CN102690626B - Single-component polyurethane sealant capable of quickly curing moisture and preparation method thereof - Google Patents
Single-component polyurethane sealant capable of quickly curing moisture and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a single-component polyurethane sealant capable of quickly curing moisture and a preparation method thereof. The polyurethane sealant comprises the following raw materials in percentage by weight: 10 to 20 percent of polyisocyanate monomer, 20 to 45 percent of polyether polyol, 1 to 10 percent of acetoacetic ester sealed end polyether prepolymer, 5 to 20 percent of plasticizer, 25 to 40 percent of modified mineral powder, 1 to 5 percent of latent curing agent, 0.1 to 2 percent of cyclodextrin wrapped environment-friendly catalyst, 0.1 to 1 percent of defoaming agent and 0.1 to 1 percent of water-removing agent, wherein the water-removing agent is one or more of mono-isocyanate compound or functionalized silane compound. The single-component polyurethane sealant avoids bubble fundamentally, can be quickly cured, is stable in storage, and can be applied to construction on damp interfaces.
Description
Technical field
The present invention relates to a kind of seal gum, particularly a kind of building field polyurethane sealant is specifically related to the quick-setting one-component polyurethane sealant of a kind of moisture.
Background technology
The commercially available building sealant of China can be divided into two big class, i.e. mineral-type and organic classes.The mineral-type seal gum namely is general putty powder and putty paste, does not have elasticity after the curing, and along with the dilatation of building slab, very fast generation bonding interface destroys or cohesive failure, and the loss of seal function.Organic class seal gum comprises silicone adhesive, polyacrylic acid ester gum, polyurethane adhesive etc., and this series products cohesive force is stronger, and flexible after solidifying, sealing effectiveness is better.Wherein polyurethane sealant has lot of advantages, as: good wear resistance, low-temperature pliability, cementability is good, and good springiness is applicable to dynamic seam.But present polyurethane sealant also has some shortcomings, as: one-component polyurethane sealant package stability packed and extraneous humidity effect bigger; The seal gum thickness of once constructing is big, and relative humidity is low in the air, and the quantity that moisture penetrates in the colloid reduces, and curing speed is slack-off thereupon, and bondline thickness is more thick, and then set time is more long; Under the elevated temperature heat environment, may produce bubble and crackle.Though silicone sealant does not exist foaming, ageing-resistant problem, because expensive and make to promote and be restricted.
At present, China is in construction industry high-speed development period, for the building sealant industry provides a huge market.Yet no matter China's building sealant is in kind quantitatively, still on mass effect, also fails to satisfy the needs in market far away.
Summary of the invention
Technical problem to be solved by this invention is to overcome the deficiencies in the prior art, and a kind of storage good stability and the quick-setting one-component polyurethane sealant of moisture are provided.
The present invention also will provide the preparation method of the quick-setting one-component polyurethane sealant of a kind of moisture simultaneously.
For solving above technical problem, a kind of technical scheme that the present invention takes is:
The quick-setting one-component polyurethane sealant of a kind of moisture, in weight percentage, its raw material is composed as follows: environment-friendly type catalyzer 0.1% ~ 2%, defoamer 0.1% ~ 1% and the water-removal agent 0.1% ~ 1% of polyisocynate monomer 10% ~ 20%, polyether glycol 20% ~ 45%, acetylacetic ester end capped polyether prepolymer 1% ~ 10%, softening agent 5% ~ 20%, modification breeze 25% ~ 40%, latent curing agent 1% ~ 5%, cyclodextrin parcel, and wherein: the modification breeze is for handling the mineral powder that the surface is coated with coating through chemical coating method; In the environment-friendly type catalyzer of described cyclodextrin parcel, the environment-friendly type catalyzer is in the lar nanometric cavities of cyclodextrin, and cyclodextrin is unmodified cyclodextrin or modified cyclodextrin or the combination of the two; Water-removal agent is to be selected from monoisocyanates compounds or the functionalized silane compounds one or more.
Among the present invention, acetylacetic ester end capped polyether prepolymer is a kind of with acetylacetic ester terminated polyether prepolymer, the Prepolymerizing process preparation of the routine that can be taked by those skilled in the art.
