CN104745066A - Preparation method of single-component polyurethane waterproofing paint - Google Patents
Preparation method of single-component polyurethane waterproofing paint Download PDFInfo
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- CN104745066A CN104745066A CN201510171599.XA CN201510171599A CN104745066A CN 104745066 A CN104745066 A CN 104745066A CN 201510171599 A CN201510171599 A CN 201510171599A CN 104745066 A CN104745066 A CN 104745066A
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- preparation
- component polyurethane
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- proof paint
- polyurethane water
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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
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4833—Polyethers containing oxyethylene units
- C08G18/4837—Polyethers containing oxyethylene units and other oxyalkylene units
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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
- C09D175/08—Polyurethanes from polyethers
Abstract
The invention relates to a preparation method of a single-component polyurethane waterproofing paint. The preparation method is mainly characterized by comprising the following steps: adding poly-functionality polyether glycol to a reaction kettle, dehydrating and adding a certain amount of isocyanate, reacting at 50-80 DEG C for 2-4h, decreasing to room temperature, adding a plasticizer, a defoaming agent, an antioxidant and an ultraviolet light absorber which are dried in advance, and uniformly mixing so as to obtain the single-component polyurethane waterproofing paint. The preparation method disclosed by the invention has the following advantages: 1) the preparation method is cheap and easily available in the adopted raw materials, simple and efficient in synthesis method, low in cost, easy in the scaling-up of an operating process and capable of achieving industrial production; and 2) the polyurethane resin is good in dispersing performance in water; a dense polyurethane elastomer coating film, which is environment-friendly and non-toxic and is highly safe, can be prepared by uniformly stirring and curing with the addition of 20-50% of water during constructing. By introducing the poly-functionality active group, a dense cross-linked network structure can be formed since being cured in water; and the waterproofing paint is excellent in mechanical performance (thin-film tensile strength is more than 10MPa and elongation at break is more than 500%), therefore, the waterproofing paint can be used as an excellent waterproofing material which is broad in application prospect.
Description
Technical field
The present invention relates to the preparation method of a kind of building trade field waterproof paint, particularly relate to a kind of preparation method of single-component polyurethane water-proof paint with high tensile, high elongation at tear.
Background technology
The WATER REPELLENT of construction work effectively can improve the working life, particularly modern architecture of buildings, and WATER REPELLENT is particularly important.Waterproof paint conventional is at present polyurethane water-proof paint, acrylate waterproof paint, modified emulsifying asphalt waterproof paint etc.Wherein polyurethane water-proof paint has elasticity and good-extensibility, tensile strength are high, cohesiveness good, volumetric shrinkage is little, film waterproof material is without seam due to its film, stronger adaptability is had to the distortion of basic crack retractility, working drawing review convenient (being amorphous viscous liquid material before polyurethane water-proof paint solidification), all be easy to construction in any baroque substrate surface, be easy to regulate the features such as component ratio, can be used for the waterproofing and leakage-stopping of buildings different sites, in waterproof field, occupy critical role.
Polyurethane water-proof protective cover mainly contains following several: asphalt polyurethane water-proof paint, mono-composition poyurethane water-proof paint, Two-component Waterproof Polyurethane Coating, aqueous polyurethane waterproof paint, spray polyurea elastomer waterproof paint.Wherein single-component polyurethane water-proof paint is because of its easy construction, eliminate the burden process before construction, the advantages such as metering mistake can not occur greatly developed at present, the patent of this respect comprises: CN201110007526.9, CN201110033097.2, CN201110333955.5, CN201210537883.0, CN201310041967.X, CN201410038016.1, CN201410210676.3, CN201410459714.9, CN201410294925.1 etc.Single-component polyurethane water-proof paint can be divided into wet-solidifying single-component polyurethane waterproof paint and single-component water cure polyurethane coating according to the difference of formula, for wet-solidifying single-component polyurethane waterproof paint, the water generally adding 20% ~ 30% during the construction of single-component water cure polyurethane coating makees solidifying agent, easy construction and nontoxic pollution-free, more environmental protection, cost is lower, and Recent study is enlivened gradually.Although certain progress that single-component polyurethane water-proof paint has been got, but still there are the following problems: tensile strength is lower, can not meet the construction related request of some construction works at present; Cost is high, is difficult to large-scale promotion application.
