CN106634534A - Anti-sagging single-ingredient polyurethane waterproof paint and preparation method thereof - Google Patents
Anti-sagging single-ingredient polyurethane waterproof paint and preparation method thereof Download PDFInfo
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- CN106634534A CN106634534A CN201611225116.0A CN201611225116A CN106634534A CN 106634534 A CN106634534 A CN 106634534A CN 201611225116 A CN201611225116 A CN 201611225116A CN 106634534 A CN106634534 A CN 106634534A
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Classifications
-
- 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
-
- 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
- C08G18/64—Macromolecular compounds not provided for by groups C08G18/42 - C08G18/63
- C08G18/6415—Macromolecular compounds not provided for by groups C08G18/42 - C08G18/63 having nitrogen
- C08G18/6423—Polyalkylene polyamines; polyethylenimines; Derivatives thereof
-
- 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
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/80—Masked polyisocyanates
- C08G18/8061—Masked polyisocyanates masked with compounds having only one group containing active hydrogen
- C08G18/8064—Masked polyisocyanates masked with compounds having only one group containing active hydrogen with monohydroxy compounds
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
Abstract
The invention relates to anti-sagging single-ingredient polyurethane waterproof paint and a preparation method thereof. An anti-sagging agent of the polyurethane waterproof paint is hyperbranched polyurea formed by hyperbranched polyethyleneimine and monoisocyanate terminated prepolymers through reaction, wherein the number of nitrogen atoms contained in the molecular structure of the hyperbranched polyethyleneimine is 10 to 30; the monoisocyanate terminated prepolymers are obtained through reaction of diisocyanate monomers and monohydric alcohol with the carbon atom number being 3 to 12. The anti-sagging single-ingredient polyurethane waterproof paint has the advantages that a production process is simple; the production efficiency is high; the construction is convenient; the sagging problem of single-ingredient polyurethane products is solved.
Description
Technical field
The present invention relates to the domatic water-repellent paint of a kind of mono-component waterproofing paint, particularly building field and its preparation side
Method.Specifically, the present invention relates to a kind of anti-sag single-component polyurethane water-proof paint and preparation method thereof.
Background technology
Monocomponent polyurethane paint is a kind of performed polymer containing isocyanates (- NCO) end group, is suitable in wet environment
Construction, can react with moisture, and further crosslinking curing forms high resiliency, robust seamless waterproof coating.Contain in film
Have substantial amounts of urea bond and amino-formate bond, due to the effect of hydrogen bond etc., film has excellent adhesive force, with it is wear-resisting,
Oil resistant, acid and alkali-resistance, impact resistance, and electrical insulating property is good.The film forming matter of such coating, is mostly by the polynary of macromolecular
Alcohol (such as PEPA, PPG) is prepared with diisocyanate addition reaction.Because the coating is to moisture-sensitive, therefore storage
Deposit requirement higher, in production and packaging process moisture is strictly controlled.Compared with dual-component coating, moisturecuring one-component gathers
Urethane coating eliminates the burden process before construction, and metering mistake will not occur, and is great development prospect using easy to operate
Kind.
However, the anti-sag single-component polyurethane water-proof paint on market comes with some shortcomings.Release on the market at present
The anti-sag single-component polyurethane water-proof paint of suitable elevation construction, typically all using aerosil, organobentonite,
Polyamide wax powder etc. is used as anti-sag agent (thixotropic agent), and these traditional thixotropic agent additions are big, and higher cutting is needed during production
Shear force just can be uniformly dispersed, and to producing, equipment requirement is high, and at present the common apparatus of production anti-sag coating is double-planet Scattered Kettle,
High equipment cost, effectively production volume is little, and existing equipment is less than 1100L on market, and low production efficiency, production operation is bothered, and
And these anti-sag auxiliary agents operate very trouble and cause dust pollution using being front required for individually carrying out dehydrating process
Problem.In recent years, occur some new anti-sag auxiliary agents, such as BYK-410 of Bi Ke companies of Germany on market, but the auxiliary agent is only
The coating of middle polarity and solvent-free system is suitable to, is unsuitable for single-component polyurethane water-proof paint system, if to reach preferably
Anti-sag effect, it is necessary to use with reference to traditional powdery anti-sag agent, and have that thixotroping system is unstable etc. to ask using in
Topic.
