CN104263289B - Automotive upholstery use adhesive and preparation method - Google Patents
Automotive upholstery use adhesive and preparation method Download PDFInfo
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- CN104263289B CN104263289B CN201410456481.7A CN201410456481A CN104263289B CN 104263289 B CN104263289 B CN 104263289B CN 201410456481 A CN201410456481 A CN 201410456481A CN 104263289 B CN104263289 B CN 104263289B
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Abstract
The present invention relates to a kind of automotive upholstery use adhesive and preparation method, is to be polymerized at a certain temperature by a certain percentage by soft monomer, hard monomer, function monomer, emulsifying agent, buffer, initator, PH conditioning agent, distilled water. Do be this product taking water as medium, safety and environmental protection, the TVOC < 50ug of product? C/g, Formaldehyde emission < 1mg/kg, far below national standard; Cohesive force to all kinds of interior trim raw materials such as nonwoven is good, and peel strength is high; Product is single-component adhesive, without adding curing agent, easy to use; Can directly use, also can use step by step, to initial bake out temperature and secondary activating temperature without harsh requirement; Product nontoxicity, use procedure safety and sanitation, to human body skin non-corrosiveness. Preparation technology is simple, a polymerization, and preparation cost is cheap. Decorative fabric and substrate bonding intensity are 299N/5cm in the time of supply of material state; After heat-resisting, be 174N/5cm; After moisture resistance, be 98N/5cm; After cold-resistant, be 82N/5cm; Total haze value 1.7mg of bonding glued membrane; 2 points of the smells of bonding glued membrane.
Description
Technical field:
The present invention relates to a kind of bonding agent, the adhesive especially using in automotive trim bonding process, relates to especiallyAnd automotive trim use acrylate adhesive, also relate to automotive trim use acrylate adhesive and systemPreparation Method.
Background technology:
At present, the automotive trim that bonds at home still uses solvent-borne type glue inflammable, poisonous, contaminated environment mostlyStick, as neoprene. Solvent-based adhesive not only causes resource serious waste, serious environment pollution, and also rightWorkmen's health causes very large threat. Along with the enhancing of sound and people's environmental consciousness of environmental regulation,Solvent-based adhesive will be replaced by environment-friendly type aqueous adhesive gradually, especially pushing away of aqueous automobile interior trim glueWide application is imperative.
Aqueous adhesive by raw material sources be mainly divided into water-based polyurethane adhesive, water polyacrylic acid is gluingAgent, polyvinyl acetate class emulsion glue, neoprene latex, aqueous epoxy resins glue etc. Water polyacrylic acid is gluingA kind of aqueous polymer adhesive with fastest developing speed since Ji Shi China eighties, it is taking water as decentralized medium,Acrylate is the adhesive that monomer forms through polymerization. Such adhesive have good ageing-resistant, weatherability,The pollution-free premium properties that waits is widely used as automotive interior trim glue. But existing esters of acrylic acid adhesive usesToxic raw materials, bring severe contamination to environment as toxic solvent, curing agent and other auxiliary agents, and existThe deficiency such as poor, the irritant smell of temperature tolerance, adhesion strength are inadequate.
CN101289529 discloses one and " can be used as the aqueous polyurethane emulsion of adhesive for automobile internal decorationPreparation method " (1) by vegetable oil polyol and isocyanates under catalyst exists, 50～80 DEG C of reactionsWithin 2～4 hours, obtain performed polymer; (2) in the performed polymer obtaining, add the compound containing hydrophilic radical, add simultaneouslyAccount for the cosolvent of emulsion cumulative volume 1～4%, at 50～60 DEG C, react 2.5～3 hours; (3) obtainingProduct in add triethylamine to carry out neutralization reaction, and this neutralization reaction product was added to water in 1～5 minuteIn after, emulsification 10 minutes; (4) in the product obtaining, add amine chainextender to make a kind of aqueous polyurethaneEmulsion.
