CN105505195A - Waterborne ultraviolet curing gloss oil and preparation method thereof - Google Patents
Waterborne ultraviolet curing gloss oil and preparation method thereof Download PDFInfo
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- CN105505195A CN105505195A CN201511018730.5A CN201511018730A CN105505195A CN 105505195 A CN105505195 A CN 105505195A CN 201511018730 A CN201511018730 A CN 201511018730A CN 105505195 A CN105505195 A CN 105505195A
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- gloss oil
- preparation
- reaction solution
- curable waterborne
- vulcabond
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- 238000002360 preparation method Methods 0.000 title claims abstract description 42
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 54
- MMCOUVMKNAHQOY-UHFFFAOYSA-N carbonoperoxoic acid Chemical compound OOC(O)=O MMCOUVMKNAHQOY-UHFFFAOYSA-N 0.000 claims abstract description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000004970 Chain extender Substances 0.000 claims abstract description 31
- 238000003756 stirring Methods 0.000 claims abstract description 31
- 150000001336 alkenes Chemical class 0.000 claims abstract description 29
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 26
- 239000004814 polyurethane Substances 0.000 claims abstract description 26
- 229920002635 polyurethane Polymers 0.000 claims abstract description 26
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 239000006185 dispersion Substances 0.000 claims abstract description 10
- 230000001804 emulsifying effect Effects 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 106
- 239000000243 solution Substances 0.000 claims description 56
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 34
- 239000003153 chemical reaction reagent Substances 0.000 claims description 28
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 23
- 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 23
- HVVWZTWDBSEWIH-UHFFFAOYSA-N [2-(hydroxymethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(COC(=O)C=C)COC(=O)C=C HVVWZTWDBSEWIH-UHFFFAOYSA-N 0.000 claims description 22
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 claims description 21
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical group CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 19
- 239000013530 defoamer Substances 0.000 claims description 17
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 16
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 14
- -1 ester ion Chemical class 0.000 claims description 14
- LHGVFZTZFXWLCP-UHFFFAOYSA-N guaiacol Chemical compound COC1=CC=CC=C1O LHGVFZTZFXWLCP-UHFFFAOYSA-N 0.000 claims description 12
- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 claims description 11
- NWVVVBRKAWDGAB-UHFFFAOYSA-N p-methoxyphenol Chemical group COC1=CC=C(O)C=C1 NWVVVBRKAWDGAB-UHFFFAOYSA-N 0.000 claims description 11
- 238000010792 warming Methods 0.000 claims description 11
- 238000013019 agitation Methods 0.000 claims description 8
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 8
- 239000000178 monomer Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 6
- 229920001610 polycaprolactone Polymers 0.000 claims description 5
- 239000004632 polycaprolactone Substances 0.000 claims description 5
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 4
- GWZMWHWAWHPNHN-UHFFFAOYSA-N 2-hydroxypropyl prop-2-enoate Chemical compound CC(O)COC(=O)C=C GWZMWHWAWHPNHN-UHFFFAOYSA-N 0.000 claims description 4
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 4
- KXBFLNPZHXDQLV-UHFFFAOYSA-N [cyclohexyl(diisocyanato)methyl]cyclohexane Chemical compound C1CCCCC1C(N=C=O)(N=C=O)C1CCCCC1 KXBFLNPZHXDQLV-UHFFFAOYSA-N 0.000 claims description 4
- 150000002009 diols Chemical class 0.000 claims description 4
- 150000002334 glycols Chemical class 0.000 claims description 4
- VLCAYQIMSMPEBW-UHFFFAOYSA-N methyl 3-hydroxy-2-methylidenebutanoate Chemical compound COC(=O)C(=C)C(C)O VLCAYQIMSMPEBW-UHFFFAOYSA-N 0.000 claims description 4
- 229920000570 polyether Polymers 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 239000008096 xylene Substances 0.000 claims description 4
- ZMARGGQEAJXRFP-UHFFFAOYSA-N 1-hydroxypropan-2-yl 2-methylprop-2-enoate Chemical compound OCC(C)OC(=O)C(C)=C ZMARGGQEAJXRFP-UHFFFAOYSA-N 0.000 claims description 3
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 3
- TUOBEAZXHLTYLF-UHFFFAOYSA-N [2-(hydroxymethyl)-2-(prop-2-enoyloxymethyl)butyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(CC)COC(=O)C=C TUOBEAZXHLTYLF-UHFFFAOYSA-N 0.000 claims description 3
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 5
- 239000012295 chemical reaction liquid Substances 0.000 abstract 8
- 239000002518 antifoaming agent Substances 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 abstract 1
- 125000005442 diisocyanate group Chemical group 0.000 abstract 1
- 239000003112 inhibitor Substances 0.000 abstract 1
- 238000006116 polymerization reaction Methods 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 238000003848 UV Light-Curing Methods 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000009775 high-speed stirring Methods 0.000 description 4
- 239000003643 water by type Substances 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- AZIQALWHRUQPHV-UHFFFAOYSA-N prop-2-eneperoxoic acid Chemical compound OOC(=O)C=C AZIQALWHRUQPHV-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000003245 working effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 125000003827 glycol group Chemical group 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- CQHKDHVZYZUZMJ-UHFFFAOYSA-N [2,2-bis(hydroxymethyl)-3-prop-2-enoyloxypropyl] prop-2-enoate Chemical group C=CC(=O)OCC(CO)(CO)COC(=O)C=C CQHKDHVZYZUZMJ-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
-
- 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
- C08G18/2815—Monohydroxy compounds
-
- 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
- C08G18/30—Low-molecular-weight compounds
- C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
- C08G18/348—Hydroxycarboxylic acids
-
- 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
- C08G18/65—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
- C08G18/6692—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/34