The content of the invention
The technical problem to be solved is to overcome the deficiencies in the prior art, there is provided a kind of improved anti-sag single group
Part polyurethane water-proof paint, on the premise of excellent sag resistance is kept, reduces paint production plant and requires, improves and produces effect
Rate.
The present invention also provides a kind of preparation method of single-component polyurethane water-proof paint, the method equipment requirement simultaneously
Low, efficiency high, cost is relatively low, and gained coating has excellent sag resistance, and thixotroping stable system.
To solve above technical problem, a kind of technical scheme that the anti-sag agent of the present invention is taken is：
A kind of anti-sag single-component polyurethane water-proof paint, comprising anti-sag agent, the anti-sag agent is hyperbranched polyethylene
Imines reacts the hyperbranched polyureas to be formed, the wherein molecular structure of hyperbranched polyethyleneimine with monoisocyanates terminated prepolymer
In the nitrogen-atoms numbers that contain be 10～30, the monoisocyanates terminated prepolymer is with carbon number by diisocyanate monomer
3～12 monohydric alcohol reaction is obtained.
Further, above-mentioned diisocyanate monomer can be commercially available conventional diisocyanate monomer, without especially limit
System, wherein it is preferred that toluene di-isocyanate(TDI) (TDI) and/or IPDI (IPDI).
Further, above-mentioned monohydric alcohol is preferably straight chain alcohol, be more preferably selected from carbon number 4～10 straight chain alcohol in
One or more of combination, specific monohydric alcohol such as n-butanol, n-amyl alcohol, n-hexyl alcohol, n-heptanol, n-octyl alcohol, nonyl alcohol, the last of the ten Heavenly stems
Alcohol etc..
Preferably, the diisocyanate monomer and the molar ratio of monohydric alcohol are 2～2.5:1.
Preferably, terminal nitrogen atom number is 5～10 in the molecular structure of the hyperbranched polyethyleneimine.
One of the invention concrete and preferred aspect, the structural formula of hyperbranched polyethyleneimine is as follows：
According to another concrete and preferred aspect of the present invention, the structural formula of hyperbranched polyethyleneimine is as follows：
Preferably, the hyperbranched polyethyleneimine and monoisocyanates terminated prepolymer are according to amino and NCO
The mol ratio of group is 1：1.05～1.2 feed intake.
Usually, mass content of the described anti-sag agent in the coating is more than or equal to 0.5%, preferably greater than or equal to
1%, most preferably 1.0%～1.5%.
A specific aspect of the invention, the preparation method of anti-sag agent is as follows：Make diisocyanate monomer and one
Under nitrogen protection, hybrid reaction 2-5h, reaction temperature 70-80 DEG C is obtained the performed polymer of monoisocyanates end-blocking to first alcohol；Will be super
Branched polyethylene imine (HBPA, Hyperbranched polyethyle imines) is dissolved in dimethylformamide and N- methyl
In the mixed solvent of pyrrolidones, the performed polymer for adding monoisocyanates to block, hybrid reaction 1-2h, reaction temperature 30-40 DEG C,
Obtain final product the anti-sag agent.
One of the invention concrete and preferred aspect, anti-sag single-component polyurethane water-proof paint, with weight percent
Content meter, its raw material composition is as follows：Polyisocynate monomer 10%～20%, PPG 20%～40%, plasticizer 5%
～15%, mineral powder modified 30%～50%, latent curing agent 1%～5%, catalyst 0.1%～2%, defoamer 0.1%～1%
With anti-sag agent 0.5%～1.5%, wherein：Described mineral powder modified is that Surface coating has bag through Chemical coating method process
Cover the mineral powder of agent.
According to the present invention, the degree of functionality of described PPG is 2～3, it is preferable that PPG is selected from poly- second
One or more in glycol ethers, polypropylene glycol ether and polyglycerol ether.Preferably, the hydroxyl value of PPG 20～
Between 200KOHmg/g, it is highly preferred that hydroxyl value is 20～58KOHmg/g.
According to the present invention, plasticizer can be type commonly used in the art.Preferably, plasticizer is propene carbonate.Cause
It is that propene carbonate and polyurethane resin can form chemical bonding, with traditional plasticizer chlorinated paraffin, the fourth of phthalic acid two
The phase specific viscosity such as ester and dioctyl phthalate is lower, and compatibility is good, will not over time migrate out coating, and it is used both may be used
To reduce system viscosity, it is also possible to improve the durability of product.
Described Chemical coating method is known, and it is referred to and led to being wrapped by material by silane coupler, stearic acid etc.