CN102061140A discloses a kind of " a kind of hot-melt pressure sensitive adhesive for automobile interior part " for AutomobileBody metal and plastics, rubber inside gadget adhering and sealing, comprise following component: styrene-isoamyl two in massAlkene-styrene block copolymer 25%～35%, styrene-ethylene-propylene-styrene block copolymer 10%～25%, tackifying resin 30%～45%, nanometer CaCO3 or Al2O3,3%～8%, titanium whitePowder 3%～8%, process auxiliaries is microwax, 3%～8%, plasticizer be trioctyl trimellitate (TOTM) 2%～5%, antioxidant 0.5%～1%; Manufacturing process: above-mentioned material is added to horizontal kneading machine in proportion successivelyIn heat kneading, after completing, the moulding of injection square dies, encapsulates with separate paper after cooling and demolding.
That CN101143999 discloses is a kind of " environment-friendly type automobile inner decoration textile materials electrostatic flocking binding agent andIts preparation " this flocking adhesive is the aqueous liquid dispersion forming after lower routine raw emulsion combined polymerization, it is formerThe parts by weight of material consist of poly-(750) the glycol methyl ether ester 2.5-4 of methacrylic acid, methyl chloride acrylic acidTrimethyl ammonia ethyl ester 2-3, DAAM 4-6, adipic dihydrazide 2-4, acrylic acid 2-8; ThirdOlefin(e) acid ester 25-35.5, S-400 emulsifying agent 2-4, potassium peroxydisulfate 0.2-0.8; Add deionized water to admittedly containingAmount is 44-46%.
CN102533185A disclose " a kind of Waterborne acrylate adhesive " with monomer, emulsifying agent, drawSending out agent, hydroxyl-terminated injecting two methyl siloxane organosilicon modifier and distilled water is that raw material is by emulsion polymerisation legal systemBecome.
CN101423734 discloses " a kind of preparation method of organosilicon modified acrylic ester binding agent " stepSuddenly be: the step of (1) modified monomer pre-polymerization, this step is by modified monomer, modified monomer catalyst, emulsifying agentCarry out pre-polymerization with deionized water, make organosilicon pre-polymerization emulsion; (2) step of emulsification, this step is by organosiliconPre-polymerization emulsion and basic monomer emulsification, make intermediate pre-emulsion; (3) acrylic ester polymerization step, by centreBody pre-emulsion and basic monomer catalyst, deionized water polymerization finished product.
CN101003715 discloses " a kind of preparation method of modified aqueous adhesion agent of polyurethane ". The methodThe epoxy resin that modifier modification epoxy resin is obtained to modification; By polynary to polyisocyanates and polyester or polyethersAlcohol reaction, then adds chain extender, obtains base polyurethane prepolymer for use as; Pre-with modified epoxy modified polyurethaneAggressiveness, obtains the base polyurethane prepolymer for use as of modification; Finally the base polyurethane prepolymer for use as of modification is added water and uses high speed dispersorDisperse, add nertralizer and crosslinking agent, obtain modified aqueous adhesion agent of polyurethane.
CN102533185A discloses " a kind of Waterborne acrylate adhesive ", described acrylic acid ester emulsionAdhesive is with monomer, emulsifying agent, initator, hydroxyl-terminated injecting two methyl siloxane organosilicon modifier and distillationWater is that raw material is made by emulsion polymerization; The consumption of described each raw material is expressed as with mass percent: monomer50～80%, emulsifying agent 1～10%, initator 0.01～0.5%, hydroxyl-terminated injecting two methyl siloxane hasMachine silica modifier 1～10%, distilled water 1～30%;
Huang Hong etc. " Packaging Engineering " 2006No5 discloses a kind of " acrylate modified aqueous polyurethane glueStick synthetic ", using trimethylolpropane etc. as crosslinking agent, adopt acrylate as modifier, syntheticModified aqueous polyurethane emulsion. The adhesive that this dairy industry Pei Jiao is made is to PVC composite package film adhesive propertyGood.
Summary of the invention:
Object of the present invention is just for above-mentioned the deficiencies in the prior art, and a kind of automotive upholstery use is providedAdhesive;
Another object of the present invention is to provide a kind of preparation method of automotive upholstery use adhesive.
The object of the invention is to be achieved through the following technical solutions:
Automotive upholstery use adhesive, its components in mass portion number is made up of following raw materials according:
Described soft monomer is ethyl acrylate, butyl acrylate, 2-ethyl hexyl acrylate, acrylic acid-2-ethyl secondAt least one in ester.
