CN113801342A - Water-based epoxy emulsion, preparation method, waterproof binding material and water-based epoxy asphalt material - Google Patents
Water-based epoxy emulsion, preparation method, waterproof binding material and water-based epoxy asphalt material Download PDFInfo
- Publication number
- CN113801342A CN113801342A CN202111083354.3A CN202111083354A CN113801342A CN 113801342 A CN113801342 A CN 113801342A CN 202111083354 A CN202111083354 A CN 202111083354A CN 113801342 A CN113801342 A CN 113801342A
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- parts
- water
- emulsion
- isocyanate
- epoxy emulsion
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- Granted
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- 239000004593 Epoxy Substances 0.000 title claims abstract description 181
- 239000000839 emulsion Substances 0.000 title claims abstract description 124
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 239000000463 material Substances 0.000 title claims abstract description 93
- 238000002360 preparation method Methods 0.000 title claims abstract description 75
- 239000010426 asphalt Substances 0.000 title claims abstract description 74
- 239000012948 isocyanate Substances 0.000 claims abstract description 56
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 54
- 239000003822 epoxy resin Substances 0.000 claims abstract description 42
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 42
- 150000003973 alkyl amines Chemical class 0.000 claims abstract description 40
- 229920005862 polyol Polymers 0.000 claims abstract description 29
- 150000003077 polyols Chemical class 0.000 claims abstract description 29
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 22
- 239000003054 catalyst Substances 0.000 claims abstract description 17
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 9
- 229920000768 polyamine Polymers 0.000 claims abstract description 9
- 230000001070 adhesive effect Effects 0.000 claims description 41
- 239000000853 adhesive Substances 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 16
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 15
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 14
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 14
- 229920000909 polytetrahydrofuran Polymers 0.000 claims description 14
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 13
- 239000003995 emulsifying agent Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- 239000002202 Polyethylene glycol Substances 0.000 claims description 8
- 229920001223 polyethylene glycol Polymers 0.000 claims description 8
- 229920001451 polypropylene glycol Polymers 0.000 claims description 8
- 238000004945 emulsification Methods 0.000 claims description 7
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 7
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 claims description 5
- PLZVEHJLHYMBBY-UHFFFAOYSA-N Tetradecylamine Chemical compound CCCCCCCCCCCCCCN PLZVEHJLHYMBBY-UHFFFAOYSA-N 0.000 claims description 5
- 229910052797 bismuth Inorganic materials 0.000 claims description 5
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 5
- 150000003335 secondary amines Chemical class 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 238000006116 polymerization reaction Methods 0.000 claims description 4
- 230000001804 emulsifying effect Effects 0.000 abstract description 11
- 239000004721 Polyphenylene oxide Substances 0.000 abstract description 3
- 229920000570 polyether Polymers 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 37
- 238000006243 chemical reaction Methods 0.000 description 28
- 238000005054 agglomeration Methods 0.000 description 18
- 230000002776 aggregation Effects 0.000 description 18
- 239000002994 raw material Substances 0.000 description 15
- 238000001879 gelation Methods 0.000 description 13
- 238000012360 testing method Methods 0.000 description 13
- 230000000694 effects Effects 0.000 description 12
- 230000009286 beneficial effect Effects 0.000 description 7
- 150000002009 diols Chemical class 0.000 description 7
- 150000001412 amines Chemical group 0.000 description 6
- 239000011230 binding agent Substances 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000003513 alkali Substances 0.000 description 4
- 125000000217 alkyl group Chemical group 0.000 description 4
- 239000002518 antifoaming agent Substances 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 238000004132 cross linking Methods 0.000 description 4
- 239000002270 dispersing agent Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 239000000080 wetting agent Substances 0.000 description 4
- 238000000227 grinding Methods 0.000 description 3
- HKUFIYBZNQSHQS-UHFFFAOYSA-N n-octadecyloctadecan-1-amine Chemical group CCCCCCCCCCCCCCCCCCNCCCCCCCCCCCCCCCCCC HKUFIYBZNQSHQS-UHFFFAOYSA-N 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 238000009736 wetting Methods 0.000 description 3
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 description 2
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- -1 alicyclic isocyanate Chemical class 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 150000005846 sugar alcohols Polymers 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920001730 Moisture cure polyurethane Polymers 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- CBTVGIZVANVGBH-UHFFFAOYSA-N aminomethyl propanol Chemical group CC(C)(N)CO CBTVGIZVANVGBH-UHFFFAOYSA-N 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 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 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- CRVGTESFCCXCTH-UHFFFAOYSA-N methyl diethanolamine Chemical compound OCCN(C)CCO CRVGTESFCCXCTH-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007665 sagging Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/2805—Compounds having only one group containing active hydrogen
- C08G18/285—Nitrogen containing compounds
- C08G18/2865—Compounds having only one primary or secondary amino group; Ammonia
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4804—Two or more polyethers of different physical or chemical nature
- C08G18/4808—Mixtures of two or more polyetherdiols
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4825—Polyethers containing two hydroxy groups
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4833—Polyethers containing oxyethylene units
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/58—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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/721—Two or more polyisocyanates not provided for in one single group C08G18/73 - C08G18/80
- C08G18/724—Combination of aromatic polyisocyanates with (cyclo)aliphatic polyisocyanates
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7614—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7614—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring
- C08G18/7621—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring being toluene diisocyanate including isomer mixtures
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- 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
- 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
- C09J195/00—Adhesives based on bituminous materials, e.g. asphalt, tar, pitch
- C09J195/005—Aqueous compositions, e.g. emulsions
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2475/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2475/04—Polyurethanes
- C08J2475/08—Polyurethanes from polyethers
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Epoxy Resins (AREA)
- Polyurethanes Or Polyureas (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a water-based epoxy emulsion, a preparation method, a waterproof binding material and a water-based epoxy asphalt material, and relates to the technical field of epoxy asphalt materials. The water-based epoxy emulsion comprises 5-13 parts of polyol, 0.02-2 parts of isocyanate, 0.05-1.5 parts of long-chain alkylamine, 0.03-0.08 part of catalyst, 85-105 parts of epoxy resin and 90-125 parts of water; the waterproof binding material comprises 10-50 parts of waterborne epoxy emulsion, 50-90 parts of emulsified asphalt, 0.5-1.47 parts of auxiliary agent and 8-12 parts of water; the water-based epoxy asphalt material comprises 70-153 parts of waterproof binding material and 2-5 parts of modified polyamine epoxy curing agent. The long-chain alkylamine is adopted, and the dosage of the polyether polyol, the isocyanate and the long-chain alkylamine is controlled within the range, so that the emulsifying effect of the water-based epoxy emulsion is improved, and the bonding property of the water-based epoxy asphalt material can be improved.
