CN106318192B - A kind of aqueous wallpaper waterproof basement membrane and preparation method thereof - Google Patents
A kind of aqueous wallpaper waterproof basement membrane and preparation method thereof Download PDFInfo
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- CN106318192B CN106318192B CN201610818081.5A CN201610818081A CN106318192B CN 106318192 B CN106318192 B CN 106318192B CN 201610818081 A CN201610818081 A CN 201610818081A CN 106318192 B CN106318192 B CN 106318192B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
-
- 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
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4202—Two or more polyesters of different physical or chemical nature
-
- 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
- C08G18/67—Unsaturated compounds having active hydrogen
- C08G18/671—Unsaturated compounds having only one group containing active hydrogen
- C08G18/672—Esters of acrylic or alkyl acrylic acid having only one group containing active hydrogen
-
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
Abstract
The present invention relates to building material technical fields, more particularly to a kind of aqueous wallpaper waterproof basement membrane and preparation method thereof, wallpaper waterproof basement membrane is made by modified polyisocyanate, long chain diol, hydroxy-functional propylene acid esters, reactive diluent, catalyst, silicon powder, silane coupling agent, flocculating agent, levelling agent, curing agent.Wallpaper waterproof basement membrane of the invention is water-based system, avoid pollution of the harmful substances such as VOC to environment, bulk concentration is accumulated close to critical size concentration, the basement membrane waterproof performance formed after drying is good, good permeability, weatherability is strong, puncture is strong, tear resistance is strong, not easy to foaming, cohesive force is strong, acid and alkali-resistance is anticorrosive strong, it is hardly damaged, adhesive force is strong, good permeability, does not blister, cracks and flakes off phenomenon.
Description
Technical field
The present invention relates to building material technical fields, and in particular to a kind of aqueous wallpaper waterproof basement membrane and preparation method thereof.
Background technique
Basement membrane be it is a kind of with alkali resistant, moisture-proof, antimildew function metope processing material, formation level can be effectively prevented
Moisture moisture and alkaline matter extravasation, avoid to wall decorative material: as wallpaper, dope layer, glued board, the getting damp of decorative panel,
The bad damages such as mouldy nigrescence.More and more however as the building problem now, crack, seepage problem are more and more tighter
Weight, common basement membrane product can not cope with wall environment severe so at all, to greatly shorten decorative material for wall surface
Service life.
There are also the materials with water-proof function on the market now, but these materials are one-component basement membrane because of the letter of its structure
Single, the degree of cross linking is not high, and waterproof effect is poor.Meanwhile also having solvent type waterproof material, waterproof effect has very big promotion, but
Again because its volumetric concentration (PVC) is below critical size concentration (CPVC), the basement membrane formed is fine and close, thus by base-material
The waterproofness of resin prevents the intrusion of outside moisture.But such basement membrane makes the moisture generated inside wall that can not penetrate basement membrane
Discharge, these moisture gather under basement membrane, reduce adhesive force between basement membrane and wall, and as the extension of time causes basement membrane
Loose, bubbling, and occur phenomena such as blistering, crack and flake off in turn.Meanwhile containing nuisances such as a large amount of benzene compounds in system
Matter has very big harm to environment and human body.
Summary of the invention
The purpose of the present invention is being directed to above-mentioned deficiency in the prior art, a kind of aqueous wallpaper waterproof basement membrane is provided, is used
Modified polyisocyanate, long chain diol, hydroxy functional acrylate, reactive diluent, catalyst obtain polyurethane propylene
Acid esters performed polymer, polyurethane acrylate prepolymer are easily made, and stable reaction, by-product is few, then by polyurethane acrylate prepolymer
Aggressiveness is added silicon powder, silane coupling agent, flocculating agent, levelling agent and is stablized, and by-product is few, and with certain waterproofness
Polyurethane acrylic resin, polyurethane acrylic resin is further reacted with curing agent is made wallpaper waterproof basement membrane, and basement membrane is fine and close
Property it is good, waterproof performance is superior, and adhesive force is strong, good permeability, do not blister, crack and flake off phenomenon, the waterproof basement membrane be aqueous body
System, avoids pollution of the harmful substances such as VOC to environment.
It is another object of the present invention to be directed to above-mentioned deficiency in the prior art, a kind of aqueous wallpaper waterproof basement membrane is provided
Preparation method, preparation process is simple, it is easy to operate, can be mass.
The purpose of the present invention is achieved through the following technical solutions:
A kind of aqueous wallpaper waterproof basement membrane, the raw material including following parts by weight:
30-40 parts of modified polyisocyanate,
15-35 parts of long chain diol,
30-40 parts of hydroxy functional acrylate,
25-40 parts of reactive diluent,
0.2-2 parts of catalyst,
10-30 parts of silicon powder,
4-8 parts of silane coupling agent,
0.5-4 parts of flocculating agent,
0.1-1 parts of levelling agent,
0.1-5 parts of curing agent
Wherein, the curing agent is made of dibenzoyl peroxide and curing accelerator with weight ratio for 3:4-1:1.
