CN101168650A - Single-component self-crosslink emulsion adhesive for dry type composite film and preparation method thereof - Google Patents
Single-component self-crosslink emulsion adhesive for dry type composite film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses single component self-cross linking emulsion tackiness agent used for dry type compound and the preparation method thereof. The invention has the preparation method as follows: firstly, part of aqueous medium, part of emulsifying agent, and part of initiating agent and baking soda are measured and added in a reactor, and are warmed up 70 to 85 DEG C; secondly, then hard monomer, soft monomer, (methyl) acrylic acid and cross linking monomer are mixed, and form pre-emulsion together with part of the emulsifying agent and water; thirdly, 1/10 pre-emulsion is added firstly to form assistant emulsion by reacting, and then the pre-emulsion and initiating agent aqueous solution are added synchronistically to perform reaction, the time lasts for 3 to 5 hours. The water emulsion tackiness agent obtained has good stability, and is free from poison and dissolving agent, and is favor of good health of a worker and environmental protection. A compound produced product obtained by utilizing the emulsion tackiness agent of the invention has the advantages that the ageing resistance is excellent, the viscous force is high, and the foaming is not existent during the impressing and sagging process, and the invention has wide application market.
Description
Technical field:
The invention belongs to the adhesive technology field, more specifically relate to a kind of single-component self-crosslink emulsion adhesive for dry type composite film and preparation method thereof.
Background technology
The dry type composite film method is present domestic the most frequently used film coating method, it is coating one deck tamanori on plastics film, remove solvent in the tamanori or water and drying through the dry drying tunnel evaporation of coating machine then, under the hot pressing state, bind again and become to answer the film product with paper printed matter.Printed matter through multiple film; because the much more surperficial thin and transparent plastics film of one deck; the level and smooth more light in surface; the glossiness and the fastness of printed matter have not only been improved; prolonged the work-ing life of printed matter, simultaneously plastics film plays provide protections such as waterproof, antifouling, wear-resisting, folding, resistance to chemical attack again.Therefore, the package printed matter behind the multiple film can significantly improve the class and the added value of commodity packaging.
Compound film adhesive be multiple membrane process key factor.Commercially available compound film adhesive mainly contains solvent-borne type and aqueous emulsion type two big classes.The solvent-type film-covered tackiness agent generally adopts cheap deleterious and volatile solvent, and this not only produces operator's health and poisons, and environment has also been caused severe contamination, and inflammable, explosive, be not easy to store and transportation, be faced with superseded now.The acrylic emulsion tackiness agent is dispersion medium with water, and eco-friendly demand has been complied with in production cost reduction on the one hand, safe in utilization on the other hand.Acrylic emulsion sticks with glue the existing commodity of agent as dry type composite film, but still has many weak points at present:
1) loss of properties on aging, it is low to hold viscous force, and stripping strength descends gradually in put procedure;
2) not good to the wettability of the low plastics film of surface energy;
3) bad with the consistency of printing-ink, ink transfer is not thorough when peeling off;
4) rate of drying is slower, can not high-speed coating;
5) multiple membrane product is prone to phenomenons such as foaming, explosion in impression, concavo-convex process.
In order to overcome the above-mentioned shortcoming of aqueous compound film adhesive, some improved linking agents have been developed in recent years, but as dispersed isocyanate, polyfunctional group azacyclopropane, polyfunctional group carbodiimide etc., make the performance of aqueous compound film adhesive be greatly improved, can match in excellence or beauty with the solvent-type film-covered tackiness agent substantially.But most of systems need the two-pack mode to store, and use inconvenient.
Summary of the invention:
The objective of the invention is to overcome the defective that prior art exists, a kind of single-component self-crosslink emulsion adhesive for dry type composite film is provided.The present invention is directed to the problems referred to above, in polymerization process, introduce the self-crosslinking group, obtain the monocomponent self-cross-linking acrylic emulsion, acrylic emulsion tackiness agent of a kind of excellent performance and preparation method thereof is provided for dry type composite film technology.Use multiple membrane product that this tackiness agent obtains have anti-old friend's voltinism can be excellent, hold the viscous force height, and in performances such as impression, concavo-convex process are non-foaming.