For overcoming the problems referred to above, this invention exploits a kind of single-component polyurethane water-proof paint based on polyfunctionality polyether glycol, well-designed by urethane resin molecular structure, control cross-linking density and cross-linked network structure, synthesize the single-component water-cured polyurethane waterproof coating with high tensile, high elongation at tear.This urethane resin is solidifying agent with water, and the water adding 20% ~ 50% during construction stirs after solidification can form fine and close polyurethane elastomer film, has tight security.Because its synthesis technique is simple, cost is low, is expected to obtain large-scale application in actual production.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of single-component polyurethane water-proof paint with high tensile, high elongation at tear, to solve the problem that existing polyurethane hydrogel is difficult to industrialization large-scale application.
For achieving the above object, this invention exploits a kind of single-component water-cured polyurethane waterproof coating based on polyfunctionality polyether glycol, its preparation method is:
Polyfunctionality polyether glycol is added in reactor, after dehydration, add a certain amount of isocyanic ester, 50-80 DEG C of reaction 2-4h, is down to room temperature, add softening agent dried in advance, defoamer, antioxidant and UV light absorber, mix rear obtained polyurethane water-proof paint; Wherein, polyfunctionality polyether glycol used is polyoxyethylene polyoxypropylene glyceryl ether or polyoxyethylene polyoxypropylene tetramethylolmethane ether, the add-on of isocyanic ester is to ensure that in polyether glycol, hydroxyl complete reaction is for benchmark, the mol ratio of preferred isocyanate group and hydroxyl is 2:1-4:1, the add-on of softening agent is the 3-8wt% of polyvalent alcohol consumption, the add-on of defoamer is the 0.5-1wt% of polyvalent alcohol consumption, the add-on of antioxidant is the 0.1-1wt% of polyvalent alcohol consumption, and the add-on of UV light absorber is the 0.1-1wt% of polyvalent alcohol consumption.
The molecular weight of described polyoxyethylene polyoxypropylene glyceryl ether is 2000-10000, and polyoxyethylated content is 10-30 wt%, and in its molecular structure, polyoxyethylene (A) and polyoxypropylene (B) are block distributed or random distribution, as follows:
The molecular weight of described polyoxyethylene polyoxypropylene tetramethylolmethane ether is 2000-10000, and polyoxyethylated content is 10-30 wt%, and in its molecular structure, polyoxyethylene (A) and polyoxypropylene (B) are block distributed or random distribution, as follows:
Described isocyanic ester is one or more mixtures in tolylene diisocyanate, '-diphenylmethane diisocyanate, poly methylene poly phenyl poly isocyanate, how vulcabond, xylylene diisocyanate, isophorone diisocyanate, hexamethylene diisocyanate.
Described softening agent is one or more mixtures in didecyl phthalate, Dinonylphthalate, Wickenol 117, dioctyl sebacate.
Described defoamer is silicone antifoam agent.
Described antioxidant is four (β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid) tetramethylolmethane, two [β (the 3-tertiary butyl-5-methyl-4-hydroxy phenyl) propionic acid] triethyleneglycol ester, three (3,5-di-tert-butyl-hydroxy phenyl) chlorinated isocyanurates, one or more mixtures in 2,6 di tert butyl 4 methyl phenol.
Described UV light absorber be ESCALOL 567 or 2-(2 '-hydroxyl-3 ', 5 '-two ［ 1,1-3,5-dimethylphenyl ］) – benzotriazole.
Compared with prior art, the present invention has the following advantages:
The present invention, from industrial raw material cheap and easy to get polypropylene glycol-polyoxyethylene glycol polyether glycol, has synthesized single-component water-cured polyurethane waterproof coating efficiently by simple chemical reaction; Synthetic method is efficiently simple and direct, and raw material used in reaction process and reagent are all cheap and easy to get, and cost is low, the amplification of easy handling process and realize suitability for industrialized production; This urethane resin has dispersing property in good water, and the water adding 20% ~ 50% during construction stirs after solidification can form fine and close polyurethane elastomer film, and environment-protecting asepsis, has tight security.Owing to introducing polyfunctionality active group, fine and close cross-linked network structure can be formed after meeting water cure, there is excellent mechanical property (film stretching intensity is greater than 10MPa, and elongation at break is greater than 500%), can be used as a kind of water-proof material of excellence, have a extensive future.
Embodiment
To contribute to understanding the present invention by following embodiment, but not limit content of the present invention.
In following examples, PEO represents polyoxyethylene, and PPO represents polyoxypropylene.