Wherein, the modified polyisocyanate is by polyester polyol, diisocyanate, stannous octoate and organic solvent, with
1-1.5:2.5-3: 0.1-0.5:0.1-0.3 mass fraction carries out reaction 2-10h than mixing at 60-90 DEG C under nitrogen protection,
It depressurizes again and steams solvent, be cooled to room temperature obtained.Wherein, the viscosity (23 DEG C) of the modified polyisocyanate: 3200-
3500mPas, NCO content: 11.5-14.5%, solid content 95-99%.The applicant's invention is constantly tested, modification is more
The viscosity (23 DEG C) of isocyanates: 3200-3500mPas, NCO content: made when 11.5-14.5%, solid content 95-99%
The volumetric concentration of the wallpaper waterproof basement membrane obtained is close to critical size concentration, and compactness when applied to basement membrane is good, and waterproof performance is good,
Gas permeability is good.Modified polyisocyanate of the invention has many advantages, such as that low volatility, small toxicity, degree of functionality are high, modified polyisocyanate cyanogen
Urea acid esters heterocycle structure assigns the excellent waterproof performance of made polyurethane acrylate resin, chemical corrosion resistance, Yi Jiliang again
The high feature of good hardness and flexibility.
Wherein, diisocyanate 4, one in 4- dicyclohexyl methyl hydride diisocyanate, meta-xylene diisocyanate
Kind is two or more.
Wherein, polyester polyol be by ethylene glycol, 1, any one of 2 one propylene glycol, 1,4-butanediol, neopentyl glycol or
The mixture and polyalcohol of the two carry out dealcoholysis by vacuum fusion method according to the molar ratio of 1.03~1.47:1 and dehydration is contracted
It is poly- to form, in vacuum fusion method, first the raw material of the above ratio is connect in 120~160 DEG C of progress initial stage 1~2h of esterification
Be warming up to 180~250 DEG C, until the hydroxyl value of polyester polyol is 18~360mgKOH/g in a manner of decompression dehydration, acid value is
0.1~2mgKOH/g.The polyester polyol and di-isocyanate reaction produced can control its viscosity, solid content and HCO well
Value makes the modified polyisocyanate produced have good stability, and volatility is low, and degree of functionality is high.NCO refers in chemical material
Isocyanate group, value refer to the quality of isocyanates (- NCO) group contained by 100g sample.NCO content uses the positive fourth of 1- bis-
Amine-n-butyl acetate method measures.Viscosity overuse capillary tube viscosity apparatus measurement.The measuring method of solid content are as follows: weigh about
0.8g sample, is accurate to 0.0002g, is placed in the weighing bottle of constant weight, careful to shake, and flows test solution naturally, in bottom of bottle shape
At one layer of uniform film.It places in drying box, is gradually heated to 120 DEG C, 20 minutes dry under (120 ± 2 DEG C), taking-up is put
Enter in drier, be cooled to room temperature, weighs.The solid content X6 indicated with mass percent is calculated as follows: X6=100* (m2-
M1)/m, wherein m1 is the quality of weighing bottle, the quality of sample and weighing bottle, the quality of m sample after m2 is dry.
Wherein, the curing agent is made of dibenzoyl peroxide and curing accelerator with weight ratio for 3:4-1:1, poly- ammonia
After ester acrylate is excited by curing agent, the free radical of generation quickly causes the polyurethane in polyurethane acrylate resin
The Raolical polymerizable of acrylate prepolymer body and reactive diluent, further crosslinking curing, it is netted to ultimately generate solid type
Dibenzoyl peroxide and curing accelerator are used in compounding by the cross linking membrane of structure, the present invention, crosslink performed polymer rapidly,
Reaction speed is fast, and the wallpaper waterproof basement membrane of formation has good puncture and tear resistance.Wherein, curing accelerator is uncle
One of butylperoxide or organosilicone compounds or two kinds of mixtures.Tert-butyl peroxide is mainly and acrylic acid
The double bond of ester resin occurs key point reaction and forms three-dimensional crosslinking structure, and cross-linking efficiency is high, and basement membrane has because amount of by-products is few
There is excellent water resistance, and there is higher glossiness, hardness and impact resistance, it is stronger to bond substrates power.Organosilicon oxygen
Hydride compounds are not spontaneously wet out by water thermally and chemically stable reagent, ageing-resistant performance outstanding, excellent hydrophobicity and are electrically insulated
Property, the solidification of acrylate can be promoted well.
