CN105061667B - A kind of acrylic acid ester emulsion and its application - Google Patents
A kind of acrylic acid ester emulsion and its application Download PDFInfo
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- CN105061667B CN105061667B CN201510489243.0A CN201510489243A CN105061667B CN 105061667 B CN105061667 B CN 105061667B CN 201510489243 A CN201510489243 A CN 201510489243A CN 105061667 B CN105061667 B CN 105061667B
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Abstract
The present invention relates to a kind of acrylic acid ester emulsion, function monomer is used as using AAEM, acetoacetic acid group reacts in the neutralization stage that emulsion is synthesized with amine generates enamine, participate in cured later crosslinking, and the shrinkage factor of function monomer is low, be conducive to alleviating internal stress when curing of coating shrinks, it is coated in polyester film surface after the solidification of high temperature cross directional stretch, be conducive to the infiltration of functional layer coating fluid, sprawl, can not fall off the adhesive force between functional coating and polyester film 100%.The optics mylar containing face coat that the present invention is provided can be used as the fields such as reflectance coating, cured film, fenestrated membrane, meet the reprocessing demand of film.
Description
Technical field
The present invention relates to a kind of acrylic acid ester emulsion of polyester film primary coat, in addition, the invention further relates to surface
It is coated with the polyester film of the emulsion.
Background technology
Polyethylene terephthalate（PET）Film is due to excellent mechanical performance, electric property and chemically-resistant
Corrosive nature, is widely used in liquid crystal display（LCD）, in-mold decoration（Such as brightness enhancement film, diffusion barrier, cured film）Deng production neck
Domain.But because the highly crystalline of polyester film surface is orientated, cause its surface property poor, with various ink, adhesive, coating
It is poor Deng cementability between material.Generally polyester resin, polyacrylic acid can be contained by the coating on thermoplastic resin film surface
The bonding modified layer of the adhesives such as esters resin, polyurethane based resin, to improve between polyester film and other functional coating interfaces
Adhesive force.
In the prior art, Chinese patent 201310515714.1 discloses a kind of acrylic acid ester emulsion, acrylate breast
Liquid has synthesized a kind of acrylic acid ester emulsion using hard monomer, soft monomer and function monomer as reaction monomers using solution polymerization process, and
Polyester film surface is coated on, to improve the surface property of polyester film, adhesive force is improved.
Although the acrylic acid ester emulsion that above-mentioned technology is provided, which is applied to polyester film surface, can improve its adhesive force, on
State acrylic acid ester emulsion and use solution polymerization, containing organic solvent, synthesized emulsion has certain smell, and dirt is caused to environment
Dye；And do not contained after the solidification of above-mentioned emulsion coated film surface and can participate in the active group of UV solidifications, priming coat and functional coating
Between be difficult to form effective chemical bonding.
The content of the invention
The technical problems to be solved by the invention are in view of the shortcomings of the prior art there is provided a kind of acrylic acid ester emulsion, and this third
Olefin(e) acid ester lotion applicator can improve the adhesive force between polyester film and other functional coatings, through UV in polyester film surface
After degradation 24h, functional coating 100% is not fallen off.
Another technical problem to be solved by this invention is to provide the polyester that surface is coated with the acrylic acid ester emulsion
Film.
In order to solve the above technical problems, the present invention is adopted the following technical scheme that：
A kind of acrylic acid ester emulsion, is prepared according to the following steps：
（1）The parts by weight of deionized water 150 ~ 250, the parts by weight of reactive emulsifier 0.5 ~ 1.5 are added in the reactor, quickly
It is uniformly mixed, obtains mixture A；Weighing the 1/5 ~ 1/2 of mixture A weight is used to dissolve 0.5 ~ 1.5 parts by weight initiator, obtains
Initiator solution；Weigh 2 ~ 5 parts by weight acrylic ester monomers containing acyl group, the hard monomer of 15 ~ 40 parts by weight, 15 ~ 40 parts by weight
Soft monomer, the functional monomer of 8 ~ 15 parts by weight, obtain mix monomer B；
（2）0.5 ~ 1.5 parts by weight pH buffer and mix monomer B weights are added in the reactor containing remaining mixture A
After the 1/5 ~ 1/10 of amount, 20 ~ 40min of pre-emulsification, temperature of reactor rises to 75 ~ 85 DEG C, and initiator solution is added dropwise, to pre-emulsion
After becoming basket, while remaining initiator solution and remaining mix monomer B is added dropwise, after both add, after 1 ~ 3h of emulsion insulation reaction, drop
Temperature is to 40 ~ 50 DEG C, and it is 7 ~ 8 to add alkali lye and be neutralized to pH value, obtains acrylic acid ester emulsion.
