CN104356911A - Method for preparing aqueous double-component polyurethane flexible coating - Google Patents

Method for preparing aqueous double-component polyurethane flexible coating Download PDF

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Publication number
CN104356911A
CN104356911A CN201410597341.1A CN201410597341A CN104356911A CN 104356911 A CN104356911 A CN 104356911A CN 201410597341 A CN201410597341 A CN 201410597341A CN 104356911 A CN104356911 A CN 104356911A
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add
stirring
soft
aqueous
component
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吴礼才
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DAZU COUNTY ZHONGKE PIPELINE EQUIPMENT Co Ltd
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DAZU COUNTY ZHONGKE PIPELINE EQUIPMENT Co Ltd
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Priority to CN201410597341.1A priority Critical patent/CN104356911A/en
Publication of CN104356911A publication Critical patent/CN104356911A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30Low-molecular-weight compounds
    • C08G18/34Carboxylic acids; Esters thereof with monohydroxyl compounds
    • C08G18/348Hydroxycarboxylic acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40High-molecular-weight compounds
    • C08G18/42Polycondensates having carboxylic or carbonic ester groups in the main chain
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/65Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/66Compounds of groups C08G18/42, C08G18/48, or C08G18/52
    • C08G18/6633Compounds of group C08G18/42
    • C08G18/6659Compounds of group C08G18/42 with compounds of group C08G18/34
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72Polyisocyanates or polyisothiocyanates
    • C08G18/721Two or more polyisocyanates not provided for in one single group C08G18/73 - C08G18/80
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72Polyisocyanates or polyisothiocyanates
    • C08G18/73Polyisocyanates or polyisothiocyanates acyclic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72Polyisocyanates or polyisothiocyanates
    • C08G18/74Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/75Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
    • C08G18/751Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
    • C08G18/752Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
    • C08G18/753Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
    • C08G18/755Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D175/00Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
    • C09D175/04Polyurethanes

Abstract

The invention relates to a method for preparing an aqueous double-component polyurethane flexible coating. The method comprises the following steps: keeping the temperature of a mixture of polyvinegar polyhydric alcohol, DMPA, N-methyl pyrrolidinone, IPDI and HDI, and DBTL, and keeping back flowing; reacting, adding TEA for neutralization, and uniformly stirring the mixture, and obtaining a polyurethane prepolymer containing hydroxyl; slowly adding a prepolymer solution into deionized water in high-speed stirring, and stirring at a high speed, and preparing uniform emulsion; pouring the emulsion into a flask, performing reduced pressure distillation, and removing acetone, and obtaining hydroxyl terminated aqueous polyurethane dispersoid; synthesizing by using the method, and obtaining aqueous polyurethane dispersoid; uniformly mixing the hydroxyl terminated aqueous polyurethane dispersoid with the aqueous polyurethane dispersoid, adding a quantitative coating additive, uniformly stirring the mixture at a high speed, adding Bayhyder3100, uniformly mixing, stirring, and discharging, and obtaining the aqueous double-component polyurethane flexible coating. The method provided by the invention is simple, low in cost and easy to control, and the synthesized aqueous double-component polyurethane flexible coating is environment-friendly and excellent in comprehensive property.