Wherein, the long chain diol is polyethylene glycol adipate dihydric alcohol, poly- six subunits carbon esterdiol, poly- adjacent benzene two
Formic acid diglycol esterdiol, poly- phthalic acid neopentyl glycol polyester-diol, polyadipate ethylene glycol butanediol ester two
The mixture of one or more of alcohol, poly (propylene carbonate) glycol, polyethylencarbonate glycol.Long chain diol is to changing
Property polyisocyanates there is dispersibility well, it is good to be formed by polyurethane acrylate resin filming performance, and suppleness is high, resistance to
Alkalinity, hydrolysis are strong, after cooperating curing agent use, have stronger flexibility with basal plane bonding, not easy to foaming, cohesive force is strong.
Wherein, the hydroxy functional acrylate is 2-hydroxyethyl methacry-late, acrylic acid -2- hydroxyl ethyl ester, methyl
2-hydroxypropyl acrylate, 2-hydroxypropyl acrylate, trimethylolpropane diacrylate, in pentaerythritol triacrylate
One or more kinds of mixtures.
Wherein, the reactive diluent is that vinyl pyrrolidone, vinylacetate, butyl acrylate, acrylic acid are different pungent
Ester, methacrylic acid hydroxy ester, 1,6- hexanediyl ester, tripropylene glycol diacrylate, neopentyl glycol diacrylate
The mixture of one or more of ester, trimethylolpropane trimethacrylate.
Reactive diluent of the invention is free radical type reactive diluent, common with reactive diluent after curing agent is added
Effect issues raw radical photopolymerization and carries out, and free radical initiation can obtain the cross-linked network of polymer after solidifying, degree of functionality is higher,
The obtained cross-linked network degree of cross linking is higher, and the hardness for obtaining cured film is higher, and the wallpaper waterproof basement membrane of formation has very strong anti-
Stampability and tear resistance.
Wherein, the reactive diluent is pressed by butyl acrylate, methacrylic acid hydroxy ester, tripropylene glycol diacrylate
Weight fraction ratio is 10:2:1~5:3:1 composition.
Wherein, the catalyst be one or both of tertiary amine, basic carboxylate salt, tin octoate, metal naphthenate with
On mixture.Preferably, catalyst is answered by tin dilaurate tin dibutyl tin and tin octoate by mass fraction ratio for 1-2:1-1.5
With forming.The catalytic rate of catalyst after compounding is fast, high-efficient, side reaction is few, is conducive to modified polyisocyanate and long-chain
The progress of diol reaction.
Wherein, the flocculating agent is ethylene glycol, propylene glycol, hexylene glycol, propandiol butyl ether, butyl glycol ether, propylene glycol second
Ether, xylyl alcohol, diethylene glycol, 2-Butoxyethyl acetate, 2, in 2,4- trimethyl -1,3- pentanediol mono isobutyrates
It is any.Flocculating agent can make polyurethane acrylate prepolymer lotion comparatively fast flocculate molding, be conducive to the formation of basement membrane and
The activity of flocculating agent is good, under conditions of soda acid also very efficiently.
Wherein, the levelling agent is any one of acrylic copolymer, organosilicon and fluorocarbon surfactant.The present invention
Levelling agent can improve flow leveling and equalization energy, eliminate shrinkage cavity and flake phenomenon, reduce tangerine peel and pin-hole phenomena, improve bottom
Material wetting is conducive to air and solvent release, keeps or increase ground recoatability and adhesive force, and levelling agent is added into performed polymer
The surface tension that performed polymer can be reduced makes wallpaper waterproof basement membrane have good wetability to ground；(2) adjustment solvent volatilization speed
Degree reduces ripe degree, improves mobility, extends flow time；(3) very thin monolayer is formed on surface, it is uniform to provide
The basement membrane of surface tension, formation is not easy to foaming, strong with the cohesive force of basal plane.Silicone levelling agent preferably, can be changed using rubbing
The serial levelling agent in 1070, the 1071 of work.
Wherein, the present invention uses silicon powder, and average grain diameter is at 0.1~0.3 micron, specific surface area are as follows: 20~28m2/ g, in
There is good wellability in pre-polymerization precursor emulsion, easily mix, no clustering phenomena, it is poly- to can be good at control polyurethane acrylate prepolymer
The volumetric concentration of body is allowed to close to critical size concentration, and making to gather has good waterproof performance by ester acrylate.Energy when use
Precipitating, lamination are reduced and eliminated, is used cooperatively with flocculating agent, flocculating result more preferably, keeps performed polymer more stable, is conducive to next
Walk hybrid reaction.