According to a preferred aspect of the present invention, acetylacetic ester end capped polyether prepolymer is reacted under catalyst action by polyether Glycols and/or polyether-tribasic alcohol and/or polyether tetrols and Acetacetic acid alkyl ester and obtains, wherein, Acetacetic acid alkyl ester is preferably and is selected from methyl aceto acetate, etheric acid n-propyl, ISOPROPYL ACETOACETATE, the positive butyl ester of etheric acid and the special butyl ester of etheric acid one or more.Further preferably, polyether Glycols is polyoxyethylene dibasic alcohol or polyoxytrimethylene dibasic alcohol; Polyether-tribasic alcohol is polyoxyethylene trivalent alcohol or polyoxytrimethylene trivalent alcohol; So, acetylacetic ester end capped polyether prepolymer can be expressed as follows with general formula:
In the general formula, R represents oxyethyl group, propoxy-or isopropoxy; X is 10 ~ 200 integer, and y is 2,3 or 4.
Should be understood that the purpose that provides above-mentioned general formula is only is clearer and understand acetylacetic ester end capped polyether prepolymer clearly for those skilled in the art.Acetylacetic ester end capped polyether prepolymer can be represented with above-mentioned general formula, be not equal to acetylacetic ester end capped polyether prepolymer and be equal to the content that this general formula is expressed fully, and should be these those skilled in the art on this general formula basis in conjunction with the confirmable content of general knowledge, for example, be appreciated that, acetylacetic ester end capped polyether prepolymer is generally the mixture of the material that satisfies above-mentioned general formula, this be since prepolymer as a kind of polymkeric substance, impossible as micromolecular compound, can be with one-component acquisition completely.
According to the present invention, described polyisocynate monomer can be the common tolylene diisocyanate in market (TDI), diphenylmethanediisocyanate (MDI), isophorone diisocyanate (IPDI), hexamethylene diisocyanate (HDI) etc.Wherein TDI and MDI are used for the non-product that exposes, and IPDI and HDI are used for exposing product.Because TDI and HDI vapour pressure height, high volatility have the strong impulse smell, take all factors into consideration from the feature of environmental protection and direct labor's security of product, the present invention is MDI and IPDI more preferably, is respectively applied to the non-product that exposes and expose.
According to an aspect of the present invention, the functionality of polyether glycol is 2 ~ 3, and preferably, polyether glycol is to be selected from polyglycol ether, polypropylene glycol ether and the polyglycerol ether one or more.Preferably, the hydroxyl value of polyether glycol is between 10～100KOHmg/g, and more preferably, hydroxyl value is 20～58KOHmg/g.
According to the present invention, softening agent can be this area type commonly used.Preferably, softening agent is propylene carbonate.Because propylene carbonate and urethane resin can form chemical bonding, lower with traditional phase specific viscosities such as softening agent clorafin, dibutyl phthalate and dioctyl phthalate (DOP), consistency is good, can be along with time-shift goes out seal gum, its use both can reduce system viscosity, also can improve durability of products.
Described chemical coating method is known, and it refers to the method for modification is carried out on the surface that is wrapped by material and is generally inorganic particulate by silane coupling agent, stearic acid etc.According to the present invention, described coating is preferably silane coupling agent.Described mineral powder includes but not limited to calcined kaolin, talcum powder, wollastonite powder and calcium carbonate etc.The modification breeze is not easy to reunite, precipitate after joining polyurethane system, can not only improve the consistency with polyurethane system, also can reduce system viscosity preferably, improve levelling.
According to the present invention, described latent curing agent is preferably the oxazole alkanes solidifying agent of hiding, rapid hydrolysis after running into water, latent curing agent takes place under the effect of catalyzer, discharge active amino, isocyanate group crosslinking curing in a part and the system, thereby stopped the generation of carbon dioxide from the source, eliminated the chemistry bubble of system.A part of oxazolidine generates water, thereby further promotes the latent curing agent hydrolysis by the rapid and acetylacetic ester terminated prepolymer reaction of polyamino oligopolymer that hydrolysis generates in addition.So as long as the seal gum system absorbs micro-moisture in the air, get final product so that the crosslinking curing of system is finished rapidly.