Described hard monomer is methyl methacrylate, methyl acrylate, vinylacetate, styrene, propyleneAt least one in nitrile.
Described function monomer is hydroxy-ethyl acrylate, methacrylic acid, acrylic acid, acrylamide, N-hydroxylAt least one in Methacrylamide, dibutyl phthalate.
Described emulsifying agent is nonionic emulsifier: anion emulsifier: cation emulsified=(2-0.01): (1-0.01): mixed emulsifier (1-0.01);
Described nonionic emulsifier is NPE;
Described anionic emulsifier be lauryl sodium sulfate, neopelex, amber sulfonate,One or more in enuatrol, carboxymethyl cellulose, polyvinyl alcohol, allyl ether series sulfonate;
Described cationic emulsifier is N-domiphen.
Described initator is potassium peroxydisulfate or ammonium persulfate;
Described buffer is dibastic sodium phosphate salt or sodium bicarbonate salt;
Described pH adjusting agent is ammoniacal liquor, sodium acid carbonate or potassium hydroxide.
The preparation method of automotive upholstery use adhesive, comprises the following steps:
A, by mass fraction get distillation 36-72 part, 4.6-32 parts of soft monomers, hard monomer 6.5-35 part,Function monomer 0.5-5 part and emulsifying agent 0.9-5 part, pack into successively with carrying out pre-breast in the flask of agitatorChange, make compound for subsequent use;
B, in the four-hole boiling flask that agitator, thermometer, reflux condenser and feeding device are housed, add distillationWater 4-8 part, soft monomer 0.4-3 part, hard monomer 0.5-3 part, function monomer 0.5-5 part, emulsifying agent 0.1-3Part and buffer 0.1-0.5 part, use heating water bath, when temperature rises to 70 while spending, adds 0.01-0.4 partInitator initiation reaction, obtains the emulsion particle seed that reacts required;
C, then slowly drips compound and the residue 0.8-1.8 part initator prepared through pre-emulsification simultaneously,Reaction temperature is controlled at 75 DEG C-85 DEG C, after pre-emulsification material dropwises, is incubated 2 hours;
D, add PH conditioning agent 0.3-1.5 part, adjust PH=6～7, filter discharging, obtain milky thicknessShape product emulsion, is automotive upholstery use adhesive.
Beneficial effect: adhesive of the present invention is mainly used in the bonding of automotive upholstery, also can be used for nonwoven carpet,Manual blanket by lining bonding, product is taking water as medium, safety and environmental protection, the TVOC < 50ugC/g of product,Formaldehyde emission < 1mg/kg, far below national standard; Cohesive force to all kinds of interior trim raw materials such as nonwoven is good,Peel strength is high; Product is single-component adhesive, without adding curing agent, easy to use; It is applied widely,Can directly use, also can use step by step, to initial bake out temperature and secondary activating temperature without harsh requirement; ProductNontoxicity, use procedure safety and sanitation, to human body skin non-corrosiveness. Preparation technology is simple, and a polymerizationCan, preparation cost is cheap. Be used for the bonding of black non-woven mat and wood flour board, decorative fabric and substrate bonding intensityIn the time of supply of material state, be 299N/5cm; After heat-resisting, be 174N/5cm; After moisture resistance, be 98N/5cm;After cold-resistant, be 82N/5cm; Total haze value 1.7mg of bonding glued membrane; 2 points of the smells of bonding glued membrane.
Detailed description of the invention:
Below in conjunction with embodiment, the present invention is described in further detail:
A kind of automotive upholstery use adhesive, is characterized in that, its components in mass portion number is by following formerMaterial is made:
Described soft monomer is ethyl acrylate, butyl acrylate, 2-ethyl hexyl acrylate, acrylic acid-2-ethyl secondAt least one in ester.
Described hard monomer is methyl methacrylate, methyl acrylate, vinylacetate, styrene, propyleneAt least one in nitrile.
Described function monomer is hydroxy-ethyl acrylate, methacrylic acid, acrylic acid, acrylamide, N-hydroxylAt least one in Methacrylamide, dibutyl phthalate.
Described emulsifying agent is nonionic emulsifier: anion emulsifier: cation emulsified=(2-0.01): (1-0.01): mixed emulsifier (1-0.01).
