CN104530298B - A kind of acrylic ester emulsion, preparation method and application thereof - Google Patents

A kind of acrylic ester emulsion, preparation method and application thereof Download PDF

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CN104530298B
CN104530298B CN201410489607.0A CN201410489607A CN104530298B CN 104530298 B CN104530298 B CN 104530298B CN 201410489607 A CN201410489607 A CN 201410489607A CN 104530298 B CN104530298 B CN 104530298B
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monomer
mixture
weight
acrylic ester
polyester film
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CN104530298A (en
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安佳丽
周守发
王旭亮
王辉
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Hefei Lucky Science and Technology Industry Co Ltd
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Hefei Lucky Science and Technology Industry Co Ltd
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Abstract

A kind of polyester film primary coat acrylic ester emulsion, preparation method and application thereof, it has following structural formula:

Description

A kind of acrylic ester emulsion, preparation method and application thereof
Technical field
The present invention relates to a kind of macromolecule emulsion preparing technical field, the particularly acrylic ester emulsion of a kind of polyester film undercoat, in addition, the present invention also relates to the polyester film that surface is coated with this emulsion.
Background technology
Two-way stretch gathers polyester film (BOPET) molecular chain rigidity, and polar group is few, which dictates that its surface energy is little, surface tension is low, the phenomenon that ink, sizing agent come off easily occurs, service requirements cannot be met, therefore its surface must be carried out modification, to improve its surface property, improve the sticking power between itself and functional coating.
In prior art, one part of Chinese patent discloses the preparation method of a kind of acrylic ester emulsion improving polyester film sticking power, and this acrylic ester emulsion adopts solution polymerization, containing organic solvent, synthesized emulsion has certain smell, it is easy to polluted by environment; And containing the unsaturated group that can react with functional coating after the solidification of above-mentioned emulsion coated film surface, be difficult to form effective chemical bonding between undercoat and functional coating, functional layer easily comes off.
Summary of the invention
Technical problem to be solved by this invention is the defect for prior art, provides a kind of acrylic ester emulsion, this acrylate contains the unsaturated group that can react with functional coating, it can improve the sticking power between polyester film and functional coating, after water boils 30 minutes, functional coating 100% does not come off.
Another two technical problems to be solved by this invention are to provide the preparation method of aforesaid propylene yogurt liquid and surface is coated with the polyester film of described ACRYLIC EMULSION.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of acrylic ester emulsion, has following structural formula:
Wherein: a is 10��25, b be 25��60, c is 20��85; D is 15��45; E is 10 ~ 35;
R1For-H or-CH3; R2ForOr; R3For-H or-CH3;
R4ForOrOr; R5For-H or-CH2CH2OH or-CH2CH(CH3) OH or-CH2CH3Or-CH2CH2CH2CH3Or-CH2CH(CH2CH3)CH2CH2CH2CH3��
A preparation method for acrylic ester emulsion, comprises the steps:
(1) add deionized water 150 ~ 250 weight part, reactive emulsifier 0.5 ~ 1.5 weight part in the reactor, obtain mixture A, for subsequent use;
(2) tri (propylene glycol) diacrylate of the functional monomer of the soft monomer of the hard monomer of 15 ~ 40 weight parts, 15 ~ 40 weight parts, 7 ~ 20 weight parts, 2 ~ 5 weight parts is mixed, obtain mix monomer B, for subsequent use;
(3) the mixture A taking 1/5 ~ 1/2 dissolves 0.5 ~ 1.5 weight part initiator, obtains initiator solution, for subsequent use;
(4) in the reactor containing remaining mixture A, add the pH buffer reagent of 0.5 ~ 1.5 weight part and the mix monomer B of 1/10 ~ 1/5, pre-emulsification 20 ~ 40min, it is warming up to 75 ~ 85 DEG C, drip and add initiator solution, after in question response device, liquid becomes basket, drip simultaneously and add remaining mix monomer B, after reacting 1.5 ~ 4h after dropwising, obtain acrylic ester emulsion C;
(5) in aforesaid propylene acid esters emulsion C, add the Resorcinol of 0.02 ~ 0.05 weight part, it is warming up to 85 ~ 100 DEG C, add the tosic acid of 0.1 ~ 0.5 weight part and the modified monomer of 1 ~ 5 weight part, after reaction 2 ~ 4h, obtain polyester film undercoat acrylic ester emulsion.
In such scheme, described reactive emulsifier is one or more mixtures in acrylamide sodium stearate, 2-acrylamide-2,2-dimethyl ethyl sulfonic acid sodium, 1-allyloxy-3-(4-nonylphenol)-2-propyl alcohol polyoxyethylene (10) ether ammonium sulfate.
In such scheme, described hard monomer is one or more mixtures in methyl methacrylate, vinyl acetate, vinyl cyanide.