A kind of preparation method of aqueous wallpaper waterproof basement membrane: include the following steps:
Step A: by long chain diol warming while stirring, making 80~120 DEG C of temperature, 90~120min of reduced pressure treatment,
40~50 DEG C are then cooled to, modified polyisocyanate is added and is warming up to 50~60 DEG C, reacts 20~30min, sequentially adds hydroxyl
Base functionalized propylene acid esters, reactive diluent, catalyst, then 65~80 DEG C, under temperature constant state are warming up to, react 3~4h, cooling
To 30 DEG C hereinafter, obtaining polyurethane acrylate prepolymer；
Step B: silicon powder, silane coupling agent, flocculating agent, levelling are sequentially added into polyurethane acrylate prepolymer
Agent is ground to fineness≤40 μm after mixing evenly, then disperses 20~35min under the revolving speed of 1500~2000r/min, obtains A
Component；
Step C: dibenzoyl peroxide is mixed with curing accelerator, is stirred 10~15min, is obtained B component；
Step D: B component is added in component A and stirs 10~15min, wallpaper waterproof basement membrane can be obtained.
Beneficial effects of the present invention:
1, the viscosity (23 DEG C) of modified polyisocyanate prepared by the present invention: 3200-3500mPas, NCO content:
11.5-14.5%, solid content 95-99%, volatility is good, degree of functionality is high, high with the cross-linking reaction degree of long chain diol, formation
Waterproof basement membrane good waterproof performance, corrosion-resistant, hardness is strong, flexibility is good.
2, a kind of aqueous wallpaper waterproof basement membrane prepared by the present invention, uses modified polyisocyanate, long chain diol, hydroxyl
Functionalized propylene acid esters, reactive diluent, catalyst obtain polyurethane acrylate prepolymer, polyurethane acrylate prepolymer
It is easily made, stable reaction, by-product is few, then silicon powder, silane coupling agent, cohesion is added in polyurethane acrylate prepolymer
Agent, levelling agent are stablized, by-product is few and the polyurethane acrylic resin with superior waterproofness, then by polyurethane third
Diluted acid resin and curing agent reaction are made, and wallpaper waterproof basement membrane product bulk concentration obtained is close to critical size concentration, shape after drying
At basement membrane waterproof performance it is good, good permeability, weatherability is strong, puncture is strong, tear resistance is strong, not easy to foaming, cohesive force is strong,
Acid and alkali-resistance is anticorrosive strong, is hardly damaged, adhesive force is strong, good permeability, does not blister, cracks and flakes off phenomenon, which is
Water-based system avoids pollution of the harmful substances such as VOC to environment.
3, preparation method step of the invention it is simple, it is easy to operate, can be mass.
Specific embodiment
The invention will be further described with the following Examples.
Embodiment 1
A kind of aqueous wallpaper waterproof basement membrane, the raw material including following parts by weight:
30 parts of modified polyisocyanate,
20 parts of long chain diol,
35 parts of hydroxy functional acrylate,
25 parts of reactive diluent,
0.5 part of catalyst,
20 parts of silicon powder,
4.5 parts of silane coupling agent,
1.5 parts of flocculating agent,
0.5 part of levelling agent,
0.1 part of curing agent,
Wherein, the curing agent is made of dibenzoyl peroxide and curing accelerator with weight ratio for 3:4, and solidification promotes
Agent is tert-butyl peroxide.
Wherein, the modified polyisocyanate is by polyester polyol, diisocyanate, stannous octoate and organic solvent, with
1:2.5: 0.2:0.1 mass fraction carries out reaction 4h, then depressurize and steam solvent than mixing at 60-90 DEG C under nitrogen protection, cold
But it is made to room temperature.
Wherein, the long chain diol is poly- six subunits carbon esterdiol.
Wherein, the hydroxy functional acrylate is 2-hydroxyethyl methacry-late, acrylic acid -2- hydroxyl ethyl ester, methyl
2-hydroxypropyl acrylate, 2-hydroxypropyl acrylate are 1:1.2:2.5:0.4 composition by mass fraction ratio.
Wherein, the reactive diluent is pressed by butyl acrylate, methacrylic acid hydroxy ester, tripropylene glycol diacrylate
Weight fraction ratio is 10:2:1 composition.
Wherein, the catalyst is made of tertiary amine, basic carboxylate salt, tin octoate by mass fraction ratio for 0.5:2.5:1.5.
Wherein, the flocculating agent propandiol butyl ether, butyl glycol ether are 1:1 composition by mass fraction ratio.
Wherein, the levelling agent is organosilicon.
Embodiment 2
A kind of aqueous wallpaper waterproof basement membrane, the raw material including following parts by weight:
35 parts of modified polyisocyanate,
30 parts of long chain diol,
40 parts of hydroxy functional acrylate,
40 parts of reactive diluent,
1.8 parts of catalyst,
30 parts of silicon powder,
8 parts of silane coupling agent,
0.5 part of flocculating agent,
1 part of levelling agent,
1 part of curing agent,
Wherein, the curing agent is made of dibenzoyl peroxide and curing accelerator with weight ratio for 1:1, and solidification promotes
Agent is organosilicone compounds.
