CN104910317A - Acrylic resin emulsion used in water-based plastic ink, and preparation method thereof - Google Patents
Acrylic resin emulsion used in water-based plastic ink, and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of high-molecular synthesis, and discloses an acrylic resin emulsion used in water-based plastic ink, and a preparation method thereof. According to the invention, commonly used acrylic acid soft and hard monomers are blended; a plurality of specific functional monomers are introduced; a small amount of co-emulsifier is used in auxiliary; and free radical polymerization is carried out under the initiation of ammonium persulfate, such that the acrylic resin emulsion is prepared. When a water-based plastic ink prepared with the acrylic resin emulsion is applied on a plastic substrate, characteristics such as good water resistance, high adhesion, excellent wet rubbing resistance, and the like are shown. The emulsion also has the advantages of low surface tension, fast drying, and excellent alcohol solubility. When the emulsion is used in plastic substrate printing, the printing effect is equivalent to that of a solvent-type plastic ink.
Description
Technical field
The present invention relates to macromolecule synthesising technology field, specifically a kind of Emulsion acrylic resin for aqueous ink used for plastic and preparation method thereof.
Background technology
Water color ink refers to the volatile-type ink making solvent with water and part alcohol etc.Ink is dry with the volatilization of moisture content, printing process environmentally safe, and ink is to human non-toxic's evil, and nonflammable, security is good.Its main application fields is flexo and gravure.
In gravure field, the gravure printing product of the U.S. 80% use water color ink, and the plastic printing of 40% adopts water color ink.Britain has made laws and has prohibitted the use the film of solvent type ink printing packaging food.But plastic rotogravure ink is still based on solvent type ink at home.In recent years, along with people are more and more stricter to environmental requirement, aqueous ink used for plastic will be the main trend of current ink used for plastic development.
But, when promoting water color ink and being applied to plastic printing, be faced with many technical bottlenecks.
First, when water color ink is applied to plastic film printing, must meets and possess good printing performance.Because the surface tension of water is comparatively large, is difficult in the flattening of film upper berth whole, therefore, other solvent must be added when preparing aqueous ink used for plastic, reduce the surface tension of ink, to reach the printing performance being equal to conventional solvent ink.
This analog assistant is mainly based on alcohols, and a small amount of silicon class leveling auxiliary agent.Therefore, require that emulsion must possess excellent alcohols consistency, that is: meet alcohols not breakdown of emulsion, not thickening, easily rush rare.
Secondly, require the emulsion preparing aqueous ink used for plastic, when being applied to plastic basis material table print, stronger sticking power and water resisting property must be had with plastic film; When being applied to the printing of plastic basis material composite membrane, stronger combined strength bination should be possessed.
Finally, in order to the production maximum benefit in the actual printing process of larger realization, improve printing efficiency, require that this emulsion possesses quick-drying, anti-not sticky characteristic.
Although on the market, early more existing aqueous ink used for plastic is released, and product performance more or less exist some shortcomings in some aspects, and over-all properties still cannot the status of replace solvents ink.The emulsion over-all properties mainly making ink of tracing sth. to its source does not reach application requiring.Therefore, aqueous ink used for plastic is thought to replace solvent-borne type ink used for plastic completely, and main problem is the over-all properties problem that will solve emulsion.
Summary of the invention
The object of the present invention is to provide a kind of Emulsion acrylic resin for aqueous ink used for plastic.
The present invention for achieving the above object, takes following technical scheme to be achieved:
For an Emulsion acrylic resin for aqueous ink used for plastic, comprise mixture A, mixture B, initiator one and initiator two,
Described mixture A comprises following component: the moon/non-composite emulsifying agent accounting for emulsion monomer quality total amount 0.5% ~ 1.0%, the sticking power accounting for emulsion monomer quality total amount 1% ~ 5% promote monomer, account for the cross-linking monomer of mixture A monomer mass total amount 1% ~ 8%, account for the functional acrylic monomer of emulsion monomer quality total amount 8% ~ 15%, account for soft, the hard monomer of emulsion monomer quality total amount 18% ~ 40% and appropriate water, and the second-order transition temperature of soft or hard monomer is at 5 DEG C ~ 25 DEG C;
Initiator one: account for mixture A monomer mass total amount 0.7% ~ 1.0%;
Described mixture B is 35% ~ 65% of emulsion monomer quality total amount, comprise following component: account for soft, the hard monomer of mixture B monomer mass total amount 98.5% ~ 99.5% and account for the cross-linking monomer of mixture B monomer mass total amount 0.5% ~ 1.5%, the second-order transition temperature of soft or hard monomer is at 0 DEG C ~ 40 DEG C;
Initiator two: account for mixture B monomer mass total amount 0.8% ~ 1.2%;
Described emulsion monomer comprises sticking power and promotes monomer, cross-linking monomer, functional acrylic monomer, soft monomer, hard monomer.