Aforesaid propylene acid esters emulsion, the reactive emulsifier is acrylamide odium stearate, 3- allyloxy -2- hydroxyls
One kind or any combination of base -1- sulfonic acid sodium salts.
Aforesaid propylene acid esters emulsion, the initiator is ammonium persulfate or one kind or any combination in potassium peroxydisulfate.
Aforesaid propylene acid esters emulsion, the acrylic ester monomer containing acyl group is acetoacetate methacrylic acid ethylene glycol
Ester, 3- benzoylacrylates or one kind or any combination in AAEM.
Aforesaid propylene acid esters emulsion, the hard monomer is methyl methacrylate or one kind in styrene or its combination.
Aforesaid propylene acid esters emulsion, the soft monomer is ethyl acrylate or one kind or its group in Isooctyl acrylate monomer
Close.
Aforesaid propylene acid esters emulsion, the function monomer is acrylic acid, methacrylic acid, DAAM, methyl
Isobornyl acrylate, THFMA, one kind or any combination of 2- phenoxyethyl acrylates.
Aforesaid propylene acid esters emulsion, the pH buffer is sodium acid carbonate or one kind or any combination in ammonium hydrogen carbonate.
Aforesaid propylene acid esters emulsion, the alkali lye is hexamethylene diamine, N, one kind of N- dimethylethanolamines or n-butylamine or is appointed
Meaning combination.
Contain the bottom that aforesaid propylene acid esters emulsion is made in a kind of polyester film, at least one surface.
Compared with prior art, the invention has the advantages that：
1. the acyl group in the acrylic acid ester emulsion that the present invention is provided, acrylic ester monomer containing acyl group is in emulsion synthesis
Enamine is generated with stage and amine reaction, cured later crosslinking is participated in, after the solidification of high temperature cross directional stretch, forms the sky of multidimensional
Between network structure, the adhesive force between functional coating and polyester film can be improved.
2. 2- phenoxyethyl acrylates used contain ehter bond in the present invention, adhesive force promotion can be played in system
The effect of agent, can improve the adhesive force between precoated shet and functional coating.
3. the present invention uses reactive emulsifier, such as：Acrylamide odium stearate, 3- allyloxy -2- hydroxyls -1-
Sulfonic acid sodium salt, it is to avoid small-molecular emulsifier, which migrates the phenomenon for causing film surface to reduce to film surface, to be occurred.Third
Amido link has the effect for improving adhesive force in acrylamide odium stearate；3- allyloxy -2- hydroxyl -1- propane sulfonic acid sodium
Contain ehter bond, hydroxyl and sulfonic group isoreactivity group in salt, complete active group is not reacted exposed to film surface, with function
Coating reaction, chemical bonding effect is formd between precoated shet and functional coating, the adhesive force between them is effectively improved.
4. contain various active group in the side-chain structure of emulsion, such as：Amino, carboxyl, amide groups etc., these functional groups
Between synergy, adhesive force can be effectively improved.Lotion applicator is consolidated in polyester film surface by high temperature cross directional stretch
After change, the spacial framework of multidimensional is formed, is conducive to the infiltration of functional coating coating fluid, sprawls, and and acrylate coatings
Close structure is formed after solidification, and the shrinkage factor of function monomer is low, is conducive to alleviating internal stress when curing of coating shrinks,
Can not fall off the adhesive force between functional coating and polyester film 100%.
5. the optics mylar containing face coat that the present invention is provided can be used as the neck such as reflectance coating, cured film, fenestrated membrane
Domain, meets the reprocessing demand of film.
Embodiment
The present invention is described in further detail below in conjunction with specific embodiment, but embodiments of the present invention are not limited to
This.