Wherein, the modified polyisocyanate is by polyester polyol, diisocyanate, stannous octoate and organic solvent, with
1.5:2.5: 0.2:0.1 mass fraction carries out reaction 8h, then depressurize and steam solvent than mixing at 90 DEG C under nitrogen protection, cold
But it is made to room temperature.
Wherein, the long chain diol by poly- six subunits carbon esterdiol, poly- phthalic acid diglycol esterdiol,
Poly- phthalic acid neopentyl glycol polyester-diol, polyadipate ethylene glycol butyl glycol ester diol, poly (propylene carbonate) glycol, poly- carbon
Sour ethyl glycol is 1:1.5:0.2:2.5:0.1:2.5 composition by mass fraction.
Wherein, the hydroxy functional acrylate is by 2-hydroxyethyl methacry-late, acrylic acid -2- hydroxyl ethyl ester, methyl
2-hydroxypropyl acrylate, 2-hydroxypropyl acrylate, trimethylolpropane diacrylate, pentaerythritol triacrylate press matter
Score ratio is measured as 2:3:0.2:5:0.1:2.5 composition.
Wherein, the reactive diluent 1,6- hexanediyl ester, tripropylene glycol diacrylate, neopentyl glycol two
Acrylate, trimethylolpropane trimethacrylate are 4:7:1.5:3.5 composition by mass fraction ratio.
Wherein, the catalyst is made of tertiary amine, tin octoate, metal naphthenate by mass fraction ratio for 2:0.1:7.
Wherein, the flocculating agent is pressed by 2-Butoxyethyl acetate, 2,2,4- trimethyl -1,3- pentanediol mono isobutyrates
Mass fraction ratio is 1:1.5:0.4 composition.
Wherein, the levelling agent is acrylic copolymer.
Embodiment 3
A kind of aqueous wallpaper waterproof basement membrane, the raw material including following parts by weight:
30 parts of modified polyisocyanate,
15 parts of long chain diol,
30 parts of hydroxy functional acrylate,
25 parts of reactive diluent,
0.2 part of catalyst,
10 parts of silicon powder,
4 parts of silane coupling agent,
3.5 parts of flocculating agent,
0.8 part of levelling agent,
2 parts of curing agent,
Wherein, the curing agent is made of dibenzoyl peroxide and curing accelerator with weight ratio for 3:4, and solidification promotes
Agent is organosilicone compounds.
Wherein, the modified polyisocyanate is by polyester polyol, diisocyanate, stannous octoate and organic solvent, with
1.5:3: 0.5:0.3 mass fraction carries out reaction 8h, then depressurize and steam solvent than mixing at 90 DEG C under nitrogen protection, cooling
It is made to room temperature.
Wherein, the long chain diol is by polyadipate ethylene glycol butyl glycol ester diol, poly (propylene carbonate) glycol, poly- carbon
Sour ethyl glycol is 1:1.5:4.5 composition by mass fraction ratio.
Wherein, the hydroxy functional acrylate is by trimethylolpropane diacrylate, three acrylic acid of pentaerythrite
Ester is 2.5:7 composition by mass fraction ratio.
Wherein, the reactive diluent by butyl acrylate, Isooctyl acrylate monomer, methacrylic acid hydroxy ester, 1,6- oneself
Omega-diol diacrylate, neopentylglycol diacrylate, trimethylolpropane trimethacrylate press 2:3.5:4:6:1.5:0.1 group
At.
Wherein, it by mass fraction ratio is 2 that the catalyst, which is tertiary amine, basic carboxylate salt, tin octoate, metal naphthenate:
3:0.5:6 composition.
Wherein, the flocculating agent is 2:1 by mass fraction ratio by ethylene glycol, propylene glycol, hexylene glycol, propandiol butyl ether:
2.5:4 composition.
Wherein, the levelling agent is fluorocarbon surfactant.
Embodiment 4
A kind of aqueous wallpaper waterproof basement membrane, the raw material including following parts by weight:
35 parts of modified polyisocyanate,
30 parts of long chain diol,
35 parts of hydroxy functional acrylate,
30 parts of reactive diluent,
1.8 parts of catalyst,
15 parts of silicon powder,
6 parts of silane coupling agent,
3.5 parts of flocculating agent,
0.5 part of levelling agent,
5 parts of curing agent,
Wherein, the curing agent is made of dibenzoyl peroxide and curing accelerator with weight ratio for 3:4, and solidification promotes
Agent is the mixture that tert-butyl peroxide and organosilicone compounds are 1:1.5 in mass ratio.
Wherein, the modified polyisocyanate is by polyester polyol, diisocyanate, stannous octoate and organic solvent, with
1.5:2.5: 0.4:0.1 mass fraction carries out reaction 5h, then depressurize and steam solvent than mixing at 80 DEG C under nitrogen protection, cold
But it is made to room temperature.