It is often the method for the modifying surface of inorganic particulate.According to the present invention, described covering is preferably silane coupler.It is described
Mineral powder include but is not limited to calcined kaolin, talcum powder, wollastonite powder and calcium carbonate etc..Mineral powder modified is added to polyurethane
It is less likely to occur to reunite after system, precipitates, the compatibility with polyurethane system can not only be improved, also can preferably reduces system and glue
Spend, improve levelling.
According to the present invention, described latent curing agent can adopt type commonly used in the art.Preferably, described latent solidification
Agent is preferably the combination of one or more of ketimide, aldimine and oxazole alkanes curing agent, after latent curing agent runs into water
There is rapid hydrolysis in the presence of catalyst, the NCO crosslinking curing in active amino, with system is discharged, so as to from source
Prevent the generation of carbon dioxide on head, eliminate the chemistry bubble of system.In addition amino generates urea with isocyanates reaction,
Make coating system that there is physically better mechanical property, and higher adhesive strength and more preferable wear-resisting ageing-resistant performance.
According to the present invention, described defoamer is mainly used in the mechanical gas that elimination system is produced in production and application process
Bubble, it can be type of anti-foam agent commonly used in the art, but preferably Siloxane-Oxyalkylene Copolymers class defoamer.
The another technical scheme that the present invention takes is：A kind of anti-sag single-component polyurethane water-proof paint as above
Preparation method, it is comprised the following steps：
(1) anti-sag agent is prepared：Make diisocyanate monomer and monohydric alcohol under nitrogen protection, hybrid reaction 2-5h, instead
Temperature 70-80 DEG C is answered, the performed polymer of monoisocyanates end-blocking is obtained；By hyperbranched polyethyleneimine be dissolved in dimethylformamide and
In the mixed solvent of 1-METHYLPYRROLIDONE, the performed polymer of monoisocyanates end-blocking, hybrid reaction 1-2h, reaction temperature are added
30-40 DEG C, obtain final product the anti-sag agent；
(2) polyurethane water-proof paint is prepared：In possessing the closed reactor of the main stirring of anchor formula and the auxiliary stirring of high speed shear,
PPG, plasticizer and the mineral powder modified of formula ratio, stirring is added to heat up, temperature control is opened at 100 DEG C～120 DEG C
Vacuum pumping negative pressure, Stress control is below -0.08MPa；Then less than 60 DEG C are cooled to, drying nitrogen are passed through and are released vacuum,
The polyisocynate monomer of formula ratio is added, temperature control carries out polymerisation at 75～85 DEG C, after polymerisation terminates, drop
Temperature adds defoamer, latent curing agent, the catalyst of formula ratio to less than 50 DEG C, is well mixed, while open main stirring stirring with auxiliary
In the case of mixing, the anti-sag agent of formula ratio is added, disperse 10-30min, obtained final product the anti-sag monocomponent polyurethane waterproof and apply
Material.
Due to the utilization of above technical scheme, the present invention has compared with prior art following advantage：
The hyperbranched polyureas anti-sag agent that the single-component polyurethane water-proof paint of the present invention is adopted, because of its super branched molecule
Structure and contained group make it have low oneself viscosity, good dispersion and thixotropy it is good the features such as, as anti-sag
Agent is added in single-component polyurethane water-proof paint, only little addition, it is possible to give coating excellent thixotropic effects, institute
The coating of preparation just can greatly facilitate construction without the need for the construction machinery utensil of specialty in oblique broken face protection operation；While by
In the hyperbranched polyureas good dispersion, so when producing coating using it, without the need for the double-planet dispersing apparatus of specialty, allowing production work
Skill becomes simple, can adopt the reactor of big volume, and production efficiency is greatly improved, and hyperbranched polyureas anti-sag agent need not
It is dried, can be directly added into system, further simplify production and avoid dust pollution.
Specific embodiment
The main innovation of the present invention is to design the new anti-sag agent for being suitable to single-component polyurethane water-proof paint application simultaneously
In being applied to single-component polyurethane water-proof paint.The anti-sag agent is that hyperbranched polyethyleneimine is blocked with monoisocyanates
The hyperbranched polyureas that prepolymer reaction is formed, the nitrogen-atoms numbers for wherein containing in the molecular structure of hyperbranched polyethyleneimine are 10
～30, the monoisocyanates terminated prepolymer is reacted by the monohydric alcohol that diisocyanate monomer and carbon number are 3～12
Arrive.Anti-sag agent has the characteristics that：I closely, in spherical, oneself viscosity is low, with good mobility, holds for () molecular structure
Easily dispersion；(ii) close structure, with 3-D solid structure, there is substantial amounts of oleophylic functional group on surface, can form unimolecule glue
Beam, the dispersion to filler is highly efficient, stable；(iii) all there is excellent thixotropy in polarity and non-polar solven system,
It is good with polyurethane resin compatibility.