According to the present invention, the environment-friendly type catalyzer of cyclodextrin parcel belongs to a kind of coated catalysts microcapsule.The preparation of this kind catalyst micro capsule is fairly simple, a concrete method is: the catalyst dissolution that will need to coat is in ethanol, the cyclodextrin or derivatives thereof is mixed with saturated solution (solution is that water and ethanol mix according to the volume ratio of 2:1), heated and stirred, temperature is controlled at 45～55 ℃, slowly joins catalyzer in the saturated solution, continuously stirring is disperseed, vacuum filtration then 50 ℃ of vacuum-dryings, namely gets the coated catalysts microcapsule with throw out.Utilize the lar nanometric cavities of cyclodextrin that catalyst pack is wrapped, reduce the reactive behavior of catalyzer, the lar nanometric cavities of cyclodextrin discharges catalyzer by expansion after running into steam.Compare with the catalyzer of routine, the employing of the environment-friendly type catalyzer of cyclodextrin parcel can make the stability of polyurethane system be greatly improved, and uses the polyurethane system storage period of this catalyzer can be above 1 year.And conventional polyurethane body series catalysts, as dibutyl tin laurate, stannous octoate, isocaprylic acid lead and isocaprylic acid zinc etc., the isocyanic ester system had advantages of high catalytic activity, if the catalyzer addition is few, the system curing speed is slower, increasing addition can the acceleration system solidify, but causes system viscosity to increase obviously easily, influences its stability in storage.
Preferably, the environment-friendly type catalyzer is organo-bismuth class complex compound, and it is gentleer that it compares other environment-friendly type catalyzer to the polyurethane system catalytic activity.
According to the present invention, described defoamer is mainly used in the mechanical bubble that the elimination system produces in production and application process, and it can be this area type of anti-foam agent commonly used, but is preferably polyether-modified polysiloxane defoamer.
According to the present invention, can be for rubigan isocyanic ester for example,-sulfinic acid phenyl isocyanate, to Methyl benzenesulfonyl isocyanate, methacrylic acid isocyanate group ethyl ester and phenyl isocyanate etc. as the monoisocyanates compounds of water-removal agent.Functionalized silane compounds as water-removal agent can be for example vinyltrimethoxy silane, vinyltriethoxysilane etc.The existence of water can cause system viscosity to increase, and is unfavorable for storing.In prescription, add water-removal agent, can improve storge quality.
The another technical scheme that the present invention takes is: a kind of preparation method of the above-mentioned quick-setting one-component polyurethane sealant of moisture, it comprises the steps:
(1), polyether glycol and the acetylacetic ester that will have 2 ~ 4 hydroxyls carry out prepolymerization reaction under catalyst action, after reaction finishes, except the alkyl alcohol that dereaction generates, obtain acetylacetic ester end capped polyether prepolymer by underpressure distillation;
(2), in closed reactor, add polyether glycol, softening agent and the modification breeze of formula ratio, stir and heat up, temperature control at 100 ℃ ~ 120 ℃, the unlatching vacuum pump is taken out negative pressure, pressure-controlling-below the 0.08MPa; Cool to then below 70 ℃, feed drying nitrogen and remove vacuum, the polyisocynate monomer that adds formula ratio, temperature control is carried out polyreaction at 75～85 ℃, after polyreaction finishes, be cooled to below 50 ℃, environment-friendly type catalyzer and the water-removal agent of the acetylacetic ester blocked prepolymer of adding formula ratio, defoamer, latent curing agent, cyclodextrin parcel mix, and namely get the quick-setting one-component polyurethane sealant of described moisture
Preparation in accordance with the present invention, in the step (1), described catalyzer can carry out for example bismuth carboxylate catalyzer of prepolymerization reaction those catalyzer commonly used for polyether glycol.The temperature of prepolymerization reaction can adopt according to the needs of real reaction, and is relevant with catalyzer usually.For example when adopting the bismuth carboxylate catalyzer, the temperature of reaction can be 130 ~ 150 ℃, more specifically, and for example 140 ℃.
Preferably, last what prepare, seal gum is packed in the nitrogen protection bottom discharge.
The quick-setting one-component polyurethane sealant of moisture provided by the invention has following characteristics:
(1) single-component packing, construction need not the field mix preparation;
(2) to concrete with metal-based layer sticking power is eager to do well in everything, snappiness good, weather-proof, hydrolysis;
(3) fast setting can be in moist basal plane construction, and the thickness of once constructing can reach 10mm and also can solidify fully in several hours, and can not bubble.Can be deployed into various colored seal gums according to the construction needs;
(4) fabulous stability in storage adopts mineral powder and the catalyzer handled through special methods, does not reunite, viscosity changes for a short time, greatly improved the stability in storage of system;
(5) high solids content does not add any diluting solvent, and adopts the new catalyst of nontoxic pollution-free, belongs to environmentally friendly machine, has widened the Application Areas of polyurethane sealant.