Wherein, the long chain diol is polyethylene glycol adipate glycol, poly- six subunits carbon esterdiol, poly- O-phthalic
Sour diglycol esterdiol is 0.1:2.5:6 composition by mass fraction ratio.
Wherein, the hydroxy functional acrylate is by acrylic acid -2- hydroxyl ethyl ester, Hydroxypropyl methacrylate, three hydroxyls
Diacrylate, pentaerythritol triacrylate are 7:4:3:1 composition by mass fraction ratio.
Wherein, the reactive diluent is pressed by butyl acrylate, methacrylic acid hydroxy ester, tripropylene glycol diacrylate
Weight fraction ratio is 5:3:1 composition.
Wherein, the catalyst is made of tertiary amine, tin octoate, metal naphthenate by mass fraction ratio for 1:1.5:2.5.
Wherein, the flocculating agent is by propandiol butyl ether, butyl glycol ether, propylene-glycol ethyl ether, xylyl alcohol, a contracting second two
Alcohol, 2-Butoxyethyl acetate are 5:2.5:1:2.1:3:1 composition by mass fraction ratio.
Wherein, the levelling agent is acrylic copolymer.
Embodiment 5
A kind of preparation method of aqueous wallpaper waterproof basement membrane, comprising the following steps:
Step A: by long chain diol warming while stirring, making temperature to 100 DEG C, reduced pressure treatment 100min, then cools down
To 40 DEG C, polyisocyanates is added and is warming up to 55 DEG C, reacts 25min, sequentially adds hydroxy functional acrylate, activity dilution
Agent, catalyst, then 70 DEG C, under temperature constant state are warming up to, 3.5h is reacted, is cooled to 30 DEG C hereinafter, obtaining urethane acrylate
Performed polymer；
Step B: silicon powder, silane coupling agent, flocculating agent, levelling are sequentially added into polyurethane acrylate prepolymer again
Agent is ground to fineness≤40 μm after mixing evenly, then disperses 25min under the revolving speed of 2000r/min, obtains component A；
Step C: dibenzoyl peroxide is mixed with curing accelerator, is stirred 10min, is obtained B component；
Step D: B component is added in component A and stirs 15min, wallpaper waterproof basement membrane can be obtained.
Embodiment 6
A kind of preparation method of aqueous wallpaper waterproof basement membrane, comprising the following steps:
Step A: by long chain diol warming while stirring, making 120 DEG C of temperature, reduced pressure treatment 120min, then cools down
To 50 DEG C, polyisocyanates is added and is warming up to 55 DEG C, reacts 25min, sequentially adds hydroxy functional acrylate, activity dilution
Agent, catalyst, then 80 DEG C, under temperature constant state are warming up to, 3h is reacted, is cooled to 30 DEG C hereinafter, obtaining polyurethane acrylate prepolymer
Aggressiveness；
Step B: silicon powder, silane coupling agent, flocculating agent, levelling are sequentially added into polyurethane acrylate prepolymer again
Agent, it is ground to fineness≤40 μm after mixing evenly, then disperse 35min under the revolving speed of 2000r/min, obtains component A；
Step C: dibenzoyl peroxide is mixed with curing accelerator, is stirred 15min, is obtained B component；
Step D: B component is added in component A and stirs 10min, wallpaper waterproof basement membrane can be obtained.
Embodiment 7
A kind of preparation method of aqueous wallpaper waterproof basement membrane, comprising the following steps:
Step A: by long chain diol warming while stirring, make 80 DEG C of temperature, reduced pressure treatment 90min is then cooled to
45 DEG C, polyisocyanates is added and is warming up to 50 DEG C, reacts 25min, sequentially adds hydroxy functional acrylate, activity dilution
Agent, catalyst, then 65 DEG C, under temperature constant state are warming up to, 3h is reacted, is cooled to 30 DEG C hereinafter, obtaining polyurethane acrylate prepolymer
Aggressiveness；
Step B: silicon powder, silane coupling agent, flocculating agent, levelling are sequentially added into polyurethane acrylate prepolymer again
Agent is ground to fineness≤40 μm after mixing evenly, then disperses 25min under the revolving speed of 1500r/min, obtains component A；
Step C: dibenzoyl peroxide is mixed with curing accelerator, is stirred 12min, is obtained B component；
Step D: B component is added in component A and stirs 15min, wallpaper waterproof basement membrane can be obtained.
