CN104448206B - A kind of environment-friendly type strippable water-soluble polyurethane resin and its preparation method and application - Google Patents
A kind of environment-friendly type strippable water-soluble polyurethane resin and its preparation method and application Download PDFInfo
- Publication number
- CN104448206B CN104448206B CN201410826926.6A CN201410826926A CN104448206B CN 104448206 B CN104448206 B CN 104448206B CN 201410826926 A CN201410826926 A CN 201410826926A CN 104448206 B CN104448206 B CN 104448206B
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- China
- Prior art keywords
- polyurethane resin
- environment
- friendly type
- soluble polyurethane
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 229920005749 polyurethane resin Polymers 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000004970 Chain extender Substances 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 16
- -1 siloxanes Chemical class 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 230000018044 dehydration Effects 0.000 claims abstract description 9
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 9
- 239000012948 isocyanate Substances 0.000 claims abstract description 8
- 150000003384 small molecules Chemical group 0.000 claims abstract description 8
- 239000004593 Epoxy Substances 0.000 claims abstract description 7
- 230000004044 response Effects 0.000 claims abstract description 7
- 125000005442 diisocyanate group Chemical group 0.000 claims abstract description 6
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 32
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 14
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 7
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 6
- 235000019260 propionic acid Nutrition 0.000 claims description 6
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 6
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 5
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 5
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 5
- 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 5
- BJZYYSAMLOBSDY-QMMMGPOBSA-N (2s)-2-butoxybutan-1-ol Chemical compound CCCCO[C@@H](CC)CO BJZYYSAMLOBSDY-QMMMGPOBSA-N 0.000 claims description 4
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 claims description 3
- 229920001610 polycaprolactone Polymers 0.000 claims description 3
- 239000004632 polycaprolactone Substances 0.000 claims description 3
- 229920001451 polypropylene glycol Polymers 0.000 claims description 3
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-L adipate(2-) Chemical compound [O-]C(=O)CCCCC([O-])=O WNLRTRBMVRJNCN-UHFFFAOYSA-L 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 229920001748 polybutylene Polymers 0.000 claims description 2
- GGHDAUPFEBTORZ-UHFFFAOYSA-N propane-1,1-diamine Chemical compound CCC(N)N GGHDAUPFEBTORZ-UHFFFAOYSA-N 0.000 claims description 2
- 125000003396 thiol group Chemical class [H]S* 0.000 claims description 2
- 229960001124 trientine Drugs 0.000 claims description 2
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 claims 2
- RNLHGQLZWXBQNY-UHFFFAOYSA-N 3-(aminomethyl)-3,5,5-trimethylcyclohexan-1-amine Chemical compound CC1(C)CC(N)CC(C)(CN)C1 RNLHGQLZWXBQNY-UHFFFAOYSA-N 0.000 claims 1
- 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 claims 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical class OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims 1
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical class OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims 1
- 229920005989 resin Polymers 0.000 abstract description 11
- 239000011347 resin Substances 0.000 abstract description 11
- 238000000034 method Methods 0.000 abstract description 6
- 150000002513 isocyanates Chemical class 0.000 abstract description 5
- 239000000839 emulsion Substances 0.000 abstract description 4
- 229920002635 polyurethane Polymers 0.000 abstract description 4
- 239000004814 polyurethane Substances 0.000 abstract description 4
- 238000004132 cross linking Methods 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract description 2
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 239000002585 base Substances 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 238000010907 mechanical stirring Methods 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N Furan Chemical compound C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000004566 building material Substances 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- HJOVHMDZYOCNQW-UHFFFAOYSA-N isophorone Chemical compound CC1=CC(=O)CC(C)(C)C1 HJOVHMDZYOCNQW-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000002633 protecting effect Effects 0.000 description 2
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 2
- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 description 1
- GTACSIONMHMRPD-UHFFFAOYSA-N 2-[4-[2-(benzenesulfonamido)ethylsulfanyl]-2,6-difluorophenoxy]acetamide Chemical compound C1=C(F)C(OCC(=O)N)=C(F)C=C1SCCNS(=O)(=O)C1=CC=CC=C1 GTACSIONMHMRPD-UHFFFAOYSA-N 0.000 description 1
- DBXBTMSZEOQQDU-UHFFFAOYSA-N 3-hydroxyisobutyric acid Chemical compound OCC(C)C(O)=O DBXBTMSZEOQQDU-UHFFFAOYSA-N 0.000 description 1
- 101710130081 Aspergillopepsin-1 Proteins 0.000 description 1