Embodiment 1
1. the preparation of acrylic acid ester emulsion
（1）Deionized water 220g, acrylamide odium stearate 1g are added in the reactor, are quickly uniformly mixed, are obtained
Mixture A；Weighing the 1/3 of mixture A weight is used to dissolve 1g potassium peroxydisulfates, obtains initiator solution；Weigh 3g acetoacetyls
EMA, 25g methyl methacrylates, 23g ethyl acrylates, 1g methacrylic acids, 2g DAAMs,
5g isobornyl methacrylates are well mixed, and obtain mix monomer B.
（2）The 1/8 of 1g sodium acid carbonates and mix monomer B weight, pre- breast are added in the reactor containing remaining mixture A
Change after 20min；Temperature of reactor rises to 80 DEG C, and is added dropwise after initiator solution to emulsion change basket, while initiator solution is added dropwise
With remaining mix monomer B, 2.5h is incubated after adding, 40 DEG C are cooled to, N is added, it is 7 that N- dimethylethanolamines, which are neutralized to pH value,
Obtain acrylic acid ester emulsion.
2. the preparation of polyester film
(1) 20g aforesaid propylene acid esters emulsion, 0.25g curing agent, 0.6g wetting agents, 0.4g silica dispersions are taken
Scattered body fluid and 80g deionized waters, are uniformly dispersed through high-shear emulsifying agent, obtain the primary coat liquid of polyester film coating；
(2) dry polyester slice melting extrusion is cooled into the casting sheet of No yield point, through 3.2 times of longitudinal stretching,
After its surface coating precoating underlying liquid, then 3.5 times of cross directional stretch is carried out, thickness is obtained for 100 μm through 230 DEG C of thermal finalization windings
Polyester film, the thickness of priming coat is 0.1 μm, surveys its performance（It is shown in Table 1）.
Embodiment 2
（1）Deionized water 200g, 0.5g 3- allyloxy -2- hydroxyl -1- sulfonic acid sodium salts are added in the reactor,
Quickly it is uniformly mixed, obtains mixture A；Weighing the 1/4 of mixture A weight is used to dissolve 0.8g ammonium persulfates, obtains initiator
Solution；Weigh 2.5g acetoacetyls methacrylic acid glycol ester, 15g methyl methacrylates, 5g styrene, 15g propylene
The different monooctyl ester of acid, 2g acrylic acid, 2g DAAMs, 6g 2- phenoxyethyl acrylates are well mixed, and obtain mix monomer
B。
（2）The 1/5 of 0.8g ammonium hydrogen carbonate and mix monomer B weight is added in the reactor containing remaining mixture A, in advance
Emulsify after 25min, be warming up to 82 DEG C, and be added dropwise after initiator solution to emulsion change basket, while initiator solution and residue is added dropwise
Mix monomer B, 1h is incubated after adding, and is cooled to 45 DEG C, and it is 8 to add hexamethylene diamine and be neutralized to pH value, obtains acrylic acid ester emulsion.
2. the preparation of polyester film
Using aforesaid propylene acid esters emulsion, prepared according to the preparation method of polyester film in embodiment 1.
Embodiment 3
（1）Deionized water 150g, 0.7g acrylamide odium stearate, 0.8g 3- allyloxys -2- are added in the reactor
Hydroxyl -1- sulfonic acid sodium salts, are quickly uniformly mixed, and obtain mixture A；Weighing the 1/2 of mixture A weight is used to dissolve
0.5g potassium peroxydisulfates, obtain initiator solution；Weigh 4g 3- benzoylacrylates, 25g methyl methacrylate, 15g
Styrene, 25g ethyl acrylate, 5g methacrylic acids, 5g THFMAs, 5g methacrylic acid isoborneols
Ester is well mixed, and obtains mix monomer B.
（2）The 1/7 of 1.5g sodium acid carbonates and mix monomer B weight is added in the reactor containing remaining mixture A, in advance
Emulsify after 30min；Temperature of reactor rises to 75 DEG C, and is added dropwise after initiator solution to emulsion change basket, while it is molten that initiator is added dropwise
Liquid and remaining mix monomer B, are incubated 2h after adding, are cooled to 47 DEG C, and it is 8 to add n-butylamine and be neutralized to pH value, obtains acrylate
Emulsion.