Embodiment 8
A kind of preparation method of aqueous wallpaper waterproof basement membrane, comprising the following steps:
Step A: by long-chain binary warming while stirring, make 80 DEG C of temperature, reduced pressure treatment 90min is then cooled to 50
DEG C, polyisocyanates is added and is warming up to 50 DEG C, reacts 20min, sequentially add hydroxy functional acrylate, reactive diluent,
Catalyst, then 80 DEG C, under temperature constant state are warming up to, 3h is reacted, 30 DEG C is cooled to and gathers hereinafter, obtaining polyurethane acrylate prepolymer
Body；
Step B: silicon powder, silane coupling agent, flocculating agent, levelling are sequentially added into polyurethane acrylate prepolymer again
Agent is ground to fineness≤40 μm after mixing evenly, then disperses 20min under the revolving speed of 2000r/min, obtains component A；
Step C: dibenzoyl peroxide is mixed with curing accelerator, is stirred 10min, is obtained B component；
Step D: B component is added in component A and stirs 10min, wallpaper waterproof basement membrane can be obtained.
Test experiment
Wallpaper is made using the preparation method of the wallpaper waterproof basement membrane of embodiment 5 in the wallpaper waterproof basement membrane of embodiment 1 to prevent
Water base film is as experimental group 1；The wallpaper waterproof basement membrane of embodiment 2 is used into the preparation method of the wallpaper waterproof basement membrane of embodiment 6
Wallpaper waterproof basement membrane is made as experimental group 2；The wallpaper waterproof basement membrane of embodiment 3 is used to the wallpaper waterproof basement membrane of embodiment 7
Preparation method be made wallpaper waterproof basement membrane as experimental group 3；The wallpaper waterproof basement membrane of embodiment 4 is used to the wall of embodiment 8
Wallpaper waterproof basement membrane is made as experimental group 4 in the preparation method of paper waterproof basement membrane；Using commercially available wallpaper waterproof basement membrane as control
Group performs the following performance tests, and the results are shown in Table 1.
1, adhesive force is tested
Draw 100 1 millimeter × 1 millimeter of square lattice on the coating surface with cross hatch device.It is produced with Minnesota Mining and Manufacturing Company
The adhesive tape of model 600 is smooth to be bonded on grid, is not stayed a gap, is then uncovered adhesive tape rapidly with 60 ° of angle,
Whether have at observation coating scratching edge and falls off.
It such as falls off without any for 5B, falling off area between 0-5% is 4B, and the area that falls off is between 5%-15%
3B, falling off area between 15%-35% is 2B, and falling off area between 35%-65% is 1B, and the area that falls off is 65% or more
For 0B.
2, hardness test
Hardness test is carried out according to method specified in chapter 4 in GB/6739T.
It is successively the pencil of 2H, 3H, 4H, 5H and 6H with Mitsubishi's (UNI) hardness, on sample, with 90 ° of angle application
The pencil of 1000 gram forces, 10 millimeters of strokes, each hardness draws 3 in different location, and whether observation appearance of coat has obvious scratch,
There is the minimum pencil hardness of scratch in record.
3, adhesion strength is tested
PH-5813 gauge head is matched using BYKPH-5811/PH-5811,0.75 millimeter of measuring head diameter, test angle is 90 °, is applied
Certain load (N) is added to streak with the speed of 1 cm/s in coating surface, whether observation coating surface has scratch, and record is drawn
The minimum load power (N) of trace.
4, water absorption rate test
The basement membrane of experimental group 1-4 is separately immersed in the sodium hydroxide that mass concentration is 10%, is impregnated 24 hours, detection
Its waterproofness.
1 performance test of table
| Project | Experimental group 1 | Experimental group 2 | Experimental group 3 | Experimental group 4 | Control group |
| Adhesive force | 5B | 5B | 5B | 5B | 4B |
| Hardness | 6H | 6H | 6H | 6H | 5H |
| Resistance to marring | 9N | 9N | 9N | 9N | 8N |
| Water absorption rate | 2.18% | 2.34% | 2.64% | 2.64% | 5.34% |
Find out from above-mentioned test data result, wallpaper waterproof basement membrane adhesive force prepared by the present invention is strong, hardness is high, scratch resistance
Property is good, water absorption rate is few, good water-proof effect.
Adhesion results determine: it is required that being qualification when adhesive force >=4B.
5B- scribing edge is smooth, at the edge and intersection of scribing line without peeling paint；
4B- has the peeling paint of small pieces in the intersection of scribing line, and the gross area that falls off is less than 5%；
3B- has the basement membrane of small pieces to fall off at the edge and intersection of scribing line, and fall off the gross area 5%~15% it
Between；
2B- has sheet of basement membrane to fall off at the edge and intersection of scribing line, and fall off the gross area 15%~35% it
Between；
1B- has sheet of basement membrane to fall off at the edge and intersection of scribing line, and fall off the gross area 35%~65% it
Between；
0B- has sheet of basement membrane to fall off at the edge and intersection of scribing line, and the gross area that falls off is greater than 65%
Finally it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than the present invention is protected
The limitation of range is protected, although explaining in detail referring to preferred embodiment to the present invention, those skilled in the art are answered
Work as understanding, it can be with modification or equivalent replacement of the technical solution of the present invention are made, without departing from the reality of technical solution of the present invention
Matter and range.