- 102100031007 Cytosolic non-specific dipeptidase Human genes 0.000 description 1
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical class NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- 241000276489 Merlangius merlangus Species 0.000 description 1
- 241000255964 Pieridae Species 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 125000003916 ethylene diamine group Chemical group 0.000 description 1
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical class OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000004922 lacquer Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C—CHEMISTRY; METALLURGY
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08G18/4277—Caprolactone and/or substituted caprolactone
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- C08G18/4808—Mixtures of two or more polyetherdiols
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- 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
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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
- 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
- C09D175/06—Polyurethanes from polyesters
-
- 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
- C09D175/08—Polyurethanes from polyethers
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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
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/20—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for coatings strippable as coherent films, e.g. temporary coatings strippable as coherent films
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Abstract
The invention belongs to aqueous polyurethane preparing technical field, a kind of environment-friendly type strippable water-soluble polyurethane resin and its preparation method and application is disclosed.The preparation method includes step in detail below：Oligomer dihydric alcohol after dehydration and diisocyanate Hybrid Heating are reacted；Add small molecule chain extender, hydrophilic chain extender, heating response；Nertralizer, latent curing agent, water, rear chain extender are sequentially added under stirring, is stirred, that is, obtains environment-friendly type strippable water-soluble polyurethane resin；Described latent curing agent includes at least one of blocked isocyanate class and the siloxanes containing epoxy radicals.Latent curing agent is added in system of the present invention; with the reaction of hydrophilic radical present in resin system so as to remove hydrophilic radical during emulsion film forming; assign resin splendid water resistance; and latent curing agent crosslinking curing again in film forming procedure; further improve the combination property of resin; there is provided permanently effective protective value for the service life of extension film.
Description
Technical field
The invention belongs to aqueous polyurethane preparing technical field, more particularly to a kind of environment-friendly type strippable water-soluble polyurethane tree
Fat and its preparation method and application.
Background technology
With the continuous improvement of living standard, people also exist to the requirement such as outward appearance, the feature of environmental protection and its performance of product
Increasingly increase.Manufacturer can be in the material surface additional layer protective coating such as glass, ceramics, metal building material, to avoid it from adding
It is scraped off during work, transport and assembling etc., so that influenceing its aesthetics, or even reduces its performance.
The base resin that most of Stripable paint is used in the market be still it is solvent type, its production, construction and
Environment and human body can be polluted and injured during use, run counter to the idea of development of environmental protection.Though there is fraction
Aqueous product is the problem of using, but also expose many：(1) in use, coating can not be bonded all the time with base material
Together, it is easy to fall off；(2) strength of coating not enough, is difficult full wafer stripping；(3) hydrophilic chain extender is as internal emulsifying agent, to emulsion
Stability plays vital effect, but after dried coating film, it easily absorbs water so that water-resistant coating is poor, after water suction
Easily whiting, greatly reduces protecting effect of the film to base material；(4) coating acid and alkali-resistance and high and low temperature resistance difference etc..
The content of the invention
In order to overcome the shortcomings and deficiencies of the prior art described above, be to provide a kind of environment-friendly type can for primary and foremost purpose of the invention
Peel off the preparation method of waterborne polyurethane resin.
Another object of the present invention is to provide environment-friendly type strippable water-soluble polyurethane resin prepared by the above method.
Still a further object of the present invention is to provide above-mentioned environment-friendly type strippable water-soluble polyurethane resin in surfacecti proteon field
Application, be particularly suitable for use in glass, ceramics and metal building material surface protection in.