Because the utilization of above technical scheme, the present invention compared with prior art has following advantage:
The polyurethane sealant of moisture-curable provided by the invention has solved the problems of stability in storage of existing one-component polyurethane sealant product, and the shelf lives can be above 1 year; In addition, the present invention also stops bubble and produces from the source, but fast setting (the thickness 10mm that once constructs also can solidify in 2h fully), and can not produce bubble in moist basal plane construction yet, can be used for various joint seal engineerings.Good, the environmental protection of Material Physics mechanical property after the curing except can be used for building field, can also be used in fields such as food, pharmacy, water works.
Embodiment
Below in conjunction with specific embodiment the present invention is described in further details.
Acetylacetic ester end capped polyether prepolymer used in following examples 1 ~ 3 is the polyether glycol composition with polyoxyethylene dibasic alcohol and polyoxytrimethylene dibasic alcohol respectively, with methyl aceto acetate be the end-blocking composition, be prepared as follows and obtain: make polyether glycol composition and methyl aceto acetate and bismuth carboxylate catalyst mix, be heated to 140 ℃, under this temperature, stirred 1 ~ 2 hour, by underpressure distillation the alkyl alcohol that generates is steamed, namely, wherein, the polyether glycol composition, the molar ratio of methyl aceto acetate is 2:1, the weight that feeds intake of bismuth carboxylate catalyzer be the polyether glycol composition weight 0.01%.
Acetylacetic ester end capped polyether prepolymer used among the embodiment 4 and 5 is the end-blocking composition with ISOPROPYL ACETOACETATE and the special butyl ester of etheric acid respectively, is the polyether glycol composition with the polyoxyethylene dibasic alcohol, prepares according to above-mentioned method and condition.
Used acetylacetic ester end capped polyether prepolymer is to be the polyether glycol composition with the polyoxytrimethylene trivalent alcohol among the embodiment 6, with the positive butyl ester of etheric acid, prepares according to above-mentioned method and condition.
Embodiment 1
Present embodiment provides quick-setting one-component polyurethane sealant of a kind of moisture and preparation method thereof.
By weight, the raw material of the quick-setting one-component polyurethane sealant of moisture consists of: diphenylmethanediisocyanate MI-50(BASF AG) 13 parts, polyether glycol (DL-4000, Shandong Lanxing Dongda Chemical Co.,Ltd) 35 part, 5 parts of acetylacetic ester blocked prepolymers, 10 parts of propylene carbonates, 35 parts of silane coupler modified calcined kaolins, 1 part in oxazolidine solidifying agent (FT-103, Zhangjiagang Fitow company), 0.5 part in the organo-bismuth complex compound (Shanghai grass tree chemical industry company limited) that cyclodextrin coats, 0.3 part of defoamer (BYK-378) and to 0.2 part of Methyl benzenesulfonyl isocyanate (Chemical Reagent Co., Ltd., Sinopharm Group).
The preparation process of the quick-setting one-component polyurethane sealant of moisture is as follows:
The first step: in closed reactor, add polyether glycol, propylene carbonate and silane coupler modified calcined kaolin, stir and heat up, temperature control at 100～120 ℃, and the unlatching vacuum pump is taken out negative pressure, pressure-controlling-below the 0.08MPa, vacuumize 1h;
Second step: cool to below 70 ℃, feed drying nitrogen and remove vacuum, add the liquefaction diphenylmethanediisocyanate, temperature is controlled at 75～85 ℃, polyreaction 3h;
The 3rd step: cool to below 50 ℃, add acetylacetic ester blocked prepolymer, defoamer BYK-378, oxazolidine FT-103, coat organo-bismuth and to Methyl benzenesulfonyl isocyanate, mix 30min, pack in the nitrogen protection bottom discharge.
Embodiment 2
Present embodiment provides quick-setting one-component polyurethane sealant of a kind of moisture and preparation method thereof.