Claims (9)
1. a kind of aqueous wallpaper waterproof basement membrane, it is characterised in that: the raw material including following parts by weight:
30-40 parts of modified polyisocyanate,
15-35 parts of long chain diol,
30-40 parts of hydroxy functional acrylate,
25-40 parts of reactive diluent,
0.2-2 parts of catalyst,
10-30 parts of silicon powder,
4-8 parts of silane coupling agent,
0.5-4 parts of flocculating agent,
0.1-1 parts of levelling agent,
0.1-5 parts of curing agent,
Wherein, the curing agent is made of dibenzoyl peroxide and curing accelerator with weight ratio for 3:4-1:1；
The modified polyisocyanate is by polyester polyol, diisocyanate, stannous octoate and organic solvent, with 1-1.5:2.5-
3: 0.1-0.5:0.1-0.3 mass fraction carries out reaction 2-10h, then depressurize and steam than mixing at 60-90 DEG C under nitrogen protection
Solvent is cooled to room temperature obtained.
2. a kind of aqueous wallpaper waterproof basement membrane according to claim 1, it is characterised in that: the diisocyanate is 4,4-
One or more kinds of mixtures of dicyclohexyl methyl hydride diisocyanate, meta-xylene diisocyanate.
3. a kind of aqueous wallpaper waterproof basement membrane according to claim 1, it is characterised in that: the polyester polyol is by second
Glycol, 1, the mixture and polyalcohol of any one of 2 one propylene glycol, 1,4-butanediol, neopentyl glycol or both are according to 1.03
The molar ratio of~1.47:1 carries out dealcoholysis by vacuum fusion method and dehydrating polycondensation forms.
4. a kind of aqueous wallpaper waterproof basement membrane according to claim 1, it is characterised in that: the hydroxyl functional acrylic
Ester be 2-hydroxyethyl methacry-late, acrylic acid -2- hydroxyl ethyl ester, Hydroxypropyl methacrylate, 2-hydroxypropyl acrylate,
The mixture of one or more of trimethylolpropane diacrylate, pentaerythritol triacrylate.
5. a kind of aqueous wallpaper waterproof basement membrane according to claim 1, it is characterised in that: the reactive diluent is ethylene
Base pyrrolidones, vinylacetate, butyl acrylate, Isooctyl acrylate monomer, methacrylic acid hydroxy ester, 1,6- hexylene glycol dipropyl
One of olefin(e) acid ester, tripropylene glycol diacrylate, neopentylglycol diacrylate, trimethylolpropane trimethacrylate or
Two or more mixtures.
6. a kind of aqueous wallpaper waterproof basement membrane according to claim 1, it is characterised in that: the catalyst is tertiary amine, alkali
The mixture of one or more of property carboxylate, tin octoate, metal naphthenate.
7. a kind of aqueous wallpaper waterproof basement membrane according to claim 1, it is characterised in that: the flocculating agent be ethylene glycol,
Propylene glycol, hexylene glycol, propandiol butyl ether, butyl glycol ether, propylene-glycol ethyl ether, xylyl alcohol, diethylene glycol, butyl glycol ether
Acetate, 2, any one of 2,4- trimethyl -1,3- pentanediol mono isobutyrates.
8. a kind of aqueous wallpaper waterproof basement membrane according to claim 1, it is characterised in that: the levelling agent is total for acrylic acid
Any one of polymers, organosilicon and fluorocarbon surfactant.
9. a kind of preparation method of aqueous wallpaper waterproof basement membrane according to claim 1: it is characterized by:
Step A: by long chain diol warming while stirring, make 80~120 DEG C of temperature, 90~120min of reduced pressure treatment, then
40~50 DEG C are cooled to, modified polyisocyanate is added and is warming up to 50~60 DEG C, reacts 20~30min, sequentially adds hydroxyl official
Acrylate, reactive diluent, catalyst can be changed, then be warming up to 65~80 DEG C, under temperature constant state, 3~4h is reacted, be cooled to 30
DEG C hereinafter, obtaining polyurethane acrylate prepolymer；
Step B: silicon powder, silane coupling agent, flocculating agent, levelling agent are sequentially added into polyurethane acrylate prepolymer, is stirred
Fineness≤40 μm are ground to after mixing uniformly, then disperse 20~35min under the revolving speed of 1500~2000r/min, obtain component A；
Step C: dibenzoyl peroxide is mixed with curing accelerator, is stirred 10~15min, is obtained B component；
Step D: B component is added in component A and stirs 10~15min, wallpaper waterproof basement membrane can be obtained.
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| CN109505389B (en) * | 2018-11-21 | 2021-02-02 | 深圳市全艺建筑工程有限公司 | Waterproof environment-friendly wallpaper and preparation method thereof |
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