-
- 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
- C08G18/67—Unsaturated compounds having active hydrogen
- C08G18/6705—Unsaturated polymers not provided for in the groups C08G18/671, C08G18/6795, C08G18/68 or C08G18/69
-
- 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
- C08G18/67—Unsaturated compounds having active hydrogen
- C08G18/671—Unsaturated compounds having only one group containing active hydrogen
- C08G18/672—Esters of acrylic or alkyl acrylic acid having only one group containing active hydrogen
- C08G18/6725—Esters of acrylic or alkyl acrylic acid having only one group containing active hydrogen containing ester groups other than acrylate or alkylacrylate ester groups
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Macromonomer-Based Addition Polymer (AREA)
Abstract
The invention relates to waterborne ultraviolet curing gloss oil and a preparation method thereof. The preparation method of the waterborne ultraviolet curing gloss oil comprises the following steps: mixing diisocyanate with dihydric alcohol, and reacting, so as to obtain a first reaction liquid; adding dihydroxy carboxylic acid and a catalyst into the first reaction liquid, reacting to obtain a second reaction liquid, mixing the second reaction liquid with a chain extender, and reacting to obtain a third reaction liquid; adding an alkene end-capping agent and a polymerization inhibitor into the third reaction liquid, reacting to obtain a fourth reaction liquid, adding triethylamine into the fourth reaction liquid, and reacting to obtain a polyurethane acrylate prepolymer; and adding deionized water into the polyurethane acrylate prepolymer, emulsifying and dispersing to obtain polyurethane acrylate dispersion, mixing the polyurethane acrylate dispersion, a photoinitiator, a defoaming agent and a levelling agent, stirring and dispersing for 15-30 minutes, so that the waterborne ultraviolet curing gloss oil is obtained. The waterborne ultraviolet curing gloss oil prepared by adopting the method has relatively high performance.
Description
Technical field
The present invention relates to paint field, particularly a kind of UV-curable waterborne gloss oil and preparation method thereof.
Background technology
Along with the sustainable development of electronic technology, touch-screen obtains and applies more and more widely on the electronicss such as mobile phone, Pad, electric paper book, automatic teller machine.Different from the input method of traditional button, keyboard-type, touch input method is by instrument or points the direct object contacting the information that realizes and input with touch-screen.Especially along with the development of capacitive touch screen, the application that hand touches input mode is more and more extensive.Therefore, the work-ing life how extending touch-screen receives to be paid close attention to widely.
The method in common prolongation touch-screen work-ing life coats insulating coating in touch screen surface, stops finger to contact with the direct of screen body producing electrical signal, thus the work-ing life of prolongation touch-screen.Normally used insulating coating is the transparent gloss oil of a class UV solidification, but the coating of current UV gloss oil is all not satisfactory at hardness, resistant, the aspect of performance such as water-fast.
Summary of the invention
Based on this, be necessary to provide a kind of method can preparing the UV-curable waterborne gloss oil of better performances.
In addition, a kind of UV-curable waterborne gloss oil is also provided.
A preparation method for UV-curable waterborne gloss oil, comprises the steps:
Under the environment of protective gas, be that vulcabond mixes with dibasic alcohol by 1:0.2 ~ 0.6 according to mol ratio, in 80 ~ 90 DEG C of stirring reactions 1 ~ 2 hour, obtain the first reaction solution;
In described first reaction solution, add dihydroxy carboxylic acids and catalyzer, in 70 ~ 80 DEG C of stirring reactions 1 ~ 2 hour, obtain the second reaction solution, wherein, the mol ratio of described dihydroxy carboxylic acids and described vulcabond was 0.1 ~ 0.5:1;
Under the condition of 50 ~ 60 DEG C, by described second reaction solution and chainextender mixing, carry out chain extending reaction 2 ~ 3 hours, obtain the 3rd reaction solution;
Under the condition of 50 ~ 60 DEG C, alkene class end-capping reagent and stopper is added in described 3rd reaction solution, react after 1 hour, be warming up to 75 ~ 85 DEG C, be adjusted to appropriate viscosity with acetone, continue reaction 2 hours, obtain the 4th reaction solution, wherein, the mol ratio of described alkene class end-capping reagent and described vulcabond is 0.1 ~ 0.6:1;
Under the condition of 40 ~ 50 DEG C, in described 4th reaction solution, add triethylamine, react 0.5 ~ 1.0 hour, obtain polyurethane acrylate prepolymer, wherein, the mol ratio of described triethylamine and described dihydroxy carboxylic acids is 1 ~ 1.5:1;
Under the condition of Keep agitation, deionized water is joined in described polyurethane acrylate prepolymer, continue stirring and emulsifying dispersion 30 ~ 40 minutes, through cooling, obtain urethane acrylate dispersoid, wherein, the mass ratio of described polyurethane acrylate prepolymer and described deionized water is 30 ~ 50:40 ~ 60;
Following component is comprised: described urethane acrylate dispersoid 90 ~ 95 parts, flow agent 0.1 ~ 2 part, defoamer 0.1 ~ 2 part and light trigger 2 ~ 6 parts according to mass fraction; ; And
By described urethane acrylate dispersoid, described flow agent, described light trigger and described defoamer, dispersed with stirring 15 ~ 30 minutes, obtains UV-curable waterborne gloss oil.
Wherein in an embodiment, described vulcabond is selected from least one in Xylene Diisocyanate, dicyclohexyl methane diisocyanate, '-diphenylmethane diisocyanate, terephthalylidene vulcabond, hexamethylene diisocyanate and isophorone diisocyanate.
Wherein in an embodiment, described dibasic alcohol is selected from least one in polyether Glycols, polycaprolactone diols and PCDL.
Wherein in an embodiment, the molecular weight of described dibasic alcohol is 500g/mol, 600g/mol or 1000g/mol.
