CN103304719B - Acrylic emulsion and preparation method and application in waterborne polyvinyl chloride (PVC) wallpaper ink thereof - Google Patents
Acrylic emulsion and preparation method and application in waterborne polyvinyl chloride (PVC) wallpaper ink thereof Download PDFInfo
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Abstract
The invention relates to the technical field of water-based ink and discloses acrylic emulsion. The acrylic emulsion comprises a first component, a second component and water; the acrylic emulsion comprises the following components in percentage by weight: the first component comprising 0-5 percent of emulsifier, 0-20 percent of styrene, 0-5 percent of cross-linking monomer and 10-40 percent of acrylate polymerization monomer; the second component comprising 5-15 percent of protection glue and 0.1-5 percent of initiator; the balance of water. The acrylic emulsion is prepared by the following steps: (1) uniformly mixing each component in the first component, thereby obtaining a solution A; (2) adding water into a reaction container, raising the temperature to be 75-95 DEG C, adding the protection glue, and stirring until the mixture is dissolved; (3) simultaneously dripping the solution A and the initiator into the reaction container, finishing dripping at a constant speed within 2-2.5 hours, and keeping the temperature for 30 minutes after dripping is finished; (4) cooling and discharging. The acrylic emulsion is high-temperature-resistant, has excellent adhesion force to polyvinyl chloride (PVC), does not contain harmful alcohol solvents and can be widely applied to the PVC wallpaper ink.
Description
Technical field
The present invention relates to water color ink technical field, specifically a kind of ACRYLIC EMULSION and preparation method thereof and the application in water-based PVC wallpaper ink.
Background technology
The wallpaper that present China produces can be divided into paper substrate paper wallpaper by material, PVC wallpaper, fabric side wallpaper, natural materials surface wallpaper, sand surface wallpaper, diatomite wallpaper, non-woven fabrics wallpaper.PVC wallpaper is base material with paper, take PVC as surface layer, and carries out Lacquer finish to PVC top layer and close, and then processes embossing printing etc. and carries out decoration to PVC wallpaper.PVC material in wallpaper printing is as a kind of non-absorbent material, mostly solvent type ink is used when printing, the volatilization of its solvent not only can cause healthy infringement to on-the-spot press operator in printing process, wallpaper is decorated in family by people, and residual solvent volatilization wherein also can cause damage to the health of kinsfolk.
Although existing acrylic emulsion PVC wallpaper gloss oil is water-based system, VOC content is lower, substantially meets environmental requirement, and the allotment of most water color ink still adds harmful alcoholic solvents such as a large amount of Virahols, still can cause certain harm to human body.Existing emulsion and PVC wallpaper ink hot sticky cold crisp simultaneously, resistance to elevated temperatures is not enough to meet the not hot sticky requirement of embossing.
Summary of the invention
For above-mentioned Problems existing, provide a kind of aqueous acrylic emulsion, it containing harmful alcohols equal solvent, high temperature resistant, to PVC, there is excellent adhesive attraction.
Another object of the present invention is to the preparation method that aforesaid propylene yogurt liquid is provided.
A further object of the invention is to provide a kind of PVC wallpaper ink containing aforesaid propylene yogurt liquid.
The present invention for achieving the above object, takes following technical scheme to be achieved:
A kind of ACRYLIC EMULSION, comprise the first component, second component and water, the weight percent that each composition in described component accounts for described emulsion is: the first component: emulsifying agent 0 ~ 5%, vinylbenzene 0 ~ 20%, cross-linking monomer 0 ~ 5%, acrylic monomer 10 ~ 40%; Second component: protecting glue 5 ~ 15%, initiator 0.1 ~ 5%; Surplus is water.
Described emulsifying agent is formed by reactive emulsifier and anionic emulsifier interworking.Anionic emulsifier comprises carboxylate salt, sulfonate, sulfuric acid, phosphate ester salt, preferably uses alkyl diphenyl ether disulphonic acid sodium, Sodium dodecylbenzene sulfonate, sodium lauryl sulphate and alkylphenol polyoxyethylene vitriol; Reactive emulsifier comprises acrylamido sodium isopropyl xanthate, containing vinyl alcohol ether sulfate, containing vinyl alcohol ether sulfosuccinates sodium salt, vinyl ether hydroxy alkyl sulfonic acid sodium.Emulsifying agent in the present invention preferably adopts mass ratio to be that the alkylphenol polyoxyethylene vitriol of 1:1 and vinyl ether hydroxy alkyl sulfonic acid sodium interworking form.
