CN109777330A - A kind of microwave oven door label acrylate pressure sensitive adhesive and preparation method thereof - Google Patents
A kind of microwave oven door label acrylate pressure sensitive adhesive and preparation method thereof Download PDFInfo
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- CN109777330A CN109777330A CN201910089428.0A CN201910089428A CN109777330A CN 109777330 A CN109777330 A CN 109777330A CN 201910089428 A CN201910089428 A CN 201910089428A CN 109777330 A CN109777330 A CN 109777330A
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Abstract
The present invention relates to macromolecule adhesive fields, and in particular to arrives a kind of microwave oven door label acrylate pressure sensitive adhesive and preparation method thereof.The microwave oven door label acrylate pressure sensitive adhesive, including following component: sticky monomer, interior polycondensation monomer, modified monomer, initiator, solvent, emulsifier, crosslinking agent, defoaming agent, levelling agent, wetting agent.Microwave oven door label acrylate pressure sensitive adhesive prepared by the present invention can be while keeping basic performance, make product that there is preferable shrinkage, it can satisfy the appearance requirement of all micro-wave oven polyester film door stickers, and it will not warp, obscure through 210 DEG C of baking back doors patch, phenomena such as peel strength reduces, therefore being highly suitable for the high-temperature-resistant microwave ovens such as barbecue type microwave oven.
Description
Technical field
The invention belongs to macromolecule adhesive technical field, more particularly it relates to which a kind of microwave oven door label is with third
Olefin(e) acid pressure sensitive adhesive and preparation method thereof.
Background technique
Plain edition micro-wave oven door patch is to be coated with acrylic acid solvent type pressure using with a thickness of the transparent polyester film surface of 0.1mm
Quick glue is compound with release polyester film after drying, final shape by die-cutting.The appearance requirement of microwave oven door label be it is transparent, clear,
Surface must not have a bad phenomenons such as scratch, scratch, bubble, and physical index is 90 ° of peel strength >=10N/25mm, and 180 DEG C of heatproof
(polyester film of surface coating solvent type pressure-sensitive adhesive is attached on micro-wave oven door-plate in the environment of 180 DEG C after heat baking 30min
Its appearance pasted must not turn yellow, warp, and clarity must not weaken, and can see No. 4 words of the Song typeface at 1 ruler of distance clearly).High temperature resistant microwave
Fire door patch then needs to reach 210 DEG C of heatproof.
If being all not difficult to accomplish from the point of view of whether appearance or physical index are single in the technical requirements that micro-wave oven is pasted with door,
There are many adhesive to be attained by requirement in the market, but all to reach requirement just difficult very big for comprehensive all indexs, has
Clarity, peel strength are not achieved again, and vice versa.Although existing adhesive formulation can satisfy above-mentioned part and want substantially
It asks, but shrinking percentage is larger, and can only be 180 DEG C of heatproof, is only applicable to plain edition micro-wave oven, still can through 210 DEG C of baking back door patches
It warps, obscures, and phenomena such as peel strength reduction.
Summary of the invention
To solve the above-mentioned problems, first aspect of the present invention provides a kind of microwave oven door label acrylate pressure sensitive adhesive,
Including following component: sticky monomer, interior polycondensation monomer, modified monomer, initiator, solvent, emulsifier, crosslinking agent, defoaming agent, levelling
Agent, wetting agent.
As a kind of perferred technical scheme, by weight, microwave oven door label acrylate pressure sensitive adhesive includes such as
Lower component: sticky monomer 60-80 parts, polycondensation monomer 5-8 parts interior, 3-6 parts of modified monomer, 0.05-1 parts of initiator, solvent 50-60
Part, 0.5-1 parts of emulsifier, 2-3.5 parts of crosslinking agent, 0.5-1 parts of defoaming agent, 0.5-1 parts of levelling agent, 0.5-1 parts of wetting agent.
As a kind of perferred technical scheme, by weight, microwave oven door label acrylate pressure sensitive adhesive includes such as
Lower component: sticky monomer 65-75 parts, polycondensation monomer 5-7 parts interior, 4-5 parts of modified monomer, 0.1-0.5 parts of initiator, solvent 53-58
Part, 0.5-0.8 parts of emulsifier, 2.5-3 parts of crosslinking agent, 0.5-0.8 parts of defoaming agent, 0.5-0.8 parts of levelling agent, wetting agent 0.5-
0.8 part.
As a kind of perferred technical scheme, the sticky monomer is selected from butyl methacrylate, isobutyl
One of ester, isobutyl acrylate, n-propyl, Isooctyl acrylate monomer are a variety of.
As a kind of perferred technical scheme, the interior polycondensation monomer is selected from methyl methacrylate, cyclohexyl acrylate, horse
Come one of acid anhydrides, styrene, acrylonitrile, vinylacetate or a variety of.
As a kind of perferred technical scheme, the modified monomer is selected from hydroxyethyl methacrylate, methacrylic acid contracts
One of water glyceride, hydroxy-ethyl acrylate are a variety of.
As a kind of perferred technical scheme, the crosslinking agent is modified melamine-formaldehyde resin.
As a kind of perferred technical scheme, the modified melamine-formaldehyde resin is butanol etherification melamino-formaldehyde
Resin microsphere.
As a kind of perferred technical scheme, the interior polycondensation monomer, the weight ratio of modified monomer are 1:(0.6-0.8).