In such scheme, described soft monomer is one or more mixtures in ethyl propenoate, butyl acrylate, Isooctyl acrylate monomer.
In such scheme, described functional monomer is one or more mixtures in vinylformic acid, methacrylic acid, diacetone-acryloamide(DAA), isobornyl methacrylate, Hydroxyethyl acrylate, Propylene glycol monoacrylate.
In such scheme, described initiator is one or more mixtures in Potassium Persulphate, ammonium persulphate.
In such scheme, described pH buffer reagent is sodium bicarbonate.
In such scheme, described modified monomer is one or more mixtures in glycidyl methacrylate, glycidyl allyl ether.
A kind of polyester film, the bottom that at least one surface is made containing aforesaid propylene acid esters emulsion.
Compared with prior art, tool has the following advantages in the present invention:
1. acrylic ester emulsion provided by the invention, by introducing active group in the structure, after being coated in polyester film surface, after high temperature longitudinal stretching, cross directional stretch are shaped, film surface contains unsaturated double-bond, and this group can participate in the ultraviolet light polymerization reaction of functional coating (blast liquid, hardening liquid), plays ligation between polyester film base material and functional coating, the sticking power of polyester film can be significantly improved, water can be prepared and boil the polyester film coating not come off for 30 minutes 100%.
2. method technique provided by the invention is simple, and reaction is easy to operation, in emulsion polymerization process, it may also be useful to reactive emulsifier, it is not necessary to remove the loaded down with trivial details operation of small-molecular emulsifier, and organic solvent-free, is conducive to environmental protection.
3. polyester film provided by the invention, sticking power is excellent, and after coating function layer, water boils rear functional layer difficult drop-off.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment 1
1. the preparation of acrylic ester emulsion
(1) add deionized water 240g, acrylamide sodium stearate 1g in the reactor, it is uniformly mixed fast, obtain mixture A;
(2) take the methyl methacrylate of 25g, the ethyl propenoate of 23g, the diacetone-acryloamide(DAA) of 10g, the tri (propylene glycol) diacrylate of 3g, 3g Hydroxyethyl acrylate join in single port bottle and mix, obtain mix monomer B;
(3) the said mixture A taking 50g, for dissolving 1g Potassium Persulphate, obtains initiator solution;
(4) in the reactor containing remaining mixture A, add the above-mentioned mix monomer B of 1g sodium bicarbonate, 10.7g, after pre-emulsification 30min, it is warming up to 80 DEG C, drip after adding initiator solution to emulsion change basket, drip simultaneously and add remaining mix monomer B, drip and it is incubated 2.5h after adding, obtain acrylic ester emulsion C;
(5) in aforesaid propylene acid esters emulsion C, add the Resorcinol of 0.03g, and it is warming up to 90 DEG C; Add 0.4g tosic acid and 3g glycidyl methacrylate again, carry out insulation reaction 3h, obtain polyester film undercoat acrylic ester emulsion.
2. the preparation of polyester film:
Get 20g aforesaid propylene acid esters emulsion, 0.2g solidifying agent, 0.5g wetting agent, 0.3g silica dispersion emulsion and 80g deionized water, it is uniformly dispersed through high-shear emulsion machine, obtain the precoating underlying liquid of polyester film coating.
Sheet is moulded in the casting that polyester slice melting is extruded cooling becomes No yield point, carries out longitudinal stretching, after its surface-coated precoating underlying liquid, then carries out cross directional stretch, and rolling obtains the optical polyester film with bottom.
Embodiment 2
1. the preparation of acrylic ester emulsion
(1) add deionized water 200g, 2-acrylamide-2,2-dimethyl ethyl sulfonic acid sodium 0.5g, acrylamide sodium stearate 0.5g in the reactor, it is uniformly mixed fast, obtains mixture A;
(2) take 18g vinyl acetate, 12g butyl acrylate, 20g Isooctyl acrylate monomer, the isobornyl methacrylate of 5g, the tri (propylene glycol) diacrylate of 2g, 3g Propylene glycol monoacrylate join in single port bottle and mix, obtain mix monomer B;
(3) the said mixture A taking 42g, for dissolving 0.8g ammonium persulphate, obtains initiator solution;
(4) in the reactor containing remaining mixture A, add the mix monomer B of 0.8g sodium bicarbonate and 7.5g, after pre-emulsification 25min, it is warming up to 75 DEG C, drip after adding initiator solution to emulsion change basket, drip simultaneously and add remaining mix monomer B, after adding, be incubated 2h, obtain acrylic ester emulsion C;
(5) in aforesaid propylene acid esters emulsion C, add the Resorcinol of 0.04g, and it is warming up to 95 DEG C; Add 0.25g tosic acid and 3g glycidyl allyl ether, 1g glycidyl methacrylate again, carry out insulation reaction 2h, obtain polyester film undercoat acrylic ester emulsion.
2. the preparation of polyester film:
Adopt aforesaid propylene acid esters emulsion, it is prepared according to the preparation method of polyester film in embodiment 1.
Embodiment 3
1. the preparation of acrylic ester emulsion
(1) add deionized water 250g, 2-acrylamide-2,2-dimethyl ethyl sulfonic acid sodium 1.5g in the reactor, it is uniformly mixed fast, obtains mixture A;
(2) take the vinyl acetate of 15g, 25g methyl methacrylate, the butyl acrylate of 16g, 2g vinylformic acid, 3g isobornyl methacrylate, the tri (propylene glycol) diacrylate of 2.5g, 2.5g Hydroxyethyl acrylate, 2.5g Propylene glycol monoacrylate join in single port bottle and mix, obtain mix monomer B;
(3) the said mixture A taking 62.5g, for dissolving 1.2g ammonium persulphate, obtains initiator solution;
(4) in the reactor containing remaining mixture A, add the mix monomer B of 1.2g sodium bicarbonate and 11.5g, after pre-emulsification 40min, it is warming up to 80 DEG C, drip after adding initiator solution to emulsion change basket, drip simultaneously and add remaining mix monomer B, after adding, be incubated 3h, obtain acrylic ester emulsion C;
(5) in aforesaid propylene acid esters emulsion C, add the Resorcinol of 0.04g, and it is warming up to 100 DEG C; Add 0.5g tosic acid and 5g glycidyl allyl ether again, carry out insulation reaction 2.5h, obtain polyester film undercoat acrylic ester emulsion.
2. the preparation of polyester film:
Adopt aforesaid propylene acid esters emulsion, it is prepared according to the preparation method of polyester film in embodiment 1.
Embodiment 4
1. the preparation of acrylic ester emulsion
(1) add deionized water 180g, 1-allyloxy-3-(4-nonylphenol)-2-propyl alcohol polyoxyethylene (10) ether ammonium sulfate 0.6g in the reactor, it is uniformly mixed fast, obtains mixture A;
(2) take 15g vinyl acetate, the ethyl propenoate of 7g, 8g Isooctyl acrylate monomer, the isobornyl methacrylate of 6g, the tri (propylene glycol) diacrylate of 2g, 2g Hydroxyethyl acrylate join in single port bottle and mix, obtain mix monomer B;
(3) the said mixture A taking 60g, for dissolving 0.5g Potassium Persulphate, obtains initiator solution;
(4) in the reactor containing remaining mixture A, add the mix monomer B of 0.6g sodium bicarbonate and 8g, after pre-emulsification 35min, it is warming up to 78 DEG C, drip after adding initiator solution to emulsion change basket, drip simultaneously and add remaining mix monomer B, after adding, be incubated 2.5h, obtain acrylic ester emulsion C;
(5) in aforesaid propylene acid esters emulsion C, add the Resorcinol of 0.02g, and it is warming up to 88 DEG C; Add 0.2g tosic acid and 2g glycidyl methacrylate again, carry out insulation reaction 2h, obtain polyester film undercoat acrylic ester emulsion.
2. the preparation of polyester film:
Adopt aforesaid propylene acid esters emulsion, it is prepared according to the preparation method of polyester film in embodiment 1.
Embodiment 5
1. the preparation of acrylic ester emulsion
(1) add deionized water 200g, 1-allyloxy-3-(4-nonylphenol)-2-propyl alcohol polyoxyethylene (10) ether ammonium sulfate 0.6g, acrylamide sodium stearate 0.8g in the reactor, it is uniformly mixed fast, obtains mixture A;
(2) take 10g methyl methacrylate, 5g vinyl acetate, 15g butyl acrylate, 25g isobornyl methacrylate, 3g methacrylic acid, 4g diacetone-acryloamide(DAA), the tri (propylene glycol) diacrylate of 4g, 2g Hydroxyethyl acrylate, 2g Propylene glycol monoacrylate join in single port bottle and mix, obtain mix monomer B;
(3) the mixture A taking 50g, for dissolving 0.8g ammonium persulphate, obtains initiator solution;
(4) in the reactor containing remaining mixture A, add 1.2g sodium bicarbonate in the mix monomer B with 8.5g, after pre-emulsification 30min, it is warming up to 80 DEG C, drip after adding initiator solution to emulsion change basket, drip simultaneously and add remaining mix monomer B, after adding, be incubated 3.5h, obtain acrylic ester emulsion C;
(5) in aforesaid propylene acid esters emulsion C, add the Resorcinol of 0.04g, and it is warming up to 90 DEG C; Add 0.4g tosic acid and 2g glycidyl methacrylate, 2g glycidyl allyl ether again, carry out insulation reaction 2.5h, obtain acrylic ester emulsion.
2. the preparation of polyester film:
Adopt aforesaid propylene acid esters emulsion, it is prepared according to the preparation method of polyester film in embodiment 1.
Adhesion performance is tested: solidify blast liquid at the surface-coated UV of above-mentioned mylar tape bottom, brightness enhancement film is obtained after UV hardening with radiation, the method specified at the surface employing GB/T9286 of brightness enhancement film draws hundred lattice, then put into 100 DEG C of boiling water to carry out water and boil 30min, survey the sticking power between polyester film and brightness enhancement film, the frame counter sticking power retained with paint film, 100% represents do not have lattice to come off, and sticking power is best. Test result is in table 1.
Table 1 sticking power test result
Embodiment Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5
Sticking power/% 100 100 100 100 100