Preferably, described the moon/non-composite emulsifying agent is undertaken composite by anion surfactant and nonionogenic tenside, and the mass ratio of described anion surfactant and nonionogenic tenside is 1/2 ~ 1/1.5.
Preferably, described anion surfactant is any one in sodium lauryl sulphate, branched dodecylbenzene sulfonic acid sodium, polyethenoxy ether sodium sulfate, branched dodecyl diphenyl oxide disulfonate, sulfo-succinic acid alkyl phenol ether ester sodium salt; Described nonionogenic tenside is any one in polyoxyethylene nonylphenol ether class, polyoxyethylene octylphenol ether class, isomery carbon tridecanol polyoxyethylene ether, alkyl alcohol block polyether.
Preferably, described sticking power promotes that monomer is the combination of a kind of in Methacrylamide ethyl ethylene-urea, nitrogen heterocyclic methacrylic ester or two kinds.
Preferably, the cross-linking monomer in described mixture A is any one in N hydroxymethyl acrylamide, N-isobutoxy methylene radical acrylamide; Or be the combination of diacetone-acryloamide(DAA) and adipic acid dihydrazide; Or be the combination of acetoacetoxyethyl (methyl) acrylate and diamines.
When cross-linking monomer is the combination of diacetone-acryloamide(DAA) and adipic acid dihydrazide, wherein, diacetone-acryloamide(DAA) consumption accounts for the 0.5%-1% of emulsion monomer gross weight, and adipic acid dihydrazide accounts for the 40%-50% of diacetone-acryloamide(DAA) consumption.
When cross-linking monomer is the combination of acetoacetoxyethyl (methyl) acrylate and diamines, wherein, acetoacetoxyethyl (methyl) acrylate consumption accounts for the 0.3%-0.8% of emulsion monomer gross weight, and diamines accounts for the 50%-60% of acetoacetoxyethyl (methyl) acrylate consumption.
Preferably, described functional acrylic monomer is one or more the combination in vinylformic acid, methacrylic acid, methylene-succinic acid, monobutyl itaconate.
Preferably, the soft monomer in described mixture A is the combination of any one or two kinds of in methyl acrylate, ethyl propenoate, Hydroxyethyl acrylate, Propylene glycol monoacrylate, and described hard monomer is methyl methacrylate.
Preferably, the cross-linking monomer in described mixture B is any one in vinylformic acid Bicvclopentyl ester, ethylene glycol bisthioglycolate (methyl) acrylate; Or be the combination of acetoacetoxyethyl (methyl) acrylate and diamines.
Preferably, the soft monomer in described mixture B is the combination of any one or 2 ~ 3 kinds in methyl acrylate, ethyl propenoate, Hydroxyethyl acrylate, Propylene glycol monoacrylate, butyl acrylate, (methyl) Isooctyl acrylate monomer; Described hard monomer is the combination of any one or more in methyl methacrylate, (methyl) isobornyl acrylate, vinylbenzene.
Another object of the present invention is to the preparation method of openly a kind of above-mentioned Emulsion acrylic resin for aqueous ink used for plastic, comprise the following steps:
(1) component each in mixture A mixed and stirs, preparing pre-emulsion A, for subsequent use;
(2) component each in mixture B mixed and stirs, preparing mix monomer B, for subsequent use;
(3) initiator one to be dissolved in suitable quantity of water and to pour reactor into, being heated to 80 DEG C ~ 85 DEG C; Pre-emulsion A is added drop-wise in reactor, controls to drip off at 2h ~ 2.5h, drip off rear insulation 0.5h ~ 1h, in reactor, add that to account for functional Acrylic Acid Monomer mass percent be the ammoniacal liquor of 80%-120%, and be incubated 10min ~ 15min;
(4) be dissolved in after in suitable quantity of water by initiator two and add reactor, drip mix monomer B, control to drip off at 2h ~ 2.5h, insulation 1h ~ 1.5h, is then cooled to room temperature, discharging.