2. the preparation of polyester film
Using aforesaid propylene acid esters emulsion, prepared according to the preparation method of polyester film in embodiment 1.
Embodiment 4
（1）Deionized water 180g, 0.8g acrylamide odium stearate, 0.4g 3- allyloxys -2- are added in the reactor
Hydroxyl -1- sulfonic acid sodium salts, are quickly uniformly mixed, and obtain mixture A；Weighing the 1/3 of mixture A weight is used to dissolve
0.7g potassium peroxydisulfates and 0.8g ammonium persulfates, obtain initiator solution；Weigh 2g AAEMs, 2g acetyl
Acetoxymethyl acrylic acid glycol ester, 1g 3- benzoylacrylates, 15g styrene, 20g ethyl acrylates, 20g
Isooctyl acrylate monomer, 3g methacrylic acids, 2g isobornyl methacrylates, the mixing of 5 g2- phenoxyethyl acrylates are equal
It is even, obtain mix monomer B.
（2）0.5g sodium acid carbonates, 0.5g ammonium hydrogen carbonate and mix monomer are added in the reactor containing remaining mixture A
After the 1/10 of B weight, pre-emulsification 40min, temperature of reactor rises to 85 DEG C, and is added dropwise after initiator solution to emulsion change basket, together
When initiator solution and remaining mix monomer B is added dropwise, be incubated 3h after adding, be cooled to 43 DEG C, add N, N- dimethylethanolamines
It is 8 to be neutralized to pH value, obtains acrylic acid ester emulsion.
2. the preparation of polyester film
Using aforesaid propylene acid esters emulsion, prepared according to the preparation method of polyester film in embodiment 1.
Embodiment 5
（1）Deionized water 250g, 0.8g 3- allyloxy -2- hydroxyl -1- sulfonic acid sodium salts are added in the reactor,
Quickly it is uniformly mixed, obtains mixture A；Weighing the 1/5 of mixture A weight is used to dissolve 1.2g ammonium persulfates, obtains initiator
Solution；Weigh 1g AAEMs, 1g 3- benzoylacrylates, 15g methyl methacrylates
Ester, 15g styrene, 10g ethyl acrylates, 16g Isooctyl acrylate monomers, 2g acrylic acid, 1g methacrylic acids, 4g diacetone acrylamides
Acid amides, 2g THFMAs, 3g isobornyl methacrylates are well mixed, and obtain mix monomer B.
（2）The 1/6 of 0.5g ammonium hydrogen carbonate and mix monomer B weight is added in the reactor containing remaining mixture A, in advance
Emulsify after 35min, temperature of reactor rises to 78 DEG C, and initiator solution to emulsion is added dropwise and become after basket, while it is molten that initiator is added dropwise
Liquid and remaining mix monomer B, are incubated 1.5h after adding, are cooled to 50 DEG C, add hexamethylene diamine and N, N- dimethylethanolamine are neutralized
It is 7 to pH value, obtains acrylic acid ester emulsion.
2. the preparation of polyester film
Using aforesaid propylene acid esters emulsion, prepared according to the preparation method of polyester film in embodiment 1.
The performance table of table 1
Properties method of testing is as follows in table：
1. adhesive force：Polyester film surface containing priming coat is coated after one layer of hardening bath, UV radiation curings, obtains interface
The cured film being firmly combined with.With UV ageing oven aging 24h, the adhesive force combined using cross-cut methods test interface, with paint film
The frame counter polyester film and the adhesive force of cured film of reservation.
2. light transmittance mist degree：Tested using Shanghai Precision Scientific Apparatus Co., Ltd WGT-S light transmittances/mist degree analyzer.