By weight, the raw material of the quick-setting one-component polyurethane sealant of moisture consists of: diphenylmethanediisocyanate MI-50(BASF AG) 13 parts, polyether glycol (DL-4000, Shandong Lanxing Dongda Chemical Co.,Ltd) 30 part, 10 parts of polyether glycols (EP-330N), 3 parts of acetylacetic ester blocked prepolymers, 10 parts of propylene carbonates, 30 parts of silane coupler modified talcum powder, 2 parts in oxazolidine solidifying agent (FT-103, Zhangjiagang Fitow company), 1 part in the organo-bismuth complex compound (Shanghai grass tree chemical industry company limited) that cyclodextrin coats, 0.5 part of defoamer (BYK-378) and to 0.5 part of Methyl benzenesulfonyl isocyanate (Chemical Reagent Co., Ltd., Sinopharm Group).
The preparation method of the quick-setting one-component polyurethane sealant of moisture is as follows:
The first step: in closed reactor, add polyether glycol DL-4000, polyether glycol EP-330N, propylene carbonate and silane coupler modified talcum powder, stir and heat up, temperature control is at 100～120 ℃, open vacuum pump and take out negative pressure, pressure-controlling-below the 0.08MPa, vacuumize 1h;
Second step: cool to below 70 ℃, feed drying nitrogen and remove vacuum, add liquefaction diphenylmethanediisocyanate MI-50, temperature is controlled at 75～85 ℃, polyreaction 3h;
The 3rd step: cool to below 50 ℃; add organo-bismuth complex compound that acetylacetic ester blocked prepolymer, defoamer BYK-378, oxazolidine solidifying agent FT-103, cyclodextrin coat and to Methyl benzenesulfonyl isocyanate; mix 30min, pack in the nitrogen protection bottom discharge.
Embodiment 3
Present embodiment provides a kind of moisture quick-setting one-component polyurethane sealant, and it prepares by the method identical with embodiment 1.By weight, the raw material of the quick-setting one-component polyurethane sealant of moisture is composed as follows:
12 parts of isophorone diisocyanates (Beyer Co., Ltd), polyether glycol (DL-4000, Shandong Lanxing Dongda Chemical Co.,Ltd) 30 part, 5 parts of polyether glycols (DL-3000), 5 parts of acetylacetic ester blocked prepolymers, 10 parts of propylene carbonates, 35 parts of silane coupler modified talcum powder, 1 part in oxazolidine solidifying agent (FT-103, Zhangjiagang Fitow company), 1 part in the organo-bismuth complex compound (Shanghai grass tree chemical industry company limited) that cyclodextrin coats, 0.5 part of defoamer (BYK-378) and to 0.5 part of Methyl benzenesulfonyl isocyanate (Chemical Reagent Co., Ltd., Sinopharm Group).
Embodiment 4
Present embodiment provides a kind of moisture quick-setting one-component polyurethane sealant, and it prepares by the method identical with embodiment 1.By weight, the raw material of the quick-setting one-component polyurethane sealant of moisture is composed as follows:
20 parts of isophorone diisocyanates (Beyer Co., Ltd), polyether glycol (DL-4000, Shandong Lanxing Dongda Chemical Co.,Ltd) 26 part, 3 parts of polyether glycols (DL-3000), 3 parts of acetylacetic ester blocked prepolymers, 10 parts of propylene carbonates, 35 parts of silane coupler modified talcum powder, 1 part in oxazolidine solidifying agent (FT-103, Zhangjiagang Fitow company), 1 part in the organo-bismuth complex compound (Shanghai grass tree chemical industry company limited) that cyclodextrin coats, 0.5 part of defoamer (BYK-378) and to 0.5 part of Methyl benzenesulfonyl isocyanate (Chemical Reagent Co., Ltd., Sinopharm Group).
Embodiment 5
Present embodiment provides a kind of moisture quick-setting one-component polyurethane sealant, and it prepares by the method identical with embodiment 1.By weight, the raw material of the quick-setting one-component polyurethane sealant of moisture is composed as follows:
10 parts of isophorone diisocyanates (Beyer Co., Ltd), polyether glycol (DL-4000, Shandong Lanxing Dongda Chemical Co.,Ltd) 25 part, 3 parts of polyether glycols (DL-3000), 6 parts of acetylacetic ester blocked prepolymers, 13 parts of propylene carbonates, 40 parts of silane coupler modified talcum powder, 1 part in oxazolidine solidifying agent (FT-103, Zhangjiagang Fitow company), 1 part in the organo-bismuth complex compound (Shanghai grass tree chemical industry company limited) that cyclodextrin coats, 0.5 part of defoamer (BYK-378) and to 0.5 part of Methyl benzenesulfonyl isocyanate (Chemical Reagent Co., Ltd., Sinopharm Group).