Description
Technical Field
The invention relates to the technical field of epoxy asphalt materials, in particular to a water-based epoxy emulsion, a preparation method, a waterproof binding material and a water-based epoxy asphalt material.
Background
The epoxy asphalt material is a bonding material prepared from emulsified asphalt, epoxy resin emulsion and a curing agent, and is generally used for road pavement. Because the epoxy asphalt material adopts the epoxy resin emulsion to modify the emulsified asphalt, compared with single emulsified asphalt, the epoxy asphalt material has stronger adhesive force and impermeability.
In order to respond to the environmental protection requirement, the emulsified asphalt is generally modified by adopting aqueous epoxy resin emulsion; the water-based epoxy resin emulsion is prepared from epoxy resin, an emulsifier and the like according to a certain proportion, wherein the emulsifier is generally a polymer emulsifier.
However, the inventors of the present invention have considered that when a polymer emulsifier having a relatively large molecular weight is used, the emulsifying effect of the aqueous epoxy resin emulsion prepared is poor due to irregular structure and low surface activity of the polymer emulsifier having a relatively large molecular weight, and when an epoxy asphalt material is prepared using such an aqueous epoxy resin emulsion, it is not preferable to improve the adhesive properties of the epoxy asphalt material.
Disclosure of Invention
In order to improve the bonding performance of the epoxy asphalt material, the application provides the water-based epoxy emulsion, the preparation method, the waterproof bonding material and the water-based epoxy asphalt material.
In a first aspect, the present application provides an aqueous epoxy emulsion, which adopts the following technical scheme:
the water-based epoxy emulsion is prepared from the following components in parts by weight: 5-13 parts of polyol, 0.02-2 parts of isocyanate, 0.05-1.5 parts of long-chain alkylamine, 0.03-0.08 part of catalyst, 85-105 parts of epoxy resin and 90-125 parts of water.
In the reaction process of the polyol and the isocyanate, the long-chain alkylamine can react with part of the isocyanate, and the reaction degree of the polyol and the isocyanate can be adjusted, so that the crosslinking degree of the prepolymer synthesized by the polyol, the isocyanate and the long-chain alkylamine can be adjusted. The application optimizes the using amounts of the polyalcohol, the isocyanate and the long-chain alkylamine through experiments; the inventors have found that controlling the amounts of the polyol, the isocyanate and the long-chain alkylamine within the above ranges can reduce the degree of crosslinking of the prepolymer, reduce the molecular weight of the prepolymer, and contribute to increasing the surface activity of the prepolymer. The prepolymer and the epoxy resin can prepare the water-based epoxy emulsion in the presence of a catalyst and water, and the surface activity of the prepolymer is relatively high, so that the emulsification effect of the water-based epoxy emulsion is enhanced.
Moreover, the long-chain alkyl amine contains long-chain alkyl, so that the long-chain alkyl can be introduced into a molecular chain of the prepolymer, and the long-chain alkyl has longer carbon chain length, which is beneficial to increasing Van der Waals force among hydrophobic groups of the prepolymer, thereby enhancing the adhesive force of the water-based epoxy emulsion; in addition, the long chain alkyl group can also enhance the water resistance of the emulsion.
Therefore, the long-chain alkylamine is adopted, and the dosage of the polyether polyol, the isocyanate and the long-chain alkylamine is controlled within the range, so that the emulsifying effect of the aqueous epoxy emulsion is improved, the adhesive force and the water resistance of the aqueous epoxy emulsion are enhanced, and the cohesiveness of the epoxy asphalt material is improved.
Preferably, the long-chain alkylamine is at least one of dioctadecylsecondary amine, hexadecylamine or tetradecylamine.
Dioctadecylsecondary amine, hexadecylamine or tetradecylamine can react with isocyanate, so that the molecular weight of the prepolymer is reduced, and the emulsifying effect of the epoxy emulsion is improved; in addition, the reaction rate of the dioctadecylsecondary amine and the isocyanate is relatively slow, the reaction process is convenient to control, the adverse phenomena of gel and the like of the prepared emulsion can be reduced, and the emulsion effect of the emulsion is further improved.
Preferably, the polyol is prepared from the following components in parts by weight: 2-5 parts of polytetrahydrofuran glycol, 2-5 parts of polyethylene glycol and 1-3 parts of polypropylene glycol.
