CN105331274A - Thixotropic bi-compound polyurethane waterproof paint capable of being constructed at high temperature and preparation method thereof - Google Patents
Thixotropic bi-compound polyurethane waterproof paint capable of being constructed at high temperature and preparation method thereof Download PDFInfo
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Abstract
The invention relates to thixotropic bi-compound polyurethane waterproof paint capable of being constructed at a high temperature and a preparation method thereof. The thixotropic bi-compound polyurethane waterproof paint is prepared by mixing a component A and a component B at the mass ratio of 1:2.5. The component A is prepared from, by component content, polyether polyol, toluene diisocyanate, diphenylmethane diisocyanate, a plasticizer, a defoaming agent and a polymerization inhibitor. The component B is prepared from extending oil, a plasticizer, pigment and filler, a solvent, a composite chain extender, a defoaming agent, an emulsifying agent, a dispersing agent, a polymerization inhibitor, a coupling agent and a thixotropic agent. Compared with the prior art, the thixotropic bi-compound polyurethane waterproof paint has the advantages of being environmentally friendly, free of peculiar smells, excellent in storage performance and convenient to construct, and being long in operable time, excellent in overall performance, obvious in cost advantage and the like in a high-temperature construction environment in summer.
Description
Technical field
The present invention relates to a kind of waterproof paint and preparation method thereof, thixotropy double-composition polyurethane waterproof paint especially relating to a kind of construction at high temperature and preparation method thereof.
Background technology
Polyurethane water-proof paint belongs to the high-elastic waterproof coating of reactive chemistry rubber, and this material has the advantage of fill a prescription easy to adjust and excellent combination property, is thus widely used at building field, in buildings waterproof field, occupies critical role.Polyurethane water-proof paint forms according to it, can be divided into the large class of single component and two-pack two, wherein two-pack because film is closely knit, excellent performance, can disposable thick painting, produce simple, the features such as low price are widely used.Because the curing speed of double-composition polyurethane waterproof paint is to very temperature sensitive, cause water-cured polyurethane waterproof coating must avoid construction at high temperature in hot weather construction, but some special engineerings must be constructed again due to the reason of each side under summer high temperature, general polyurethane water-proof paint summer high temperature working viscosity rises very fast, blade coating difficulty, cannot construction requirement be reached at all, which limits the application in the summer high temperature period of urethane., often there is settlement issues in the B component of double-composition polyurethane waterproof paint, even produce the caking of hard-caked sediment time serious in storage process, causes constant to use, sometimes even can cause deterioration in material properties.In the polyurethane water-proof paint new national standard that in August, 2014 implements, I new type merged into by I type in old-national being marked and II type, performance index require to have also been made corresponding raising, the waterproof paint performance index of I type bring up to tensile strength 2.0MPa, elongation at break 500%, tear strength 15N/mm, watertightness requires 0.3MPa, 120min are waterproof, and index of correlation requires stricter.Patent at present for polyurethane water-proof paint is a lot, and as patent CN104559734A reports a kind of two component chemical reaction thixotropic polyurethane water-proof paint and preparation method, the feature of environmental protection of this kind of waterproof paint to polyurethane water-proof paint is not improved.Patent CN104403547A reports environment-friendly type high performance polyurethane water-proof paint and preparation method thereof, and in fact the environment-friendly type of this kind of waterproof paint is not very significantly improved.
Summary of the invention
Object of the present invention be exactly provide a kind of in order to overcome defect that above-mentioned prior art exists and have that environment-protective no-smell, storge quality are excellent, easy construction and under summer high temperature construction environment the thixotropy double-composition polyurethane waterproof paint and preparation method thereof of tool operable time length, excellent combination property, the obvious construction at high temperature of cost advantage.
Object of the present invention can be achieved through the following technical solutions:
The thixotropy double-composition polyurethane waterproof paint of construction at high temperature, by component A and B component in mass ratio for 1:2.5 is mixed to get,
Described component A is prepared by the raw material of following component and weight part content:
Polyether glycol 50-75, tolylene diisocyanate 5-10, diphenylmethanediisocyanate 20-35, softening agent 10-20, defoamer 0.1-0.5, stopper 0.005-0.05;
Described B component is prepared by the raw material of following component and weight part content:
Extending oil 30-50, softening agent 10-30, color stuffing 30-50, solvent 5-10, compound chainextender 5-10, defoamer 0.1-0.5, emulsifying agent 1-5, dispersion agent 0.1-0.5, stopper 0.005-0.05, coupling agent 1-5, thixotropic agent 0.1-0.5.