Embodiment 6
Present embodiment provides a kind of moisture quick-setting one-component polyurethane sealant, and it prepares by the method identical with embodiment 1.By weight, the raw material of the quick-setting one-component polyurethane sealant of moisture is composed as follows:
Diphenylmethanediisocyanate MI-50(BASF AG) 12 part, polyether glycol (DL-4000, Shandong Lanxing Dongda Chemical Co.,Ltd) 29 part, 10 parts of polyether glycols (EP-330N), 9 parts of acetylacetic ester blocked prepolymers, 8 parts of propylene carbonates, 28 parts of silane coupler modified talcum powder, 2 parts in oxazolidine solidifying agent (FT-103, Zhangjiagang Fitow company), 1 part in the organo-bismuth complex compound (Shanghai grass tree chemical industry company limited) that cyclodextrin coats, 0.5 part of defoamer (BYK-378) and to 0.5 part of Methyl benzenesulfonyl isocyanate (Chemical Reagent Co., Ltd., Sinopharm Group).
Comparative Examples 1
The quick-setting one-component polyurethane sealant of a kind of moisture, it prepares as follows:
The first step: in closed reactor, the calcined kaolin that adds DL-4000,10 parts of propylene carbonates and 35 parts of modifications of 35 parts of Shandong Lanxing Dongda Chemical Co.,Ltd, stir and heat up, temperature control is at 100～120 ℃, open vacuum pump and take out negative pressure, pressure-controlling-below the 0.08MPa, vacuumize 1h;
Second step: cool to below 70 ℃, feed drying nitrogen and remove vacuum, add the liquefaction diphenylmethanediisocyanate MI-50 of 17 parts of basf companies, temperature is controlled at 75～85 ℃, polyreaction 3h;
The 3rd step: cool to below 50 ℃; add the coating organo-bismuth of the oxazolidine solidifying agent FT-103 of 0.3 part of defoamer BYK-378,1 part of Zhangjiagang Fitow company, 1.5 parts of Shanghai grass tree chemical industry company limiteds and 0.2 part of Chemical Reagent Co., Ltd., Sinopharm Group to Methyl benzenesulfonyl isocyanate; mix 30min, pack in the nitrogen protection bottom discharge.
Comparative Examples 2
The quick-setting one-component polyurethane sealant of a kind of moisture, it prepares as follows:
The first step: in closed reactor, DL-4000,10 parts of propylene carbonates and 35 parts of calcined kaolins of adding 35 parts of Shandong Lanxing Dongda Chemical Co.,Ltd, stir and heat up, temperature control is at 100～120 ℃, open vacuum pump and take out negative pressure, pressure-controlling-below the 0.08MPa, vacuumize 1h;
Second step: cool to 60 ℃, feed drying nitrogen and remove vacuum, add the liquefaction diphenylmethanediisocyanate MI-50 of 18 parts of basf companies, temperature is controlled at 75～85 ℃, polyreaction 3h;
The 3rd step: cool to below 50 ℃; add the dibutyl tin laurate of 0.3 part of BYK-378,1.5 parts of Shanghai grass tree chemical industry company limiteds and 0.2 part of Chemical Reagent Co., Ltd., Sinopharm Group to Methyl benzenesulfonyl isocyanate; mix 30min, in nitrogen protection bottom discharge packing, namely.
Every performance index to the quick-setting one-component polyurethane sealant of moisture of above-described embodiment 1 ~ 6 and Comparative Examples 1 ~ 2 are tested, and the result is referring to table 1.
The The performance test results of the quick-setting one-component polyurethane sealant of table 1 moisture
Annotate: test is carried out under standard test condition, once becomes glue thickness 10mm.