The influence of different types of polyols and the use amount thereof on the emulsion is analyzed through experiments. The inventors have found that when the amount of the long-chain alkylamine is controlled within the above range, the use of a polyol obtained by mixing polytetrahydrofuran glycol, polyethylene glycol and polypropylene glycol and the amount of the polytetrahydrofuran glycol, polyethylene glycol and polypropylene glycol is controlled within the above range, contributes to the reduction in the molecular weight of the prepolymer, and can further improve the emulsifying effect of the aqueous epoxy emulsion.
In addition, polytetrahydrofuran glycol, polyethylene glycol and polypropylene glycol are easy to obtain, have stable performance, and are beneficial to controlling the production period and the product performance of the aqueous epoxy emulsion.
Preferably, the isocyanate is prepared from the following components in parts by weight: 0.01-1 part of toluene diisocyanate and 0.01-1 part of isophorone diisocyanate.
Isophorone diisocyanate is alicyclic isocyanate and has the characteristics of low reaction activity and good flexibility, but the market price of isophorone diisocyanate is higher, and only isophorone diisocyanate is used for preparing epoxy emulsion, so that the preparation cost of aqueous epoxy emulsion is not reduced.
The toluene diisocyanate is aromatic isocyanate and has the characteristic of low market price, but the toluene diisocyanate has high reaction activity and high strength, and the epoxy emulsion prepared by only using the toluene diisocyanate can cause the over-high reaction rate in the reaction process and has potential safety hazard.
According to the application, isophorone diisocyanate and toluene diisocyanate are used in a matched manner, and the use amounts of the isophorone diisocyanate and the toluene diisocyanate are controlled within the above range, so that the manufacturing cost of the water-based epoxy emulsion can be reduced, and the potential safety hazard in the production process can be reduced.
Preferably, the catalyst is an organic bismuth catalyst.
Compared with the prior art, the organic bismuth catalyst has the characteristics of environmental protection and high cost performance, and can reduce the manufacturing cost of the aqueous epoxy emulsion and the harm to workers and the environment in the manufacturing process.
Compared with other environment-friendly catalysts, the organic bismuth catalyst has lower catalytic activity, is beneficial to reducing the emulsification rate of the epoxy resin, reducing the phenomena of gelation and emulsion breaking of the aqueous epoxy emulsion and further enhancing the adhesive force of the epoxy emulsion.
In a second aspect, the present application provides a method for preparing an aqueous epoxy emulsion, which adopts the following technical scheme:
a preparation method of the water-based epoxy emulsion comprises the following steps:
pre-polymerization: heating polyol to liquid state, mixing isocyanate with the liquid polyol, reacting at 80-85 ℃ for 2.5-3.5h, adding long-chain alkylamine, and reacting for 1.5-2.5h to obtain a prepolymer;
preparation: dividing the epoxy resin into two parts, mixing the prepolymer and the first part of the epoxy resin at the temperature of 80-85 ℃, reacting, mixing with a catalyst, and reacting to obtain an emulsifier with the isocyanate content of 0;
emulsification: and (3) mixing and heating the emulsifier and the second part of epoxy resin at 70-80 ℃ to obtain an emulsified mixture, and dripping water into the emulsified mixture under stirring to obtain the water-based epoxy emulsion.
According to the method, the epoxy resin in the raw materials is divided into two parts of epoxy resin, so that when the first part of epoxy resin or the second part of epoxy resin is reacted, the emulsifier in the reaction system is in an excessive state relative to the epoxy resin, the reaction rate of the epoxy resin is improved, the epoxy resin is also facilitated to be completely reacted, the phenomena of gelation and emulsion breaking of the emulsion can be reduced, the emulsification effect of the water-based epoxy emulsion is improved, and the adhesive force of the water-based epoxy emulsion is enhanced.
Preferably, in the prepolymerization step, the content of isocyanate in the prepolymer is 0-0.8%.
Tests show that when the residual amount of isocyanate in the prepolymer is 0-0.8%, the surface activity of the prepolymer is high, and the emulsifying effect of the prepared water-based epoxy emulsion is good.
Preferably, in the prepolymerization step, when the residual amount of the isocyanate is 0 to 2.0%, a long-chain alkylamine is further added.
When the residual amount of the isocyanate is 0-2.0%, adding long-chain alkylamine, so that the residual amount of the isocyanate in the prepolymer is adjusted to 0-0.8%. And when the residual quantity of the isocyanate is 0-2.0%, most of the isocyanate is polymerized with the polyol, but the crosslinking degree of a polymerization product is smaller, and at the moment, the long-chain alkylamine is added, and the long-chain alkylamine reacts with a part of residual isocyanate, so that the crosslinking degree of the prepolymer can be controlled, the molecular weight of the prepolymer is kept at a smaller level, and the surface activity of the prepolymer is improved.
In a third aspect, the present application provides a waterproof adhesive material using a water-based epoxy emulsion, which adopts the following technical scheme:
a waterproof binding material using a water-based epoxy emulsion is prepared from the following components in parts by weight: 10-50 parts of water-based epoxy emulsion, 50-90 parts of emulsified asphalt, 0.5-1.47 parts of auxiliary agent and 8-12 parts of water.
The waterborne epoxy emulsion prepared by the method is emulsified with emulsified asphalt, so that the bonding property and the water resistance of the prepared waterproof bonding material can be improved. Water is used to adjust the viscosity of the waterproof binder to the desired viscosity. The auxiliary agent can reduce the phenomena of shrinkage cavity and dark bubble of the waterproof binding material.