The second aspect of the present invention provides a kind of preparation method of microwave oven door label acrylate pressure sensitive adhesive, step packet
It includes:
(1) the sticky monomer, interior polycondensation monomer, modified monomer, crosslinking agent, solvent, emulsifier are added in reaction kettle
Stirring is warming up to 85 ± 2 DEG C, keeps the temperature 1.5h；
(2) reaction kettle is cooled to 75 ± 2 DEG C, the initiator of 1/3 parts by weight is then added, after 3-6h is reacted in heating, point
Continue the initiator that remaining 2/3 parts by weight are added dropwise three times, it is 0.5h that interval time is added dropwise every time, 1-2h is reacted after dripping off, then
Cool the temperature to 60 DEG C；
(3) defoaming agent, levelling agent, wetting agent are put into the system of step (2), after stirring 30-60min, are cooled to 40
DEG C filtering obtains the Acrylic Pressure Sensitive Adhesive.
The utility model has the advantages that microwave oven door label acrylate pressure sensitive adhesive prepared by the present invention can keep the same of basic performance
When, make product that there is preferable shrinkage, can satisfy the appearance requirement of all micro-wave oven polyester film door stickers, and through 210 DEG C
Phenomena such as baking back door patch will not warp, obscure, peel strength reduces, therefore it is resistance to be highly suitable for barbecue type microwave oven etc.
High temperature microwave furnace.
Specific embodiment
It is further clear, complete that the technical characteristic work in technical solution is provided to the present invention With reference to embodiment
Description, not to the limitation of its protection scope.
Word " preferred ", " preferred " in the present invention etc. refer to, can provide in some cases certain beneficial to effect
The embodiment of the present invention of fruit.However, other embodiments are also likely to be preferred under identical circumstances or in the case of other
's.In addition, do not imply that other embodiments are unavailable to the statement of one or more preferred embodiments, be also not intended to by
Other embodiments exclude except the scope of the present invention.
When a numberical range disclosed herein, above range is considered as continuously, and the minimum value including the range and most
Big value and each value between this minimum value and maximum value.Further, when range refers to integer, including the model
Each integer between minimum value and maximum value enclosed.In addition, when providing multiple range Expressive Features or characteristic, Ke Yihe
And the range.In other words, unless otherwise specified, otherwise all ranges disclosed herein are understood to include and are wherein included into
Any and all subrange.For example, should be regarded as including between minimum value 1 and maximum value 10 from the specified range of " 1 to 10 "
Any and all subrange.The Exemplary range of range 1 to 10 include but is not limited to 1 to 6.1,3.5 to 7.8,5.5 to
10 etc..
To solve the above-mentioned problems, first aspect of the present invention provides a kind of microwave oven door label acrylate pressure sensitive adhesive,
Including following component: sticky monomer, interior polycondensation monomer, modified monomer, initiator, solvent, emulsifier, crosslinking agent, defoaming agent, levelling
Agent, wetting agent.
In a preferred embodiment, by weight, microwave oven door label acrylate pressure sensitive adhesive includes such as
Lower component: sticky monomer 60-80 parts, polycondensation monomer 5-8 parts interior, 3-6 parts of modified monomer, 0.05-1 parts of initiator, solvent 50-60
Part, 0.5-1 parts of emulsifier, 2-3.5 parts of crosslinking agent, 0.5-1 parts of defoaming agent, 0.5-1 parts of levelling agent, 0.5-1 parts of wetting agent.
In a preferred embodiment, by weight, microwave oven door label acrylate pressure sensitive adhesive includes such as
Lower component: sticky monomer 65-75 parts, polycondensation monomer 5-7 parts interior, 4-5 parts of modified monomer, 0.1-0.5 parts of initiator, solvent 53-58
Part, 0.5-0.8 parts of emulsifier, 2.5-3 parts of crosslinking agent, 0.5-0.8 parts of defoaming agent, 0.5-0.8 parts of levelling agent, wetting agent 0.5-
0.8 part.
Sticky monomer
Viscosity monomer of the present invention refers to simple function (methyl) of the homopolymer glass transition temperature at least below -20 DEG C
Alkyl acrylate.
In a preferred embodiment, above-mentioned example of enumerating includes but is not limited to: ethyl acrylate, acrylic acid positive third
Ester, isopropyl acrylate, n-butyl acrylate, butyl methacrylate, Isobutyl methacrylate, isobutyl acrylate, third
Olefin(e) acid n-pentyl ester, isoamyl acrylate, acrylic acid n-hexyl ester, 4- methyl -2- acrylate, 2- ethylhexyl acrylic acid
The different nonyl ester of ester, 2- methyl hexyl acrylate, n-octyl, Isooctyl acrylate monomer, acrylic acid, isoamyl acrylate, third
The positive last of the ten Heavenly stems ester of olefin(e) acid, isodecyl acrylate, acrylic acid 2- Propylheptyl, dodecyl acrylate, heptadecane acrylate, 18
One of alkyl acrylate, 2- octydecyl acrylate are a variety of.
In a preferred embodiment, the sticky monomer is selected from butyl methacrylate, isobutyl
One of ester, isobutyl acrylate, n-propyl, Isooctyl acrylate monomer are a variety of.
In a preferred embodiment, the sticky monomer is butyl methacrylate.