There are following features using the single-component polyurethane water-proof paint of anti-sag agent of the present invention：I () coating is designed as list
Component is packed, and without the need for live mixed preparing, form of construction work is various, can brush and spray for construction；(ii) anti-sag agent oneself viscosity
Low, good dispersion, without the need for the double-planet dispersing apparatus of specialty, allows production technology to become simple, can adopt the reaction of big volume
Kettle, is greatly improved production efficiency；(iii) when producing, anti-sag agent can be directly added into system, further without the need for being individually dried
Simplify production and avoid dust pollution；(iv) coating has fabulous storage stability：Hyperbranched anti-sag agent system is glued
Spend low, functional group many, improve the dispersion efficiency of filler, system is not allowed to be also easy to produce precipitated and separated phenomenon；V the agent of () anti-sag adds
Dosage is few, and thixotropic effects are good, saved production cost.Easy construction, just can tiltedly break without the need for the construction machinery utensil of specialty
Operation is protected in face.
The present invention is described in further details below in conjunction with specific embodiment.
Raw materials used material is commercially available in following examples, and wherein hyperbranched polyethyleneimine structural formula is as follows：
Not marked condition is conventional laboratory conditions in following examples.When without special instruction, represent " % " of content
For weight/mass percentage composition.
Embodiment 1
This example provides a kind of preparation method of hyperbranched polyureas anti-sag agent, implements as follows：
By diisocyanate monomer IPDI and butanol according to 2.2:1 mol ratio feeds intake, in 75 DEG C of nitrogen protection and temperature
Lower hybrid reaction 3h, is obtained monoisocyanates terminated prepolymer；
Hyperbranched polyethyleneimine is dissolved in into dimethylformamide and 1-METHYLPYRROLIDONE mixed solvent (volume ratio 1:
1) monoisocyanates terminated prepolymer, is added, isocyanate groups are 1.1 with amide proton molar ratio：1, hybrid reaction
1.5h, reaction temperature 30-40 DEG C obtains final product hyperbranched polyureas anti-sag agent.
Embodiment 2
This example provides a kind of preparation method of hyperbranched polyureas anti-sag agent, implements as follows：
By diisocyanate monomer TDI and hexanol according to 2.2:1 mol ratio feeds intake, at 80 DEG C of nitrogen protection and temperature
Hybrid reaction 2.5h, is obtained monoisocyanates terminated prepolymer；
Hyperbranched polyethyleneimine is dissolved in into dimethylformamide and 1-METHYLPYRROLIDONE mixed solvent (volume ratio 1:
1) monoisocyanates terminated prepolymer, is added, isocyanate groups are 1.1 with amide proton molar ratio：1, hybrid reaction
2h, reaction temperature 30-40 DEG C obtains final product hyperbranched polyureas anti-sag agent.
Embodiment 3
The present embodiment provides a kind of anti-sag single-component polyurethane water-proof paint and preparation method thereof.
By weight, the raw material of polyurethane water-proof paint is consisted of：Methyl diphenylene diisocyanate TDI (BASFs
Company's T -80) 18 parts, 35 parts of PPG (DL-2000, Shandong Lanxing Dongda Chemical Co., Ltd), propene carbonate
10 parts, 35 parts of silane coupler modified calcined kaolin, (MS-201, Qingdao perseverance section new material science and technology is limited for oxazolidine curing agent
Company) 1 part, 0.5 part of organic bismuth catalyst (Shanghai grass tree Chemical Co., Ltd.), defoamer (BYK-1790, German Bi Ke) 0.3
0.8 part of part and anti-sag agent (prepared by embodiment 1).