Described nonionic emulsifier is NPE;
Described anionic emulsifier be lauryl sodium sulfate, neopelex, amber sulfonate,One or more in enuatrol, carboxymethyl cellulose, polyvinyl alcohol, allyl ether series sulfonate;
Described cationic emulsifier is N-domiphen.
Described initator is potassium peroxydisulfate or ammonium persulfate;
Described buffer is dibastic sodium phosphate salt or sodium bicarbonate salt;
Described pH adjusting agent is ammoniacal liquor, sodium acid carbonate or potassium hydroxide.
A preparation method for automotive upholstery use adhesive, is characterized in that, comprises the following steps:
A, by mass fraction get distillation 36-72 part, 4.6-32 parts of soft monomers, hard monomer 6.5-35 part,Function monomer 0.5-5 part and emulsifying agent 0.9-5 part, pack into successively with carrying out pre-breast in the flask of agitatorChange, make compound for subsequent use;
B, in the four-hole boiling flask that agitator, thermometer, reflux condenser and feeding device are housed, add distillationWater 4-8 part, soft monomer 0.4-3 part, hard monomer 0.5-3 part, function monomer 0.5-5 part, emulsifying agent 0.1-3Part and buffer 0.1-0.5 part, use heating water bath, when temperature rises to 70 while spending, adds 0.01-0.4 partInitator initiation reaction, obtains the emulsion particle seed that reacts required;
C, then slowly drips compound and the residue 0.8-1.8 part initator prepared through pre-emulsification simultaneously,Reaction temperature is controlled at 75 DEG C-85 DEG C, after pre-emulsification material dropwises, is incubated 2 hours;
D, add PH conditioning agent 0.3-1.5 part, adjust PH=6～7, filter discharging, obtain milky thicknessShape product emulsion, is automotive upholstery use adhesive.
Embodiment 1
A, get 72ml distilled water, 4.6g ethyl acrylate, 6.5g methyl methacrylate, 3.8g propyleneAcid hydroxyl ethyl ester, emulsifying agent are pressed NPE: lauryl sodium sulfate: N-domiphen=1:0.5:0.5 is made into compound emulsifying agent 2.6g, adds successively dress with carrying out pre-emulsification in the flask of agitator,Make compound for subsequent use;
B, in the four-hole boiling flask that agitator, thermometer, reflux condenser and feeding device are housed, add 8mlDistilled water, 0.5g ethyl acrylate, 0.7g methyl methacrylate, 0.5g hydroxy-ethyl acrylate, 0.3gCompound emulsifying agent and 0.1g dibastic sodium phosphate salt, with heating water bath, when temperature rises to 70 while spending, add 0.01gPotassium peroxydisulfate initiation reaction, obtains the emulsion particle seed that reacts required;
C, compound and residue 0.09g potassium peroxydisulfate that then slowly dropping is prepared through pre-emulsification, reaction temperatureBe controlled at 75 DEG C, after pre-emulsification material dropwises, be incubated 2 hours;
D, add 0.3g ammoniacal liquor, adjust pH=6, filter discharging, obtain the thick product emulsion of milky,For automotive upholstery use adhesive.
Embodiment 2
A gets 59ml distilled water, 5g ethyl acrylate, 5g butyl acrylate, 7.5g methyl acrylate, 7.5gStyrene, 2.35g acrylic acid, emulsifying agent are pressed NPE: neopelex: N-Domiphen=1.6:0.8:0.8 is made into compound emulsifying agent 2g, adds successively the burning of dress with agitatorIn bottle, carry out pre-emulsification, make compound for subsequent use;
B, in the four-hole boiling flask that agitator, thermometer, reflux condenser and feeding device are housed, add 6.7mlDistilled water, 0.55g ethyl acrylate, 0.55g butyl acrylate, 0.85g methyl acrylate, 0.85gStyrene, 0.5g acrylic acid, 0.15g compound emulsifying agent and 0.2g sodium bicarbonate salt, with heating water bath, whenTemperature rises to 70 while spending, adds the initiation reaction of 0.05g ammonium persulfate, obtains the emulsion particle seed that reacts required;
C, then slowly drips compound and the residue 0.45g ammonium persulfate prepared through pre-emulsification simultaneously, anti-Answer temperature to be controlled at 80 DEG C, after pre-emulsification material dropwises, be incubated 2 hours;
D, add 0.8g sodium acid carbonate, adjust pH=7, filter discharging, obtain the thick product emulsion of milky,Be automotive upholstery use adhesive.