When cross-linking monomer is two component, a kind of function monomer of polymerizability and the combination of corresponding linking agent, as the combination of diacetone-acryloamide(DAA) and adipic acid dihydrazide, or the combination of acetoacetoxyethyl (methyl) acrylate and diamines.Wherein, the function monomer (diacetone-acryloamide(DAA) or acetoacetoxyethyl (methyl) acrylate) of polymerizability can participate in polymerization, corresponding linking agent (adipic acid dihydrazide or diamines) is then the material of band bifunctional, added and the corresponding function monomer generation chemical reaction that take part in polymerization by the later stage, play crosslinked action, make emulsion possess stronger water resisting property and combined strength bination.
In step (1), when in mixture A, cross-linking system is two-pack, the function monomer (diacetone-acryloamide(DAA) or acetoacetoxyethyl (methyl) acrylate) of wherein polymerizability is mixed with each component in mixture A, prepare pre-emulsion A, for subsequent use.The corresponding linking agent (adipic acid dihydrazide or diamines) of this combination then added in reaction solution before step (4) discharging, after stirring 15min, completed crosslinked.
In step (2), when in mixture B, cross-linking system is two-pack, the function monomer (diacetone-acryloamide(DAA) or acetoacetoxyethyl (methyl) acrylate) of wherein polymerizability is mixed with each component in mixture B, prepare mix monomer B, for subsequent use.The corresponding linking agent (adipic acid dihydrazide or diamines) of this combination then added in reaction solution before step (4) discharging, after stirring 15min, completed crosslinked.
Wherein, the mass concentration of ammoniacal liquor is 25%.
Compared with prior art, beneficial effect of the present invention is as follows:
Preparation technology of the present invention is relatively simple, and controllability is strong, the good emulsion stability prepared, low bubble.In emulsion preparation process, monomer is promoted by introducing the sticking power that can provide hydrogen bond and intermolecular reactive force, and this function monomer has the emulsion particle structure of improvement system, reduce emulsion interface tension force and effective infiltrate a color stuffing material and by the characteristic on adhering substrate surface, thus giving sticking power and the printing performance of emulsion excellence.Meanwhile, in this emulsion, introduce a certain amount of cross-linking monomer, effectively improve the water resisting property of emulsion.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated:
Embodiment 1
The obtained compound emulsifying agent aqueous solution in the water of 100g will be dissolved under the isomery carbon tridecanol polyoxyethylene ether strong stirring of 1g polyethenoxy ether sodium sulfate and 2g, take 80g methyl acrylate, 30g methyl methacrylate, 40g methacrylic acid, 3g N-isobutoxy methylene radical acrylamide, 15g Methacrylamide ethyl ethylene-urea pour in the compound emulsifying agent aqueous solution after mixing, strong stirring 15min, obtained pre-emulsion A, for subsequent use.
Take 150g butyl acrylate, after 90g methyl methacrylate, 3.5g vinylformic acid Bicvclopentyl ester mix, obtained monomer mixture B, for subsequent use.
1.5g ammonium persulfate is dissolved in 400g water, pours in reactor and be heated to 83 DEG C while stirring.Then drip pre-emulsion A while stirring, control to drip off at about 2h.After dripping off, insulation 1h.Then, add 40g ammoniacal liquor (mass concentration is 25%) in reactor, insulation 15min.
2.6g ammonium persulfate is dissolved in 40g water, pours in reactor, and drip monomer mixture B, control to drip off at about 2h.After dripping off, insulation 1h, be cooled to less than 40 DEG C, discharging can obtain target emulsion.