Embodiment 1 ~ 6 is seal gum provided by the invention, as can be seen from Table 1, moisture curing one-component polyurethane sealant of the present invention, it is very fast that product is done solid work speed behind the interpolation acetylacetic ester blocked prepolymer, add the system that coats organic bismuth catalyst and store quite stable, surpassing 12 months system viscosities increases not quite, still can be from levelling.Comparative Examples 1 is not used the acetylacetic ester blocked prepolymer, and the system rate of drying of causing is very slow, surpasses 22h.Comparative Examples 2 causes system initial stage viscosity higher owing to use unmodified mineral filler, and precipitation easily, uses conventional organotin catalysts to cause system storage process viscosity to rise obviously, less than just occurring gelling in 6 months.
More than the present invention has been done detailed description; the explanation of embodiment just is used for helping to understand method of the present invention and core concept thereof; its purpose is to allow the personage that is familiar with this art can understand content of the present invention and is implemented; can not limit protection scope of the present invention with this; the equivalence that all spirit according to the present invention are done changes or modifies, and all should be encompassed in protection scope of the present invention.
Claims (10)
1. quick-setting one-component polyurethane sealant of moisture, it is characterized in that: in weight percentage, the raw material of described polyurethane sealant is composed as follows: polyisocynate monomer 10% ~ 20%, polyether glycol 20% ~ 45%, acetylacetic ester end capped polyether prepolymer 1% ~ 10%, softening agent 5% ~ 20%, modification breeze 25% ~ 40%, latent curing agent 1% ~ 5%, the environment-friendly type catalyzer 0.1% ~ 2% of cyclodextrin parcel, defoamer 0.1% ~ 1% and water-removal agent 0.1% ~ 1%, described modification breeze is for handling the mineral powder that the surface is coated with coating through chemical coating method; In the environment-friendly type catalyzer of described cyclodextrin parcel, the environment-friendly type catalyzer is in the lar nanometric cavities of cyclodextrin, and described cyclodextrin is unmodified cyclodextrin or modified cyclodextrin or the combination of the two; Described water-removal agent is to be selected from monoisocyanates compounds or the functionalized silane compounds one or more.
2. the quick-setting one-component polyurethane sealant of moisture according to claim 1, it is characterized in that: described acetylacetic ester end capped polyether prepolymer is reacted under catalyst action by polyether Glycols and/or polyether-tribasic alcohol and/or polyether tetrols and Acetacetic acid alkyl ester and obtains, and described Acetacetic acid alkyl ester is to be selected from the special butyl ester of methyl aceto acetate, etheric acid n-propyl, ISOPROPYL ACETOACETATE, the positive butyl ester of etheric acid and etheric acid one or more.
3. the quick-setting one-component polyurethane sealant of moisture according to claim 2, it is characterized in that: described polyether Glycols is polyoxyethylene dibasic alcohol or polyoxytrimethylene dibasic alcohol; Described polyether-tribasic alcohol is polyoxyethylene trivalent alcohol or polyoxytrimethylene trivalent alcohol.
4. the quick-setting one-component polyurethane sealant of moisture according to claim 1, it is characterized in that: described mineral powder is one or more the mixture that is selected from calcined kaolin, talcum powder, wollastonite powder and the calcium carbonate, and described coating is silane coupling agent.
5. the quick-setting one-component polyurethane sealant of moisture according to claim 1, it is characterized in that: described environment-friendly type catalyzer is organo-bismuth class complex compound.
6. the quick-setting one-component polyurethane sealant of moisture according to claim 1 is characterized in that: described monoisocyanates compound be selected from rubigan isocyanic ester,-sulfinic acid phenyl isocyanate, in Methyl benzenesulfonyl isocyanate, methacrylic acid isocyanate group ethyl ester and the phenyl isocyanate one or more; Described functionalized silane compounds is vinyltrimethoxy silane or vinyltriethoxysilane.
7. the quick-setting one-component polyurethane sealant of moisture according to claim 1 is characterized in that: described polyisocynate monomer is one or more the combination that is selected from tolylene diisocyanate, diphenylmethanediisocyanate, isophorone diisocyanate and the hexamethylene diisocyanate; Described polyether glycol is one or more the combination that is selected from polyglycol ether, polypropylene glycol ether and the polyglycerol ether.
8. the quick-setting one-component polyurethane sealant of moisture according to claim 1, it is characterized in that: described softening agent is propylene carbonate.
9. the quick-setting one-component polyurethane sealant of moisture according to claim 1, it is characterized in that: described latent curing agent is oxazole alkanes solidifying agent.