Interior polycondensation monomer
Interior polycondensation monomer of the present invention refers to that homopolymer glass transition temperature is at least above 50 DEG C of simple function methyl-prop
Olefin(e) acid Arrcostab, acrylate base ester, acrylic acid bicyclic alkyl ester or aryl methacrylate.
In a preferred embodiment, above-mentioned example of enumerating includes but is not limited to: methyl methacrylate, methyl-prop
Olefin(e) acid ethyl ester, n propyl methacrylate, isopropyl methacrylate, cyclohexyl acrylate, (methyl) isobornyl acrylate,
One of 2- phenoxyethyl methacrylate is a variety of.
In a preferred embodiment, the interior polycondensation monomer is selected from methyl methacrylate, cyclohexyl acrylate, horse
Come one of acid anhydrides, styrene, acrylonitrile, vinylacetate or a variety of.
In a preferred embodiment, the interior polycondensation monomer is maleic anhydride.
Modified monomer
Modified monomer of the present invention refers to simple function (methyl) crylic acid hydroxy ester, including but not limited to: acrylic acid hydroxyl
Ethyl ester, hydroxyethyl methacrylate, hydroxypropyl acrylate, hydroxy propyl methacrylate, polyethylene glycol monomethacrylate, 2-
One of hydroxyl -3- phenoxypropylacrylate, glycidyl methacrylate are a variety of.
In a preferred embodiment, the modified monomer is selected from hydroxyethyl methacrylate, methacrylic acid contracts
One of water glyceride, hydroxy-ethyl acrylate are a variety of.
In a preferred embodiment, the modified monomer is glycidyl methacrylate, and generation is faced upward in purchase certainly
Chemistry is subordinate to Shanghai Yang Shi Industrial Co., Ltd..
In a preferred embodiment, the interior polycondensation monomer, the weight ratio of modified monomer are 1:(0.6-0.8).
When present inventor is had found in the course of the study using herein described modified monomer and interior polycondensation monomer, institute
The cohesive strength for the acrylate pressure sensitive adhesive being prepared enhances, and product has excellent peel strength.Inventor speculates that it may
The reason of be modified monomer by the effect of initiator, crosslinking agent, crosslink chemical reaction, formation cross-linked polymer, simultaneously
Due to the steric effect of modified monomer, the effect between main chain can be weakened, so as to improve the cohesive strength of pressure sensitive adhesive.
Initiator
Initiator of the present invention is also known as radical initiator, refer to it is a kind of be easy to be thermally decomposed into free radical (it is i.e. primary from
By base) compound, can be used for causing alkenes, the free radical polymerization of double vinyl monomers and copolymerization, it can also be used to insatiable hunger
It is reacted with the crosslinking curing and high molecular crosslink of polyester.
In a preferred embodiment, the initiator is selected from ammonium persulfate, potassium peroxydisulfate, sodium peroxydisulfate, special fourth
One of base hydrogen peroxide is a variety of.
In a preferred embodiment, the initiator is ammonium persulfate.
Solvent
Solvent of the present invention is selected from one of alcohols, esters, ethers, ketone, benzene class or a variety of.
In a preferred embodiment, the solvent is water.
Emulsifier
Emulsifier of the present invention is can to improve the various surface tension constituted between phase in emulsion, is allowed to be formed
The substance of even stable dispersion or emulsion.
In a preferred embodiment, the emulsifier is selected from allyloxy nonyl phenol propyl alcohol polyoxyethylene ether sulfuric acid
Ammonium, allyloxy Nonylphenoxy propyl alcohol polyoxyethylene ether ammonium sulfate, allyloxy Nonylphenoxy propyl alcohol polyoxyethylene ether, alkene
One of oxyl sulfonate is a variety of.
In a preferred embodiment, the emulsifier is DNS-86, and purchase has from Chinese section, Qingxin County chemical science and technology
Limit company.
Crosslinking agent
Crosslinking agent of the present invention is used primarily in high molecular material (rubber and thermosetting resin).Because of high molecular material
The molecular structure line long just as a rule, intensity is low when not being crosslinked, and easily breaks, and without elasticity, the effect of crosslinking agent is exactly
Chemical bond is generated between the molecule of line style, is connected with each other linear molecule, reticular structure is formed, enhances product performance.
In a preferred embodiment, the crosslinking agent is modified melamine-formaldehyde resin.
In a kind of preferred embodiment, the crosslinking agent is butyl alcohol etherified melamine-formaldehyde resin microballoon；Institute
Butyl alcohol etherified melamine-formaldehyde resin microballoon is stated to be made by the steps to obtain:
(1) formaldehyde is added in four-hole bottle, adjusting pH value with triethylamine is 8.5, melamine is added, aqueous solution slowly rises
Temperature is dissolved to 70 DEG C to melamine, and system becomes clarification, and the reaction was continued 20min is cooled to 50 DEG C, butanol is added, and use hydrochloric acid
It adjusts pH value and carries out etherificate polycondensation for 4.5, react 1-1.5h, obtain butanol etherification melamino-formaldehyde prepolymer；
(2) suitable PVA concentrated solution is taken to be added in above-mentioned prepolymer, until its concentration is 4 × 10-3G/mL uses dilute hydrochloric acid
It adjusts when pH value of solution is stirred to react constant to microspherulite diameter for 4.5,60 DEG C and stops reaction, be washed with deionized after centrifugation 3 times,
60 DEG C of low temperature dryings obtain butyl alcohol etherified melamine-formaldehyde resin microballoon.
Present inventor has found in the course of the study using butyl alcohol etherified melamine-formaldehyde resin microballoon as crosslinking agent,
The acrylic resin that its spherical structure is prepared is more three-dimensional, and butyl alcohol etherified melamine-formaldehyde resin is as in crosslinking
The heart, cohesive force is stronger, and caking property has more bonding points than aspherical butyl alcohol etherified melamine-formaldehyde resin.