Embodiment 2
The obtained compound emulsifying agent aqueous solution in the water of 100g is dissolved under 1g being gathered the isomery carbon tridecanol polyoxyethylene ether strong stirring of branched dodecylbenzene sulfonic acid sodium and 1.5g, take 60g methyl acrylate, 15g Hydroxyethyl acrylate, 20g methyl methacrylate, 40g methacrylic acid, 3.0g N hydroxymethyl acrylamide, 15g nitrogen heterocyclic methacrylic ester pour in the compound emulsifying agent aqueous solution after mixing, strong stirring 15min, obtained pre-emulsion A, for subsequent use.
Take 130g butyl acrylate, 70g methyl methacrylate, 40g vinylbenzene, 3g ethylene glycol bisthioglycolate (methyl) crylic acid ester mixture evenly after, obtained monomer mixture B, for subsequent use.
1.5g ammonium persulfate is dissolved in 400g water, pours in reactor and be heated to 83 DEG C while stirring.Then drip pre-emulsion A while stirring, control to drip off at about 2h.After dripping off, insulation 1h.Then, add 43g ammoniacal liquor (mass concentration is 25%) in reactor, insulation 15min.
2.8g ammonium persulfate is dissolved in 40g water, pours in reactor, and drip monomer mixture B, control to drip off at about 2h.After dripping off, insulation 1h, be cooled to less than 40 DEG C, discharging can obtain target emulsion.
Embodiment 3
The obtained compound emulsifying agent aqueous solution in the water of 100g will be dissolved under the isomery carbon tridecanol polyoxyethylene ether strong stirring of 1g branched dodecyl diphenyl oxide disulfonate and 1.8g, take 40g ethyl propenoate, 25g Hydroxyethyl acrylate, 20g methyl methacrylate, 40g methacrylic acid, 5g diacetone-acryloamide(DAA), 15g nitrogen heterocyclic methacrylic ester pour in the compound emulsifying agent aqueous solution after mixing, strong stirring 15min, obtained pre-emulsion A, for subsequent use.
Take 180g butyl acrylate, 40g methyl methacrylate, 30g isobornyl acrylate, 3.5g vinylformic acid Bicvclopentyl ester, after mixing, obtained monomer mixture B, for subsequent use.
1.4g ammonium persulfate is dissolved in 400g water, pours in reactor and be heated to 83 DEG C while stirring.Then drip pre-emulsion A while stirring, control to drip off at about 2h.After dripping off, insulation 1h.Then, add 43g ammoniacal liquor (mass concentration is 25%) in reactor, insulation 15min.
3.0g ammonium persulfate is dissolved in 40g water, pours in reactor, and drip monomer mixture B, control to drip off at about 2h.After dripping off, insulation 1h, be cooled to less than 40 DEG C and go out, then add 2.5g adipic acid dihydrazide, then after stirring 15min, discharging can obtain target emulsion.
Embodiment 4
The obtained compound emulsifying agent aqueous solution in the water of 100g is dissolved under 1g being gathered the polyoxyethylene nonylphenol ether strong stirring of branched dodecylbenzene sulfonic acid sodium and 1.5g, take 30g methyl acrylate, 25g Propylene glycol monoacrylate, 40g methyl methacrylate, 45g monobutyl itaconate, 5g diacetone-acryloamide(DAA), 15g Methacrylamide ethyl ethylene-urea pour in the compound emulsifying agent aqueous solution after mixing, strong stirring 15min, obtained pre-emulsion A, for subsequent use.
Take 200g butyl acrylate, 40g isobornyl acrylate, 3g ethylene glycol bisthioglycolate (methyl) acrylate, after mixing, obtained monomer mixture B, for subsequent use.
1.5g ammonium persulfate is dissolved in 400g water, pours in reactor and be heated to 83 DEG C while stirring.Then drip pre-emulsion A while stirring, control to drip off at about 2h.After dripping off, insulation 1h.Then, add 43g ammoniacal liquor (mass concentration is 25%) in reactor, insulation 15min.
2.8g ammonium persulfate is dissolved in 40g water, pours in reactor, and drip monomer mixture B, control to drip off at about 2h.After dripping off, insulation 1h, be cooled to less than 40 DEG C and go out, then add 2.5g adipic acid dihydrazide, then after stirring 15min, discharging can obtain target emulsion.