Described cross-linking monomer is one or more the mixture in (methyl) Hydroxyethyl acrylate, (methyl) Propylene glycol monoacrylate, acrylamide, N hydroxymethyl acrylamide, N, N-diacetone-acryloamide(DAA), glycidyl methacrylate and phosphoric acid ester function monomer.
Described acrylic monomer, to refer in vinylformic acid, (methyl) vinylformic acid, acrylate or (methyl) acrylate more than one mixture.Preferably, acrylic monomer is more than one mixture in vinylformic acid, (methyl) vinylformic acid, (methyl) methyl acrylate, (methyl) ethyl propenoate, (methyl) butyl acrylate, (methyl) Isooctyl acrylate monomer and isobornyl methacrylate.More preferably, acrylic monomer is more than one mixture in (methyl) vinylformic acid, butyl acrylate, Isooctyl acrylate monomer, (methyl) methyl acrylate.
Described protecting glue is any one in polyvinyl alcohol, styrene-maleic anhydride copolymer, acrylate copolymer and acrylic-styrene copolymer.The present invention preferably uses acrylate copolymer or acrylic-styrene copolymer.
Described initiator is any one in inorganic peroxide initiator, organic peroxide evocating agent, azo-initiator and redox type initiators.Conventional inorganic peroxide initiator has Potassium Persulphate, ammonium persulphate; Conventional organic peroxide evocating agent has benzoyl peroxide, tertbutyl peroxide; Conventional azo-initiator then has Diisopropyl azodicarboxylate; Initiator system of ammonium persulfate of the present invention, Potassium Persulphate are as initiator.
The Tg of described ACRYLIC EMULSION is 20 DEG C ~ 80 DEG C, can the high temperature of resistance to 220 DEG C, has excellent adhesive attraction to PVC base.
Aqueous acrylic emulsion in the present invention synthesizes especially for the application of PVC wallpaper ink, with common water borne ACRYLIC EMULSION unlike introducing phosphinylidyne-containing amine group and the special cross-linking monomer containing vinyl phosphate, adding of these special cross-linking monomers, improve the thermotolerance of emulsion and the sticking power to PVC base.
Another technical scheme of the present invention is as follows: a kind of preparation method of aforesaid propylene yogurt liquid, comprises the following steps:
(1) composition each in the first component is mixed, obtain solution A;
(2) in reaction vessel, add water, be warming up to 75 DEG C ~ 95 DEG C, add protecting glue, high-speed stirring is to dissolving completely;
(3) in reaction vessel, drip solution A and initiator simultaneously, at the uniform velocity drip in 2 ~ 2.5h, drip off insulation 30min;
(4) lower the temperature, discharging.
Preferably first be cooled to 70 DEG C in step (4), add the removing residual monomers such as tertbutyl peroxide, and then lower the temperature, discharging.
Another technical scheme of the present invention is as follows: a kind of water-based PVC wallpaper ink containing aforesaid propylene yogurt liquid, comprise the following component of mass percent: ethanol 0 ~ 10%, ACRYLIC EMULSION 30% ~ 70%, aqueous color paste 10% ~ 50%, wetting agent 0.5% ~ 3%, flow agent 0.5% ~ 3%, film coalescence aid 0.5% ~ 3%, defoamer 0.1% ~ 1%, wear-resistant scraping-resistant agent 0.5% ~ 5%, surplus is water.
Described aqueous color paste is water soluble acrylic acid ester solution or waterborne polyester solution, the environmental-friendly pigment of 10 ~ 50%, the water of 10% ~ 40% of 10% ~ 60% by mass percent, and environmental protection dispersion agent, 0.1% ~ 1% defoamer of 0 ~ 5% grind and form in sand mill.
Described wetting agent is nonionogenic tenside or polyether siloxane copolymer.The present invention is preferably acetylenic diols nonionogenic tenside.
Described flow agent is any one in fluorin modified crylic acid ester copolymer, polyether modified siloxane and phosphate modified acrylic copolymer.The present invention preferably adopts polyether modified siloxane as flow agent.
Described film coalescence aid is any one in propylene glycol monomethyl ether, dipropylene glycol methyl ether, propandiol butyl ether, Trivalin SF, diethylene glycol monobutyl ether, butyl and dipropylene.The preferred butyl of the present invention or dipropylene are as film coalescence aid.
Described defoamer is any one in polysiloxane, mineral oil, polyethers, higher alcohols and vegetables oil.The present invention preferably adopts polyethers defoamer.
Described wear-resistant scraping-resistant agent is one or more the mixture in polyethylene wax slurry, tetrafluoroethylene wax slurry, organic silicon surfactant.The tetrafluoroethylene wax that the preferred fusing point of the present invention is higher is starched as anti-wear agent.