The purpose of the present invention is realized by following proposal：
A kind of preparation method of environment-friendly type strippable water-soluble polyurethane resin, including step in detail below：
(1) the oligomer dihydric alcohol after dehydration and diisocyanate Hybrid Heating are reacted；
(2) small molecule chain extender, hydrophilic chain extender, heating response are added；
(3) nertralizer, latent curing agent, water, rear chain extender are sequentially added under stirring, is stirred, that is, obtaining environment-friendly type can
Peel off waterborne polyurethane resin.
Described latent curing agent includes at least one of blocked isocyanate class and the siloxanes containing epoxy radicals.It is preferred that
The mass ratio of ground, latent curing agent used and oligomer dihydric alcohol is (0.5~1.5):(20~60).
In order to which the present invention is better achieved, the siloxanes containing epoxy radicals is without amino, hydroxyl or mercapto etc.
Group with active hydrogen.
Oligomer polyol of the present invention is preferably the polyester-type or polyether-type binary that molecular weight is 400~4000
Alcohol, it may include polybutylene glyool adipate, polycaprolactone glycol, PCDL, PTMG and poly-
At least one of propane diols etc., including at least one PPG.
Preferably, there is no particular restriction for diisocyanate of the present invention, it is known to use diisocyanate, can
For IPDI (IPDI), hexamethylene-diisocyanate (HDI), toluene di-isocyanate(TDI) (TDI) and 4,4-
At least one of dicyclohexyl methyl hydride diisocyanate (H12-MDI) etc..
Preferably, there is no particular restriction for small molecule chain extender of the present invention, it is known to use small molecule chain extender it is equal
Can, in order to which the present invention is better achieved, described small molecule chain extender is preferably BDO (BDO), neopentyl glycol
(NPG), at least one of 1,6- hexylene glycols (HEG) and diglycol, its consumption are catalytic amount.
Preferably, there is no particular restriction for hydrophilic chain extender of the present invention, it is known to use hydrophilic chain extender, be
The present invention is better achieved, described hydrophilic chain extender is preferably dihydromethyl propionic acid, dimethylolpropionic acid and double hydroxyl sulphurs
At least one of hydrochlorate, its consumption is catalytic amount.
Nertralizer of the present invention is used for the pH value for adjusting reaction system to alkalescent, can arbitrarily be commonly used for this area
Alkali lye, such as trimethylamine, triethylamine, ammoniacal liquor.
There is no particular restriction for rear chain extender of the present invention, it is known to use rear chain extender, in order to preferably real
The existing present invention, described rear chain extender is preferably ethylenediamine, propane diamine, 1,6- hexamethylene diamines, diethylenetriamines, isophorone two
At least one of amine and trien.
In order to which the consumption that each component during the present invention, above-mentioned preparation method is further better achieved is preferably：
Above-mentioned preparation method is carried out preferably under inert gas shielding.
Heating response described in step (1) is preferably at 60~90 DEG C, the h of stirring reaction 1.5~2.5.
Dehydration described in step (1) is preferably dehydrated 2 h at 80~140 DEG C.
The temperature of preferred reduction reaction system is to 40~60 DEG C before reagent addition in step (2).
Heating response described in step (2) is preferably heated to 70~85 DEG C, reacts 2.5~4.5 h.
The temperature of preferred reduction reaction system is to less than 50 DEG C before reagent addition in step (3).
Step sequentially adds nertralizer, latent curing agent, water, rear chain extender described in (3), and a kind of reagent is preferably added every time
Carry out being sufficiently stirred for adding a kind of lower reagent afterwards, be preferably added to after nertralizer, latent curing agent stir 1~5 min respectively, add
The min of high-speed stirred 10~30 is distinguished after water, rear chain extender, adding progress high-speed stirred after water can make system fully emulsified.
The middle addition water of step (3) is mainly used in consolidating for regulation system and contained, and can carry out arbitrary bar according to needs of production
Part, therefore its consumption can adjust as needed, it is appropriate, preferably use 120~280 parts by weight.
Preferably, the total amount of above-mentioned small molecule chain extender used and hydrophilic chain extender is 2.5~7.5 parts by weight.
