CN112724904A - Graphene heating floor tile adhesive and preparation method thereof - Google Patents
Graphene heating floor tile adhesive and preparation method thereof Download PDFInfo
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- CN112724904A CN112724904A CN202011642446.6A CN202011642446A CN112724904A CN 112724904 A CN112724904 A CN 112724904A CN 202011642446 A CN202011642446 A CN 202011642446A CN 112724904 A CN112724904 A CN 112724904A
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- 239000000853 adhesive Substances 0.000 title claims abstract description 45
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 45
- 238000010438 heat treatment Methods 0.000 title claims abstract description 44
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000005011 phenolic resin Substances 0.000 claims abstract description 46
- 150000003505 terpenes Chemical class 0.000 claims abstract description 30
- 235000007586 terpenes Nutrition 0.000 claims abstract description 30
- 239000011347 resin Substances 0.000 claims abstract description 23
- 229920005989 resin Polymers 0.000 claims abstract description 23
- 239000003607 modifier Substances 0.000 claims abstract description 17
- 239000004611 light stabiliser Substances 0.000 claims abstract description 13
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910000077 silane Inorganic materials 0.000 claims abstract description 12
- 239000000945 filler Substances 0.000 claims abstract description 7
- 239000004014 plasticizer Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 239000000314 lubricant Substances 0.000 claims abstract description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 60
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 43
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 20
- 239000011858 nanopowder Substances 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 229910052710 silicon Inorganic materials 0.000 claims description 12
- 239000010703 silicon Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 239000000413 hydrolysate Substances 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000005543 nano-size silicon particle Substances 0.000 claims description 6
- 235000012239 silicon dioxide Nutrition 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 241000110847 Kochia Species 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 2
- 238000012545 processing Methods 0.000 abstract description 3
- -1 polyethylene Polymers 0.000 description 8
- 239000004698 Polyethylene Substances 0.000 description 7
- 229920000573 polyethylene Polymers 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 108010009736 Protein Hydrolysates Proteins 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- WTEOIRVLGSZEPR-UHFFFAOYSA-N boron trifluoride Chemical compound FB(F)F WTEOIRVLGSZEPR-UHFFFAOYSA-N 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- 229910015900 BF3 Inorganic materials 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 235000013873 oxidized polyethylene wax Nutrition 0.000 description 1
- 239000004209 oxidized polyethylene wax Substances 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 238000012643 polycondensation polymerization Methods 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000001993 wax Substances 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
- C09J171/00—Adhesives based on polyethers obtained by reactions forming an ether link in the main chain; Adhesives based on derivatives of such polymers
-
- 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
- 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
- C09J11/08—Macromolecular additives
-
- 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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- 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)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a graphene heating floor tile adhesive which comprises the following raw materials in parts by weight: 50-60 parts of silane end-capped resin, 5-10 parts of organosilicon modified terpene phenol resin, 50-60 parts of filler, 20-30 parts of plasticizer, 5-10 parts of nano modifier, 0-1 part of lubricant and 0-1 part of ultraviolet light stabilizer. The invention also discloses a preparation method of the graphene heating floor tile adhesive. The adhesive disclosed by the invention has excellent thermal stability, can keep excellent bonding strength at high temperature, and is suitable for bonding processing of graphene heating floor tiles.
Description
Technical Field
The invention relates to the technical field of adhesives, and particularly relates to a graphene heating floor tile adhesive and a preparation method thereof.
Background
The graphene heating floor is an electric floor heating floor which takes a floor as a carrier and is processed by arranging a two-dimensional graphene heating chip inside the floor, and can continuously generate and release heat after being electrified so as to achieve the purpose of quick and efficient heating. The ground temperature can reach 40 ℃ after the graphene heating floor is electrified, and the graphene heating floor has the advantages of good heat supply effect, uniform heat supply, long service life, energy conservation and environmental protection, and has good market prospect. The graphene heating floor, as an interior decoration building material, has high requirements on the safety performance, so that an environment-friendly, safe and nontoxic formaldehyde-free water-based adhesive needs to be adopted during processing. At present, common water-based adhesives for floor bonding comprise water-based polyurethane adhesives, water-based acrylate adhesives and the like, and the adhesives generally have the problems of poor thermal stability, poor heat resistance and low adhesive strength, are not suitable for being applied to graphene heating floors with high surface temperature for a long time, and become important factors for limiting the service performance and the service life of the graphene heating floors. Therefore, the development of the water-based adhesive suitable for the graphene heating floor is of great significance.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a graphene heating floor tile adhesive and a preparation method thereof.