Embodiment 3
A, get 45ml distilled water, 15g 2-ethyl hexyl acrylate, 15g vinylacetate, 5g by mass percentMethyl methacrylate, 4g methacrylic acid, emulsifying agent are pressed NPE: amber sulfonate:N-domiphen=0.8:0.4:0.4 is made into compound emulsifying agent 5g, adds successively dress with agitatorIn flask, carry out pre-emulsification, make compound for subsequent use;
B, in the four-hole boiling flask that agitator, thermometer, reflux condenser and feeding device are housed, add 4mlDistilled water, 1.7g 2-ethyl hexyl acrylate, 1.65g vinylacetate, 1.65 methyl methacrylates, 0.5gMethacrylic acid, 0.6g compound emulsifying agent and 0.3g dibastic sodium phosphate salt, with heating water bath, when temperature rises to70 when spend, adds the initiation reaction of 0.13g ammonium persulfate, obtains the emulsion particle seed that reacts required;
C, then slowly drips compound and the residue 1.17g ammonium persulfate prepared through pre-emulsification simultaneously, anti-Answer temperature to be controlled at 85 DEG C, after pre-emulsification material dropwises, be incubated 2 hours;
D, add 0.3g potassium hydroxide, adjust pH=6.5, filter discharging, obtain the thick emulsion of milky and produceProduct, are automotive upholstery use adhesive.
Embodiment 4
A, by mass percent get 40ml distilled water, 32g acrylic acid-2-ethyl ethyl ester, 5g acrylonitrile,3.9g styrene, 1g dibutyl phthalate, 2g acrylic acid, emulsifying agent are pressed NPE:Carboxymethyl cellulose: N-domiphen=0.5:0.25:0.25 is made into compound emulsifying agent 5g, adds successivelyEnter dress with carrying out pre-emulsification in the flask of agitator, make compound for subsequent use;
B, in the four-hole boiling flask that agitator, thermometer, reflux condenser and feeding device are housed, add 4mlDistilled water, 3.6g acrylic acid-2-ethyl ethyl ester, 0.56g acrylonitrile, 0.44g styrene, the adjacent benzene of 0.15gDibutyl carboxylic acid, 0.35g acrylic acid, 0.6g compound emulsifying agent and 0.4g sodium bicarbonate salt, add with water-bathHeat, when temperature rises to 70 while spending, adds the initiation reaction of 0.07g ammonium sulfate, obtains the emulsion particle that reacts requiredSeed;
C, then slowly drips compound and the residue 0.63g ammonium sulfate prepared through pre-emulsification, reaction temperature simultaneouslyBe controlled at 80 DEG C, after pre-emulsification material dropwises, be incubated 2 hours;
D, add 0.3g ammoniacal liquor, adjust pH=6.3, filter discharging, obtain the thick product emulsion of milky,Be automotive upholstery use adhesive.
Embodiment 5
A, by mass percent get 36ml distilled water, 1.8g butyl acrylate, 2.8g ethyl acrylate,5g styrene, 20g methyl methacrylate, 10g acrylonitrile, 2.3gN-NMA, 2.7gAcrylamide, emulsifying agent are pressed NPE: allyl ether series sulfonate: N-dodecyl diformazanAmine=0.1:0.05:0.05 is made into compound emulsifying agent 2.25g, adds successively in the flask of dress with agitatorRow pre-emulsification, makes compound for subsequent use;
B, in the four-hole boiling flask that agitator, thermometer, reflux condenser and feeding device are housed, add 4mlDistilled water and 0.2g butyl acrylate, 0.3g ethyl acrylate, 0.6g styrene, 2.2g methacrylic acidMethyl esters, 1.1g acrylonitrile, 2.3gN-NMA, 2.7g acrylamide, 0.25g composite emulsifyingAgent and 0.26g dibastic sodium phosphate salt, with heating water bath, when temperature rises to 70 while spending, add 0.18g over cureThe initiation reaction of acid ammonium, obtains the emulsion particle seed that reacts required;
C, then slowly drips compound and the residue 1.56g ammonium persulfate prepared through pre-emulsification simultaneously, anti-Answer temperature to be controlled at 85 DEG C, after pre-emulsification material dropwises, be incubated 2 hours;
D, add 1.5g sodium acid carbonate, adjust pH=7.1, filter discharging, obtain the thick emulsion of milky and produceProduct, are automotive upholstery use adhesive.