In a kind of preferred embodiment, the crosslinking agent is the butanol etherification melamine first containing ferroso-ferric oxide
Urea formaldehyde microballoon；The butyl alcohol etherified melamine-formaldehyde resin microballoon containing ferroso-ferric oxide is made by the steps
It arrives:
(1)Fe2+The absorption of ion: the butyl alcohol etherified melamine-formaldehyde resin microballoon after taking centrifugation to wash is ultrasonic in water
50 DEG C of heating stirrings of continuation are uniform after dispersing 5min；By FeCl2Solution is slowly added thereto, so that Fe in solution2+Ion concentration
Fe is centrifugated to obtain after 60 DEG C of heating stirrings react 1h for 1.2mol/L2+The resin microsphere of ionic adsorption；
(2)Fe2+The conversion of ion: gained resin microsphere is dispersed in water, and pH to 10.0 is adjusted with ammonium hydroxide, by mixed liquor
The static heating 5h at 70 DEG C, washing sample after Magneto separate, must contain the butanol etherification melamine of ferroso-ferric oxide after being repeated 5 times
Formaldehyde resin microballoon；Wherein, the concentration of the butyl alcohol etherified melamine-formaldehyde resin after the centrifugation washing in water is 28g/
L。
In addition, present inventor is found surprisingly that since the application crosslinking agent surface has ferroso-ferric oxide, have certain
Microwave absorption characteristic, after absorbing microwave, polar group generates friction and vibration, forms " hot spot " to stimulating metering system
Acid glycidyl ester and maleic anhydride are had an effect, at the same the complete modified melamine-formaldehyde resin of unreacted can generate it is extra
Free formaldehyde can eliminate part formaldehyde after absorbing microwave, slow down the generation of security risk, to obtain high temperature resistant
Acrylate pressure sensitive adhesive.
Defoaming agent
Defoaming agent of the present invention, also referred to as defomaing agent are to reduce surface tension in process, inhibit foam generate or
Eliminate the additive for having generated foam.
In a preferred embodiment, the defoaming agent is selected from silicone emulsion, the fatty acid ester compounded object of higher alcohols, gathers
Ethylene oxide polyoxypropylene pentaerythrite ether, polyoxyethylene polyoxy propyl alcohol amidogen ether, polypropylene glycerol aether and polyoxypropylene polyoxy second
One of alkene glycerin ether, dimethyl silicone polymer are a variety of.
In a preferred embodiment, the defoaming agent is fatty alcohol and polyethers defoaming agent, is bought from crop field
It learns, model D-90.
Levelling agent
Levelling agent of the present invention is a kind of common commercial auxiliaries, it can promote coating to be formed during the drying and film forming process
One smooth, smooth, uniform film can be effectively reduced and cover with paint, lacquer, colour wash, etc. liquid surface tension, improve one kind of its levelability and uniformity
Substance.A possibility that it can improve the permeability for covering with paint, lacquer, colour wash, etc. liquid, generate spot and spot when can be reduced brushing, increases spreadability, makes
Film forming is uniform, natural.
In a preferred embodiment, the levelling agent is selected from fluorine-containing surfactant polymer B YK340, polyethers
Modified dimethyl siloxane BYK333, acrylic acid modified fluorine-carbon macromolecule compound EFKA3500 and fluorine-carbon modified organosilicon oxygen
One of alkane EFKA3034 or a variety of.
In a preferred embodiment, the levelling agent is BYK333, is bought limited at safe trade from Shenzhen pool
Company.
Wetting agent
Wetting agent of the present invention refers to the substance that solid material can be made to be easier to be soaked in water.By reducing its surface tension
Or interfacial tension, the substance for allowing the water to be deployed on solid material surface, or penetrate its surface, and solid material being soaked.
In a preferred embodiment, the wetting agent is selected from organic silicon polyether copolymer, anionic surface
One of activating agent, nonionic surfactant are a variety of.
In a preferred embodiment, the wetting agent is BYK346, is bought limited at safe trade from Shenzhen pool
Company.
The second aspect of the present invention provides a kind of preparation method of microwave oven door label acrylate pressure sensitive adhesive, step packet
It includes:
(1) the sticky monomer, interior polycondensation monomer, modified monomer, crosslinking agent, solvent, emulsifier are added in reaction kettle
Stirring is warming up to 85 ± 2 DEG C, keeps the temperature 1.5h；
(2) reaction kettle is cooled to 75 ± 2 DEG C, the initiator of 1/3 parts by weight is then added, after 3-6h is reacted in heating, point
Continue the initiator that remaining 2/3 parts by weight are added dropwise three times, it is 0.5h that interval time is added dropwise every time, 1-2h is reacted after dripping off, then
Cool the temperature to 60 DEG C；
(3) defoaming agent, levelling agent, wetting agent are put into the system of step (2), after stirring 30-60min, are cooled to 40
DEG C filtering obtains the Acrylic Pressure Sensitive Adhesive.