Description

A kind of aqueous double-component polyurethane soft-feel coating preparation method
Technical field
The present invention relates to a kind of synthetic technology of organic coating, particularly relate to a kind of aqueous double-component polyurethane soft-feel coating preparation method.
Background technology
Soft-feel coating can provide a kind of outward appearance of luxury and warm, soft hand tactile qualities owing to having relative to ice-cold hard plastics, metal products, obtains more and more widespread use in recent years.The special soft feeling of aqueous two-component polyurethane soft-feel coating is the existence due to aqueous polyurethane dispersion, instead of caused by interpolation elasticity auxiliary agent.By the combination of hydroxy component and aqueous one-component polyurethane dispersions, and with the resin system being cross-linked to form this coating of hydrophilic isocyanate curing agent.Aqueous double-component polyurethane soft-feel coating can reduce the release of plastic coating volatile matter effectively, is a kind of brand-new environment-friendly type soft-feel coating.
Summary of the invention
It is simple that technical problem to be solved by this invention is to provide a kind of method, and cost is low, easy to control, the aqueous double-component polyurethane soft-feel coating environmental protection of synthesis, the synthetic method of excellent combination property.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of aqueous double-component polyurethane soft-feel coating preparation method, comprises the steps:
Poly-vinegar polyvalent alcohol, DMPA, N-methyl are adjoined and irons alkane ketone, the mixture of IPDI and HDI and DBTL, be incubated and keep backflow;
Add people TEA after reaction to neutralize, stir, obtain the polyurethane prepolymer of hydroxyl;
By pre-polymer solution, add in deionized water under high velocity agitation lentamente, high-speed stirring, form uniform emulsion;
By underpressure distillation in the emulsion flask of falling people, removing acetone, obtains terminal hydroxy group water-based polyurethane dispersion;
Adopt aforesaid method, synthesis obtains water-based polyurethane dispersion;
Terminal hydroxy group water-based polyurethane dispersion mixed with water-based polyurethane dispersion, add the quantitative coatings additive(s) high-speed stirring of people even, add Bayhyder3100 and mix, after stirring, discharging, obtains aqueous dual-component and gathers the cruel soft-feel coating of ammonia.
On the basis of technique scheme, the present invention can also do following improvement.
Further, described poly-vinegar polyvalent alcohol, DMPA, N-methyl being adjoined, irons alkane ketone, the mixture of IPDI and HDI and DBTL, is incubated and keeps being implemented as follows of reflow step:
The poly-vinegar polyvalent alcohol of 90 ~ 95g, the DMPA of 6.02 ~ 6.35g, the N-methyl of 3 ~ 5g are adjoined and irons alkane ketone, pass into nitrogen, 100 ~ 120 DEG C of backflow 0.5 ~ 1h are warmed up under whipped state, add the mixture of the IPDI of 2.58 ~ 2.66g and the HDI of 2.56 ~ 2.84g and the DBTL of 2 ~ 5, be incubated and keep backflow.
Further, add people TEA after described reaction and neutralize, stir, obtain being implemented as follows of the polyurethane prepolymer step of hydroxyl:
After reaction 1 ~ 3h, be cooled to 20 ~ 40 DEG C, add in the TEA of people 4.02 ~ 5.35g and 10 ~ 30min, stir, obtain the polyurethane prepolymer of hydroxyl.
Further, described by pre-polymer solution, add in deionized water under high velocity agitation lentamente, high-speed stirring, form being implemented as follows of uniform emulsion step:
By pre-polymer solution, add in 300 ~ 320ml deionized water under high velocity agitation lentamente, with 1500 ~ 2000r/min high-speed stirring, 1 ~ 2h, form uniform emulsion.
Further, described terminal hydroxy group water-based polyurethane dispersion to be mixed with water-based polyurethane dispersion, add people's quantitative coatings additive(s) high-speed stirring even, add Bayhyder3100 to mix, after stirring, discharging, obtains aqueous dual-component and gathers being implemented as follows of the cruel soft-feel coating step of ammonia:
The terminal hydroxy group water-based polyurethane dispersion of 20 ~ 26% is mixed with 30 ~ 36% water-based polyurethane dispersions, add the coatings additive(s) high-speed stirring 30 ~ 45min of people 5 ~ 8%, add 10 ~ 15%Bayhyder3100 to mix, after stirring 0.5 ~ 1h, discharging, obtains aqueous dual-component and gathers the cruel soft-feel coating of ammonia.
The invention has the beneficial effects as follows: method is simple, and cost is low, easy to control, the aqueous double-component polyurethane soft-feel coating environmental protection of synthesis, excellent combination property.
Embodiment