In a fourth aspect, the present application provides a water-based epoxy asphalt material using a waterproof binder, which adopts the following technical scheme:
a water-based epoxy asphalt material applying a waterproof binding material is prepared from the following components in parts by weight: 70-153 parts of waterproof binding material and 2-5 parts of modified polyamine epoxy curing agent.
The waterproof adhesive is prepared from the waterborne epoxy emulsion, so that the adhesive property and the water resistance of the prepared waterborne epoxy asphalt material can be improved, and the waterproof adhesive is a waterborne system, so that the modified polyamine epoxy curing agent has high tolerance to water, and the waterproof adhesive is favorably cured into the waterborne epoxy asphalt material.
In summary, the present application has the following beneficial effects:
1. according to the method, long-chain alkylamine is adopted, and the use amounts of polyether polyol, isocyanate and the long-chain alkylamine are controlled within the range, so that the emulsifying effect of the water-based epoxy emulsion is improved, and the bonding property of the emulsified asphalt material is further improved;
2. the application preferably selects dioctadecyl secondary amine, can reduce the adverse phenomena of gel and the like of the prepared emulsion, preferably selects polytetrahydrofuran glycol, polyethylene glycol and polypropylene glycol, is beneficial to reducing the molecular weight of the prepolymer, and can further improve the emulsification effect of the water-based epoxy emulsion;
3. according to the preparation method of the water-based epoxy emulsion, the epoxy resin in the raw materials is divided into two parts for reaction, so that the phenomena of gelation and emulsion breaking of the emulsion can be reduced, and the emulsion effect and the adhesive force of the emulsion can be improved;
4. the waterproof adhesive is prepared from the water-based epoxy emulsion, so that the adhesive property and the water resistance of the prepared waterproof adhesive are improved;
5. the water-based epoxy asphalt material is prepared from the waterproof binding material and the modified polyamine epoxy curing agent, the waterproof binding material is beneficial to improving the binding property and the water resistance of the prepared water-based epoxy asphalt material, and the modified polyamine epoxy curing agent is convenient to play a role in a water-based system.
Detailed Description
The present application will be described in further detail with reference to examples.
The starting materials used in the following examples are commercially available unless otherwise specified. Wherein the polytetrahydrofuran diol is polytetrahydrofuran diol 1000; isophorone diisocyanate is purchased from Wuhan Gixin Yibang Biotech Co., Ltd, and is 4098-71-9; e20 epoxy resin is purchased from Balin petrochemical and is CYD-011; e51 epoxy resin is obtained from the country of the Ling petrochemical company and is CYD-128; the F51 epoxy resin is purchased from Jinan Bai evolutionary engineering technology, Inc., and has a product number of F51; NPEF-170 epoxy resin is available from south Asia plastics industries, Inc.; dioctadecyl secondary amine was purchased from Jiangsu Runfeng synthetic science and technology company; hexadecylamine is purchased from Hubei Handa Biotech, Inc., with a purity of 95%; tetradecylamine was purchased from Shandong Jiapeng New materials, Inc., model 16; diphenylmethane diisocyanate was purchased from cigarette Taiwanhua polyurethane, Inc.; the emulsified asphalt is purchased from RHLQ003 of Shandong Honggong waterproof material Co.Ltd; the substrate wetting agent is TEGO-4100; selecting K4000 as a defoaming agent; BYK-190 is selected as the wetting dispersant; the multifunctional auxiliary agent is AMP-95; the leveling agent is KMT-5510S, and the modified polyamine epoxy curing agent is 5304A.
Preparation example
Preparation example 1
The preparation example provides a water-based epoxy emulsion which is prepared from the following components: polyol, isocyanate, long-chain alkylamine, catalyst, epoxy resin and water. Wherein the polyhydric alcohol is polytetrahydrofuran diol; the isocyanate is selected from toluene diisocyanate; the epoxy resin is E20 epoxy resin; the long-chain alkylamine is dioctadecyl secondary amine; the catalyst is organic bismuth catalyst DY-20.
The raw materials of the water-based epoxy emulsion are used in the amount shown in the table one, and are prepared according to the following steps:
pre-polymerization: putting polyol into a reaction kettle, heating the reaction kettle to 80 ℃, heating for 1h, heating the reaction kettle to 120 ℃, pumping the reaction kettle to a vacuum state, keeping the vacuum state for 1.5h, reducing the temperature of the reaction kettle to 70 ℃, adding isocyanate into the reaction kettle, slowly heating the reaction kettle to 80 ℃, testing the content of the isocyanate according to a method in HG/T2409-1992 determination of the content of isocyanate groups in polyurethane prepolymer in the reaction process of the isocyanate and the polyol, reacting for 3h until the content of the isocyanate is 0.1%, adding long-chain alkylamine into the reaction kettle, and reacting the long-chain alkylamine with the prepolymer for 2h to obtain the prepolymer with the content of the isocyanate being 0.
Preparation: dividing the epoxy resin into two parts, keeping the temperature of the reaction kettle at 80 ℃, adding the first part of the epoxy resin into the reaction kettle, reacting the epoxy resin with the prepolymer for 1h, adding the catalyst into the reaction kettle, and continuously reacting for 1h to obtain the emulsifier with the isocyanate content of 0.