Wherein in an embodiment, described dihydroxy carboxylic acids is at least one in dimethylol propionic acid and dimethylolpropionic acid; Described catalyzer is dibutyl tin laurate.
Wherein in an embodiment, the mass ratio of described catalyzer and described dihydroxy carboxylic acids is 0.1 ~ 1:2 ~ 10.
Wherein in an embodiment, described alkene class end-capping reagent is selected from least one in hydroxyethyl methylacrylate, Hydroxyethyl acrylate, pentaerythritol triacrylate, Rocryl 410, Propylene glycol monoacrylate, trimethylolpropane diacrylate; Described stopper is p methoxy phenol.
Wherein in an embodiment, the mass ratio of described stopper and described alkene class end-capping reagent is 0.1 ~ 0.5:8 ~ 60.
Wherein in an embodiment, also comprise the preparation process of described chainextender:
Pentaerythritol triacrylate, methoxyphenol and acetone are mixed, under the condition of 45 DEG C, add isophorone diisocyanate and dibutyl tin laurate, then rise to 40 ~ 60 DEG C of reactions until the content of isocyanic ester ion is 8%, obtain the first mixed solution wherein; The acetone soln of TriMethylolPropane(TMP) is added in described first mixed solution, in 60 ~ 75 DEG C of reactions until isocyano ion disappears, obtain double bond containing glycol monomer, wherein, the mol ratio of described pentaerythritol triacrylate, described isophorone diisocyanate and described TriMethylolPropane(TMP) is 1:1:1.
The UV-curable waterborne gloss oil that the preparation method of above-mentioned UV-curable waterborne gloss oil prepares.
The preparation method of above-mentioned UV-curable waterborne gloss oil is simple to operate, is easy to suitability for industrialized production.Above-mentioned UV-curable waterborne gloss oil adopts with vulcabond, dibasic alcohol, dihydroxy carboxylic acids, chainextender, hydroxy acrylate and triethylamine as main raw material has prepared polyurethane acrylate prepolymer, by introducing UV curing groups containing double bond dibasic alcohol at molecular backbone chain side base, obtain a kind of double bond containing glycol chain extender, by introducing UV curing groups containing double bond dibasic alcohol at molecular backbone chain side base, prepare high-performance UV solidfication water polyurethane acrylate, and then obtain a kind of high performance UV-curable waterborne gloss oil.
Accompanying drawing explanation
Fig. 1 is the schema of the preparation method of the UV-curable waterborne gloss oil of an embodiment.
Embodiment
Mainly in conjunction with the drawings and the specific embodiments UV-curable waterborne gloss oil and preparation method thereof is described in further detail below.
As shown in Figure 1, the preparation method of the UV-curable waterborne gloss oil of an embodiment, comprises the steps:
Step S110: under the environment of protective gas is that vulcabond mixes with dibasic alcohol by 1:0.2 ~ 0.6 according to mol ratio, in 80 ~ 90 DEG C of stirring reactions 1 ~ 2 hour, obtains the first reaction solution.
Wherein, protective gas can be nitrogen or rare gas element.
Wherein, vulcabond is selected from least one in Xylene Diisocyanate, dicyclohexyl methane diisocyanate, '-diphenylmethane diisocyanate, terephthalylidene vulcabond, hexamethylene diisocyanate and isophorone diisocyanate.
Wherein, dibasic alcohol is selected from least one in polyether Glycols, polycaprolactone diols and PCDL.And the molecular weight of dibasic alcohol is 500g/mol, 600g/mol, 1000g/mol.
Step S120: add dihydroxy carboxylic acids and catalyzer in the first reaction solution, in 70 ~ 80 DEG C of stirring reactions 1 ~ 2 hour, obtains the second reaction solution.
Wherein, the mol ratio of dihydroxy carboxylic acids and vulcabond is 0.1 ~ 0.5:1.
Wherein, dihydroxy carboxylic acids is at least one in dimethylol propionic acid and dimethylolpropionic acid.
Wherein, catalyzer is dibutyl tin laurate.Wherein, the mass ratio of catalyzer and dihydroxy carboxylic acids is 0.1 ~ 1:2 ~ 10.
Step S130: under the condition of 50 ~ 60 DEG C, by the second reaction solution and chainextender mixing, carries out chain extending reaction 2 ~ 3 hours, obtains the 3rd reaction solution.
Wherein, chainextender is double bond containing glycol monomer.
Concrete, chainextender prepares by following preparation process: pentaerythritol triacrylate, methoxyphenol and acetone are mixed, under the condition of 45 DEG C, add isophorone diisocyanate and dibutyl tin laurate, then rise to 40 ~ 60 DEG C of reactions until the content of isocyanic ester ion is 8%, obtain the first mixed solution wherein; The acetone soln of TriMethylolPropane(TMP) is added in the first mixed solution, in 60 ~ 75 DEG C of reactions until isocyanic ester ion disappears, obtain double bond containing glycol monomer.Wherein, the mol ratio of pentaerythritol triacrylate, isophorone diisocyanate and TriMethylolPropane(TMP) is 1:1:1.
Wherein, the quality of methoxyphenol and the mass ratio of pentaerythritol triacrylate are 0.5:100.
Wherein, the mass ratio of dibutyl tin laurate and isophorone diisocyanate is 0.08:100.
Wherein, the mol ratio of chainextender and vulcabond is 0.1 ~ 0.3:1.
Wherein, the synthesis path of chainextender is as follows: step S140: under the condition of 50 ~ 60 DEG C, in the 3rd reaction solution, add alkene class end-capping reagent and stopper, react after 1 hour, be warming up to 75 ~ 85 DEG C, be adjusted to appropriate viscosity with acetone, continue reaction 2 hours, obtain the 4th reaction solution.
