 10-60 min; finally, adding calcium carbonate, tungsten carbide and gas-phase white carbon black, continuously stirring (stirring for 10-40min), cooling, stopping stirring for 30min, and then stopping vacuumizing to obtain a component B; and/or
S3 specifically includes: preparing the two-component stone joint sealant: and respectively bottling the component A and the component B according to the mass ratio of 1:1.0-1.5 (preferably 1:1.1-1.3) to obtain the two-component stone crack filling adhesive.
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| CN102786903A (en) * | 2012-06-26 | 2012-11-21 | 湖南柯盛新材料有限公司 | Modified epoxy adhesive for stone combination and preparation method thereof |
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2021
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| CN102786903A (en) * | 2012-06-26 | 2012-11-21 | 湖南柯盛新材料有限公司 | Modified epoxy adhesive for stone combination and preparation method thereof |
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