The invention provides a graphene heating floor tile adhesive which comprises the following raw materials in parts by mass: 50-60 parts of silane end-capped resin, 5-10 parts of organosilicon modified terpene phenol resin, 50-60 parts of filler, 20-30 parts of plasticizer, 5-10 parts of nano modifier, 0-1 part of lubricant and 0-1 part of ultraviolet light stabilizer.
Preferably, the silane-terminated resin is japanese Kochia S303H resin.
Preferably, the preparation method of the organosilicon modified terpene phenol resin comprises the following steps:
s1, adding the silane coupling agent KH-560 into absolute ethyl alcohol, and stirring for 1-2h to obtain silane coupling agent hydrolysate;
and S2, mixing the terpene-phenol resin, the silane coupling agent hydrolysate and the toluene, heating for reaction, and drying in vacuum after the reaction is finished to obtain the terpene-phenol resin silane coupling agent.
Preferably, the mass ratio of the silane coupling agent KH-560 to the absolute ethyl alcohol is 1: (3-5); the mass ratio of the terpene phenol resin to the silane coupling agent KH-560 is 1: (0.5-1); the mass ratio of the terpene phenol resin to the toluene is 1: (10-20).
Preferably, in the step S2, the heating reaction temperature is 85-95 ℃ and the time is 3-5 h.
Wherein, the terpene phenol resin is prepared by the reaction of sigma-pinene and phenol in the presence of boron trifluoride or hydrochloric acid catalyst.
Preferably, the preparation method of the nano modifier comprises the following steps: mixing nano silicon dioxide and nano aluminum oxide according to the mass ratio of 1: (0.15-0.25) to obtain nano powder, then adding the nano powder and a silane coupling agent KH-560 into toluene, heating and reacting at 110-120 ℃ for 2-4h, centrifuging and drying to obtain the product.
Preferably, the mass ratio of the nano powder to the silane coupling agent KH-560 is 1: (0.1-0.15), wherein the mass ratio of the nano powder to the toluene is 1: (20-30).
Preferably, the filler is nano calcium carbonate.
Preferably, the plasticizer is DOP.
Preferably, the lubricant is at least one of polyethylene wax, oxidized polyethylene wax, polyamide wax, and polytetrafluoroethylene wax.
Preferably, the ultraviolet light stabilizer is a light stabilizer UV-531.
The preparation method of the graphene heating floor tile adhesive comprises the following steps: weighing the silane end-capped resin, the organic silicon modified terpene phenol resin, the filler, the plasticizer, the nano modifier, the lubricant and the ultraviolet light stabilizer according to the mass parts, stirring for 20-40min at the temperature of 115-125 ℃, and cooling to obtain the modified terpene phenol resin.
The invention has the following beneficial effects:
the adhesive of the invention adopts silane terminated resin as matrix resin and organosilicon modified terpene phenol resin as tackifying resin, and is compounded according to a proper proportion, wherein the silane terminated resin adopts Japanese Korea S303H resin, has high activity, can be rapidly crosslinked and cured by contacting with water vapor at room temperature, forms a network structure which takes Si-O-Si bond as crosslinking point and is connected by flexible long chain, has the advantages of environmental protection and low odor, and has rapid curing speed and good durability, the organosilicon modified terpene phenol resin adopts silane coupling agent KH-560 as modifier to modify terpene phenol resin formed by copolymerization of sigma-pinene and phenol, and the silane coupling agent KH-560 and phenolic hydroxyl in the terpene phenol resin are subjected to condensation polymerization, so that the obtained organosilicon modified terpene phenol resin and the silane terminated resin have good compatibility, a uniform and stable adhesive system can be obtained, and the organic silicon modified terpene-phenol resin has good thermal stability, can play a better role in tackifying at high temperature, and improves the bonding strength of the adhesive at high temperature; meanwhile, the silane coupling agent KH-560 surface modified nano silicon dioxide and nano aluminum oxide are added into the adhesive, so that the mechanical strength and the thermal conductivity of the adhesive can be improved, and a better heat dissipation effect is achieved, thereby reducing the accumulation of heat in the adhesive, and further improving the thermal stability of the adhesive and the bonding property of the adhesive at high temperature. The adhesive disclosed by the invention has excellent thermal stability, can keep excellent bonding strength at high temperature, and is suitable for bonding processing of graphene heating floor tiles.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
The graphene heating floor tile adhesive comprises the following raw materials in parts by mass: 50 parts of Japanese Kochia S303H resin, 5 parts of organic silicon modified terpene phenol resin, 50 parts of nano calcium carbonate, 20 parts of DOP and 5 parts of nano modifier.