The environment-friendly type strippable water-soluble polyurethane resin that above-mentioned preparation method is obtained, with environmentally friendly easily peelable, stability it is good,
Persistently peelable, intensity is high, water resistance is splendid, good resistance to acids and bases and the low advantage of high and low temperature resistance, product cost, is
Environment-friendly type stripping lacquer provides the base resin of high performance-price ratio, can be widely used in surfacecti proteon field, be particularly suitable for use in
In glass, ceramics and metal building material surface protection.
The present invention mechanism be：
The environment-friendly type strippable water-soluble polyurethane resin selection of the present invention is original and different, and latent curing agent is added in system,
With the reaction of hydrophilic radical present in resin system so as to remove the parent introduced in preparation process during emulsion film forming
Water base group, so as to assign resin splendid water resistance, and eliminates a large amount of free parents present in existing aqueous polyurethane system
Water base group and cause resin easily to absorb water so that water-resistant coating is poor, easily whitens after water suction, greatly reduces film to base material
Protecting effect influence, and due to the presence of these acidic hydrophilic groups, cause the anti-hydrolytic performance of film to decline, reduce
The service life of film, the defencive function for preventing it permanently effective from providing；And the latent curing agent of the present invention is in film forming procedure
Crosslinking curing again is understood, so as to further increase the combination property of environment-friendly type strippable water-soluble polyurethane resin.Meanwhile, this hair
Bright PPG and the PEPA of preferably using carries out being mixed with resin, so as to obtain excellent properties.
The present invention has the following advantages and beneficial effect relative to prior art：
(1) latent curing agent is added in environment-friendly type strippable water-soluble polyurethane resin of the invention, in emulsion film forming process
In hydrophilic radical both in elimination system, be cross-linked with each other solidification again, so as to improve the properties of resin.
(2) environment-friendly type strippable water-soluble polyurethane resin synthesis technique of the invention is simple, and controllability is strong, and equipment is wanted
Obvious reduction is asked, while avoiding many influence factors that multiple modified product is brought in building-up process.
(3) environment-friendly type strippable water-soluble polyurethane resin decentralized medium of the invention is water, and cost is relatively low, is aqueous, environmental protective
Base resin of the preparation of Stripable paint there is provided high performance-price ratio.
Embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
Embodiment 1：The preparation of environment-friendly type strippable water-soluble polyurethane resin
Under the protection of dry nitrogen, by 80 grams of PTMG after the h of vacuum dehydration 2 at 120 DEG C, different Fo Er
26.7 grams of ketone diisocyanate, is added in reactor, controls temperature to carry out reaction 2 hours at 70~90 DEG C under mechanical stirring；
5.6 grams of diglycol is added, 3.5 grams of dihydromethyl propionic acid reacts 3 hours at 70~85 DEG C；It is down to less than 50 DEG C, addition
It is alkalescent to measure 2.45 grams of regulation system pH of triethylamine, continues to stir 5 minutes；Add blocked isocyanate class latent curing agent
(TPA-B80X) 0.7 gram, continue to stir 5 minutes；200 grams of water is added, (rotating speed preferably >=1200 r/min) is scattered 10 points at a high speed
Clock；1.5 grams of ethylenediamine is added, continues scattered 30 minutes at a high speed, you can obtain environment-friendly type strippable water-soluble polyurethane resin.
Embodiment 2：The preparation of environment-friendly type strippable water-soluble polyurethane resin
Under the protection of dry nitrogen, by 40 grams of PTMG after the h of vacuum dehydration 2 at 120 DEG C, poly- the third two
40 grams of alcohol, 44.4 grams of IPDI is added in reactor, controls temperature to enter at 70~90 DEG C under mechanical stirring
Row reaction 2 hours；4.0 grams of diglycol is added, 5.0 grams of dihydromethyl propionic acid reacts 3 hours at 70~85 DEG C；It is down to
Less than 50 DEG C, 2.45 grams of triethylamine of metering is added, continues to stir 5 minutes；Add blocked isocyanate class latent curing agent (TPA-
B80X) 4.5 grams, continue to stir 5 minutes；200 grams of water is added, it is scattered 10 minutes at a high speed；1.5 grams of ethylenediamine is added, is continued at a high speed
It is scattered 30 minutes, you can to obtain environment-friendly type strippable water-soluble polyurethane resin.