10. preparation method as the quick-setting one-component polyurethane sealant of the described moisture of each claim in the claim 1 to 9, it is characterized in that: described preparation method comprises the steps:
(1), polyether glycol and the acetylacetic ester that will have 2 ~ 4 hydroxyls carry out prepolymerization reaction under catalyst action, after reaction finishes, except the alkyl alcohol that dereaction generates, obtain described acetylacetic ester end capped polyether prepolymer by underpressure distillation;
(2), in closed reactor, add polyether glycol, softening agent and the modification breeze of formula ratio, stir and heat up, temperature control at 100 ℃ ~ 120 ℃, the unlatching vacuum pump is taken out negative pressure, pressure-controlling-below the 0.08MPa; Cool to then below 70 ℃, feed drying nitrogen and remove vacuum, the polyisocynate monomer that adds formula ratio, temperature control is carried out polyreaction at 75～85 ℃, after polyreaction finishes, be cooled to below 50 ℃, environment-friendly type catalyzer and the water-removal agent of the acetylacetic ester blocked prepolymer of adding formula ratio, defoamer, latent curing agent, cyclodextrin parcel mix, and namely get the quick-setting one-component polyurethane sealant of described moisture.
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| CN 201210170531 CN102690626B (en) | 2012-05-29 | 2012-05-29 | Single-component polyurethane sealant capable of quickly curing moisture and preparation method thereof |
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| CN103554428B (en) * | 2013-11-18 | 2015-05-13 | 中国林业科学研究院林产化学工业研究所 | Core-shell synergistic flame retardant polyurethane microencapsulation expandable graphite and application thereof in rigid polyurethane foaming plastic |
| CN104312523A (en) * | 2014-10-09 | 2015-01-28 | 广东新展化工新材料有限公司 | Room-temperature fast-setting single-component polyurethane sealant and preparation method thereof |
| CN105199657A (en) * | 2015-11-12 | 2015-12-30 | 三友（天津）高分子技术有限公司 | Polyurethane sealant and preparation method thereof |
| CN106634788B (en) * | 2016-12-27 | 2019-07-30 | 苏州中材非金属矿工业设计研究院有限公司 | Assembled architecture polyurethane sealant and preparation method thereof |
| CN107141437B (en) * | 2017-06-20 | 2020-03-03 | 万华化学集团股份有限公司 | Crystallization-controllable thermoplastic polyurethane material and preparation method thereof |
| CN107841274A (en) * | 2017-11-21 | 2018-03-27 | 上海天洋热熔粘接材料股份有限公司 | The preparation technology of moisture-curable polyurethane hot melt adhesive |
| CN107841277B (en) * | 2017-12-11 | 2020-08-28 | 山东北方现代化学工业有限公司 | Preparation method of fast-curing and high-strength single-component silane modified polyurethane sealant |
| CN108276949B (en) * | 2018-01-31 | 2021-03-23 | 广州吉必盛科技实业有限公司 | Two-component polyurethane pouring sealant and preparation method and use method thereof |
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| CN109536117A (en) * | 2018-12-10 | 2019-03-29 | 福建中意铁科新型材料有限公司 | A kind of fast curable type polyurethane sealant and preparation method thereof |
| CN111364892B (en) * | 2020-03-11 | 2022-02-25 | 盐城耀晖人防防护设备科技有限公司 | Civil air defense door processing technology based on right-angle civil air defense profile steel and vulcanized fusion joint rubber strip |
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| CN114196366B (en) * | 2021-12-21 | 2023-04-07 | 日丰企业集团有限公司 | Single-component polyurethane glass cement and preparation method and application thereof |
| CN115124964B (en) * | 2022-07-27 | 2024-03-26 | 北京长润化工有限公司 | Moisture-curing polyurethane hot melt adhesive and preparation method and application thereof |
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| US5714563A (en) * | 1996-01-16 | 1998-02-03 | Depompei; Michael Frederick | One-part, low viscosity, moisture curable composition |
| CN101402845B (en) * | 2008-11-11 | 2011-05-18 | 北京市化学工业研究院 | Process for producing flame-proof fluid sealant for construction |
| CN101987950A (en) * | 2009-08-05 | 2011-03-23 | 任绍志 | Single-component polyurethane termite-resistant building sealant |
| CN101885957A (en) * | 2010-07-09 | 2010-11-17 | 山东北方现代化学工业有限公司 | Room-temperature moisture cured one-component water-expansion polyurethane sealant |
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