The preparation method of the organic silicon modified terpene phenol resin comprises the following steps:
s1, adding the silane coupling agent KH-560 into absolute ethyl alcohol, and stirring for 1h to obtain silane coupling agent hydrolysate, wherein the mass ratio of the silane coupling agent KH-560 to the absolute ethyl alcohol is 1: 3;
s2, mixing the terpene-phenol resin, the silane coupling agent hydrolysate and toluene, heating at 85 ℃ for reaction for 5 hours, and performing vacuum drying after the reaction is finished to obtain the terpene-phenol resin silane coupling agent KH-560 with the mass ratio of 1: 0.5, the mass ratio of the terpene-phenol resin to the toluene is 1: 10.
the preparation method of the nano modifier comprises the following steps: mixing nano silicon dioxide and nano aluminum oxide according to the mass ratio of 1: 0.15, uniformly mixing to obtain nano powder, then adding the nano powder and a silane coupling agent KH-560 into toluene, heating and reacting for 4 hours at 110 ℃, centrifuging, and drying to obtain the silane coupling agent KH-560, wherein the mass ratio of the nano powder to the silane coupling agent KH-560 is 1: 0.1, the mass ratio of the nano powder to the toluene is 1: 20.
the preparation method of the graphene heating floor tile adhesive comprises the following steps: weighing silane terminated resin, organic silicon modified terpene phenol resin, nano calcium carbonate, DOP and nano modifier according to the mass parts, stirring for 40min at 115 ℃, and cooling to obtain the product.
Example 2
The graphene heating floor tile adhesive comprises the following raw materials in parts by mass: 50-60 parts of Japanese bellied S303H resin, 10 parts of organosilicon modified terpene phenol resin, 60 parts of nano calcium carbonate, 30 parts of DOP, 10 parts of nano modifier, 1 part of polyethylene wax and UV-5311 parts of light stabilizer.
The preparation method of the organic silicon modified terpene phenol resin comprises the following steps:
s1, adding the silane coupling agent KH-560 into absolute ethyl alcohol, and stirring for 2 hours to obtain silane coupling agent hydrolysate, wherein the mass ratio of the silane coupling agent KH-560 to the absolute ethyl alcohol is 1: 5;
s2, mixing the terpene-phenol resin, the silane coupling agent hydrolysate and toluene, heating to react at 95 ℃ for 3 hours, and drying in vacuum after the reaction is finished to obtain the terpene-phenol resin silane coupling agent KH-560 with the mass ratio of 1: 0.5, the mass ratio of the terpene-phenol resin to the toluene is 1: 10.
the preparation method of the nano modifier comprises the following steps: mixing nano silicon dioxide and nano aluminum oxide according to the mass ratio of 1: 0.15, uniformly mixing to obtain nano powder, then adding the nano powder and a silane coupling agent KH-560 into toluene, heating and reacting for 2 hours at 120 ℃, centrifuging, and drying to obtain the silane coupling agent KH-560, wherein the mass ratio of the nano powder to the silane coupling agent KH-560 is 1: 0.15, the mass ratio of the nano powder to the toluene is 1: 30.
the preparation method of the graphene heating floor tile adhesive comprises the following steps: weighing silane end-capped resin, organic silicon modified terpene phenol resin, nano calcium carbonate, DOP, nano modifier, polyethylene wax and light stabilizer UV-531 according to the mass parts, stirring for 20min at 125 ℃, and cooling to obtain the modified terpene phenol resin.
Example 3
The graphene heating floor tile adhesive comprises the following raw materials in parts by mass: 55 parts of Japanese bellied S303H resin, 7.5 parts of organosilicon modified terpene phenol resin, 55 parts of nano calcium carbonate, 25 parts of DOP, 7.5 parts of nano modifier, 0.5 part of polyethylene wax and UV-5310.5 parts of light stabilizer.
The preparation method of the organic silicon modified terpene phenol resin comprises the following steps:
s1, adding the silane coupling agent KH-560 into absolute ethyl alcohol, and stirring for 1.5h to obtain silane coupling agent hydrolysate, wherein the mass ratio of the silane coupling agent KH-560 to the absolute ethyl alcohol is 1: 4;
s2, mixing the terpene-phenol resin, the silane coupling agent hydrolysate and toluene, heating at 90 ℃ for reaction for 4 hours, and after the reaction is finished, drying in vacuum to obtain the terpene-phenol resin silane coupling agent KH-560 with the mass ratio of 1: 0.8, the mass ratio of the terpene-phenol resin to the toluene is 1: 15.
the preparation method of the nano modifier comprises the following steps: mixing nano silicon dioxide and nano aluminum oxide according to the mass ratio of 1: 0.2, uniformly mixing to obtain nano powder, then adding the nano powder and a silane coupling agent KH-560 into toluene, heating and reacting for 3 hours at 115 ℃, centrifuging and drying to obtain the silane coupling agent KH-560, wherein the mass ratio of the nano powder to the silane coupling agent KH-560 is 1: 0.12, the mass ratio of the nano powder to the toluene is 1: 25.
the preparation method of the graphene heating floor tile adhesive comprises the following steps: weighing silane end-capped resin, organic silicon modified terpene phenol resin, nano calcium carbonate, DOP, nano modifier, polyethylene wax and light stabilizer UV-531 according to the mass parts, stirring for 30min at 120 ℃, and cooling to obtain the modified terpene phenol resin.