Described polyether glycol is PPG class polyether glycol, and molecular weight is 500-5000, hydroxyl value 40-400mgKOH/g.
Described softening agent be selected from clorafin, citrate, dioctyl phthalate (DOP), dibutyl phthalate or diisononyl phthalate class softening agent one or more.
Described defoamer is silicone based defoamer.
Described stopper is one or more in ortho-phosphoric acid, tartrate, Benzoyl chloride or phenylformic acid.
Described extending oil is liquid petroleum resin.
Described color stuffing is one or more in carbon black, red iron oxide, iron oxide brown, titanium dioxide, kaolin, cement, coarse whiting, fine particle calcium carbonate, calcium oxide, calcium hydroxide, wollastonite or talcum powder.
Described solvent is 200# solvent oil.
Described compound chainextender is one or more in water, BDO, 4,4'-diamino-3,3'-dichloro diphenyl methanes or trolamine.
Described emulsifying agent is water-in-oil type emulsifier.
Described dispersion agent is polyacrylate(s) dispersion agent.
Described coupling agent is one or more in silane coupling agent or titanate coupling agent.
Described thixotropic agent is one or more in aerosil, organobentonite, polyamide wax or attapulgite.
The preparation method of the thixotropy double-composition polyurethane waterproof paint of construction at high temperature, adopts following steps:
(1) component A preparation:
(1-1) add polyether glycol and softening agent, stir intensification 105 DEG C-115 DEG C, vacuum hydro-extraction 2-3h;
(1-2) said mixture is cooled to 60-70 DEG C, adds after stopper stirs and first add tolylene diisocyanate again, 70 DEG C-80 DEG C reaction 1.5h, add diphenylmethanediisocyanate, 70 DEG C-80 DEG C reaction 1.5h;
(1-3) cool the temperature to 50 DEG C-60 DEG C, add defoamer, stir half an hour, be cooled to 40 DEG C of-45 DEG C of dischargings, obtain component A;
(2) B component preparation: add extending oil, softening agent, dispersion agent, emulsifying agent, defoamer and coupling agent in the reactor, after stirring 0.5-1h under normal temperature, add compound chainextender, color stuffing, thixotropic agent, after stirring 1-3h, add solvent and stopper, discharging after stirring 0.5-1h, namely obtains B component;
(3) control temperature is 45 ~ 55 DEG C, by component A and B component in mass ratio for 1:2.5 mixes and stir, namely prepares the thixotropy double-composition polyurethane waterproof paint of construction at high temperature.
The present invention in order to operable time under realizing construction at high temperature long, solve the problem of normal temperature storage poor stability, mainly it carried out to the improvement of following two aspects.
(1) in component A, the TDI of high reaction activity is first added in reaction system and react, the MDI adding low reaction activity after reaction for some time again reacts, in system, the TDI of high reaction activity first reacts, now in reaction system, the TDI content of free state is extremely low, the MDI of the low reaction activity added subsequently continues and the reactive with active hydrogen in system, feel in such system that most NCO has the MDI of low reaction activity to provide, not only reduce the TDI of free state like this, and the stopper of the low reaction activity MDI of free state and trace not only ensure that this coating has excellent mechanical property, and environmental protection aspect is much improved, what is more important extends the class operating time of construction at high temperature.
(2) thixotropy paste is obtained under the emulsifying agent in B component, thixotropic agent and compound chainextender synergy, the introducing of emulsifying agent and compound chainextender can improve the stability of paste, the introducing of thixotropic agent makes system have thixotropy, thus solves the problem of sedimentation in B component storage.