Beneficial effect of the present invention is as follows: the aqueous acrylic emulsion synthetic method in the present invention is consistent with prior synthesizing method, easy and simple to handle, is easy to control, and the product emulsion of synthesis is stablized.Aqueous acrylic emulsion of the present invention synthesizes especially for the application of PVC wallpaper ink, with common water borne ACRYLIC EMULSION unlike introducing phosphinylidyne-containing amine group and the special cross-linking monomer containing vinyl phosphate, adding of these special cross-linking monomers, improve the thermotolerance of emulsion and the sticking power to PVC base, simultaneously amide group and phosphate-basedly very easily occurs to be cross-linked after drying loses amino with the carboxyl contained by acrylic monomer, emulsion film forming after crosslinked is good, transparency is high, attachment fastness is good, water resisting property is good, be applied in PVC wallpaper ink and make it possess corresponding advantage.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment 1 ~ 5:
According to formula preparation ACRYLIC EMULSION described in table 1:
Table 1 ACRYLIC EMULSION formula table (parts by weight)
In embodiment 1 ~ 5, emulsifying agent is formed by reactive emulsifier and anionic emulsifier interworking.Anionic emulsifier comprises carboxylate salt, sulfonate, sulfuric acid, phosphate ester salt, preferably uses alkyl diphenyl ether disulphonic acid sodium, Sodium dodecylbenzene sulfonate, sodium lauryl sulphate and alkylphenol polyoxyethylene vitriol; Reactive emulsifier comprises acrylamido sodium isopropyl xanthate, containing vinyl alcohol ether sulfate, containing vinyl alcohol ether sulfosuccinates sodium salt, vinyl ether hydroxy alkyl sulfonic acid sodium.Preferred employing mass ratio is that the alkylphenol polyoxyethylene vitriol of 1:1 and vinyl ether hydroxy alkyl sulfonic acid sodium interworking form.
Cross-linking monomer is one or more the mixture in (methyl) Hydroxyethyl acrylate, (methyl) Propylene glycol monoacrylate, acrylamide, N hydroxymethyl acrylamide, N, N-diacetone-acryloamide(DAA), glycidyl methacrylate and phosphoric acid ester function monomer.
Acrylic monomer, to refer in vinylformic acid, (methyl) vinylformic acid, acrylate or (methyl) acrylate more than one mixture.Preferably, acrylic monomer is more than one mixture in vinylformic acid, (methyl) vinylformic acid, (methyl) methyl acrylate, (methyl) ethyl propenoate, (methyl) butyl acrylate, (methyl) Isooctyl acrylate monomer and isobornyl methacrylate.More preferably, acrylic monomer is more than one mixture in (methyl) vinylformic acid, butyl acrylate, Isooctyl acrylate monomer, (methyl) methyl acrylate.
Protecting glue is any one in polyvinyl alcohol, styrene-maleic anhydride copolymer, acrylate copolymer and acrylic-styrene copolymer.Preferred use acrylate copolymer or acrylic-styrene copolymer.
Initiator is any one in inorganic peroxide initiator, organic peroxide evocating agent, azo-initiator and redox type initiators.Conventional inorganic peroxide initiator has Potassium Persulphate, ammonium persulphate; Conventional organic peroxide evocating agent has benzoyl peroxide, tertbutyl peroxide; Conventional azo-initiator then has Diisopropyl azodicarboxylate; Initiator system of ammonium persulfate, Potassium Persulphate are as initiator.
Embodiment 6
The preparation method of the ACRYLIC EMULSION that table 1 provides, comprises the following steps:
(1) each composition of the first component in embodiment 1 ~ 5 is mixed in header tank, obtain solution A;
(2) in the four-hole boiling flask that heating jacket, stirring arm, condenser, header tank are housed, add water, start stirring, be warming up to 75 DEG C, add protecting glue, high-speed stirring is to dissolving completely;
(3) in four-hole boiling flask, drip solution A and initiator simultaneously, at the uniform velocity drip in 2h, drip off insulation 30min;
(4) lower the temperature, discharging.
Preferably first be cooled to 70 DEG C in step (4), add appropriate tertbutyl peroxide removing residual monomer, and then lower the temperature, discharging.
The Tg of obtained ACRYLIC EMULSION is 20 DEG C ~ 80 DEG C, can the high temperature of resistance to 220 DEG C, and have excellent adhesive attraction to PVC base, good film-forming property, transparency are high, water resisting property is good.