In examples 1 to 3, the terpene-phenol resin was prepared by the method described in "Nanjing university of forestry" 1989,13(1), which is a research and development of terpene-phenol resin.
Comparative example 1
The graphene heating floor tile adhesive comprises the following raw materials in parts by mass: 62.5 parts of Japanese Kochia S303H resin, 62.5 parts of nano calcium carbonate, 25 parts of DOP, 0.5 part of polyethylene wax and UV-5310.5 parts of light stabilizer.
The preparation method of the graphene heating floor tile adhesive comprises the following steps: weighing the silane terminated resin, the nano calcium carbonate, the DOP, the polyethylene wax and the light stabilizer UV-531 according to the mass parts, stirring for 30min at 120 ℃, and cooling to obtain the silicon-based epoxy resin.
The adhesives prepared in examples 1-3 and comparative example 1 were used for bonding a graphene chip and a floor substrate, and then cured for 7 days at 40 + -2 ℃ and 50 + -5% relative humidity, and the peel strength was measured, and the test results are shown in table 1:
TABLE 1 adhesive peel Strength
| Example 1 | Example 2 | Example 3 | Comparative example 1 | |
| Peel strength (MPa) | 1.53 | 1.56 | 1.61 | 1.27 |
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (9)
1. The graphene heating floor tile adhesive is characterized by comprising the following raw materials in parts by mass: 50-60 parts of silane end-capped resin, 5-10 parts of organosilicon modified terpene phenol resin, 50-60 parts of filler, 20-30 parts of plasticizer, 5-10 parts of nano modifier, 0-1 part of lubricant and 0-1 part of ultraviolet light stabilizer.
2. The graphene heat-generating floor tile adhesive according to claim 1, wherein the silane-terminated resin is Japanese Kochia S303H resin.
3. The graphene heating floor tile adhesive according to claim 1 or 2, wherein the preparation method of the organic silicon modified terpene phenol resin is as follows:
s1, adding the silane coupling agent KH-560 into absolute ethyl alcohol, and stirring for 1-2h to obtain silane coupling agent hydrolysate;
and S2, mixing the terpene-phenol resin, the silane coupling agent hydrolysate and the toluene, heating for reaction, and drying in vacuum after the reaction is finished to obtain the terpene-phenol resin silane coupling agent.
4. The graphene heating floor tile adhesive according to claim 3, wherein the mass ratio of the silane coupling agent KH-560 to the absolute ethyl alcohol is 1: (3-5); the mass ratio of the terpene phenol resin to the silane coupling agent KH-560 is 1: (0.5-1); the mass ratio of the terpene phenol resin to the toluene is 1: (10-20).
5. The graphene exothermic floor tile adhesive according to claim 3 or 4, wherein the heating reaction temperature in step S2 is 85-95 ℃ for 3-5 h.
6. The graphene exothermic floor tile adhesive according to any one of claims 1 to 5, wherein the nano modifier is prepared by the following steps: mixing nano silicon dioxide and nano aluminum oxide according to the mass ratio of 1: (0.15-0.25) to obtain nano powder, then adding the nano powder and a silane coupling agent KH-560 into toluene, heating and reacting at 110-120 ℃ for 2-4h, centrifuging and drying to obtain the product.
7. The graphene heating floor tile adhesive according to claim 6, wherein the mass ratio of the nano powder to the silane coupling agent KH-560 is 1: (0.1-0.15), wherein the mass ratio of the nano powder to the toluene is 1: (20-30).
8. The graphene exothermic floor tile adhesive according to any of claims 1 to 7, wherein the filler is nano calcium carbonate; the plasticizer is DOP.
9. A method for preparing graphene exothermic floor tile adhesive according to any one of claims 1 to 8, comprising the steps of: weighing the silane end-capped resin, the organic silicon modified terpene phenol resin, the filler, the plasticizer, the nano modifier, the lubricant and the ultraviolet light stabilizer according to the mass parts, stirring for 20-40min at the temperature of 115-125 ℃, and cooling to obtain the modified terpene phenol resin.
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2020
- 2020-12-31 CN CN202011642446.6A patent/CN112724904A/en active Pending
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|---|---|---|---|---|
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