The preparation method of polyurethane water-proof paint is as follows：
The first step：In closed reactor, DL-2000, propene carbonate and silane coupler modified calcining kaolinite are added
Soil, stirring heats up, and temperature control opens vacuum pumping negative pressure at 100～120 DEG C, and Stress control takes out true below -0.08MPa
Empty 1h；
Second step：Less than 60 DEG C are cooled to, drying nitrogen is passed through and is released vacuum, add T-80, temperature control is 75～85
DEG C, polymerisation 3h；
3rd step：Less than 50 DEG C are cooled to, BYK-1790, latent curing agent MS-201, organo-bismuth, stirring mixing is added
30min；
4th step：High speed shear is opened, hyperbranched anti-sag agent, 400rpm dispersion 10min is added；
5th step：Discharging under nitrogen protection is packed.
Embodiment 4
The present embodiment provides a kind of anti-sag single-component polyurethane water-proof paint and preparation method thereof.
By weight, the raw material of anti-sag single-component polyurethane water-proof paint is consisted of：Diphenylmethane diisocyanate
16 parts of ester T-80 (BASF AG), 30 parts of PPG (DL-2000, Shandong Lanxing Dongda Chemical Co., Ltd),
10 parts of PPG (EP-330N), 10 parts of propene carbonate, 30 parts of silane coupler modified talcum powder, oxazolidine curing agent
2 parts of (MS-201, Qingdao Heng Ke new materials Science and Technology Ltd.), 1 part of organo-bismuth (Shanghai grass tree Chemical Co., Ltd.), defoamer
0.3 part of (FT-301, Suzhou Fei Te new materials Science and Technology Ltd.) and 1 part of anti-sag agent (prepared by embodiment 1).
The preparation method of anti-sag single-component polyurethane water-proof paint is as follows：
The first step：In closed reactor, DL-2000, EP-330N, propene carbonate and silane coupler modified are added
Talcum powder, stirring heat up, temperature control at 100～120 DEG C, open vacuum pumping negative pressure, Stress control below -0.08MPa,
Vacuumize 1h；
Second step：Less than 60 DEG C are cooled to, drying nitrogen is passed through and is released vacuum, add T-80, temperature control is 75～85
DEG C, polymerisation 3h；
3rd step：Less than 50 DEG C are cooled to, FT-301, oxazolidine curing agent MS-201, organic bismuth complex, stirring is added
Mixing 30min；
4th step：High speed shear is opened, hyperbranched anti-sag agent, 400rpm dispersion 20min is added；
5th step：Discharging under nitrogen protection is packed.
Embodiment 5
The present embodiment provides a kind of anti-sag single-component polyurethane water-proof paint, and it is by method same as Example 3
Prepare.By weight, the raw material composition of anti-sag single-component polyurethane water-proof paint is as follows：IPDI (Beyer Co., Ltd) 12
Part, 30 parts of PPG (DL-2000, Shandong Lanxing Dongda Chemical Co., Ltd), PPG (DL-3000) 5
Part, 10 parts of propene carbonate, 40 parts of silane coupler modified talcum powder, latent curing agent (MS-201, Qingdao perseverance section new material science and technology
Co., Ltd) 2 parts, 1 part of organotin (T-12, Shanghai grass tree Chemical Co., Ltd.), 0.5 part of defoamer (BYK-1790) and anti-
1.5 parts of sagging agent (prepared by embodiment 2).
Comparative example 1
A kind of single-component polyurethane water-proof paint, it is made by the steps and obtains：
The first step：In closed reactor, the DL-2000 of 35 parts of Shandong Lanxing Dongda Chemical Co., Ltd of addition,
10 parts of propene carbonates and 35 parts of modified calcined kaolins, stirring heats up, and temperature control opens vavuum pump at 100～120 DEG C
Negative pressure is taken out, Stress control vacuumizes 1h below -0.08MPa；
Second step：Less than 60 DEG C are cooled to, drying nitrogen is passed through and is released vacuum, add the T-80 of 18 parts of basf companies, temperature
Degree control at 75～85 DEG C, polymerisation 3h；
3rd step：Cool to less than 50 DEG C, add 0.3 part of BYK-1790,1.5 parts of Shanghai grass tree Chemical Co., Ltd.s to have
Machine bismuth, stirring mixing 30min, under nitrogen protection discharging is packed.