Embodiment 5
The obtained compound emulsifying agent aqueous solution in the water of 100g will be dissolved under the polyoxyethylene nonylphenol ether strong stirring of 1g polyethenoxy ether sodium sulfate and 2g, take 60g methyl acrylate, 35g ethyl propenoate, 40g methyl methacrylate, 40g methacrylic acid, 3g N-isobutoxy methylene radical acrylamide, 15g nitrogen heterocyclic methacrylic ester pour in the compound emulsifying agent aqueous solution after mixing, strong stirring 15min, obtained pre-emulsion A, for subsequent use.
Take 120g butyl acrylate, 40g isobornyl acrylate, 30g vinylbenzene, 1.3g acetoacetoxyethyl (methyl) acrylate, after mixing, obtained monomer mixture B, for subsequent use.
1.8g ammonium persulfate is dissolved in 400g water, pours in reactor and be heated to 83 DEG C while stirring.Then drip pre-emulsion A while stirring, control to drip off at about 2h.After dripping off, insulation 1h.Then, add 40g ammoniacal liquor (mass concentration is 25%) in reactor, insulation 15min.
2.2g ammonium persulfate is dissolved in 40g water, pours in reactor, and drip monomer mixture B, control to drip off at about 2h.After dripping off, insulation 1h, be cooled to less than 40 DEG C and go out, then add 0.7g diamines, then after stirring 15min, discharging can obtain target emulsion.
The TLAY1 quick-dry type aqueous color paste that the emulsion prepared by above-described embodiment 1-5 is produced with Guangdong Sky Dragon Printing Ink Group Co., Ltd. successively, and add appropriate ethanol and prepare corresponding aqueous ink used for plastic 1-5.And to this aqueous ink used for plastic be applied to respectively plastic basis material table print printing and composite membrane printing carry out a series of performance test, its result is as following table:
Table 1 aqueous ink used for plastic 1-5 performance test table
As can be seen from the above table, emulsion 1-5 of the present invention prepares the aqueous ink used for plastic 1-5 obtained and is applied on plastic basis material and shows: quick-drying, anti-sticky, water resisting property is good, strong adhesion, wet-rub resistance can the printing performances of excellent, stronger combined strength bination and excellence.
In addition, with the addition of ethanol in proper amount during emulsion of the present invention modulation aqueous ink used for plastic, possess excellent alcohols consistency, meet alcohols not breakdown of emulsion, not thickening, easily rush rare.
To sum up, the emulsion excellent combination property that the present invention produces, makes it to be applied to the printing effect that printing effect that plastic basis material printing shows and solvent-borne type ink used for plastic show suitable.
Only as described above, be only the preferred embodiment of the present invention, when can not limit the scope of the present invention with this, namely generally according to equivalence change simple done by the content described in the claims in the present invention and specification sheets and modification, be all still covered by the claims of the invention.In addition, summary part and title are only used to the use of auxiliary patent document search, are not used for the interest field of restriction the present invention.
Claims (10)
1. for an Emulsion acrylic resin for aqueous ink used for plastic, it is characterized in that, comprise mixture A, mixture B, initiator one and initiator two,
Described mixture A comprises following component: the moon/non-composite emulsifying agent accounting for emulsion monomer quality total amount 0.5% ~ 1.0%, the sticking power accounting for emulsion monomer quality total amount 1% ~ 5% promote monomer, account for the cross-linking monomer of mixture A monomer mass total amount 1% ~ 8%, account for the functional acrylic monomer of emulsion monomer quality total amount 8% ~ 15%, account for soft, the hard monomer of emulsion monomer quality total amount 18% ~ 40% and appropriate water, and wherein the second-order transition temperature of soft or hard monomer is at 5 DEG C ~ 25 DEG C;
Initiator one: account for mixture A monomer mass total amount 0.7% ~ 1.0%;
Described mixture B is 35% ~ 65% of emulsion monomer quality total amount, comprise following component: account for soft, the hard monomer of mixture B monomer mass total amount 98.5% ~ 99.5% and account for the cross-linking monomer of mixture B monomer mass total amount 0.5% ~ 1.5%, the second-order transition temperature of soft or hard monomer is at 0 DEG C ~ 40 DEG C;
Initiator two: account for mixture B monomer mass total amount 0.8% ~ 1.2%;
Described emulsion monomer comprises sticking power and promotes monomer, cross-linking monomer, functional acrylic monomer, soft monomer, hard monomer.