Embodiment 1:
20g polyoxyethylene polyoxypropylene glyceryl ether (Mn=2000, PEO wt%=30%, PEO and PPO block distributed) is added in reaction flask, 120 DEG C of vacuum hydro-extraction 2h, be cooled to 50 DEG C, add tolylene diisocyanate 10.4g, 50 DEG C of reaction 2h, be down to room temperature, add pyrocatechol formic acid didecyl 0.6g, silicon-type defoamer 0.1g, four (β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid) tetramethylolmethane 0.02g, ESCALOL 567 0.02g.Stir 10min, discharging, sealing is preserved.
Embodiment 2:
20g polyoxyethylene polyoxypropylene glyceryl ether (Mn=10000, PEO wt%=10%, PEO and PPO are block distributed) is added in reaction flask, 120 DEG C of vacuum hydro-extraction 2h, be cooled to 50 DEG C, add tolylene diisocyanate 4.2g, 80 DEG C of reaction 4h, be down to room temperature, add pyrocatechol formic acid didecyl 1.6g, silicon-type defoamer 0.2g, four (β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid) tetramethylolmethane 0.2g, ESCALOL 567 0.2g.Stir 10min, discharging, sealing is preserved.
Embodiment 3:
20g polyoxyethylene polyoxypropylene glyceryl ether (Mn=6000, PEO wt%=20%, PEO and PPO are random distribution) is added in reaction flask, 120 DEG C of vacuum hydro-extraction 2h, be cooled to 60 DEG C, add tolylene diisocyanate 5.2g, 60 DEG C of reaction 3h, be down to room temperature, add pyrocatechol formic acid two ester in ninth of the ten Heavenly Stems 1.2g, silicon-type defoamer 0.1g, four (β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid) tetramethylolmethane 0.1g, ESCALOL 567 0.1g.Stir 10min, discharging, sealing is preserved.
Embodiment 4:
20g polyoxyethylene polyoxypropylene tetramethylolmethane ether (Mn=2000, PEO wt%=30%, PEO and PPO are random distribution) is added in reaction flask, 120 DEG C of vacuum hydro-extraction 2h, be cooled to 60 DEG C, add hexamethylene diisocyanate 13.4g, 50 DEG C of reaction 3h, be down to room temperature, add Wickenol 117 0.6g, silicon-type defoamer 0.02g, four (β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid) tetramethylolmethane 0.02g, ESCALOL 567 0.02g.Stir 10min, discharging, sealing is preserved.
Embodiment 5:
20g polyoxyethylene polyoxypropylene tetramethylolmethane ether (Mn=10000 is added in reaction flask, PEO wt%=10%, PEO and PPO is block distributed), 120 DEG C of vacuum hydro-extraction 2h, be cooled to 60 DEG C, add hexamethylene diisocyanate 5.4g, 80 DEG C of reaction 4h, are down to room temperature, add pyrocatechol formic acid didecyl 1.6g, silicon-type defoamer 0.2g, three (3,5-di-tert-butyl-hydroxy phenyl) chlorinated isocyanurates 0.2g ,-(2 '-hydroxyl-3 ', 5 '-two ［ 1,1-3,5-dimethylphenyl ］) – benzotriazole 0.2g.Stir 10min, discharging, sealing is preserved.
Embodiment 6:
20g polyoxyethylene polyoxypropylene tetramethylolmethane ether (Mn=6000 is added in reaction flask, PEO wt%=20%, PEO and PPO is block distributed), 120 DEG C of vacuum hydro-extraction 2h, 120 DEG C of vacuum hydro-extraction 2h, be cooled to 60 DEG C, add tolylene diisocyanate 5.2g, 60 DEG C of reaction 3h, are down to room temperature, add pyrocatechol formic acid two ester in ninth of the ten Heavenly Stems 1.2g, silicon-type defoamer 0.1g, four (β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid) tetramethylolmethane 0.1g, ESCALOL 567 0.1g.Stir 10min, discharging, sealing is preserved.
Claims (8)
1. the preparation method of a single-component polyurethane water-proof paint, it is characterized in that preparation process is: in reactor, add polyfunctionality polyether glycol, a certain amount of isocyanic ester is added after dehydration, 50-80 DEG C of reaction 2-4h, be down to room temperature, add softening agent dried in advance, defoamer, antioxidant and UV light absorber, mix rear obtained polyurethane water-proof paint; Wherein, polyfunctionality polyether glycol used is polyoxyethylene polyoxypropylene glyceryl ether or polyoxyethylene polyoxypropylene tetramethylolmethane ether, the add-on of isocyanic ester is to ensure that in polyether glycol, hydroxyl complete reaction is for benchmark, the mol ratio of preferred isocyanate group and hydroxyl is 2:1-4:1, the add-on of softening agent is the 3-8wt% of polyvalent alcohol consumption, the add-on of defoamer is the 0.5-1wt% of polyvalent alcohol consumption, the add-on of antioxidant is the 0.1-1wt% of polyvalent alcohol consumption, and the add-on of UV light absorber is the 0.1-1wt% of polyvalent alcohol consumption.