Embodiment 3：The preparation of environment-friendly type strippable water-soluble polyurethane resin
Under the protection of dry nitrogen, by 40 grams of polycaprolactone glycol after the h of vacuum dehydration 2 at 120 DEG C, polyadipate fourth
40 grams of glycol esterdiol, 34.8 grams of toluene di-isocyanate(TDI) is added in reactor, and temperature is controlled under mechanical stirring 70~90
DEG C carry out reaction 2 hours；5.6 grams of diglycol is added, 3.5 grams of dihydromethyl propionic acid reacts 3 hours at 70~85 DEG C；
Less than 50 DEG C are down to, 2.45 grams of triethylamine of metering is added, continues to stir 5 minutes；Add epoxy radicals type siloxane latent curing agent
(OS-9012) 2.8 grams, continue to stir 5 minutes；200 grams of water is added, it is scattered 10 minutes at a high speed；1.5 grams of ethylenediamine is added, is continued
It is scattered 30 minutes at a high speed, you can to obtain environment-friendly type strippable water-soluble polyurethane resin.
Embodiment 4：The preparation of environment-friendly type strippable water-soluble polyurethane resin
Under the protection of dry nitrogen, by 40 grams of PCDL after the h of vacuum dehydration 2 at 120 DEG C, poly- tetrahydrochysene furan
Mutter 40 grams of ether glycol, 22.2 grams of IPDI, 16.8 grams of hexamethylene-diisocyanate is added in reactor,
Control temperature carries out reaction 2 hours at 70~90 DEG C under mechanical stirring；Add 4.75 grams of BDO, dihydromethyl propionic acid
3.5 grams, reacted 3 hours at 70~85 DEG C；Less than 50 DEG C are down to, 2.45 grams of triethylamine of metering is added, continues to stir 5 minutes；Plus
Enter 6.0 grams of blocked isocyanate class latent curing agent (TPA-B80X), continue to stir 5 minutes；200 grams of water is added, it is scattered at a high speed
10 minutes；1.5 grams of ethylenediamine is added, continues scattered 30 minutes at a high speed, you can obtain environment-friendly type strippable water-soluble polyurethane resin.
Embodiment 5：The preparation of environment-friendly type strippable water-soluble polyurethane resin
Under the protection of dry nitrogen, by 40 grams of PCDL after the h of vacuum dehydration 2 at 120 DEG C, poly- tetrahydrochysene furan
Mutter 40 grams of ether glycol, 4,4- 104.8 grams of dicyclohexyl methyl hydride diisocyanates, 16.8 grams of hexamethylene-diisocyanate is added
In reactor, temperature is controlled to carry out reaction 2 hours at 70~90 DEG C under mechanical stirring；Add 17.5 grams of BDO, two
10.0 grams of hydroxymethyl propionic acid, reacts 3 hours at 70~85 DEG C；Less than 50 DEG C are down to, 2.45 grams of triethylamine of metering is added, continues to stir
Mix 5 minutes；1.8 grams of epoxy radical siloxane (OS-9012) is added, continues to stir 5 minutes；200 grams of water is added, it is scattered 10 points at a high speed
Clock；1.5 grams of ethylenediamine is added, continues scattered 30 minutes at a high speed, you can obtain environment-friendly type strippable water-soluble polyurethane resin.
Above-described embodiment is preferably embodiment, but embodiments of the present invention are not by above-described embodiment of the invention
Limitation, other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (9)
1. a kind of preparation method of environment-friendly type strippable water-soluble polyurethane resin, it is characterised in that including step in detail below：
（1）Oligomer dihydric alcohol after dehydration and diisocyanate Hybrid Heating are reacted；
（2）Add small molecule chain extender, hydrophilic chain extender, heating response；
（3）Nertralizer, latent curing agent, water, rear chain extender are sequentially added under stirring, is stirred, that is, obtains environment-friendly type peelable
Waterborne polyurethane resin；
Described latent curing agent is the siloxanes OS-9012 containing epoxy radicals.