Emulsification: and adding an emulsifier and a second part of epoxy resin into an emulsifying kettle, heating the emulsifying kettle to 75 ℃, heating for 1h to obtain an emulsified mixture, dripping water into the emulsifying kettle, controlling the dripping time of the water within 3h, and continuously stirring for 1h after the water is completely dripped to obtain the water-based epoxy emulsion.
Table-raw material consumption table of preparation example 1
Preparation example 2
This preparation example differs from preparation example 1 in that the amount of polytetrahydrofuran diol used was 9 kg; in the prepolymerization step, after isocyanate reacts with polyol for 3 hours, the content of the isocyanate is 0, long-chain alkylamine is added into a reaction kettle, and after the long-chain alkylamine reacts with the prepolymer for 2 hours, the prepolymer with the content of the isocyanate being 0 is obtained.
Preparation example 3
This preparation example differs from preparation example 1 in that the amount of polytetrahydrofuran diol used was 13 kg; in the prepolymerization step, after isocyanate reacts with polyol for 3 hours, the content of the isocyanate is 0, long-chain alkylamine is added into a reaction kettle, and after the long-chain alkylamine reacts with the prepolymer for 2 hours, the prepolymer with the content of the isocyanate being 0 is obtained.
Preparation example 4
This preparation differs from preparation 2 in that the polytetrahydrofuran diol is replaced by the same amount of polyethylene glycol.
Preparation example 5
This preparation differs from preparation 2 in that the polytetrahydrofuran diol is replaced by the same amount of polypropylene glycol.
Preparation example 6
The preparation example differs from preparation example 2 in that the amount of toluene diisocyanate used was 0.12 kg; in the prepolymerization step, after isocyanate reacts with polyol for 3 hours, the content of the isocyanate is 0.8 percent, long-chain alkylamine is added into a reaction kettle, and after the long-chain alkylamine reacts with the prepolymer for 2 hours, the prepolymer with the content of the isocyanate of 0.2 percent is obtained.
Preparation example 7
The present preparation example differs from preparation example 6 in that the amount of toluene diisocyanate used was 2 kg; in the prepolymerization step, after isocyanate reacts with polyol for 3 hours, the content of the isocyanate is 2.0 percent, long-chain alkylamine is added into a reaction kettle, and after the long-chain alkylamine reacts with the prepolymer for 2 hours, the prepolymer with the content of the isocyanate of 0.8 percent is obtained.
Preparation example 8
This preparation differs from preparation 6 in that toluene diisocyanate is replaced by an equal amount of isophorone diisocyanate.
Preparation example 9
The difference between the preparation example and the preparation example 6 is that in the prepolymerization step, the dosage of the toluene diisocyanate is 0.06kg, the isocyanate also comprises 0.06kg of isophorone diisocyanate, and the isophorone diisocyanate and the toluene diisocyanate are added into the reaction kettle after being uniformly mixed.
Preparation example 10
This preparation differs from preparation 9 in that the secondary dioctadecylamine is replaced by the same amount of primary hexadecylamine.
Preparation example 11
This preparation differs from preparation 9 in that the secondary dioctadecylamine is replaced by the same amount of tetradecylamine.
Preparation example 12
This preparation example differs from preparation example 9 in that toluene diisocyanate and isophorone diisocyanate are replaced with the same amount of diphenylmethane diisocyanate.
Preparation example 13
This preparation differs from preparation 9 in that the first part of epoxy resin is composed of 2.5kg of E20, 2.5kg of E51 and 2.5kg of F51, and the second part of epoxy resin is composed of 29.3kg of E20, 29.1kg of F51 and 29.1kg of NPEF-170.
Examples
Example 1
The present embodiment provides a waterproof adhesive. The waterproof binding material is prepared from the following components: the water-based epoxy emulsion, the emulsified asphalt, the auxiliary agent and water. Wherein the waterborne epoxy emulsion obtained in preparation example 1 is adopted as the waterborne epoxy emulsion; the auxiliary agent comprises a base material wetting agent, a defoaming agent, a wetting dispersant, a multifunctional auxiliary agent and a flatting agent.
The raw material formulation of the waterproof adhesive is shown in table two, and the waterproof adhesive is prepared according to the following steps: dividing the water into two parts horizontally, putting the first part of water into a material jar, stirring the water in the material jar at the rotating speed of 1000r/min, sequentially adding a wetting dispersant, a defoaming agent, a base material wetting agent, a multifunctional assistant and a flatting agent into the material jar, stirring for 15min, reducing the rotating speed to 500r/min, adding the aqueous epoxy emulsion and the emulsified asphalt into the material jar, stirring for 20min, adding the second part of water into the material jar, and stirring for 20min to obtain the waterproof binding material.
Table two raw material proportioning table of example 1
Example 2
This example differs from example 1 in that the aqueous epoxy emulsion obtained in preparation example 2 was used as the aqueous epoxy emulsion.
Example 3
This example differs from example 1 in that the aqueous epoxy emulsion obtained in preparation example 3 was used as the aqueous epoxy emulsion.
Example 4
This example differs from example 1 in that the aqueous epoxy emulsion obtained in preparation example 4 was used as the aqueous epoxy emulsion.
Example 5
This example differs from example 1 in that the aqueous epoxy emulsion obtained in preparation example 5 was used as the aqueous epoxy emulsion.
Example 6
This example differs from example 1 in that the aqueous epoxy emulsion obtained in preparation example 6 was used as the aqueous epoxy emulsion.
Example 7
This example differs from example 1 in that the aqueous epoxy emulsion obtained in preparation example 7 was used as the aqueous epoxy emulsion.