Claims (9)
1. a kind of acrylic acid ester emulsion, it is characterised in that prepare according to the following steps：
(1) parts by weight of deionized water 150~250, the parts by weight of reactive emulsifier 0.5~1.5 are added in the reactor, are quickly stirred
Mix well mixed, obtain mixture A；Weighing the 1/5~1/2 of mixture A weight is used to dissolve 0.5~1.5 parts by weight initiator, obtains
Initiator solution；Weigh 2~5 parts by weight acrylic ester monomers containing acyl group, the hard monomer of 15~40 parts by weight, 15~40 weight
The soft monomer, the functional monomer of 8~15 parts by weight of part, obtain mix monomer B；
(2) 0.5~1.5 parts by weight pH buffer, 1/5~1/10 parts by weight are added in the reactor containing remaining mixture A
Mix monomer B, after 20~40min of pre-emulsification, temperature of reactor rises to 75~85 DEG C, and initiator solution is added dropwise, to pre- breast
After liquid becomes basket, while remaining initiator solution and remaining mix monomer B, after both add, 1~3h of emulsion insulation reaction is added dropwise
Afterwards, 40~50 DEG C are cooled to, it is 7~8 to add alkali lye and be neutralized to pH value, obtains acrylic acid ester emulsion；
The reactive emulsifier is acrylamide odium stearate, one kind of 3- allyloxy -2- hydroxyl -1- sulfonic acid sodium salts
Or any combination.
2. acrylic acid ester emulsion according to claim 1, it is characterised in that described initiator is ammonium persulfate or over cure
One kind of sour potassium or its combination.
3. acrylic acid ester emulsion according to claim 2, it is characterised in that described acrylic ester monomer containing acyl group is
In acetoacetyl methacrylic acid glycol ester, 3- benzoylacrylates or AAEM
One kind or any combination.
4. acrylic acid ester emulsion according to claim 3, it is characterised in that described hard monomer is methyl methacrylate
Or one kind in styrene or its combination.
5. acrylic acid ester emulsion according to claim 4, it is characterised in that described soft monomer is ethyl acrylate or third
One kind or its combination in the different monooctyl ester of olefin(e) acid.
6. acrylic acid ester emulsion according to claim 5, it is characterised in that described function monomer is acrylic acid, methyl
Acrylic acid, DAAM, isobornyl methacrylate or one kind of 2- phenoxyethyl acrylates or any group
Close.
7. acrylic acid ester emulsion according to claim 6, it is characterised in that described pH buffer is sodium acid carbonate or carbon
One kind of sour hydrogen ammonium or its combination.
8. acrylic acid ester emulsion according to claim 7, it is characterised in that the alkali lye is hexamethylene diamine, N, N- dimethyl
One kind or any combination of monoethanolamine or n-butylamine.
9. a kind of polyester film, it is characterised in that contain the propylene as any one of claim 1-8 at least one surface
The bottom that acid esters emulsion is made.
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| CN108239297A (en) * | 2018-01-31 | 2018-07-03 | 苏州维洛克电子科技有限公司 | A kind of preparation method of anti-ultraviolet polyester sheet material |
| CN108440708B (en) * | 2018-02-28 | 2020-11-03 | 合肥乐凯科技产业有限公司 | Preparation method of emulsion pressure-sensitive adhesive and polarizer protective film |
| CN109651550A (en) * | 2018-12-06 | 2019-04-19 | 成都杰晟蜀邦新材料科技有限公司 | A kind of fatty acid modified acrylic emulsion and preparation method thereof |
| CN110746892B (en) * | 2019-11-13 | 2021-09-24 | 合肥乐凯科技产业有限公司 | Surfactant for protective film and preparation method thereof |
| CN111775253A (en) * | 2020-07-17 | 2020-10-16 | 安徽三和工艺品有限公司 | Preparation method of impregnating resin for wickerwork |
| CN114369198B (en) * | 2022-01-26 | 2023-03-31 | 上海应用技术大学 | 3-benzoyl ethyl acrylate diesel pour point depressant, diesel pour point depressant composition, preparation and application |
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| CN102391411A (en) * | 2011-08-29 | 2012-03-28 | 华南理工大学 | Low-temperature self-crosslinking polyacrylate pigment printing binding agent and preparation method thereof |
| CN102924987A (en) * | 2012-10-16 | 2013-02-13 | 广东工业大学 | Thermal-ultraviolet dual-curing water-based colored coating composition |
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| CN103554340B (en) * | 2013-10-27 | 2016-06-15 | 合肥乐凯科技产业有限公司 | For improving acrylic acid ester emulsion of mylar adhesive force and preparation method thereof |
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