Wherein, the mol ratio of alkene class end-capping reagent and vulcabond is 0.1 ~ 0.6:1.
Wherein, alkene class end-capping reagent is selected from least one in hydroxyethyl methylacrylate, Hydroxyethyl acrylate, pentaerythritol triacrylate, Rocryl 410, Propylene glycol monoacrylate, trimethylolpropane diacrylate.
Wherein, stopper is p methoxy phenol.
Wherein, the mass ratio of stopper and alkene class end-capping reagent is 0.1 ~ 0.5:8 ~ 60.
Step S150: under the condition of 40 ~ 50 DEG C, adds triethylamine in described 4th reaction solution, reacts 0.5 ~ 1.0 hour, obtains polyurethane acrylate prepolymer.
Wherein, the mol ratio of triethylamine and dihydroxy carboxylic acids is 1 ~ 1.5:1.
Step S160: under the condition of Keep agitation, joins deionized water in polyurethane acrylate prepolymer, continues stirring and emulsifying dispersion 30 ~ 40 minutes, through cooling, obtains urethane acrylate dispersoid.
Wherein, the mass ratio of polyurethane acrylate prepolymer and deionized water is 30 ~ 50:40 ~ 60.
In step S160, it is 300 ~ 400 revs/min in the speed of the condition of Keep agitation; Continuing the stirring and emulsifying dispersion stirring velocity of 30 ~ 40 minutes is 400 ~ 600 revs/min.
Step S170: comprise following component according to mass fraction: described urethane acrylate dispersoid 90 ~ 95 parts, flow agent 0.1 ~ 2 part, defoamer 0.1 ~ 2 part and light trigger 2 ~ 6 parts.。
Wherein, flow agent is selected from least one in BYK346, BYK333, BYK301 and BYK307.Defoamer is the defoamer that this area is commonly used, and defoamer is selected from least one in BYK024, BYK028, BYK022 and BYK093.
Wherein, light trigger is selected from least one in 907,184,1173,2959 and 754.
Step S180: by urethane acrylate dispersoid, flow agent, light trigger and defoamer, dispersed with stirring 15 ~ 30 minutes, obtains UV-curable waterborne gloss oil.
The preparation method of above-mentioned UV-curable waterborne gloss oil is simple to operate, is easy to suitability for industrialized production.Above-mentioned UV-curable waterborne gloss oil adopts with vulcabond, dibasic alcohol, dihydroxy carboxylic acids, chainextender, hydroxy acrylate and triethylamine as main raw material has prepared polyurethane acrylate prepolymer, by introducing UV curing groups containing double bond dibasic alcohol at molecular backbone chain side base, prepare high performance UV-curable waterborne gloss oil.
A kind of UV-curable waterborne gloss oil prepared by the preparation method of above-mentioned UV-curable waterborne gloss oil.Above-mentioned UV-curable waterborne gloss oil adopts with vulcabond, dibasic alcohol, dihydroxy carboxylic acids, chainextender, hydroxy acrylate and triethylamine as main raw material has prepared polyurethane acrylate prepolymer, by introducing UV curing groups containing double bond dibasic alcohol at molecular backbone chain side base, obtain a kind of double bond containing glycol chain extender, by introducing UV curing groups containing double bond dibasic alcohol at molecular backbone chain side base, prepare high-performance UV solidfication water polyurethane acrylate, and then obtain a kind of high performance UV-curable waterborne gloss oil.
It is below specific embodiment part.
Embodiment 1
The preparation process of the UV-curable waterborne gloss oil of the present embodiment is as follows:
(1) preparation of chainextender: pentaerythritol triacrylate and methoxyphenol (MEHQ) are proceeded to the acetone of 10g in the there-necked flask that thermometer, prolong and agitator are housed, wherein, the quality of methoxyphenol and the mass ratio of pentaerythritol triacrylate are 0.5:100; Then be placed in 45 DEG C of waters bath with thermostatic control, constant pressure funnel is utilized dropwise to be joined in there-necked flask by isophorone diisocyanate, add dibutyl tin laurate (DBTAL) simultaneously and carry out catalysis, then rise to 55 DEG C of reaction 2h, the content to the isocyanic ester ion in system is 8%.By in TriMethylolPropane(TMP) constant voltage instillation reaction system, be warming up to 65 DEG C of reaction 3h, isocyanic ester ion in question response system disappears, discharging, obtain colourless or lurid double bond containing glycol monomer, be chainextender, wherein, the mass ratio of dibutyl tin laurate and isophorone diisocyanate is 0.08:100; The mol ratio of pentaerythritol triacrylate, isophorone diisocyanate and TriMethylolPropane(TMP) is 1:1:1.
(2) preparation of urethane acrylate dispersoid:
1, under logical nitrogen protection condition, to in the four mouthfuls of round reaction flasks being placed with thermometer, prolong, stirring rod, add vulcabond and dibasic alcohol, 80 DEG C of stirring reactions 2 hours, obtain the first reaction solution, wherein, the mol ratio of vulcabond and dibasic alcohol is 1:0.6, and vulcabond is selected from Xylene Diisocyanate; Dibasic alcohol is selected from polyether Glycols; The molecular weight of dibasic alcohol is 1000g/mol.
2, in the first reaction solution, add dihydroxy carboxylic acids and catalyzer, in 70 DEG C of stirring reactions 2 hours, obtain the second reaction solution.Wherein, the mol ratio of dihydroxy carboxylic acids and vulcabond is 0.1:1, and dihydroxy carboxylic acids is dimethylol propionic acid, and catalyzer is dibutyl tin laurate, and the mass ratio of catalyzer and dihydroxy carboxylic acids is 0.1:2.
3, be cooled to 50 DEG C, adopt constant pressure funnel to add in the second reaction solution by chainextender prepared by step (1), carry out chain extending reaction 2 hours, obtain the 3rd reaction solution.Wherein, the mol ratio of chainextender and vulcabond is 0.1:1.