Example 8
This example differs from example 1 in that the aqueous epoxy emulsion obtained in preparation example 8 was used as the aqueous epoxy emulsion.
Example 9
This example differs from example 1 in that the aqueous epoxy emulsion obtained in preparation example 9 was used as the aqueous epoxy emulsion.
Example 10
This example differs from example 1 in that the aqueous epoxy emulsion obtained in preparation example 10 was used as the aqueous epoxy emulsion.
Example 11
This example differs from example 1 in that the aqueous epoxy emulsion obtained in preparation example 11 was used as the aqueous epoxy emulsion.
Example 12
This example differs from example 1 in that the aqueous epoxy emulsion obtained in preparation example 12 was used as the aqueous epoxy emulsion.
Example 13
This example differs from example 1 in that the aqueous epoxy emulsion obtained in preparation example 13 was used as the aqueous epoxy emulsion.
Examples 14 to 19
As shown in table three, examples 14 to 19 are different from example 9 mainly in the ratio of raw materials for preparing the waterproof binder.
TABLE III raw material proportioning tables for examples 14-19
Application example
Application examples 1 to 19
The water-based epoxy asphalt materials of application examples 1 to 19 were prepared by sequentially blending the waterproof adhesive obtained in examples 1 to 19 with the modified epoxy curing agent, wherein the weight of the waterproof adhesive in application examples 1 to 19 was 27kg, and the weight of the modified epoxy curing agent was 1 kg.
The water-based epoxy asphalt material is prepared according to the following steps:
and adding the waterproof binding material and the modified polyamine epoxy curing agent into a charging basket, and uniformly stirring to obtain the water-based epoxy asphalt material.
Application example 20
This application example was different from application example 9 in that the weight of the waterproof adhesive was 71kg and the weight of the modified epoxy curing agent was 3 kg.
Application example 21
This application example was different from application example 9 in that the weight of the waterproof adhesive was 151kg and the weight of the modified epoxy curing agent was 3 kg.
Comparative example
Comparative example 1
The comparative example provides a waterproof adhesive, and differs from example 9 in that the aqueous epoxy emulsion used in the preparation process uses the same amount of N-methyldiethanolamine instead of dioctadecylsecondary amine.
Comparative examples 2 to 7
Comparative examples 2 to 7 each provide a waterproof adhesive, and comparative examples 2 to 7 are different from example 9 in the ratio of raw materials in the preparation process of the aqueous epoxy emulsion used, and the aqueous epoxy emulsions used in comparative examples 2 to 7 were prepared in the ratios shown in table four.
TABLE IV raw material proportioning tables for aqueous epoxy emulsions used in comparative examples 2 to 7
Comparative application example
Comparative application examples 1 to 7
The waterproof bonding materials obtained in comparative examples 1 to 7 and the modified epoxy curing agent are sequentially adopted to be matched to prepare the waterborne epoxy asphalt materials of comparative application examples 1 to 7, wherein the weight of the waterproof bonding materials in comparative application examples 1 to 7 is 27kg, and the weight of the modified epoxy curing agent is 1 kg.
The water-based epoxy asphalt material is prepared according to the following steps:
and adding the waterproof binding material and the modified polyamine epoxy curing agent into a charging basket, and uniformly stirring to obtain the water-based epoxy asphalt material.
Comparative application example 8
The water-based epoxy asphalt coating of the comparative application example is prepared by the following method: as shown in table five, deionized water, a pH regulator, an anti-sagging auxiliary agent, a wetting agent, a dispersing agent and a defoaming agent are sequentially added into a stirring tank, and stirred at a medium speed of 600r/min for 30 min; then adding the talcum powder, the precipitated barium sulfate, the carbon black, the iron oxide black and the anti-rust pigment into a stirring tank under the stirring of 600r/min, and stirring at a high speed of 1200r/min for 30 min. Then pouring the mixture into a grinder for grinding, wherein the grinding temperature is 5-40 ℃, the grinding fineness is less than 30 mu m, adding the mixture into a dispersion tank, then adding epoxy resin, propylene glycol methyl ether, a flatting agent, an anti-flash rust agent, a thickening agent, a coupling agent and emulsified asphalt into the dispersion tank in the stirring process of 600r/min, stirring at the medium speed of 600r/min for 30min, adding silica sol, stirring for 10min, and filtering at the particle size of 200 mu m to obtain the component A. The component B is a curing agent with the model of ARADUR3986, and the component A and the component B are uniformly mixed according to the mass ratio of 12:1 to obtain the water-based epoxy asphalt coating.
Table five raw material proportioning table for comparison application example 8
Performance test
For the aqueous epoxy emulsions used in application examples 1 to 21 and comparative application examples 1 to 7, the Nano-zs Nano-particle size and Zeta potential analyzer were used to measure the particle size of the aqueous epoxy emulsion at room temperature, and the test data are shown in table six.
Aiming at the aqueous epoxy asphalt materials provided in application examples 1-21 and comparative application examples 1-8, the adhesive force pull strength, the composite pull strength, the water impermeability, the alkali resistance and the salt water resistance of the aqueous epoxy asphalt material are detected according to the detection standard of Q/JSZL-002-.
Blade coating tests were performed on the waterborne epoxy asphalt materials provided in application examples 3-6, application examples 8-13, and comparative application examples 1-8, and the test results are shown in Table seven. Wherein, the required test sample amount is weighed, and after the sample is stirred evenly, the appearance of the sample is observed firstly. Then, an aluminum plate with a clean surface was taken, the sample was coated on the aluminum plate 3 times at intervals of 8 hours, the coating area was 100mm × 50mm, the total thickness was 1.5 ± 0.2mm, and the surface was scraped off the last time. And (3) maintaining for 120h under the test conditions of 25 ℃ and 60% of relative humidity, then maintaining for 48h in an electrothermal blowing dry box at 40 ℃, taking out the test piece, and observing the surface of the test piece.