Compared with prior art, it is long that the polyurethane water-proof paint that the present invention prepares has construction operation time under summer high temperature, and stability in storage is excellent, and mechanical property is given prominence to, and free from extraneous odour, TDI content is extremely low, and toxicity is reduced to greatest extent.Experiment proves: polyurethane water-proof paint of the present invention is at 23 ~ 30 DEG C of operable time 60 ~ 75min, 50 ~ 55 DEG C of construction section operating times of high temperature, 45 ~ 55 DEG C of min, meet the special construction engineering that some hot weather construction temperature are higher, expand the application of polyurethane water-proof paint.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
The preparation method of the thixotropy double-composition polyurethane waterproof paint of construction at high temperature, adopts following steps:
Component A be prepared in the 1000mL four-hole boiling flask that agitator, prolong, thermometer, constant pressure funnel are housed, first polyether Glycols (2000D) 60 parts, polyether-tribasic alcohol (330N) 15 parts and clorafin 10 parts is added, stir intensification 105 DEG C-115 DEG C, vacuum hydro-extraction 2-3 hour; Said mixture is cooled to 60-70 DEG C, adds after stopper stirs and first add tolylene diisocyanate 5 parts again, 70 DEG C-80 DEG C reactions after 1.5 hours, then add diphenylmethanediisocyanate 20 parts, and 70 DEG C-80 DEG C are reacted 1.5 hours; Cool the temperature to 50 DEG C-60 DEG C, add defoamer 0.1 part, stir half an hour, be cooled to 40 DEG C of-45 DEG C of dischargings, obtain component A;
Add liquid petroleum resin 50 parts, clorafin 30 parts, dispersion agent 0.5 part, emulsifying agent 1 part, defoamer 0.1 part and silane coupling agent 1 part in the reactor, after stirring 0.5h under normal temperature, add compound chainextender 5 parts, coarse whiting 15 parts, talcum powder 10 parts, fine particle calcium carbonate 5 parts, 15 parts, calcium oxide, 5 parts, calcium hydroxide, polyamide wax 0.1 part, stir 1h to even, add 200# solvent 10 parts and stopper 0.005 part, discharging after stirring, namely obtains B component.
During use, control temperature is 45 DEG C, by the 1:2.5 ratio uniform mixing in mass ratio of A, B component, can obtain polyurethane waterproof coating.
Embodiment 2
The preparation method of the thixotropy double-composition polyurethane waterproof paint of construction at high temperature, adopts following steps:
Component A be prepared in the 1000mL four-hole boiling flask that agitator, prolong, thermometer, constant pressure funnel are housed, first polyether Glycols (2000D) 65 parts, polyether-tribasic alcohol (330N) 10 parts and clorafin 10 parts is added, stir intensification 105 DEG C-115 DEG C, vacuum hydro-extraction 2-3 hour; Said mixture is cooled to 60-70 DEG C, adds after stopper stirs and first add tolylene diisocyanate 5 parts again, 70 DEG C-80 DEG C reactions, after 1.5 hours, are adding diphenylmethanediisocyanate 25 parts, and 70 DEG C-80 DEG C are reacted 1.5 hours; Cool the temperature to 50 DEG C-60 DEG C, add defoamer 0.1 part, stir half an hour, be cooled to 40 DEG C of-45 DEG C of dischargings, obtain component A;
Add liquid petroleum resin 50 parts, clorafin 30 parts, dispersion agent 0.5 part, emulsifying agent 1 part, defoamer 0.1 part and silane coupling agent 1 part in the reactor, after abundant stirring, add compound chainextender 5 parts, coarse whiting 15 parts, talcum powder 10 parts, fine particle calcium carbonate 5 parts, 15 parts, calcium oxide, 5 parts, calcium hydroxide, organobentonite 0.1 part, be stirred to evenly, add 200# solvent 10 parts and stopper 0.005 part, discharging after stirring, namely obtains B component.
During use, control temperature is 50 DEG C, by the 1:2.5 ratio uniform mixing in mass ratio of A, B component, can obtain polyurethane waterproof coating.