4, under the condition of 50 DEG C, in the 3rd reaction solution, add alkene class end-capping reagent and stopper, react after 1 hour, be warming up to 75 DEG C, be adjusted to appropriate viscosity with acetone, continue reaction 2 hours, obtain the 4th reaction solution.Wherein, the mol ratio of alkene class end-capping reagent and vulcabond is 0.2:1; Alkene class end-capping reagent is selected from hydroxyethyl methylacrylate; Stopper is p methoxy phenol; The mass ratio of stopper and alkene class end-capping reagent is 0.1:8.
5, under the condition of 40 DEG C, in described 4th reaction solution, add triethylamine, react 0.5 hour, obtain transparent polyurethane acrylate prepolymer.Wherein, the mol ratio of triethylamine and dihydroxy carboxylic acids is 1:1.
6, under the condition of 300 revs/min of Keep agitation, deionized water is joined in polyurethane acrylate prepolymer, continue to disperse 30 minutes with the speed stirring and emulsifying of 400 revs/min, through cooling, obtain urethane acrylate dispersoid.
(3) preparation of UV-curable waterborne gloss oil:
1, following component is taken according to mass fraction:
2, according to said ratio, urethane acrylate dispersoid, light trigger, flow agent and defoamer are added in dispersion cylinder and mixes, high-speed stirring disperses 15 minutes, cross 200 mesh sieves, namely obtain UV-curable waterborne gloss oil, wherein, light trigger is selected from 907, defoamer is selected from BYK024, and flow agent is selected from BYK346.
The performance of the UV-curable waterborne gloss oil UV-light of the present embodiment is in table 1.
Embodiment 2
The preparation process of the UV-curable waterborne gloss oil of the present embodiment is as follows:
(1) preparation of chainextender: pentaerythritol triacrylate and methoxyphenol (MEHQ) are proceeded to the acetone of 10g in the there-necked flask that thermometer, prolong and agitator are housed, wherein, the quality of methoxyphenol and the mass ratio of pentaerythritol triacrylate are 0.5:100; Then be placed in 45 DEG C of waters bath with thermostatic control, constant pressure funnel is utilized dropwise to be joined in there-necked flask by isophorone diisocyanate, add dibutyl tin laurate (DBTAL) simultaneously and carry out catalysis, then rise to 55 DEG C of reaction 2h, the content to the isocyanic ester ion in system is 8%.By in TriMethylolPropane(TMP) constant voltage instillation reaction system, be warming up to 65 DEG C of reaction 3h, isocyanic ester ion in question response system disappears, discharging, obtain colourless or lurid double bond containing glycol monomer, be chainextender, wherein, the mass ratio of dibutyl tin laurate and isophorone diisocyanate is 0.08:100; The mol ratio of pentaerythritol triacrylate, isophorone diisocyanate and TriMethylolPropane(TMP) is 1:1:1.
(2) preparation of urethane acrylate dispersoid:
1, under logical nitrogen protection condition, to in the four mouthfuls of round reaction flasks being placed with thermometer, prolong, stirring rod, add vulcabond and dibasic alcohol, 90 DEG C of stirring reactions 1 hour, obtain the first reaction solution, wherein, the mol ratio of vulcabond and dibasic alcohol is 1:0.3, and vulcabond is selected from dicyclohexyl methane diisocyanate; Dibasic alcohol is selected from polycaprolactone diols; The molecular weight of dibasic alcohol is 500g/mol.
2, in the first reaction solution, add dihydroxy carboxylic acids and catalyzer, in 80 DEG C of stirring reactions 1 hour, obtain the second reaction solution.Wherein, the mol ratio of dihydroxy carboxylic acids and vulcabond is 0.4:1, and dihydroxy carboxylic acids is in dimethylolpropionic acid, and catalyzer is dibutyl tin laurate, and the mass ratio of catalyzer and dihydroxy carboxylic acids is 1:10.
3, be cooled to 60 DEG C, adopt constant pressure funnel to add in the second reaction solution by chainextender prepared by step (1), carry out chain extending reaction 3 hours, obtain the 3rd reaction solution.Wherein, the mol ratio of chainextender and vulcabond is 0.3:1.
4, under the condition of 60 DEG C, in the 3rd reaction solution, add alkene class end-capping reagent and stopper, react after 1 hour, be warming up to 85 DEG C, with acetone adjusting viscosity to suitable, continue reaction 2 hours, obtain the 4th reaction solution.Wherein, the mol ratio of alkene class end-capping reagent and vulcabond is 0.1:1; Alkene class end-capping reagent is selected from Hydroxyethyl acrylate; Stopper is p methoxy phenol; The mass ratio of stopper and alkene class end-capping reagent is 0.5:80.
5, under the condition of 50 DEG C, in described 4th reaction solution, add triethylamine, react and obtain transparent polyurethane acrylate prepolymer in 1.0 hours.Wherein, the mol ratio of triethylamine and dihydroxy carboxylic acids is 1.5:1.
6, under the condition of 400 revs/min of Keep agitation, deionized water is joined in polyurethane acrylate prepolymer, continue to disperse 40 minutes with the speed stirring and emulsifying of 600 revs/min, through cooling, obtain urethane acrylate dispersoid.
(3) preparation of UV-curable waterborne gloss oil:
1, following component is taken according to mass fraction:
2, according to said ratio, urethane acrylate dispersoid, light trigger, flow agent and defoamer are added in dispersion cylinder and mixes, high-speed stirring disperses 30 minutes, cross 400 mesh sieves, namely obtain UV-curable waterborne gloss oil, wherein, light trigger is selected from 184, defoamer is selected from BYK028, and flow agent is selected from BYK346.