Be described principle of the present invention and feature below in conjunction with example, example, only for explaining the present invention, is not intended to limit scope of the present invention.
A kind of aqueous double-component polyurethane soft-feel coating preparation method, comprises the steps:
Poly-vinegar polyvalent alcohol, DMPA, N-methyl are adjoined and irons alkane ketone, the mixture of IPDI and HDI and DBTL, be incubated and keep backflow;
Add people TEA after reaction to neutralize, stir, obtain the polyurethane prepolymer of hydroxyl;
By pre-polymer solution, add in deionized water under high velocity agitation lentamente, high-speed stirring, form uniform emulsion;
By underpressure distillation in the emulsion flask of falling people, removing acetone, obtains terminal hydroxy group water-based polyurethane dispersion;
Adopt aforesaid method, synthesis obtains water-based polyurethane dispersion;
Terminal hydroxy group water-based polyurethane dispersion mixed with water-based polyurethane dispersion, add the quantitative coatings additive(s) high-speed stirring of people even, add Bayhyder3100 and mix, after stirring, discharging, obtains aqueous dual-component and gathers the cruel soft-feel coating of ammonia.
Embodiment 1:
The N-methyl of the poly-vinegar polyvalent alcohol of 90g, DMPA, 3g of 6.02g is adjoined and irons alkane ketone, pass into nitrogen, be warmed up to 100 DEG C of backflow 0.5h under whipped state, add the mixture of the HDI of IPDI and the 2.56g of 2.58g and the DBTL of 2, be incubated and keep backflow; After reaction 1h, be cooled to 20 DEG C, add in the TEA of people 4.02g and 10min, stir, obtain the polyurethane prepolymer of hydroxyl; By pre-polymer solution, add in 300ml deionized water under high velocity agitation lentamente, with 1500r/min high-speed stirring 1h, form uniform emulsion; By underpressure distillation in the emulsion flask of falling people, removing acetone, obtains terminal hydroxy group water-based polyurethane dispersion; Adopt aforesaid method, synthesis obtains water-based polyurethane dispersion; The terminal hydroxy group water-based polyurethane dispersion of 20% is mixed with 30% water-based polyurethane dispersion, add the coatings additive(s) high-speed stirring 30min of people 5%, add 10%Bayhyder3100 and mix, after stirring 0.5h, discharging, obtains aqueous dual-component and gathers the cruel soft-feel coating of ammonia.
Embodiment 2:
The N-methyl of the poly-vinegar polyvalent alcohol of 92g, DMPA, 3.5g of 6.30g is adjoined and irons alkane ketone, pass into nitrogen, be warmed up to 110 DEG C of backflow 0.8h under whipped state, add the mixture of the HDI of IPDI and the 2.75g of 2.60g and the DBTL of 3, be incubated and keep backflow; After reaction 2h, be cooled to 30 DEG C, add in the TEA of people 4.88g and 20min, stir, obtain the polyurethane prepolymer of hydroxyl; By pre-polymer solution, add in 310ml deionized water under high velocity agitation lentamente, with 1800r/min high-speed stirring 1.5h, form uniform emulsion; By underpressure distillation in the emulsion flask of falling people, removing acetone, obtains terminal hydroxy group water-based polyurethane dispersion; Adopt aforesaid method, synthesis obtains water-based polyurethane dispersion; The terminal hydroxy group water-based polyurethane dispersion of 23% is mixed with 33% water-based polyurethane dispersion, add the coatings additive(s) high-speed stirring 40min of people 6%, add 12%Bayhyder3100 and mix, after stirring 0.6h, discharging, obtains aqueous dual-component and gathers the cruel soft-feel coating of ammonia.
Embodiment 3:
The N-methyl of the poly-vinegar polyvalent alcohol of 95g, DMPA, 5g of 6.35g is adjoined and irons alkane ketone, pass into nitrogen, be warmed up to 120 DEG C of backflow 1h under whipped state, add the mixture of the HDI of IPDI and the 2.84g of 2.66g and the DBTL of 5, be incubated and keep backflow; After reaction 3h, be cooled to 40 DEG C, add in the TEA of people 5.35g and 30min, stir, obtain the polyurethane prepolymer of hydroxyl; By pre-polymer solution, add in 320ml deionized water under high velocity agitation lentamente, with 2000r/min high-speed stirring 2h, form uniform emulsion; By underpressure distillation in the emulsion flask of falling people, removing acetone, obtains terminal hydroxy group water-based polyurethane dispersion; Adopt aforesaid method, synthesis obtains water-based polyurethane dispersion; The terminal hydroxy group water-based polyurethane dispersion of 26% is mixed with 36% water-based polyurethane dispersion, add the coatings additive(s) high-speed stirring 45min of people 8%, add 15%Bayhyder3100 and mix, after stirring 1h, discharging, obtains aqueous dual-component and gathers the cruel soft-feel coating of ammonia.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (5)