The present invention is specifically described below by embodiment, in addition, if without other explanations, it is raw materials used to be all
It is commercially available.
Embodiment
Embodiment 1
Embodiment 1 provides a kind of microwave oven door label acrylate pressure sensitive adhesive, by weight, including following component: it is viscous
Property 60 parts of monomer, 5 parts of interior polycondensation monomer, 3 parts of modified monomer, 0.05 part of initiator, 50 parts of solvent, 0.5 part of emulsifier, crosslinking agent 2
Part, 0.5 part of defoaming agent, 0.5 part of levelling agent, 0.5 part of wetting agent.
The viscosity monomer is butyl methacrylate.
The interior polycondensation monomer is maleic anhydride.
The modified monomer is glycidyl methacrylate, and purchase is subordinate to Shanghai to face upward generation industry limited from facing upward generation chemistry
Company.
The initiator is ammonium persulfate.
The solvent is water.
The emulsifier is DNS-86, is bought from Qingxin County Hanke Chemical Technology Co., Ltd..
The crosslinking agent is butyl alcohol etherified melamine-formaldehyde resin microballoon；It is made by the steps to obtain:
(1) formaldehyde is added in four-hole bottle, adjusting pH value with triethylamine is 8.5, melamine is added, aqueous solution slowly rises
Temperature is dissolved to 70 DEG C to melamine, and system becomes clarification, and the reaction was continued 20min is cooled to 50 DEG C, butanol is added, and use hydrochloric acid
It adjusts pH value and carries out etherificate polycondensation for 4.5, react 1-1.5h, obtain butanol etherification melamino-formaldehyde prepolymer；
(2) it takes suitable PVA concentrated solution to be added in above-mentioned prepolymer, until its concentration is 4 × 10-3g/mL, uses dilute hydrochloric acid
It adjusts when pH value of solution is stirred to react constant to microspherulite diameter for 4.5,60 DEG C and stops reaction, be washed with deionized after centrifugation 3 times,
60 DEG C of low temperature dryings obtain butyl alcohol etherified melamine-formaldehyde resin microballoon.
The defoaming agent is fatty alcohol and polyethers defoaming agent, and purchase is chemical from crop field, model D-90.
The levelling agent is BYK333, is bought from Ze Chengtai trade Co., Ltd, Shenzhen.
The wetting agent is BYK346, is bought from Ze Chengtai trade Co., Ltd, Shenzhen.
The preparation method of the microwave oven door label acrylate pressure sensitive adhesive, step include:
(1) the sticky monomer, interior polycondensation monomer, modified monomer, crosslinking agent, solvent, emulsifier are added in reaction kettle
Stirring is warming up to 85 ± 2 DEG C, keeps the temperature 1.5h；
(2) reaction kettle is cooled to 75 ± 2 DEG C, the initiator of 1/3 parts by weight is then added, after 4h is reacted in heating, divide three
The secondary initiator for continuing that remaining 2/3 parts by weight are added dropwise, it is 0.5h that interval time is added dropwise every time, and 1h is reacted after dripping off, then will be warm
Degree is down to 60 DEG C；
(3) defoaming agent, levelling agent, wetting agent are put into the system of step (2), after stirring 60min, are cooled to 40 DEG C of mistakes
Filter obtains the Acrylic Pressure Sensitive Adhesive.
Embodiment 2
Embodiment 2 provides a kind of microwave oven door label acrylate pressure sensitive adhesive, by weight, including following component: it is viscous
80 parts of monomer of property, 8 parts of interior polycondensation monomer, 6 parts of modified monomer, 1 part of initiator, 60 parts of solvent, 1 part of emulsifier, 3.5 parts of crosslinking agent,
1 part of defoaming agent, 1 part of levelling agent, 1 part of wetting agent.
The viscosity monomer is butyl methacrylate.
The interior polycondensation monomer is maleic anhydride.
The modified monomer is glycidyl methacrylate, and purchase is subordinate to Shanghai to face upward generation industry limited from facing upward generation chemistry
Company.
The initiator is ammonium persulfate.
The solvent is water.
The emulsifier is DNS-86, is bought from Qingxin County Hanke Chemical Technology Co., Ltd..
The crosslinking agent is butyl alcohol etherified melamine-formaldehyde resin microballoon, and the preparation method is the same as that of Example 1.
The defoaming agent is fatty alcohol and polyethers defoaming agent, and purchase is chemical from crop field, model D-90.
The levelling agent is BYK333, is bought from Ze Chengtai trade Co., Ltd, Shenzhen.
The wetting agent is BYK346, is bought from Ze Chengtai trade Co., Ltd, Shenzhen.
The preparation method of the microwave oven door label acrylate pressure sensitive adhesive, step is the same as embodiment 1.
Embodiment 3
Embodiment 3 provides a kind of microwave oven door label acrylate pressure sensitive adhesive, by weight, including following component: it is viscous
Property 65 parts of monomer, 5 parts of interior polycondensation monomer, 4 parts of modified monomer, 0.1 part of initiator, 53 parts of solvent, 0.5 part of emulsifier, crosslinking agent 2.5
Part, 0.5 part of defoaming agent, 0.5 part of levelling agent, 0.5 part of wetting agent.