2. the preparation method of a kind of single-component polyurethane water-proof paint according to claim 1, it is characterized in that the molecular weight of described polyoxyethylene polyoxypropylene glyceryl ether is 2000-10000, polyoxyethylated content is 10-30 wt%, in its molecular structure, polyoxyethylene (A) and polyoxypropylene (B) are block distributed or random distribution, as follows.
3. the preparation method of a kind of single-component polyurethane water-proof paint according to claim 1, the molecular weight that it is characterized in that described polyoxyethylene polyoxypropylene tetramethylolmethane ether is 2000-10000, polyoxyethylated content is 10-30 wt%, in its molecular structure, polyoxyethylene (A) and polyoxypropylene (B) are block distributed or random distribution, as follows.
4. the preparation method of a kind of single-component polyurethane water-proof paint according to claim 1, is characterized in that described isocyanic ester is one or more mixtures in tolylene diisocyanate, '-diphenylmethane diisocyanate, poly methylene poly phenyl poly isocyanate, how vulcabond, xylylene diisocyanate, isophorone diisocyanate, hexamethylene diisocyanate.
5. the preparation method of a kind of single-component polyurethane water-proof paint according to claim 1, is characterized in that described softening agent is one or more mixtures in didecyl phthalate, Dinonylphthalate, Wickenol 117, dioctyl sebacate.
6. the preparation method of a kind of single-component polyurethane water-proof paint according to claim 1, is characterized in that described defoamer is silicone antifoam agent.
7. the preparation method of a kind of single-component polyurethane water-proof paint according to claim 1, it is characterized in that described antioxidant is four (β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid) tetramethylolmethane, two [β (the 3-tertiary butyl-5-methyl-4-hydroxy phenyl) propionic acid] triethyleneglycol ester, three (3,5-di-tert-butyl-hydroxy phenyl) chlorinated isocyanurates, one or more mixtures in 2,6 di tert butyl 4 methyl phenol.
8. the preparation method of a kind of single-component polyurethane water-proof paint according to claim 1, it is characterized in that described UV light absorber be ESCALOL 567 or 2-(2 '-hydroxyl-3 ', 5 '-two ［ 1,1-3,5-dimethylphenyl ］) – benzotriazole.
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| CN201510171599.XA CN104745066A (en) | 2015-04-13 | 2015-04-13 | Preparation method of single-component polyurethane waterproofing paint |
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| CN201510171599.XA CN104745066A (en) | 2015-04-13 | 2015-04-13 | Preparation method of single-component polyurethane waterproofing paint |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105111843A (en) * | 2015-08-13 | 2015-12-02 | 蚌埠南自仪表有限公司 | Anti-oxidation heat-dissipation paint and preparation method therefor |
| CN108299619A (en) * | 2018-01-19 | 2018-07-20 | 河南建筑职业技术学院 | A kind of coupling agent modified coal ash for manufacturing for one-can urethane coating method |
| CN110452347A (en) * | 2019-07-10 | 2019-11-15 | 广东德美精细化工集团股份有限公司 | A kind of urethane intermediates and preparation method thereof with waterproof performance |
| CN110551445A (en) * | 2019-09-18 | 2019-12-10 | 江苏凯伦建材股份有限公司 | Water-repellent coating and use thereof |
-
2015
- 2015-04-13 CN CN201510171599.XA patent/CN104745066A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105111843A (en) * | 2015-08-13 | 2015-12-02 | 蚌埠南自仪表有限公司 | Anti-oxidation heat-dissipation paint and preparation method therefor |
| CN108299619A (en) * | 2018-01-19 | 2018-07-20 | 河南建筑职业技术学院 | A kind of coupling agent modified coal ash for manufacturing for one-can urethane coating method |
| CN108299619B (en) * | 2018-01-19 | 2020-12-22 | 河南建筑职业技术学院 | Method for preparing single-component polyurethane coating from coupling agent modified fly ash |
| CN110452347A (en) * | 2019-07-10 | 2019-11-15 | 广东德美精细化工集团股份有限公司 | A kind of urethane intermediates and preparation method thereof with waterproof performance |
| CN110551445A (en) * | 2019-09-18 | 2019-12-10 | 江苏凯伦建材股份有限公司 | Water-repellent coating and use thereof |
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