1. an aqueous double-component polyurethane soft-feel coating preparation method, is characterized in that, comprises the steps:
Poly-vinegar polyvalent alcohol, DMPA, N-methyl are adjoined and irons alkane ketone, the mixture of IPDI and HDI and DBTL, be incubated and keep backflow;
Add people TEA after reaction to neutralize, stir, obtain the polyurethane prepolymer of hydroxyl;
By pre-polymer solution, add in deionized water under high velocity agitation lentamente, high-speed stirring, form uniform emulsion;
By underpressure distillation in the emulsion flask of falling people, removing acetone, obtains terminal hydroxy group water-based polyurethane dispersion;
Adopt aforesaid method, synthesis obtains water-based polyurethane dispersion;
Terminal hydroxy group water-based polyurethane dispersion mixed with water-based polyurethane dispersion, add the quantitative coatings additive(s) high-speed stirring of people even, add Bayhyder3100 and mix, after stirring, discharging, obtains aqueous dual-component and gathers the cruel soft-feel coating of ammonia.
2. a kind of aqueous double-component polyurethane soft-feel coating preparation method according to claim 1, it is characterized in that, described poly-vinegar polyvalent alcohol, DMPA, N-methyl being adjoined, irons alkane ketone, the mixture of IPDI and HDI and DBTL, is incubated and keeps being implemented as follows of reflow step:
The poly-vinegar polyvalent alcohol of 90 ~ 95g, the DMPA of 6.02 ~ 6.35g, the N-methyl of 3 ~ 5g are adjoined and irons alkane ketone, pass into nitrogen, 100 ~ 120 DEG C of backflow 0.5 ~ 1h are warmed up under whipped state, add the mixture of the IPDI of 2.58 ~ 2.66g and the HDI of 2.56 ~ 2.84g and the DBTL of 2 ~ 5, be incubated and keep backflow.
3. a kind of aqueous double-component polyurethane soft-feel coating preparation method according to claim 1, is characterized in that, add people TEA and neutralize, stir, obtain being implemented as follows of the polyurethane prepolymer step of hydroxyl after described reaction:
After reaction 1 ~ 3h, be cooled to 20 ~ 40 DEG C, add in the TEA of people 4.02 ~ 5.35g and 10 ~ 30min, stir, obtain the polyurethane prepolymer of hydroxyl.
4. a kind of aqueous double-component polyurethane soft-feel coating preparation method according to claim 1, it is characterized in that, described by pre-polymer solution, add in deionized water under high velocity agitation lentamente, high-speed stirring, forms being implemented as follows of uniform emulsion step:
By pre-polymer solution, add in 300 ~ 320ml deionized water under high velocity agitation lentamente, with 1500 ~ 2000r/min high-speed stirring, 1 ~ 2h, form uniform emulsion.
5. a kind of aqueous double-component polyurethane soft-feel coating preparation method according to claim 1, it is characterized in that, described terminal hydroxy group water-based polyurethane dispersion to be mixed with water-based polyurethane dispersion, add people's quantitative coatings additive(s) high-speed stirring even, add Bayhyder3100 to mix, after stirring, discharging, obtains aqueous dual-component and gathers being implemented as follows of the cruel soft-feel coating step of ammonia:
The terminal hydroxy group water-based polyurethane dispersion of 20 ~ 26% is mixed with 30 ~ 36% water-based polyurethane dispersions, add the coatings additive(s) high-speed stirring 30 ~ 45min of people 5 ~ 8%, add 10 ~ 15%Bayhyder3100 to mix, after stirring 0.5 ~ 1h, discharging, obtains aqueous dual-component and gathers the cruel soft-feel coating of ammonia.
CN201410597341.1A 2014-10-26 2014-10-26 Method for preparing aqueous double-component polyurethane flexible coating Pending CN104356911A (en)

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Application Number Priority Date Filing Date Title
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106118441A (en) * 2016-06-30 2016-11-16 太仓市金新涂料有限公司 A kind of environment protection damp-proof anticorrosion antiwear polyurethane primer and preparation method thereof
CN106243957A (en) * 2016-08-03 2016-12-21 常州浩阳水性新材料有限公司 A kind of aqueous two-component polyurethane elastic coating and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106118441A (en) * 2016-06-30 2016-11-16 太仓市金新涂料有限公司 A kind of environment protection damp-proof anticorrosion antiwear polyurethane primer and preparation method thereof
CN106243957A (en) * 2016-08-03 2016-12-21 常州浩阳水性新材料有限公司 A kind of aqueous two-component polyurethane elastic coating and preparation method thereof
CN106243957B (en) * 2016-08-03 2018-07-24 常州浩阳水性新材料有限公司 A kind of aqueous two-component polyurethane elastic coating and preparation method thereof

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Application publication date: 20150218