Embodiment 3
The preparation method of the thixotropy double-composition polyurethane waterproof paint of construction at high temperature, adopts following steps:
Component A be prepared in the 1000mL four-hole boiling flask that agitator, prolong, thermometer, constant pressure funnel are housed, first polyether Glycols (2000D) 60 parts, polyether-tribasic alcohol (330N) 15 parts and clorafin 10 parts is added, stir intensification 105 DEG C-115 DEG C, vacuum hydro-extraction 2-3 hour; Said mixture is cooled to 60-70 DEG C, adds after stopper stirs and first add tolylene diisocyanate 5 parts again, 70 DEG C-80 DEG C reactions, after 1.5 hours, are adding diphenylmethanediisocyanate 30 parts, and 70 DEG C-80 DEG C are reacted 1.5 hours; Cool the temperature to 50 DEG C-60 DEG C, add defoamer 0.5 part, stir half an hour, be cooled to 40 DEG C of-45 DEG C of dischargings, obtain component A;
Add liquid petroleum resin 50 parts, clorafin 30 parts, dispersion agent 0.5 part, emulsifying agent 1 part, defoamer 0.1 part and titanate coupling agent 1 part in the reactor, after abundant stirring, add compound chainextender 5 parts, coarse whiting 10 parts, talcum powder 10 parts, fine particle calcium carbonate 10 parts, 10 parts, calcium oxide, 10 parts, calcium hydroxide, attapulgite 0.1 part, be stirred to evenly, add 200# solvent 10 parts and stopper 0.005 part, discharging after stirring, namely obtains B component.
During use, control temperature is 55 DEG C, by the 1:2.5 ratio uniform mixing in mass ratio of A, B component, can obtain polyurethane waterproof coating.
Embodiment 4
The preparation method of the thixotropy double-composition polyurethane waterproof paint of construction at high temperature, adopts following steps:
Component A be prepared in the 1000mL four-hole boiling flask that agitator, prolong, thermometer, constant pressure funnel are housed, first polyether Glycols (2000D) 40 parts, polyether Glycols (1000D) 20 parts, polyether-tribasic alcohol (330N) 10 parts and clorafin 10 parts is added, stir intensification 105 DEG C-115 DEG C, vacuum hydro-extraction 2-3 hour; Said mixture is cooled to 60-70 DEG C, adds after stopper stirs and first add tolylene diisocyanate 5 parts again, 70 DEG C-80 DEG C reactions, after 1.5 hours, are adding diphenylmethanediisocyanate 35 parts, and 70 DEG C-80 DEG C are reacted 1.5 hours; Cool the temperature to 50 DEG C-60 DEG C, add defoamer 0.5 part, stir half an hour, be cooled to 40 DEG C of-45 DEG C of dischargings, obtain component A;
Add liquid petroleum resin 50 parts, clorafin 30 parts, dispersion agent 0.5 part, emulsifying agent 1 part, defoamer 0.1 part and titanate coupling agent 1 part in the reactor, after abundant stirring, add compound chainextender 5 parts, talcum powder 10 parts, fine particle calcium carbonate 15 parts, 20 parts, calcium oxide, 5 parts, calcium hydroxide, aerosil 0.1 part, be stirred to evenly, add 200# solvent 10 parts and stopper 0.005 part, discharging after stirring, namely obtains B component.
During use, by the 1:2.5 ratio uniform mixing in mass ratio of A, B component, polyurethane waterproof coating can be obtained.
Respectively Performance Detection is carried out to the Two-component Waterproof Polyurethane Coating that above-described embodiment obtains, the results are shown in Table 1.
Table 1 embodiment 1 ~ 4 double-composition polyurethane waterproof paint carries out performance test results
As shown in Table 1, embodiment 1 ~ 4 double-composition polyurethane waterproof paint, at 23 ~ 30 DEG C of operable time about 40 ~ 75min, the construction operable time of high temperature 50 ~ 55 DEG C is about 31 ~ 55min, meet the special construction engineering that some hot weather construction temperature are higher, expand the application of polyurethane water-proof paint.
Can draw from upper table, the technical indicator that the GB/T19250-2013 that product properties prepared by example 1,2,3,4 all can reach this area requires.
Embodiment 5
The thixotropy double-composition polyurethane waterproof paint of construction at high temperature, by component A and B component in mass ratio for 1:2.5 is mixed to get.Component A is prepared by the raw material of following component and content: polyether glycol 50g, tolylene diisocyanate 5g, diphenylmethanediisocyanate 20g, softening agent 10g, defoamer 0.1g, stopper 0.005g; B component is prepared by the raw material of following component and content: extending oil 30g, softening agent 10g, color stuffing 30g, solvent 5g, compound chainextender 5g, defoamer 0.1g, emulsifying agent 1g, dispersion agent 0.1g, stopper 0.005g, coupling agent 1g, thixotropic agent 0.1g.