The viscosity monomer is butyl methacrylate.
The interior polycondensation monomer is maleic anhydride.
The modified monomer is glycidyl methacrylate, and purchase is subordinate to Shanghai to face upward generation industry limited from facing upward generation chemistry
Company.
The initiator is ammonium persulfate.
The solvent is water.
The emulsifier is DNS-86, is bought from Qingxin County Hanke Chemical Technology Co., Ltd..
The crosslinking agent is butyl alcohol etherified melamine-formaldehyde resin microballoon, and the preparation method is the same as that of Example 1.
The defoaming agent is fatty alcohol and polyethers defoaming agent, and purchase is chemical from crop field, model D-90.
The levelling agent is BYK333, is bought from Ze Chengtai trade Co., Ltd, Shenzhen.
The wetting agent is BYK346, is bought from Ze Chengtai trade Co., Ltd, Shenzhen.
The preparation method of the microwave oven door label acrylate pressure sensitive adhesive, step is the same as embodiment 1.
Embodiment 4
Embodiment 4 provides a kind of microwave oven door label acrylate pressure sensitive adhesive, by weight, including following component: it is viscous
Property 75 parts of monomer, 7 parts of interior polycondensation monomer, 5 parts of modified monomer, 0.5 part of initiator, 58 parts of solvent, 0.8 part of emulsifier, crosslinking agent 3
Part, 0.8 part of defoaming agent, 0.8 part of levelling agent, 0.8 part of wetting agent.
The viscosity monomer is butyl methacrylate.
The interior polycondensation monomer is maleic anhydride.
The modified monomer is glycidyl methacrylate, and purchase is subordinate to Shanghai to face upward generation industry limited from facing upward generation chemistry
Company.
The initiator is ammonium persulfate.
The solvent is water.
The emulsifier is DNS-86, is bought from Qingxin County Hanke Chemical Technology Co., Ltd..
The crosslinking agent is butyl alcohol etherified melamine-formaldehyde resin microballoon, and the preparation method is the same as that of Example 1.
The defoaming agent is fatty alcohol and polyethers defoaming agent, and purchase is chemical from crop field, model D-90.
The levelling agent is BYK333, is bought from Ze Chengtai trade Co., Ltd, Shenzhen.
The wetting agent is BYK346, is bought from Ze Chengtai trade Co., Ltd, Shenzhen.
The preparation method of the microwave oven door label acrylate pressure sensitive adhesive, step is the same as embodiment 1.
Embodiment 5
Embodiment 5 provides a kind of microwave oven door label acrylate pressure sensitive adhesive, by weight, including following component: it is viscous
Property 70 parts of monomer, 6 parts of interior polycondensation monomer, 4.5 parts of modified monomer, 0.3 part of initiator, 55 parts of solvent, 0.6 part of emulsifier, crosslinking agent 3
Part, 0.6 part of defoaming agent, 0.5 part of levelling agent, 0.5 part of wetting agent.
The viscosity monomer is butyl methacrylate.
The interior polycondensation monomer is maleic anhydride.
The modified monomer is glycidyl methacrylate, and purchase is subordinate to Shanghai to face upward generation industry limited from facing upward generation chemistry
Company.
The initiator is ammonium persulfate.
The solvent is water.
The emulsifier is DNS-86, is bought from Qingxin County Hanke Chemical Technology Co., Ltd..
The crosslinking agent is butyl alcohol etherified melamine-formaldehyde resin microballoon, and the preparation method is the same as that of Example 1.
The defoaming agent is fatty alcohol and polyethers defoaming agent, and purchase is chemical from crop field, model D-90.
The levelling agent is BYK333, is bought from Ze Chengtai trade Co., Ltd, Shenzhen.
The wetting agent is BYK346, is bought from Ze Chengtai trade Co., Ltd, Shenzhen.
The preparation method of the microwave oven door label acrylate pressure sensitive adhesive, step is the same as embodiment 1.
Embodiment 6
Embodiment 6 provides a kind of microwave oven door label acrylate pressure sensitive adhesive, by weight, including following component: it is viscous
Property 70 parts of monomer, 6 parts of interior polycondensation monomer, 4.5 parts of modified monomer, 0.3 part of initiator, 55 parts of solvent, 0.6 part of emulsifier, crosslinking agent 3
Part, 0.6 part of defoaming agent, 0.5 part of levelling agent, 0.5 part of wetting agent.
The viscosity monomer is butyl methacrylate.
The interior polycondensation monomer is maleic anhydride.
The modified monomer is glycidyl methacrylate, and purchase is subordinate to Shanghai to face upward generation industry limited from facing upward generation chemistry
Company.
The initiator is ammonium persulfate.
The solvent is water.
The emulsifier is DNS-86, is bought from Qingxin County Hanke Chemical Technology Co., Ltd..