Comparative example 2
A kind of anti-sag single-component polyurethane water-proof paint, it is made by the steps and obtains：
The first step：In closed reactor, the DL-2000 of 35 parts of Shandong Lanxing Dongda Chemical Co., Ltd of addition,
10 parts of propene carbonates and 35 parts of calcined kaolins, stirring heats up, and temperature control is opened vacuum pumping and born at 100～120 DEG C
Pressure, Stress control vacuumizes 1h below -0.08MPa；
Second step：60 DEG C are cooled to, drying nitrogen is passed through and is released vacuum, add the liquefaction diphenylmethyl of 18 parts of basf companies
Alkane diisocyanate MI-50, temperature control at 75～85 DEG C, polymerisation 3h；
3rd step：Cool to less than 50 DEG C, add 0.3 part of BYK-1790, the two of 1.5 parts of Shanghai grass tree Chemical Co., Ltd.s
Dibutyl tin laurate, stirring mixing 30min；
4th step：Under nitrogen protection material is transferred to double-planet Scattered Kettle, adds 5 parts of aerosil (Cabots
580, before adding aerosil, need to carry out dehydrating process in other equipment), take 1500rpm rotating speeds to disperse
Mixing 20min, discharging packaging is obtained final product.
The property indices of above-described embodiment 3～5 and the single-component polyurethane water-proof paint of comparative example 1～2 are carried out
Test, as a result referring to table 1.
The performance test results of the polyurethane water-proof paint of table 1
As it can be seen from table 1 for the aerosil that compares, the anti-sag agent of the present invention is anti-to monocomponent polyurethane
Water paint system viscosity affects not being too big, for the specific anti-sag agent of embodiment addition, when addition reaches 1%
Flowing down problems can be just fully solved, while filler precipitated and separated can be solved the problems, such as.Although also not existed using aerosil
Flowing down problems and sedimentation problem, but its work in-process must adopt double-planet Scattered Kettle, and equipment requirement is high, low production efficiency,
And the aerosil amount to be added is larger, and need individually to be dried aerosil process, troublesome poeration
And have a dust pollution.In addition the dope viscosity using aerosil is big, and blade coating is only suitable for during construction, is unsuitable for mechanical spray
Apply.
The present invention is described in detail above, the explanation of embodiment be only intended to help understand the method for the present invention and
Its core concept, its object is to allow the personage for being familiar with this art will appreciate that present disclosure and be carried out, and
Can not be limited the scope of the invention with this, equivalence changes or modification that all Spirit Essences of the invention are made, all should
Cover within the scope of the present invention.
Claims (10)
1. a kind of anti-sag single-component polyurethane water-proof paint, comprising anti-sag agent, it is characterised in that：Described anti-sag agent is
Hyperbranched polyethyleneimine reacts the hyperbranched polyureas to be formed with monoisocyanates terminated prepolymer, and the hyperbranched polyethylene is sub-
The nitrogen-atoms numbers contained in the molecular structure of amine are 10 ~ 30, and the monoisocyanates terminated prepolymer is by diisocyanate monomer
Obtain for 3 ~ 12 monohydric alcohol reaction with carbon number.
2. anti-sag single-component polyurethane water-proof paint according to claim 1, it is characterised in that：The diisocyanate
Monomer is toluene di-isocyanate(TDI) and/or IPDI.
3. anti-sag single-component polyurethane water-proof paint according to claim 1, it is characterised in that：The monohydric alcohol is choosing
The combination of one or more from the straight chain alcohol that carbon number is 4 ~ 10.
4. anti-sag single-component polyurethane water-proof paint according to claim 1, it is characterised in that：The hyperbranched poly second
Terminal nitrogen atom number is 5 ~ 10 in the molecular structure of alkene imines.
5. anti-sag single-component polyurethane water-proof paint according to claim 1, it is characterised in that：The diisocyanate
Monomer is 2 ~ 2.5 with the molar ratio of monohydric alcohol:1；The hyperbranched polyethyleneimine and monoisocyanates terminated prepolymer
Mol ratio according to amino and isocyanate groups is 1：1.05 ~ 1.2 feed intake.
6. anti-sag single-component polyurethane water-proof paint according to claim 1, it is characterised in that：Described anti-sag agent
Mass content in the coating is 0.5% ~ 1.5%.
7. anti-sag single-component polyurethane water-proof paint according to claim 6, it is characterised in that：Described anti-sag agent
Mass content in the coating is 1.0% ~ 1.5%.
8. the anti-sag single-component polyurethane water-proof paint according to any one of claim 1-6 claim, its feature
It is：With weight, the raw material composition of described polyurethane water-proof paint is as follows：Polyisocynate monomer 10% ~
20%th, PPG 20% ~ 40%, plasticizer 5% ~ 15%, mineral powder modified 30% ~ 50%, latent curing agent 1% ~ 5%, catalyst 0.1% ~
2%th, defoamer 0.1% ~ 1% and anti-sag agent 0.5% ~ 1.5%, wherein：Described mineral powder modified be through Chemical coating method process and
Surface coating has the mineral powder of covering.