Another object of the present invention is to provide the preparation method of this single-component self-crosslink emulsion adhesive for dry type composite film.
For achieving the above object, the present invention has taked following technical scheme:
The present invention adopts seeded emulsion polymerization and pre-emulsification technology.The portion water medium that in the four-hole bottle that agitator, prolong, nitrogen protection and feeding device are housed, adds metering, partial emulsifier, part initiator and sodium bicarbonate, and be warming up to 65～80 ℃.Hard monomer, soft monomer, (methyl) vinylformic acid, cross-linking monomer are mixed and partial emulsifier and water formation pre-emulsion.Add earlier the reaction of part pre-emulsion and form seed emulsion, drip pre-emulsion and initiator solution then synchronously, the time is 3～5 hours, get final product single-component self-crosslink emulsion adhesive for dry type composite film.Its composition and parts by weight proportioning are as follows:
Hard monomer 10～25
Soft monomer 25～40
(methyl) vinylformic acid 0.5～2.0
Cross-linking monomer 0.5～3.0
Composite emulsifier 0.5～2.0
Initiator 0.25～0.5
Sodium bicarbonate 0.1～0.5
Functional agent 0.01～1.0
Water 45～55.
In technique scheme, it is pointed out that hard monomer is methyl methacrylate, cinnamic a kind or both and usefulness; Soft monomer is made up of 1～2 kind of monomer in ethyl propenoate, butyl acrylate, 2-EHA, the Jia Jibingxisuanyizhi, and based on butyl acrylate; A kind of in (methyl) vinylformic acid and the methacrylic acid; Initiator is a kind of in Potassium Persulphate and the ammonium persulphate; Composite emulsifier is made of anionic emulsifier and nonionic emulsifier, anionic emulsifier is a Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate, ethoxy alcohol sulfonic acid disodium succinate a kind of or a kind of with a mixture, nonionic emulsifying agent is Nonyl pheno (10～30) ether and octyl phenol polyoxy ethene (10～30) ether or its mixture, and the quality proportioning of anionic emulsifier and nonionic emulsifier is 2: 1～1: 2; Cross-linking monomer is a N hydroxymethyl acrylamide, glycidyl acrylate, glycidyl methacrylate, vinyltrimethoxy silane, vinyltriethoxysilane, vinyl silane triisopropoxide, a kind or 2 kinds of methacryloxypropyl three isopropoxy silane, functional agent is sulfo-succinic acid di-isooctyl sodium and non-silicone mineral oil.
Single-component self-crosslink emulsion adhesive for dry type composite film of the present invention and preparation method thereof may further comprise the steps:
(1) gets the emulsifying agent of composite emulsifier total amount 20～50% and the water of water inventory 10～30%, place pre-emulsion tank, hard monomer, soft monomer, (methyl) vinylformic acid is after cross-linking monomer mixes, slowly join and carry out emulsification in the pre-emulsion tank, emulsification times 30～60min, standby;
(2) add the water of water inventory 0～70%, the emulsifying agent of composite emulsifier total amount 0～50% in reactor, the initiator of initiator total amount 30～40%, sodium bicarbonate be as kettle base solution, stirs temperature of reaction kettle to 65～80 ℃ of raising simultaneously;
(3) add 10% pre-emulsion, in 65～80 ℃, be incubated then to blue light and occur;
(4) after insulation half an hour, the initiator of initiator total amount 60～70% is dissolved in the water of water inventory 5～20%, and with step (1) in the residue pre-emulsion drip simultaneously, the dropping time is 3～4h;
(5) be warming up to 85 ℃ at last, reaction 1～2h is cooled to room temperature, regulates the pH value, and adds functional agent.