Embodiment 7
The preparation method of the ACRYLIC EMULSION that table 1 provides, comprises the following steps:
(1) each composition of the first component in embodiment 1 ~ 5 is mixed in header tank, obtain solution A;
(2) in the four-hole boiling flask that heating jacket, stirring arm, condenser, header tank are housed, add water, start stirring, be warming up to 80 DEG C, add protecting glue, high-speed stirring is to dissolving completely;
(3) in four-hole boiling flask, drip solution A and initiator simultaneously, at the uniform velocity drip in 2.5h, drip off insulation 30min;
(4) lower the temperature, discharging.
Preferably first be cooled to 70 DEG C in step (4), add appropriate tertbutyl peroxide removing residual monomer, and then lower the temperature, discharging.
The Tg of obtained ACRYLIC EMULSION is 20 DEG C ~ 80 DEG C, can the high temperature of resistance to 220 DEG C, and have excellent adhesive attraction to PVC base, good film-forming property, transparency are high, water resisting property is good.
Embodiment 8
The preparation method of the ACRYLIC EMULSION that table 1 provides, comprises the following steps:
(1) each composition of the first component in embodiment 1 ~ 5 is mixed in header tank, obtain solution A;
(2) in the four-hole boiling flask that heating jacket, stirring arm, condenser, header tank are housed, add water, start stirring, be warming up to 95 DEG C, add protecting glue, high-speed stirring is to dissolving completely;
(3) in four-hole boiling flask, drip solution A and initiator simultaneously, at the uniform velocity drip in 2.2h, drip off insulation 30min;
(4) lower the temperature, discharging.
Preferably first be cooled to 70 DEG C in step (4), add appropriate tertbutyl peroxide removing residual monomer, and then lower the temperature, discharging.
The Tg of obtained ACRYLIC EMULSION is 20 DEG C ~ 80 DEG C, can the high temperature of resistance to 220 DEG C, and have excellent adhesive attraction to PVC base, good film-forming property, transparency are high, water resisting property is good.
Embodiment 9 ~ 13
According to formula preparation water-based PVC wallpaper ink described in table 2:
Table 2 water-based PVC wallpaper ink formulations table (parts by weight)
ACRYLIC EMULSION in embodiment 9 ~ 13 is prepared from by embodiment 6 ~ 8.
Ethanol is the solvent of nonessential interpolation, only provides quick-drying and a little levelling effect, for national legislation allows the non-toxicity solvent of interpolation.
Wetting agent is nonionogenic tenside or polyether siloxane copolymer.Be preferably acetylenic diols nonionogenic tenside.
Flow agent is any one in fluorin modified crylic acid ester copolymer, polyether modified siloxane and phosphate modified acrylic copolymer.Preferred employing polyether modified siloxane is as flow agent.
Film coalescence aid is any one in propylene glycol monomethyl ether, dipropylene glycol methyl ether, propandiol butyl ether, Trivalin SF, diethylene glycol monobutyl ether, butyl and dipropylene.Preferred butyl or dipropylene are as film coalescence aid.
Defoamer is any one in polysiloxane, mineral oil, polyethers, higher alcohols and vegetables oil.Preferred employing polyethers defoamer.
Wear-resistant scraping-resistant agent is one or more the mixture in polyethylene wax slurry, tetrafluoroethylene wax slurry, organic silicon surfactant.The tetrafluoroethylene wax that preferred fusing point is higher is starched as anti-wear agent.
Aqueous color paste is water soluble acrylic acid ester solution or waterborne polyester solution, the environmental-friendly pigment of 10 ~ 50%, the water of 10% ~ 40% of 10% ~ 60% by mass percent, and environmental protection dispersion agent, 0.1% ~ 1% defoamer of 0 ~ 5% grind and form in sand mill.
Aqueous color paste can be prepared according to formula described in table 3:
Table 3 aqueous color paste formula table (parts by weight)
In iron flask by table 3 fill a prescription deployed after add granulated glass sphere by 1:1 weight, high speed dispersion 3 hours on wobbler, i.e. obtained aqueous color paste, mill base main performance index is in table 4:
Table 4 aqueous color paste performance table
ACRYLIC EMULSION in the mill base utilizing waterborne polyester solution to prepare and embodiment 9 ~ 13 stripping strength of arranging in pairs or groups can reach 100%, ACRYLIC EMULSION in the mill base utilizing water-borne acrylic resin solution to prepare and embodiment 9 ~ 13 stripping strength of arranging in pairs or groups is then 93%, has partial exfoliation.