2. a kind of Emulsion acrylic resin for aqueous ink used for plastic according to claim 1, it is characterized in that, described the moon/non-composite emulsifying agent is undertaken composite by anion surfactant and nonionogenic tenside, and the mass ratio of described anion surfactant and nonionogenic tenside is 1/2 ~ 1/1.5.
3. a kind of Emulsion acrylic resin for aqueous ink used for plastic according to claim 2, it is characterized in that, described anion surfactant is any one in sodium lauryl sulphate, branched dodecylbenzene sulfonic acid sodium, polyethenoxy ether sodium sulfate, branched dodecyl diphenyl oxide disulfonate, sulfo-succinic acid alkyl phenol ether ester sodium salt; Described nonionogenic tenside is any one in polyoxyethylene nonylphenol ether class, polyoxyethylene octylphenol ether class, isomery carbon tridecanol polyoxyethylene ether, alkyl alcohol block polyether.
4. a kind of Emulsion acrylic resin for aqueous ink used for plastic according to claim 1, is characterized in that, described sticking power promotes that monomer is the combination of a kind of in Methacrylamide ethyl ethylene-urea, nitrogen heterocyclic methacrylic ester or two kinds.
5. a kind of Emulsion acrylic resin for aqueous ink used for plastic according to claim 1, is characterized in that, the cross-linking monomer in described mixture A is any one in N hydroxymethyl acrylamide, N-isobutoxy methylene radical acrylamide; Or be the combination of diacetone-acryloamide(DAA) and adipic acid dihydrazide; Or be the combination of acetoacetoxyethyl (methyl) acrylate and diamines.
6. a kind of Emulsion acrylic resin for aqueous ink used for plastic according to claim 1, it is characterized in that, described functional acrylic monomer is one or more the combination in vinylformic acid, methacrylic acid, methylene-succinic acid, monobutyl itaconate.
7. a kind of Emulsion acrylic resin for aqueous ink used for plastic according to claim 1, it is characterized in that, soft monomer in described mixture A is the combination of any one or two kinds of in methyl acrylate, ethyl propenoate, Hydroxyethyl acrylate, Propylene glycol monoacrylate, and described hard monomer is methyl methacrylate.
8. a kind of Emulsion acrylic resin for aqueous ink used for plastic according to claim 1, is characterized in that, the cross-linking monomer in described mixture B is any one in vinylformic acid Bicvclopentyl ester, ethylene glycol bisthioglycolate (methyl) acrylate; Or be the combination of acetoacetoxyethyl (methyl) acrylate and diamines.
9. a kind of Emulsion acrylic resin for aqueous ink used for plastic according to claim 1, it is characterized in that, the soft monomer in described mixture B is the combination of any one or 2 ~ 3 kinds in methyl acrylate, ethyl propenoate, Hydroxyethyl acrylate, Propylene glycol monoacrylate, butyl acrylate, (methyl) Isooctyl acrylate monomer; Described hard monomer is the combination of any one or more in methyl methacrylate, (methyl) isobornyl acrylate, vinylbenzene.
10. a preparation method for a kind of Emulsion acrylic resin for aqueous ink used for plastic described in any one of claim 1 ~ 9, is characterized in that, comprise the following steps:
(1) component each in mixture A mixed and stirs, preparing pre-emulsion A, for subsequent use;
(2) component each in mixture B mixed and stirs, preparing mix monomer B, for subsequent use;
(3) initiator one to be dissolved in suitable quantity of water and to pour reactor into, being heated to 80 DEG C ~ 85 DEG C; Pre-emulsion A is added drop-wise in reactor, controls to drip off at 2h ~ 2.5h, drip off rear insulation 0.5h ~ 1h, in reactor, add that to account for functional Acrylic Acid Monomer mass percent be the ammoniacal liquor of 80%-120%, and be incubated 10min ~ 15min;
(4) initiator two is dissolved in after in suitable quantity of water adds reactor, drip mix monomer B, control to drip off at 2h ~ 2.5h, insulation 1h ~ 1.5h, discharging.
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