In above raw material, polyether glycol is PPG class polyether glycol, and molecular weight is 500, hydroxyl value 40mgKOH/g.Softening agent is clorafin.Defoamer is silicone based defoamer.Stopper is ortho-phosphoric acid.Extending oil is liquid petroleum resin.Color stuffing is carbon black.Solvent is 200# solvent oil.Compound chainextender is water.Emulsifying agent is water-in-oil type emulsifier.Dispersion agent is polyacrylate(s) dispersion agent.Coupling agent is silane coupling agent.Thixotropic agent is aerosil.
The preparation method of the thixotropy double-composition polyurethane waterproof paint of construction at high temperature, adopts following steps:
(1) component A preparation:
(1-1) add polyether glycol and softening agent, stir intensification 105 DEG C, vacuum hydro-extraction 3h;
(1-2) said mixture is cooled to 60 DEG C, adds after stopper stirs and first add tolylene diisocyanate again, 70 DEG C of reaction 1.5h, add diphenylmethanediisocyanate, 70 DEG C of reaction 1.5h;
(1-3) cool the temperature to 50 DEG C, add defoamer, stir half an hour, be cooled to 40 DEG C of dischargings, obtain component A;
(2) B component preparation: add extending oil, softening agent, dispersion agent, emulsifying agent, defoamer and coupling agent in the reactor, after stirring 0.5h under normal temperature, add compound chainextender, color stuffing, thixotropic agent, after stirring 1h, add solvent and stopper, discharging after stirring 0.5h, namely obtains B component;
(3) control temperature is 45 DEG C, by component A and B component in mass ratio for 1:2.5 mixes and stir, namely prepares the thixotropy double-composition polyurethane waterproof paint of construction at high temperature.
Embodiment 6
The thixotropy double-composition polyurethane waterproof paint of construction at high temperature, by component A and B component in mass ratio for 1:2.5 is mixed to get, component A is prepared by the raw material of following component and content: polyether glycol 75g, tolylene diisocyanate 10g, diphenylmethanediisocyanate 35g, softening agent 20g, defoamer 0.5g, stopper 0.05g; B component is prepared by the raw material of following component and content: extending oil 50g, softening agent 30g, color stuffing 50g, solvent 10g, compound chainextender 10g, defoamer 0.5g, emulsifying agent 5g, dispersion agent 0.5g, stopper 0.05g, coupling agent 5g, thixotropic agent 0.5g.
In above raw material, polyether glycol is PPG class polyether glycol, and molecular weight is 5000, hydroxyl value 400mgKOH/g.Softening agent is the mixture of dioctyl phthalate (DOP), dibutyl phthalate.Defoamer is silicone based defoamer.Stopper is tartrate.Extending oil is liquid petroleum resin.Color stuffing is red iron oxide.Solvent is 200# solvent oil.Compound chainextender is BDO.Emulsifying agent is water-in-oil type emulsifier.Dispersion agent is polyacrylate(s) dispersion agent.Coupling agent is titanate coupling agent.Thixotropic agent is organobentonite.
The preparation method of the thixotropy double-composition polyurethane waterproof paint of construction at high temperature, adopts following steps:
(1) component A preparation:
(1-1) add polyether glycol and softening agent, stir intensification 115 DEG C, vacuum hydro-extraction 3h;
(1-2) said mixture is cooled to 60-70 DEG C, adds after stopper stirs and first add tolylene diisocyanate again, 80 DEG C of reaction 1.5h, add diphenylmethanediisocyanate, 80 DEG C of reaction 1.5h;
(1-3) cool the temperature to 60 DEG C, add defoamer, stir half an hour, be cooled to 45 DEG C of dischargings, obtain component A;
(2) B component preparation: add extending oil, softening agent, dispersion agent, emulsifying agent, defoamer and coupling agent in the reactor, after stirring 1h under normal temperature, add compound chainextender, color stuffing, thixotropic agent, after stirring 3h, add solvent and stopper, discharging after stirring 1h, namely obtains B component;
(3) control temperature is 55 DEG C, by component A and B component in mass ratio for 1:2.5 mixes and stir, namely prepares the thixotropy double-composition polyurethane waterproof paint of construction at high temperature.