The identical testing method of embodiment 1 is adopted to obtain the performance of the UV-curable waterborne gloss oil of the present embodiment in table 1.
Embodiment 3
The preparation process of the UV-curable waterborne gloss oil of the present embodiment is as follows:
(1) preparation of chainextender: pentaerythritol triacrylate and methoxyphenol (MEHQ) are proceeded to the acetone of 10g in the there-necked flask that thermometer, prolong and agitator are housed, wherein, the quality of methoxyphenol and the mass ratio of pentaerythritol triacrylate are 0.5:100; Then be placed in 45 DEG C of waters bath with thermostatic control, constant pressure funnel is utilized dropwise to be joined in there-necked flask by isophorone diisocyanate, add dibutyl tin laurate DBTAL simultaneously) carry out catalysis, then rise to 55 DEG C of reaction 2h, the content to the isocyanic ester ion in system is 8%.By in TriMethylolPropane(TMP) constant voltage instillation reaction system, be warming up to 65 DEG C of reaction 3h, isocyanic ester ion in question response system disappears, discharging, obtain colourless or lurid double bond containing glycol monomer, be chainextender, wherein, the mass ratio of dibutyl tin laurate and isophorone diisocyanate is 0.08:100; The mol ratio of pentaerythritol triacrylate, isophorone diisocyanate and TriMethylolPropane(TMP) is 1:1:1.
(2) preparation of urethane acrylate dispersoid:
1, under logical nitrogen protection condition, to in the four mouthfuls of round reaction flasks being placed with thermometer, prolong, stirring rod, add vulcabond and dibasic alcohol, 82 DEG C of stirring reactions 1.5 hours, obtain the first reaction solution, wherein, the mol ratio of vulcabond and dibasic alcohol is 1:0.2, and vulcabond is selected from '-diphenylmethane diisocyanate; Dibasic alcohol is selected from PCDL; The molecular weight of dibasic alcohol is 1000g/mol.
2, in the first reaction solution, add dihydroxy carboxylic acids and catalyzer, in 75 DEG C of stirring reactions 1.5 hours, obtain the second reaction solution.Wherein, the mol ratio of dihydroxy carboxylic acids and vulcabond is 0.2:1, and dihydroxy carboxylic acids is at least one in dimethylol propionic acid and dimethylolpropionic acid, and catalyzer is dibutyl tin laurate, and the mass ratio of catalyzer and dihydroxy carboxylic acids is 0.5:8.
3, be cooled to 55 DEG C, adopt constant pressure funnel to add in the second reaction solution by chainextender prepared by step (1), carry out chain extending reaction 2.5 hours, obtain the 3rd reaction solution.Wherein, the mol ratio of chainextender and vulcabond is 0.2:1.
4, under the condition of 55 DEG C, in the 3rd reaction solution, add alkene class end-capping reagent and stopper, react after 1 hour, be warming up to 80 DEG C, with acetone adjusting viscosity to suitable, continue reaction 2 hours, obtain the 4th reaction solution.Wherein, the mol ratio of alkene class end-capping reagent and vulcabond is 0.4:1; Alkene class end-capping reagent is selected from pentaerythritol diacrylate; Stopper is p methoxy phenol; The mass ratio of stopper and alkene class end-capping reagent is 0.3:40.
5, under the condition of 45 DEG C, in described 4th reaction solution, add triethylamine, react 0.6 hour, obtain transparent polyurethane acrylate prepolymer.Wherein, the mol ratio of triethylamine and dihydroxy carboxylic acids is 1.2:1.
6, under the condition of 350 revs/min of Keep agitation, deionized water is joined in polyurethane acrylate prepolymer, continue to disperse 35 minutes with the speed stirring and emulsifying of 500 revs/min, through cooling, obtain urethane acrylate dispersoid.
(3) preparation of UV-curable waterborne gloss oil:
1, following component is taken according to mass fraction:
2, according to said ratio, urethane acrylate dispersoid, light trigger, flow agent and defoamer are added in dispersion cylinder and mixes, high-speed stirring disperses 15 minutes, cross 400 mesh sieves, namely obtain UV-curable waterborne gloss oil, wherein, light trigger is selected from 2959, defoamer is selected from BYK093, and flow agent is selected from least one in BYK307.
The identical testing method of embodiment 1 is adopted to obtain the performance of the UV-curable waterborne gloss oil of the present embodiment in table 1.
Embodiment 4
The preparation process of the UV-curable waterborne gloss oil of the present embodiment is as follows:
(1) preparation of chainextender: pentaerythritol triacrylate and methoxyphenol (MEHQ) are proceeded to the acetone of 10g in the there-necked flask that thermometer, prolong and agitator are housed, wherein, the quality of methoxyphenol and the mass ratio of pentaerythritol triacrylate are 0.5:100; Then be placed in 45 DEG C of waters bath with thermostatic control, constant pressure funnel is utilized dropwise to be joined in there-necked flask by isophorone diisocyanate, add dibutyl tin laurate (DBTAL) simultaneously and carry out catalysis, then rise to 55 DEG C of reaction 2h, the content to the isocyanic ester ion in system is 8%.65 DEG C of reaction 3h are warming up to by TriMethylolPropane(TMP) constant voltage instillation reaction system, isocyanic ester ion in question response system disappears, discharging, obtain colourless or lurid double bond containing glycol monomer, be chainextender, wherein, the mass ratio of dibutyl tin laurate and isophorone diisocyanate is 0.08:100; The mol ratio of pentaerythritol triacrylate, isophorone diisocyanate and TriMethylolPropane(TMP) is 1:1:1.