9. anti-sag single-component polyurethane water-proof paint according to claim 8, it is characterised in that：Described mineral powder
It is the mixture of one or more in calcined kaolin, talcum powder, wollastonite powder and calcium carbonate, described covering is silicon
Alkane coupling agent, described catalyst is organotin or organo-bismuth or both mixture, and described latent curing agent is solid for oxazole alkanes
Agent.
10. a kind of preparation method of anti-sag single-component polyurethane water-proof paint as claimed in claim 8 or 9, its feature exists
In comprising the following steps：
（1）Prepare anti-sag agent：Make diisocyanate monomer and monohydric alcohol under nitrogen protection, hybrid reaction 2-5h, reaction temperature
70-80 DEG C of degree, is obtained the performed polymer of monoisocyanates end-blocking；Hyperbranched polyethyleneimine is dissolved in into dimethylformamide and N- first
In the mixed solvent of base pyrrolidones, the performed polymer of monoisocyanates end-blocking, hybrid reaction 1-2h, reaction temperature 30-40 are added
DEG C, obtain final product the anti-sag agent；
（2）Prepare polyurethane water-proof paint：In possessing the closed reactor of the main stirring of anchor formula and the auxiliary stirring of high speed shear, add
The PPG of formula ratio, plasticizer and mineral powder modified, stirring heats up, and temperature control opens vavuum pump at 100 DEG C ~ 120 DEG C
Negative pressure is taken out, Stress control is below -0.08MPa；Then less than 60 DEG C are cooled to, drying nitrogen is passed through and is released vacuum, addition is matched somebody with somebody
The polyisocynate monomer of side's amount, temperature control carries out polymerisation, after polymerisation terminates, is cooled to 50 at 75～85 DEG C
Below DEG C, defoamer, latent curing agent, the catalyst of formula ratio is added, be well mixed, while opening main stirring and auxiliary stirring state
Under, the anti-sag agent of formula ratio is added, disperse 10-30min, obtain final product the anti-sag single-component polyurethane water-proof paint.
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| CN107987713A (en) * | 2017-12-22 | 2018-05-04 | 杭州之江有机硅化工有限公司 | A kind of lacquer painting silane coupling agent and its application |
| CN108300253A (en) * | 2017-07-31 | 2018-07-20 | 王敏 | A kind of modified mono-composition poyurethane water-proof paint |
| CN108440739A (en) * | 2018-03-19 | 2018-08-24 | 济南大学 | A kind of hyperbranched anti-sag agent and the application in mono-composition poyurethane water-proof paint |
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| CN112341925A (en) * | 2020-12-01 | 2021-02-09 | 远大洪雨（唐山）防水材料有限公司 | Anti-sagging solvent-free single-component polyurethane waterproof coating and preparation method thereof |
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| CN111087914A (en) * | 2019-12-21 | 2020-05-01 | 雨中情防水技术集团有限责任公司 | Single-component polyurethane waterproof coating for pasting waterproof coiled material for high-speed railway concrete bridge deck waterproofing and preparation method thereof |
| CN111662630A (en) * | 2020-06-22 | 2020-09-15 | 安徽三棵树涂料有限公司 | Low-VOC polyurethane waterproof coating and preparation method thereof |
| CN112341925A (en) * | 2020-12-01 | 2021-02-09 | 远大洪雨（唐山）防水材料有限公司 | Anti-sagging solvent-free single-component polyurethane waterproof coating and preparation method thereof |
| CN112341925B (en) * | 2020-12-01 | 2022-05-20 | 远大洪雨（唐山）防水材料有限公司 | Anti-sagging solvent-free type single-component polyurethane waterproof paint and preparation method thereof |
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Effective date of registration: 20220718 Address after: Suzhou City, Jiangsu province 215008 Guangji Road No. 284 Patentee after: China building materials Suzhou waterproofing Research Institute Co.,Ltd. Address before: No. 169 Anyang Road, Hushuguan, Suzhou hi tech Zone, Suzhou, Jiangsu 215151 Patentee before: SUZHOU SINOMA DESIGN AND RESEARCH INSTITUTE OF NON-METALLIC MINERALS INDUSTRY CO.,LTD. |