Claims (5)

1. a polyester film undercoat acrylic ester emulsion, it is characterised in that, there is following structural formula:
Wherein: a is 10��25, b be 25��60, c is 20��85; D is 15��45; E is 10��35;
R1For-H or-CH3; R2ForR3For-H or-CH3;
R4For
R5For-H or-CH2CH2OH��-CH2CH(CH3)OH��-CH2CH3��-CH2CH2CH2CH3Or-CH2CH(CH2CH3)CH2CH2CH2CH3��
2. the preparation method of a polyester film undercoat acrylic ester emulsion as claimed in claim 1, it is characterised in that, preparation comprises the steps:
A, add deionized water 150��250 weight part, reactive emulsifier 0.5��1.5 weight part in the reactor, obtain mixture A, for subsequent use;
B, the tri (propylene glycol) diacrylate of the functional monomer of the soft monomer of the hard monomer of 15��40 weight parts, 15��40 weight parts, 7��20 weight parts, 2��5 weight parts is mixed, obtain mix monomer B, for subsequent use;
C, the mixture A taking 1/5��1/2 dissolve 0.5��1.5 weight part initiator, obtain initiator solution, for subsequent use;
D, the pH buffer reagent adding 0.5��1.5 weight part in the reactor containing remaining mixture A and 1/10��1/5 mix monomer B, pre-emulsification 20��40min, it is warming up to 75��85 DEG C, drip and add initiator solution, after in question response device, liquid becomes basket, drip simultaneously and add remaining mix monomer B, after reacting 1.5��4h after dropwising, obtain acrylic ester emulsion C;
E, the Resorcinol adding 0.02��0.05 weight part in aforesaid propylene acid esters emulsion C, it is warming up to 85��100 DEG C, adding the tosic acid of 0.1��0.5 weight part and the modified monomer of 1��5 weight part, reaction 2��4h, obtains polyester film undercoat acrylic ester emulsion;
Described hard monomer is the mixture of methyl methacrylate and vinyl acetate;
Described soft monomer is one or more the mixture in ethyl propenoate, butyl acrylate, Isooctyl acrylate monomer;
Described functional monomer is one or more the mixture in vinylformic acid, diacetone-acryloamide(DAA), Hydroxyethyl acrylate;
Described modified monomer is one or both the mixture in glycidyl methacrylate or glycidyl allyl ether;
Described reactive emulsifier is one or both the mixture in acrylamide sodium stearate or 2-acrylamide-2,2-dimethyl ethyl sulfonic acid sodium.
3. preparation method according to claim 2, it is characterised in that, described initiator is one or both the mixture in Potassium Persulphate, ammonium persulphate.
4. preparation method according to claim 2, it is characterised in that, described pH buffer reagent is sodium bicarbonate.
5. a polyester film, it is characterised in that, at least one surface is containing the undercoat that acrylic ester emulsion is made as claimed in claim 1.
CN201410489607.0A 2014-09-23 2014-09-23 A kind of acrylic ester emulsion, preparation method and application thereof Active CN104530298B (en)