The crosslinking agent is the butyl alcohol etherified melamine-formaldehyde resin microballoon containing ferroso-ferric oxide, is made by the following method
It is standby to obtain:
(1)Fe2+The absorption of ion: the butyl alcohol etherified melamine-formaldehyde resin microballoon after taking centrifugation to wash is ultrasonic in water
50 DEG C of heating stirrings of continuation are uniform after dispersing 5min；By FeCl2Solution is slowly added thereto, so that Fe in solution2+Ion concentration
Fe is centrifugated to obtain after 60 DEG C of heating stirrings react 1h for 1.2mol/L2+The resin microsphere of ionic adsorption；
(2)Fe2+The conversion of ion: gained resin microsphere is dispersed in water, and pH to 10.0 is adjusted with ammonium hydroxide, by mixed liquor
The static heating 5h at 70 DEG C, washing sample after Magneto separate, must contain the butanol etherification melamine of ferroso-ferric oxide after being repeated 5 times
Formaldehyde resin microballoon；Wherein, the concentration of the butyl alcohol etherified melamine-formaldehyde resin after the centrifugation washing in water is 28g/
L；The preparation method is the same as that of Example 1 for butyl alcohol etherified melamine-formaldehyde resin microballoon.
The defoaming agent is fatty alcohol and polyethers defoaming agent, and purchase is chemical from crop field, model D-90.
The levelling agent is BYK333, is bought from Ze Chengtai trade Co., Ltd, Shenzhen.
The wetting agent is BYK346, is bought from Ze Chengtai trade Co., Ltd, Shenzhen.
The preparation method of the microwave oven door label acrylate pressure sensitive adhesive, step is the same as embodiment 1.
Comparative example 1
Comparative example 1 provides a kind of microwave oven door label acrylate pressure sensitive adhesive, by weight, including following component: it is viscous
Property 70 parts of monomer, 0.1 part of interior polycondensation monomer, 4.5 parts of modified monomer, 0.3 part of initiator, 55 parts of solvent, 0.6 part of emulsifier, crosslinking
3 parts of agent, 0.6 part of defoaming agent, 0.5 part of levelling agent, 0.5 part of wetting agent.
The microwave oven door label acrylate pressure sensitive adhesive prepares raw material with embodiment 6, the difference is that only raw material
Parts by weight.
Comparative example 2
Comparative example 2 provides a kind of microwave oven door label acrylate pressure sensitive adhesive, by weight, including following component: it is viscous
Property 70 parts of monomer, 30 parts of interior polycondensation monomer, 4.5 parts of modified monomer, 0.3 part of initiator, 55 parts of solvent, 0.6 part of emulsifier, crosslinking agent
3 parts, 0.6 part of defoaming agent, 0.5 part of levelling agent, 0.5 part of wetting agent.
The microwave oven door label acrylate pressure sensitive adhesive prepares raw material with embodiment 6, the difference is that only raw material
Parts by weight.
Comparative example 3
Comparative example 3 provides a kind of microwave oven door label acrylate pressure sensitive adhesive, by weight, including following component: it is viscous
Property 70 parts of monomer, 6 parts of interior polycondensation monomer, 0.1 part of modified monomer, 0.3 part of initiator, 55 parts of solvent, 0.6 part of emulsifier, crosslinking agent 3
Part, 0.6 part of defoaming agent, 0.5 part of levelling agent, 0.5 part of wetting agent.
The microwave oven door label acrylate pressure sensitive adhesive prepares raw material with embodiment 6, the difference is that only raw material
Parts by weight.
Comparative example 4
Comparative example 4 provides a kind of microwave oven door label acrylate pressure sensitive adhesive, by weight, including following component: it is viscous
Property 70 parts of monomer, 6 parts of interior polycondensation monomer, 30 parts of modified monomer, 0.3 part of initiator, 55 parts of solvent, 0.6 part of emulsifier, crosslinking agent 3
Part, 0.6 part of defoaming agent, 0.5 part of levelling agent, 0.5 part of wetting agent.
The microwave oven door label acrylate pressure sensitive adhesive prepares raw material with embodiment 6, the difference is that only raw material
Parts by weight.
Comparative example 5
Comparative example 5 provides a kind of microwave oven door label acrylate pressure sensitive adhesive, by weight, including following component: it is viscous
Property 70 parts of monomer, 6 parts of interior polycondensation monomer, 4.5 parts of modified monomer, 0.3 part of initiator, 55 parts of solvent, 0.6 part of emulsifier, crosslinking agent
0.1 part, 0.6 part of defoaming agent, 0.5 part of levelling agent, 0.5 part of wetting agent.
The microwave oven door label acrylate pressure sensitive adhesive prepares raw material with embodiment 6, the difference is that only raw material
Parts by weight.
Comparative example 6
Comparative example 6 provides a kind of microwave oven door label acrylate pressure sensitive adhesive, by weight, including following component: it is viscous
Property 70 parts of monomer, 6 parts of interior polycondensation monomer, 4.5 parts of modified monomer, 0.3 part of initiator, 55 parts of solvent, 0.6 part of emulsifier, crosslinking agent
30 parts, 0.6 part of defoaming agent, 0.5 part of levelling agent, 0.5 part of wetting agent.
The microwave oven door label acrylate pressure sensitive adhesive prepares raw material with embodiment 6, the difference is that only raw material
Parts by weight.
Comparative example 7
Comparative example 7 provides a kind of microwave oven door label acrylate pressure sensitive adhesive, by weight, including following component: it is viscous
Property 70 parts of monomer, 6 parts of interior polycondensation monomer, 4.5 parts of modified monomer, 0.3 part of initiator, 55 parts of solvent, 0.6 part of emulsifier, crosslinking agent 3
Part, 0.6 part of defoaming agent, 0.5 part of levelling agent, 0.5 part of wetting agent.