TABLE six test data tables of application examples 1 to 21 and comparative application examples 1 to 8
TABLE seven scrape coating test results table
| Performance of | Appearance of the sample | Surface appearance of test piece |
| Application example 2 | No color difference, no gel and no agglomeration | No shrinkage cavity and no dark bubble |
| Application example 4 | No color difference, no gel and no agglomeration | No shrinkage cavity and no dark bubble |
| Application example 5 | No color difference, no gel and no agglomeration | No shrinkage cavity and no dark bubble |
| Application example 6 | No color difference, no gel and no agglomeration | No shrinkage cavity and no dark bubble |
| Application example 8 | No color difference, no gel and no agglomeration | No shrinkage cavity and no dark bubble |
| Application example 9 | No color difference, no gel and no agglomeration | No shrinkage cavity and no dark bubble |
| Application example 10 | No color difference, gel and agglomeration | No shrinkage cavity and no dark bubble |
| Application example 11 | No color difference, gel and agglomeration | No shrinkage cavity,Without dark bubble |
| Application example 12 | Has color difference, no gel and no agglomeration | No shrinkage cavity and no dark bubble |
| Application example 13 | No color difference, no gel and no agglomeration | No shrinkage cavity and no dark bubble |
| Comparative application example 1 | No color difference, gel and caking | With shrinkage cavity and dark bubble |
| Comparative application example 2 | No color difference, gel and agglomeration | With shrinkage cavity and without dark bubble |
| Comparative application example 3 | No color difference, gel and agglomeration | With shrinkage cavity and without dark bubble |
| Comparative application example 4 | No color difference, gel and agglomeration | With shrinkage cavity and without dark bubble |
| Comparative application example 5 | No color difference, gel and agglomeration | With shrinkage cavity and without dark bubble |
| Comparative application example 6 | No color difference, gel and agglomeration | With shrinkage cavity and without dark bubble |
| Comparative application example 7 | No color difference, gel and agglomeration | With shrinkage cavity and without dark bubble |
| Comparative application example 8 | Has color difference, no gel and no agglomeration | No shrinkage cavity and no dark bubble |
The present application is described in detail below with reference to the test data provided in tables six and seven.
From the data in Table six, it was found that the particle diameters of the aqueous epoxy emulsions prepared in preparation examples 1 to 13 were all within 0.3 to 0.5. mu.m, which indicates that the preparation method of the present application can prepare aqueous epoxy emulsions having uniform particle diameters.
Application examples 1-9 and comparative application example 8 were compared for different routes of preparation of waterborne epoxy asphalt materials. As a result, it was found that the adhesive properties and water resistance of the aqueous epoxy asphalt materials prepared in application examples 1 to 9 were significantly improved as compared with those of comparative application example 8. This demonstrates that the preparation route of the present application helps to improve the adhesive property and water resistance of the aqueous epoxy asphalt material.
Example 9 and comparative example 1 are compared for the type of amine selected for use in preparing an aqueous epoxy emulsion. The result shows that compared with the application example 9, the adhesive force drawing strength and the composite drawing strength of the water-based epoxy asphalt material prepared in the comparative application example 1 are both obviously reduced, and the water impermeability, the alkali resistance and the salt water resistance are all obviously deteriorated; in addition, compared with the water-based epoxy asphalt material prepared in application example 1, the water-based epoxy asphalt material has the phenomena of gelation and agglomeration, and the formed paint film has shrinkage cavities and dark bubbles on the surface. The long-chain alkylamine is selected when the aqueous epoxy emulsion is prepared, so that the emulsifying effect of the aqueous epoxy emulsion is improved, and the improvement of the bonding property of the aqueous epoxy asphalt material is facilitated.
Example 9 and comparative examples 2-7 are comparative comparisons of the ratios of polyol, isocyanate and long chain alkylamine in the preparation of an aqueous epoxy emulsion. As a result, it was found that, as compared with application example 9, the adhesive force pull strength and the composite pull strength of the aqueous epoxy asphalt materials prepared in comparative application examples 2 to 7 were small, and the water impermeability, the alkali resistance and the salt water resistance were poor, and that the gel phenomenon occurred in the aqueous epoxy asphalt materials prepared in comparative application examples 2 to 7, and the surface of the formed paint film had shrinkage cavities. This shows that when preparing the aqueous epoxy emulsion, controlling the ratio of the polyol, the isocyanate and the long-chain alkylamine under the conditions of example 9 helps to improve the binding performance of the aqueous epoxy asphalt material.
Examples 1-9 are comparative with respect to the raw material ratios used in the preparation of the aqueous epoxy emulsion. As a result, the water-based epoxy asphalt materials prepared in application examples 1-9 all have high adhesive force pull strength and composite pull strength, and are good in water impermeability, alkali resistance and salt water resistance. This shows that the waterproof adhesive prepared by the aqueous epoxy emulsions of preparation examples 1 to 9 is helpful for improving the adhesion and water resistance of the aqueous epoxy asphalt material; furthermore, the water-based epoxy emulsion prepared by the raw material ratios of the preparation examples 1 to 9 is beneficial to preparing the epoxy asphalt material with better adhesive property.