2. the preparation method of environment-friendly type strippable water-soluble polyurethane resin according to claim 1, it is characterised in that：It is described
The siloxanes containing epoxy radicals be free of amino, hydroxyl or mercapto the group with active hydrogen.
3. the preparation method of environment-friendly type strippable water-soluble polyurethane resin according to claim 1, it is characterised in that：It is used
The mass ratio of latent curing agent and oligomer dihydric alcohol is（0.5~1.5）:（20~60）.
4. the preparation method of environment-friendly type strippable water-soluble polyurethane resin according to claim 1, it is characterised in that：It is described
Oligomer dihydric alcohol include molecular weight be 400~4000 polyester-type or polyether-type dihydric alcohol.
5. the preparation method of environment-friendly type strippable water-soluble polyurethane resin according to claim 1, it is characterised in that：It is described
Oligomer dihydric alcohol include polybutylene glyool adipate, polycaprolactone glycol, PCDL, PTMG
At least one of glycol and polypropylene glycol, including at least one PPG.
6. the preparation method of environment-friendly type strippable water-soluble polyurethane resin according to claim 1, it is characterised in that：It is described
Diisocyanate include IPDI, hexamethylene-diisocyanate, toluene di-isocyanate(TDI) and 4,4- bis-
At least one of diphenylmethane diisocyanate；Described small molecule chain extender includes 1,4- butanediols, neopentyl glycol, 1,
At least one of 6- hexylene glycols and diglycol；Described hydrophilic chain extender includes dihydromethyl propionic acid, dihydroxymethyl
At least one of butyric acid and double hydroxy sulfonates；Described rear chain extender includes ethylenediamine, propane diamine, 1,6- hexamethylene diamines, two
At least one of ethylenetriamine, isophorone diamine and trien.
7. the preparation method of environment-friendly type strippable water-soluble polyurethane resin according to claim 1, it is characterised in that：Step
（1）Described in heating response refer at 60~90 DEG C, the h of stirring reaction 1.5~2.5；Step（2）Described in heating response
To be heated to 70~85 DEG C, 2.5~4.5 h are reacted.
8. a kind of environment-friendly type strippable water-soluble polyurethane resin, it is characterised in that the ring according to any one of claim 1~7
The preparation method of guarantor's type strippable water-soluble polyurethane resin is obtained.
9. application of the environment-friendly type strippable water-soluble polyurethane resin according to claim 8 in surfacecti proteon field.
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| CN106085188A (en) * | 2016-06-16 | 2016-11-09 | 南昌航空大学 | The preparation method of two kinds of aqueous peelable dispersions of polyurethanes |
| CN106519170B (en) * | 2016-10-25 | 2019-02-26 | 广州冠志新材料科技有限公司 | A kind of woodcare paint repairs color waterborne polyurethane resin and preparation method thereof |
| CN107142003B (en) * | 2017-07-05 | 2019-11-12 | 北京科技大学 | A preparation method for peelable reinforced protective coating system for connection parts |
| CN107501497A (en) * | 2017-08-28 | 2017-12-22 | 同光（江苏）新材料科技有限公司 | A kind of Che Yiyong strippable water-solubles polyurethane resin synthetic method |
| CN107722687B (en) * | 2017-09-19 | 2020-02-07 | 河北晨阳工贸集团有限公司 | Water-based peelable resin and preparation method thereof |
| CN109207049A (en) * | 2018-08-22 | 2019-01-15 | 青岛汇智领先新材料科技有限公司 | A kind of two-component modified polyurethane Stripable paint and preparation method thereof |
| CN109486402A (en) * | 2018-11-19 | 2019-03-19 | 山东天庆科技发展有限公司 | Aqueous peelable resin of one kind and preparation method thereof |
| CN109554102B (en) * | 2018-12-03 | 2021-04-30 | 宁夏银珠蓝箭建材科技有限公司 | Waterproof coating for waterproofing buildings and preparation method thereof |
| CN112250818A (en) * | 2020-09-27 | 2021-01-22 | 长春一汽富维东阳汽车塑料零部件有限公司 | Recyclable water-based polyurethane shielding material and preparation method thereof |
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