The microwave oven door label acrylate pressure sensitive adhesive prepares raw material with embodiment 6, the difference is that only the friendship
Connection agent is butyl alcohol etherified melamine-formaldehyde resin, and model 20SE-60 is bought from Shanghai Kai Yin Chemical Co., Ltd..
Comparative example 8
Comparative example 8 provides a kind of microwave oven door label acrylate pressure sensitive adhesive, by weight, including following component: it is viscous
Property 70 parts of monomer, 6 parts of interior polycondensation monomer, 4.5 parts of modified monomer, 0.3 part of initiator, 55 parts of solvent, 0.6 part of emulsifier, crosslinking agent 3
Part, 0.6 part of defoaming agent, 0.5 part of levelling agent, 0.5 part of wetting agent.
The microwave oven door label acrylate pressure sensitive adhesive prepares raw material with embodiment 6, the difference is that only the friendship
Connection agent is melamine resin, is bought from Jining Hua Kai resin Co., Ltd.
Performance evaluation
1. 90 ° of peel strength tests: being measured by GB/T2792-2014.
2. high temperature test: placing 30min in 210 DEG C of baking ovens, whether observation sample occurs xanthochromia, warp, and according to GB/
T2792-2014 measures 90 ° of peel strength tests.
3. microwave test: placing 30min in microwave, whether observation sample occurs xanthochromia, warp.
4. shrinking percentage is tested: sample is pasted on smooth clean glass plate, 10 days under the conditions of placing it in 80 DEG C,
Measure the variation of its dimensioned area.
Table 1
Claims (10)
1. a kind of microwave oven door label acrylate pressure sensitive adhesive, which is characterized in that including following component: sticky monomer, interior polycondensation monomer,
Modified monomer, initiator, solvent, emulsifier, crosslinking agent, defoaming agent, levelling agent, wetting agent.
2. microwave oven door label acrylate pressure sensitive adhesive according to claim 1, which is characterized in that by weight, including
Following component: sticky monomer 60-80 parts, polycondensation monomer 5-8 parts interior, 3-6 parts of modified monomer, 0.05-1 parts of initiator, solvent 50-60
Part, 0.5-1 parts of emulsifier, 2-3.5 parts of crosslinking agent, 0.5-1 parts of defoaming agent, 0.5-1 parts of levelling agent, 0.5-1 parts of wetting agent.
3. microwave oven door label acrylate pressure sensitive adhesive according to claim 2, which is characterized in that by weight, including
Following component: sticky monomer 65-75 parts, polycondensation monomer 5-7 parts interior, 4-5 parts of modified monomer, 0.1-0.5 parts of initiator, solvent 53-
58 parts, 0.5-0.8 parts of emulsifier, 2.5-3 parts of crosslinking agent, 0.5-0.8 parts of defoaming agent, 0.5-0.8 parts of levelling agent, wetting agent 0.5-
0.8 part.
4. microwave oven door label acrylate pressure sensitive adhesive according to claim 1, which is characterized in that the viscosity monomer is selected from
Butyl methacrylate, Isobutyl methacrylate, isobutyl acrylate, n-propyl, one in Isooctyl acrylate monomer
Kind is a variety of.
5. microwave oven door label acrylate pressure sensitive adhesive according to claim 1, which is characterized in that the interior polycondensation monomer is selected from
One of methyl methacrylate, cyclohexyl acrylate, maleic anhydride, styrene, acrylonitrile, vinylacetate are a variety of.
6. microwave oven door label acrylate pressure sensitive adhesive according to claim 1, which is characterized in that the modified monomer is selected from
One of hydroxyethyl methacrylate, glycidyl methacrylate, hydroxy-ethyl acrylate are a variety of.
7. microwave oven door label acrylate pressure sensitive adhesive according to claim 1, which is characterized in that the crosslinking agent is to be modified
Melamine resin.
8. microwave oven door label acrylate pressure sensitive adhesive according to claim 7, which is characterized in that the modified cyanurotriamide
Formaldehyde resin is butyl alcohol etherified melamine-formaldehyde resin microballoon.
9. microwave oven door label acrylate pressure sensitive adhesive according to claim 1, which is characterized in that the interior polycondensation monomer changes
Property monomer weight ratio be 1:(0.6-0.8).
10. a kind of preparation method of microwave oven door label acrylate pressure sensitive adhesive according to claim 1, which is characterized in that
Step includes:
(1) the sticky monomer, interior polycondensation monomer, modified monomer, crosslinking agent, solvent, emulsifier are added in reaction kettle and are stirred
85 ± 2 DEG C are warming up to, 1.5h is kept the temperature；
(2) reaction kettle is cooled to 75 ± 2 DEG C, the initiator of 1/3 parts by weight is then added, after 3-6h is reacted in heating, in three times
Continue the initiator that remaining 2/3 parts by weight are added dropwise, it is 0.5h that interval time is added dropwise every time, and 1-2h is reacted after dripping off, then will be warm
Degree is down to 60 DEG C；
(3) defoaming agent, levelling agent, wetting agent are put into the system of step (2), after stirring 30-60min, are cooled to 40 DEG C of mistakes
Filter obtains the Acrylic Pressure Sensitive Adhesive.
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