Utilize mill base prepared by waterborne polyester solution, be prepared into water-based PVC wallpaper ink according to table 2 formula, as shown in table 5 with external product performance comparison:
Table 5 performance comparison table
The water-based PVC wallpaper ink good film-forming property made, transparency is high, attachment fastness good, water resisting property is good.
Above the technical scheme that the embodiment of the present invention provides is described in detail, apply specific case herein to set forth the principle of the embodiment of the present invention and embodiment, the explanation of above embodiment is only applicable to the principle helping to understand the embodiment of the present invention; Meanwhile, for one of ordinary skill in the art, according to the embodiment of the present invention, embodiment and range of application all will change, and in sum, this description should not be construed as limitation of the present invention.
Claims (5)
1. an ACRYLIC EMULSION, is characterized in that, comprises the first component, second component and water, the weight percent that each composition in described component accounts for described emulsion is: the first component: emulsifying agent 0 ~ 5%, vinylbenzene 0 ~ 20%, cross-linking monomer 0 ~ 5%, acrylic monomer 10 ~ 40%; Second component: protecting glue 5 ~ 15%, initiator 0.1 ~ 5%; Surplus is water;
Described emulsifying agent is that the alkylphenol polyoxyethylene vitriol of 1:1 and vinyl ether hydroxy alkyl sulfonic acid sodium interworking form by mass ratio;
Described cross-linking monomer is one or more the mixture in (methyl) Hydroxyethyl acrylate, (methyl) Propylene glycol monoacrylate, acrylamide, N hydroxymethyl acrylamide, N, N-diacetone-acryloamide(DAA), glycidyl methacrylate and phosphoric acid ester function monomer;
Described acrylic monomer is more than one mixture in (methyl) vinylformic acid, butyl acrylate, Isooctyl acrylate monomer, (methyl) methyl acrylate;
Described protecting glue is any one in polyvinyl alcohol, styrene-maleic anhydride copolymer, acrylate copolymer and acrylic-styrene copolymer;
Described initiator is ammonium persulphate or Potassium Persulphate.
2. a preparation method for ACRYLIC EMULSION according to claim 1, is characterized in that, comprises the following steps:
(1) composition each in the first component is mixed, obtain solution A;
(2) in reaction vessel, add water, be warming up to 75 DEG C ~ 95 DEG C, add protecting glue, high-speed stirring is to dissolving completely;
(3) in reaction vessel, drip solution A and initiator simultaneously, at the uniform velocity drip in 2 ~ 2.5h, drip off insulation 30min;
(4) lower the temperature, discharging.
3. the water-based PVC wallpaper ink containing ACRYLIC EMULSION according to claim 1, it is characterized in that, comprise the following component of mass percent: ethanol 0 ~ 10%, ACRYLIC EMULSION 30% ~ 70%, aqueous color paste 10% ~ 50%, wetting agent 0.5% ~ 3%, flow agent 0.5% ~ 3%, film coalescence aid 0.5% ~ 3%, defoamer 0.1% ~ 1%, wear-resistant scraping-resistant agent 0.5% ~ 5%, surplus is water.
4. water-based PVC wallpaper ink according to claim 3, it is characterized in that, described aqueous color paste is water soluble acrylic acid ester solution or waterborne polyester solution, the environmental-friendly pigment of 10 ~ 50%, the water of 10% ~ 40% of 10% ~ 60% by mass percent, and environmental protection dispersion agent, 0.1% ~ 1% defoamer of 0 ~ 5% grind and form in sand mill.
5. water-based PVC wallpaper ink according to claim 3, is characterized in that, described wetting agent is acetylenic diols nonionogenic tenside; Described flow agent is any one in fluorin modified crylic acid ester copolymer, polyether modified siloxane and phosphate modified acrylic copolymer; Described film coalescence aid is any one in propylene glycol monomethyl ether, dipropylene glycol methyl ether, propandiol butyl ether, Trivalin SF, diethylene glycol monobutyl ether, butyl and dipropylene; Described defoamer is any one in polysiloxane, mineral oil, polyethers, higher alcohols and vegetables oil; Described wear-resistant scraping-resistant agent is one or more the mixture in polyethylene wax slurry, tetrafluoroethylene wax slurry, organic silicon surfactant.
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Effective date of registration: 20170713 Address after: 526108 Guangdong city of Zhaoqing Province Gaoyao district town of clay highway entrance Patentee after: Guangdong Tianlong Printing Ink Co., Ltd. Address before: 526108 Industrial Park, Zhaoqing, Guangdong Patentee before: Guangdong Sky Dragon Printing Ink Group Co., Ltd. |