Claims (7)
1. an automotive upholstery use adhesive, is characterized in that, its components in mass portion number is made up of following raw materials according:
Described emulsifying agent is nonionic emulsifier: anion emulsifier: cationic emulsifier=(2-0.01): (1-0.01): mixed emulsifier (1-0.01).
2. according to automotive upholstery use adhesive claimed in claim 1, it is characterized in that, described soft monomer is at least one in ethyl acrylate, butyl acrylate, 2-ethyl hexyl acrylate.
3. according to automotive upholstery use adhesive claimed in claim 1, it is characterized in that, described hard monomer is methyl methacrylate, at least one in methyl acrylate, vinylacetate, styrene, acrylonitrile.
4. according to automotive upholstery use adhesive claimed in claim 1, it is characterized in that, described function monomer is at least one in hydroxy-ethyl acrylate, methacrylic acid, acrylic acid, acrylamide, N hydroxymethyl acrylamide, dibutyl phthalate.
5. according to automotive upholstery use adhesive claimed in claim 1, it is characterized in that, described nonionic emulsifier is NPE;
Described anionic emulsifier is one or more in lauryl sodium sulfate, neopelex, amber sulfonate, enuatrol, carboxymethyl cellulose, polyvinyl alcohol, allyl ether series sulfonate;
Described cationic emulsifier is N-domiphen.
6. according to automotive upholstery use adhesive claimed in claim 1, it is characterized in that, described initator is potassium peroxydisulfate or ammonium persulfate;
Described buffer is dibastic sodium phosphate salt or sodium bicarbonate salt;
Described pH adjusting agent is ammoniacal liquor, sodium acid carbonate or potassium hydroxide.
7. a preparation method for automotive upholstery use adhesive, is characterized in that, comprises the following steps:
A, get distilled water 36-72 part, 4.6-32 parts of soft monomers, hard monomer 6.5-35 part, function monomer 0.5-5 part and emulsifying agent 0.9-5 part by mass fraction, pack into successively with carrying out pre-emulsification in the flask of agitator, make compound for subsequent use;
B, in the four-hole boiling flask that agitator, thermometer, reflux condenser and feeding device are housed, add successively distilled water 4-8 part, soft monomer 0.4-3 part, hard monomer 0.5-3 part, function monomer 0.5-5 part, emulsifying agent 0.1-3 part and buffer 0.1-0.5 part, with heating water bath, when temperature rises to 70 while spending, add the initiation reaction of 0.01-0.4 part initator, obtain emulsion particle seed;
C, then slowly drips compound and the residue 0.8-1.8 part initator prepared through pre-emulsification simultaneously, and reaction temperature is controlled at 75 DEG C-85 DEG C, after pre-emulsification material dropwises, is incubated 2 hours;
D, add pH adjusting agent 0.3-1.5 part, adjust pH=6～7, filter discharging, obtain the thick product emulsion of milky, be automotive upholstery use adhesive.
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| CN101748617B (en) * | 2008-12-05 | 2012-11-07 | 上海洁润丝新材料股份有限公司 | Anti-sticking soft dope printing adhesive and preparation method |
| CN101434819B (en) * | 2008-12-10 | 2010-11-03 | 广东恒大新材料科技有限公司 | Aqueous adhesive for binding rubber and metal and preparation thereof |
| CN102140321B (en) * | 2010-10-26 | 2012-12-12 | 北京高盟新材料股份有限公司 | Water-based aluminized film composite glue and preparation method thereof |
| CN102516470B (en) * | 2011-11-21 | 2013-09-04 | 北京高盟新材料股份有限公司 | Aqueous acrylate electrostatic flocking bonding agent and preparation method thereof |
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