(2) preparation of urethane acrylate dispersoid:
1, under logical nitrogen protection condition, to in the four mouthfuls of round reaction flasks being placed with thermometer, prolong, stirring rod, add vulcabond and dibasic alcohol, 85 DEG C of stirring reactions 1.5 hours, obtain the first reaction solution, wherein, the mol ratio of vulcabond and dibasic alcohol is 1:0.2, and vulcabond is selected from isophorone diisocyanate; Dibasic alcohol is selected from poly-polycaprolactone; The molecular weight of dibasic alcohol is 1000g/mol.
2, in the first reaction solution, add dihydroxy carboxylic acids and catalyzer, in 70 DEG C of stirring reactions 1.5 hours, obtain the second reaction solution.Wherein, the mol ratio of dihydroxy carboxylic acids and vulcabond is 0.3:1, and dihydroxy carboxylic acids is dimethylol propionic acid, and catalyzer is dibutyl tin laurate, and the mass ratio of catalyzer and dihydroxy carboxylic acids is 0.6:7.
3, be cooled to 55 DEG C, adopt constant pressure funnel to add in the second reaction solution by chainextender prepared by step (1), carry out chain extending reaction 2.5 hours, obtain the 3rd reaction solution.Wherein, the mol ratio of chainextender and vulcabond is 0.2:1.
4, under the condition of 55 DEG C, in the 3rd reaction solution, add alkene class end-capping reagent and stopper, react after 1 hour, be warming up to 80 DEG C, be adjusted to appropriate viscosity with acetone, continue reaction 2 hours, obtain the 4th reaction solution.Wherein, the mol ratio of alkene class end-capping reagent and vulcabond is 0.4:1; Alkene class end-capping reagent is selected from Propylene glycol monoacrylate; Stopper is p methoxy phenol; The mass ratio of stopper and alkene class end-capping reagent is 0.4:55.
5, under the condition of 45 DEG C, in described 4th reaction solution, add triethylamine, react 0.6 hour, obtain transparent polyurethane acrylate prepolymer.Wherein, the mol ratio of triethylamine and dihydroxy carboxylic acids is 1.3:1.
6, under the condition of 300 revs/min of Keep agitation, deionized water is joined in polyurethane acrylate prepolymer, continue to disperse 30 minutes with the speed stirring and emulsifying of 400 revs/min, through cooling, obtain urethane acrylate dispersoid.
(3) preparation of UV-curable waterborne gloss oil:
1, following component is taken according to mass fraction:
2, according to said ratio, urethane acrylate dispersoid, light trigger, flow agent and defoamer are added in dispersion cylinder and mixes, high-speed stirring disperses 15 minutes, cross 200 mesh sieves, namely obtain UV-curable waterborne gloss oil, wherein, light trigger is selected from 754, defoamer is selected from BYK093, and flow agent is selected from BYK307.
The identical testing method of embodiment 1 is adopted to obtain the performance of the UV-curable waterborne gloss oil of the present embodiment in table 1.
What table 1 represented is the performance of the UV-curable waterborne gloss oil of embodiment 1 ~ 4.
Table 1
Obvious above-mentioned UV-curable waterborne gloss oil possesses good performance.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a preparation method for UV-curable waterborne gloss oil, is characterized in that, comprises the steps:
Under the environment of protective gas, be that vulcabond mixes with dibasic alcohol by 1:0.2 ~ 0.6 according to mol ratio, in 80 ~ 90 DEG C of stirring reactions 1 ~ 2 hour, obtain the first reaction solution;
In described first reaction solution, add dihydroxy carboxylic acids and catalyzer, in 70 ~ 80 DEG C of stirring reactions 1 ~ 2 hour, obtain the second reaction solution, wherein, the mol ratio of described dihydroxy carboxylic acids and described vulcabond was 0.1 ~ 0.5:1;
Under the condition of 50 ~ 60 DEG C, by described second reaction solution and chainextender mixing, carry out chain extending reaction 2 ~ 3 hours, obtain the 3rd reaction solution;
Under the condition of 50 ~ 60 DEG C, alkene class end-capping reagent and stopper is added in described 3rd reaction solution, react after 1 hour, be warming up to 75 ~ 85 DEG C, be adjusted to appropriate viscosity with acetone and continue reaction 2 hours, obtain the 4th reaction solution, wherein, the mol ratio of described alkene class end-capping reagent and described vulcabond is 0.1 ~ 0.6:1;
Under the condition of 40 ~ 50 DEG C, in described 4th reaction solution, add triethylamine, react 0.5 ~ 1.0 hour, obtain polyurethane acrylate prepolymer, wherein, the mol ratio of described triethylamine and described dihydroxy carboxylic acids is 1 ~ 1.5:1;
Under the condition of Keep agitation, deionized water is joined in described polyurethane acrylate prepolymer, continue stirring and emulsifying dispersion 30 ~ 40 minutes, through cooling, obtain urethane acrylate dispersoid, wherein, the mass ratio of described polyurethane acrylate prepolymer and described deionized water is 30 ~ 50:40 ~ 60;
Following component is comprised: described urethane acrylate dispersoid 90 ~ 95 parts, flow agent 0.1 ~ 2 part, defoamer 0.1 ~ 2 part and light trigger 2 ~ 6 parts according to mass fraction; And
By described urethane acrylate dispersoid, described flow agent, described light trigger and described defoamer, dispersed with stirring 15 ~ 30 minutes, obtains UV-curable waterborne gloss oil.
2. the preparation method of UV-curable waterborne gloss oil according to claim 1, it is characterized in that, described vulcabond is selected from least one in Xylene Diisocyanate, dicyclohexyl methane diisocyanate, '-diphenylmethane diisocyanate, terephthalylidene vulcabond, hexamethylene diisocyanate and isophorone diisocyanate.
3. the preparation method of UV-curable waterborne gloss oil according to claim 1, is characterized in that, described dibasic alcohol is selected from least one in polyether Glycols, polycaprolactone diols and PCDL.