Examples 9-11 are comparative with respect to the type of long chain alkyl amine used in preparing the aqueous epoxy emulsion. As a result, it was found that the aqueous epoxy asphalt materials prepared in application examples 10 and 11 were inferior in adhesive property to those prepared in application example 9, and that the aqueous epoxy asphalt materials prepared in application examples 10 and 11 were poor in gelation. This demonstrates that the use of secondary dioctadecylamine helps to reduce the gelling of the aqueous epoxy emulsion and the aqueous epoxy asphalt material.
Example 2, example 4 and example 5 are compared for the type of polyol used in preparing the aqueous epoxy emulsion. As a result, the application examples 2, 4 and 5 show that the prepared waterborne epoxy asphalt material has good adhesive property and water impermeability. This shows that, when the aqueous epoxy emulsion is prepared, in the case of using dioctadecyl secondary amine, polytetrahydrofuran glycol, polyethylene glycol or polypropylene glycol is selected, which is helpful to improve the binding property and water impermeability of the aqueous epoxy asphalt material.
Example 6, example 8, example 9 and example 12 are compared for the type of isocyanate used in preparing the aqueous epoxy emulsion. As a result, it was found that the adhesive properties and water impermeability of the aqueous epoxy asphalt materials prepared in application example 6, application example 8 and example 12 were inferior to those of application example 9. This shows that when the waterborne epoxy emulsion is prepared, the adhesive property of the waterborne epoxy asphalt material can be improved by using the isophorone diisocyanate and the toluene diisocyanate together.
Examples 9 and 13 are compared for the type of epoxy resin used in preparing the aqueous epoxy emulsion. As a result, it was found that the water-based epoxy asphalt material prepared in application example 13 was better in adhesive property than in application example 9. This shows that, when using dioctadecylsecondary amine, the combination of the epoxy resins of example 12 can improve the adhesive property of the waterborne epoxy asphalt material.
Example 9 and examples 14-19 are compared to the raw material ratios used in the preparation of the waterproof binder. As a result, the waterborne epoxy asphalt material prepared in the application example 9 and the application examples 14 to 19 has better bonding property. This shows that the waterproof binder prepared in the range of the raw material mixture ratio of example 9 and examples 14-19 can improve the binding performance of the water-based epoxy asphalt material.
Application example 9 and application examples 20-21 are directed to comparing the amount of waterproof binder employed in preparing the aqueous epoxy asphalt material. As a result, the water-based epoxy asphalt material prepared in application example 9 and application examples 19 to 20 has good adhesive property and water impermeability. This indicates that the aqueous epoxy asphalt material having good adhesive properties and water impermeability can be prepared in the range of the amount in application example 9 and application examples 19 to 20.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. The water-based epoxy emulsion is characterized by being prepared from the following components in parts by weight: 5-13 parts of polyol, 0.02-2 parts of isocyanate, 0.05-1.5 parts of long-chain alkylamine, 0.03-0.08 part of catalyst, 85-105 parts of epoxy resin and 90-125 parts of water.
2. The aqueous epoxy emulsion of claim 1, wherein: the long-chain alkylamine is at least one of dioctadecyl secondary amine, hexadecylamine and tetradecylamine.
3. The aqueous epoxy emulsion of claim 2, wherein: the polyol is prepared from the following components in parts by weight: 2-5 parts of polytetrahydrofuran glycol, 2-5 parts of polyethylene glycol and 1-3 parts of polypropylene glycol.
4. The aqueous epoxy emulsion of claim 1, wherein: the isocyanate is prepared from the following components in parts by weight: 0.01-1 part of toluene diisocyanate and 0.01-1 part of isophorone diisocyanate.
5. The aqueous epoxy emulsion of claim 1, wherein: the catalyst is organic bismuth catalyst.
6. A method of preparing the aqueous epoxy emulsion of any one of claims 1-5 comprising the steps of:
pre-polymerization: heating polyol to liquid state, mixing isocyanate with the liquid polyol, reacting at 80-85 ℃ for 2.5-3.5h, adding long-chain alkylamine, and reacting for 1.5-2.5h to obtain a prepolymer;
preparation: dividing the epoxy resin into two parts, mixing the prepolymer and the first part of the epoxy resin at the temperature of 80-85 ℃, reacting, mixing with a catalyst, and reacting to obtain an emulsifier with the isocyanate content of 0;
emulsification: and (3) mixing and heating the emulsifier and the second part of epoxy resin at 70-80 ℃ to obtain an emulsified mixture, and dripping water into the emulsified mixture under stirring to obtain the water-based epoxy emulsion.
7. The method of preparing an aqueous epoxy emulsion according to claim 6, characterized in that: in the prepolymerization step, the content of isocyanate in the prepolymer is 0-0.8%.
8. The method of preparing an aqueous epoxy emulsion according to claim 7, characterized in that: in the prepolymerization step, when the residual amount of the isocyanate is 0-2.0%, the long-chain alkylamine is added.
9. The waterproof adhesive applying the water-based epoxy emulsion as claimed in any one of claims 1 to 5, which is characterized by being prepared from the following components in parts by weight: 10-50 parts of water-based epoxy emulsion, 50-90 parts of emulsified asphalt, 0.5-1.47 parts of auxiliary agent and 8-12 parts of water.
10. The water-based epoxy asphalt material applying the waterproof binding material of claim 9 is characterized by being prepared from the following components in parts by weight: 70-153 parts of waterproof binding material and 2-5 parts of modified polyamine epoxy curing agent.
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