Claims (9)
1. the thixotropy double-composition polyurethane waterproof paint of construction at high temperature, is characterized in that, this waterproof paint by component A and B component in mass ratio for 1:2.5 is mixed to get,
Described component A is prepared by the raw material of following component and weight part content:
Polyether glycol 50-75, tolylene diisocyanate 5-10, diphenylmethanediisocyanate 20-35, softening agent 10-20, defoamer 0.1-0.5, stopper 0.005-0.05;
Described B component is prepared by the raw material of following component and weight part content:
Extending oil 30-50, softening agent 10-30, color stuffing 30-50, solvent 5-10, compound chainextender 5-10, defoamer 0.1-0.5, emulsifying agent 1-5, dispersion agent 0.1-0.5, stopper 0.005-0.05, coupling agent 1-5, thixotropic agent 0.1-0.5.
2. the thixotropy double-composition polyurethane waterproof paint of construction at high temperature according to claim 1, is characterized in that, described polyether glycol is PPG class polyether glycol, and molecular weight is 500-5000, hydroxyl value 40-400mgKOH/g.
3. the thixotropy double-composition polyurethane waterproof paint of construction at high temperature according to claim 1, it is characterized in that, described softening agent be selected from clorafin, citrate, dioctyl phthalate (DOP), dibutyl phthalate or diisononyl phthalate class softening agent one or more.
4. the thixotropy double-composition polyurethane waterproof paint of construction at high temperature according to claim 1, it is characterized in that, described defoamer is silicone based defoamer, and described stopper is one or more in ortho-phosphoric acid, tartrate, Benzoyl chloride or phenylformic acid.
5. the thixotropy double-composition polyurethane waterproof paint of construction at high temperature according to claim 1, it is characterized in that, described extending oil is liquid petroleum resin, and described color stuffing is one or more in carbon black, red iron oxide, iron oxide brown, titanium dioxide, kaolin, cement, coarse whiting, fine particle calcium carbonate, calcium oxide, calcium hydroxide, wollastonite or talcum powder.
6. the thixotropy double-composition polyurethane waterproof paint of construction at high temperature according to claim 1, it is characterized in that, described solvent is 200# solvent 0 oil, described compound chainextender is water, 1,4-butyleneglycol, 4, one or more in 4'-diamino-3,3'-dichloro diphenyl methane or trolamine.
7. the thixotropy double-composition polyurethane waterproof paint of construction at high temperature according to claim 1, is characterized in that, described emulsifying agent is water-in-oil type emulsifier, and described dispersion agent is polyacrylate(s) dispersion agent.
8. the thixotropy double-composition polyurethane waterproof paint of construction at high temperature according to claim 1, it is characterized in that, described coupling agent is one or more in silane coupling agent or titanate coupling agent, and described thixotropic agent is one or more in aerosil, organobentonite, polyamide wax or attapulgite.
9. the preparation method of the thixotropy double-composition polyurethane waterproof paint of construction at high temperature as claimed in claim 1, is characterized in that, the method adopts following steps:
(1) component A preparation:
(1-1) add polyether glycol and softening agent, stir intensification 105 DEG C-115 DEG C, vacuum hydro-extraction 2-3h;
(1-2) said mixture is cooled to 60-70 DEG C, adds after stopper stirs and first add tolylene diisocyanate again, 70 DEG C-80 DEG C reaction 1.5h, add diphenylmethanediisocyanate, 70 DEG C-80 DEG C reaction 1.5h;
(1-3) cool the temperature to 50 DEG C-60 DEG C, add defoamer, stir half an hour, be cooled to 40 DEG C of-45 DEG C of dischargings, obtain component A;
(2) B component preparation: add extending oil, softening agent, dispersion agent, emulsifying agent, defoamer and coupling agent in the reactor, after stirring 0.5-1h under normal temperature, add compound chainextender, color stuffing, thixotropic agent, after stirring 1-3h, add solvent and stopper, discharging after stirring 0.5-1h, namely obtains B component;
(3) control temperature is 45 ~ 55 DEG C, by component A and B component in mass ratio for 1:2.5 mixes and stir, namely prepares the thixotropy double-composition polyurethane waterproof paint of construction at high temperature.
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