4. the preparation method of UV-curable waterborne gloss oil according to claim 1, is characterized in that, the molecular weight of described dibasic alcohol is 500g/mol, 600g/mol or 1000g/mol.
5. the preparation method of UV-curable waterborne gloss oil according to claim 1, is characterized in that, described dihydroxy carboxylic acids is at least one in dimethylol propionic acid and dimethylolpropionic acid; Described catalyzer is dibutyl tin laurate.
6. the preparation method of UV-curable waterborne gloss oil according to claim 5, is characterized in that, the mass ratio of described catalyzer and described dihydroxy carboxylic acids is 0.1 ~ 1:2 ~ 10.
7. the preparation method of UV-curable waterborne gloss oil according to claim 1, it is characterized in that, described alkene class end-capping reagent is selected from least one in hydroxyethyl methylacrylate, Hydroxyethyl acrylate, pentaerythritol triacrylate, Rocryl 410, Propylene glycol monoacrylate, trimethylolpropane diacrylate; Described stopper is p methoxy phenol.
8. the preparation method of UV-curable waterborne gloss oil according to claim 1, is characterized in that, the mass ratio of described stopper and described alkene class end-capping reagent is 0.1 ~ 0.5:8 ~ 60.
9. the preparation method of UV-curable waterborne gloss oil according to claim 1, is characterized in that, also comprises the preparation process of described chainextender:
Pentaerythritol triacrylate, methoxyphenol and acetone are mixed, under the condition of 45 DEG C, add isophorone diisocyanate and dibutyl tin laurate, then rise to 50 ~ 60 DEG C of reactions until the content of isocyanic ester ion is 8%, obtain the first mixed solution wherein; The acetone soln of TriMethylolPropane(TMP) is added in described first mixed solution, in 60 ~ 75 DEG C of reactions until isocyano ion disappears, obtain double bond containing glycol monomer, wherein, the mol ratio of described pentaerythritol triacrylate, described isophorone diisocyanate and described TriMethylolPropane(TMP) is 1:1:1.
10. the UV-curable waterborne gloss oil for preparing of the preparation method of a UV-curable waterborne gloss oil as claimed in any one of claims 1 to 9 wherein.
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| CN110105865A (en) * | 2019-05-30 | 2019-08-09 | 江苏美乔科技有限公司 | A kind of environment protection damp-proof UV oil polish and preparation method thereof |
| CN117210119A (en) * | 2023-10-19 | 2023-12-12 | 湖南汇华新材料有限公司 | Water-based UV preprinting gloss oil |
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| CN1844182A (en) * | 2006-03-22 | 2006-10-11 | 中国科学技术大学 | Process for preparing ultraviolet curable aqueous polyurethane resin |
| CN101423677A (en) * | 2008-12-18 | 2009-05-06 | 江南大学 | Method for preparing transparent and heat insulating water ultraviolet curing coating |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1844182A (en) * | 2006-03-22 | 2006-10-11 | 中国科学技术大学 | Process for preparing ultraviolet curable aqueous polyurethane resin |
| CN101423677A (en) * | 2008-12-18 | 2009-05-06 | 江南大学 | Method for preparing transparent and heat insulating water ultraviolet curing coating |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110105865A (en) * | 2019-05-30 | 2019-08-09 | 江苏美乔科技有限公司 | A kind of environment protection damp-proof UV oil polish and preparation method thereof |
| CN117210119A (en) * | 2023-10-19 | 2023-12-12 | 湖南汇华新材料有限公司 | Water-based UV preprinting gloss oil |
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| TA01 | Transfer of patent application right |
Effective date of registration: 20180227 Address after: 246400 Taihu County Anhui province Anqing City Jin Xi Zhen Jin Hu villa 1 Building 1, room 71 Applicant after: Jia Xueming Address before: 518000 Guangdong city of Shenzhen province Futian District Che Kung Temple Cheonan Digital City Futian Tian technology building A room 402 Applicant before: Sword Defense Technology Group Limited |
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| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Liu Jian Inventor after: Yao Zhigang Inventor after: Jing Mei Inventor after: Zhang Junhua Inventor after: Jia Xueming Inventor before: Liu Jian Inventor before: Yao Zhigang Inventor before: Jing Mei Inventor before: Zhang Junhua |
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| CI02 | Correction of invention patent application | ||
| CI02 | Correction of invention patent application |
Correction item: Inventor Correct: Liu Jian|Yao Zhigang|Jing Mei|Zhang Junhua False: Liu Jian|Yao Zhigang|Jing Mei|Jia Xueming Number: 11-02 Volume: 34 Correction item: Applicant|Address Correct: Sword Defense Technology Group Limited|518000 Guangdong city of Shenzhen province Futian District Che Kung Temple Cheonan Digital City Futian Tian technology building A room 402 False: Jia Xueming|246400 Taihu County Anhui province Anqing City Jin Xi Zhen Jin Hu villa 1 Building 1, room 71 Number: 11-02 Volume: 34 |
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| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20180322 Address after: 246400 Taihu County Anhui province Anqing City Jin Xi Zhen Jin Hu villa 1 Building 1, room 71 Applicant after: Jia Xueming Address before: 518000 Guangdong city of Shenzhen province Futian District Che Kung Temple Cheonan Digital City Futian Tian technology building A room 402 Applicant before: Sword Defense Technology Group Limited |
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| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20190508 Address after: 518172 Gekeng Industrial Park, 12 Huanping Road, Gaoqiao Community, Pingdi Street, Longgang District, Shenzhen City, Guangdong Province Patentee after: Shenzhen Li Jian Bona Technology Co., Ltd. Address before: 246400 71, room 1, Jinhu villa, Jinxi Town, Taihu County, Anqing, Anhui, China, 1 Patentee before: Jia Xueming |