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CN104961857B (en) * 2015-06-30 2018-02-16 中国乐凯集团有限公司 One kind is modified(Methyl)Acrylate and preparation method thereof
CN105153348B (en) * 2015-07-30 2017-10-27 南京京锦元科技实业有限公司 A kind of modified ethylene acetate acrylate copolymer emulsion of high-dissolvability and high glass transition temperature and preparation method thereof
CN105061667B (en) * 2015-08-11 2017-10-10 合肥乐凯科技产业有限公司 A kind of acrylic acid ester emulsion and its application
CN105153353A (en) * 2015-08-11 2015-12-16 合肥乐凯科技产业有限公司 Acrylate emulsion as well as preparation method and application thereof
CN106349453B (en) * 2016-08-27 2020-02-18 合肥乐凯科技产业有限公司 Polyurethane emulsion and application thereof
CN107033715B (en) * 2017-04-27 2019-05-07 广东工业大学 A kind of emulsion-type polyacrylate coating agent and preparation method thereof
CN108285543A (en) * 2018-01-31 2018-07-17 苏州维洛克电子科技有限公司 A kind of preparation method of antibacterial polyester sheet

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WO2010045250A1 (en) * 2008-10-13 2010-04-22 Eastern Michigan University Conventional latex / nanolatex blends
CN101967211A (en) * 2010-09-29 2011-02-09 北京化工大学 Preparation method of low molecular weight polyacrylic ester acrylic ester for photo-curing
CN102585072A (en) * 2012-01-11 2012-07-18 南京瑞固聚合物有限公司 Room temperature self-crosslinking acrylic ester emulsion
CN103396508B (en) * 2013-07-29 2016-01-13 华南理工大学 A kind of low-temperature self-crosslinking waterborne acrylic paint and preparation method thereof and application
CN103694403B (en) * 2013-12-23 2016-01-27 合肥工业大学 A kind of preparation method of self-crosslinking polyester film silane coupling agent acrylic ester emulsion

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