The salient features of single-component self-crosslink emulsion adhesive for dry type composite film of the present invention is as follows:
Solid content: 45%～55%
PH value: 7.0～8.0
Viscosity: 100～300mPaS
Freeze-thaw stability: qualified
Stability in storage:＞6 months
Stripping strength:＞400N/m
Ratio of printing ink transfer: 100%
High low-temperature test: qualified
Impression, concavo-convex test: non-foaming
Compared with prior art, the present invention has following beneficial effect:
Single-component self-crosslink emulsion adhesive for dry type composite film solid content height provided by the invention, viscosity is low, and stability is high.Do not contain solvent, nontoxic, the healthy and environmental friendliness that helps the operator.Intensity was big when the multiple membrane product of using single-component self-crosslink emulsion adhesive for dry type composite film provided by the invention preparation was peeled off, printing ink ratio of printing ink transfer 100% has the ageing-resistant performance excellence, holds the viscous force height, and, has wide application market in performance such as impression, concavo-convex process be non-foaming.
Embodiment:
Below come by specific embodiment that the invention will be further described.
Embodiment 1:
In the 1000ml four-hole bottle of agitator, prolong, nitrogen protection and feeding device is housed; add deionized water 160g, Sodium dodecylbenzene sulfonate 1.0g, Nonyl pheno (20) ether 2.0g; with sodium bicarbonate 1.5g, Potassium Persulphate (KPS) 0.8g also heats up.Methyl methacrylate 75.0g, butyl acrylate 208.5g, vinylformic acid 6.0g and vinyltrimethoxy silane 4.5g are mixed.With N hydroxymethyl acrylamide 9.0g, Sodium dodecylbenzene sulfonate 1.0g, Nonyl pheno (20) ether 2.0g is dissolved in the 100.0g deionized water, slowly adds above-mentioned monomer mixture again and forms pre-emulsion.Add about 1/10 pre-emulsion earlier to reaction flask, 70 ℃ of reactions 0.5 hour.Be dissolved in KPS 1.6g in the 40g deionized water then and pre-emulsion drips synchronously, the time is 4.5 hours. be warming up to 90 ℃ at last, reacted 1.5 hours.Be cooled to below 50 ℃, regulate pH to 7.0 with ammoniacal liquor, add sulfo-succinic acid di-isooctyl sodium 1.2g and non-silicone mineral oil antifoam agent 0.6g then, product filters with 250 mesh filter screens.The solid content of gained emulsion adhesive is 50%, and viscosity is 240mPaS, freeze-thaw stability: qualified, and stability in storage:＞6 months.
Embodiment 2:
In the 1000ml four-hole bottle of agitator, prolong, nitrogen protection and feeding device is housed; add deionized water 160g, Sodium dodecylbenzene sulfonate 1.0g, Nonyl pheno (20) ether 2.0g; with sodium bicarbonate 1.5g, Potassium Persulphate (KPS) 0.8g also heats up.Vinylbenzene 75.0g, butyl acrylate 208.5g, vinylformic acid 6.0g and vinyltrimethoxy silane 4.5g are mixed.With N hydroxymethyl acrylamide 9.0g, Sodium dodecylbenzene sulfonate 1.0g, Nonyl pheno (20) ether 2.0g is dissolved in the 100.0g deionized water, slowly adds above-mentioned monomer mixture again and forms pre-emulsion.Add about 1/10 pre-emulsion earlier to four-hole bottle, 70 ℃ of reactions 0.5 hour.Be dissolved in KPS 1.6g in the 40g deionized water then and pre-emulsion drips synchronously, the time is 4.5 hours. be warming up to 90 ℃ at last, reacted 1.5 hours.Be cooled to below 50 ℃, regulate pH to 7.0 with ammoniacal liquor, add sulfo-succinic acid di-isooctyl sodium 1.2g and non-silicone mineral oil antifoam agent 0.6g then, product filters with 250 mesh filter screens.The solid content of gained emulsion adhesive is 50%, and viscosity is 230mPaS, freeze-thaw stability: qualified, and stability in storage:＞6 months.
Embodiment 3:
In the 1000ml four-hole bottle of agitator, prolong, nitrogen protection and feeding device is housed; add deionized water 160g, Sodium dodecylbenzene sulfonate 1.0g, Nonyl pheno (20) ether 2.0g; with sodium bicarbonate 1.5g, Potassium Persulphate (KPS) 0.8g also heats up.Vinylbenzene 75.0g, butyl acrylate 208.5g, vinylformic acid 6.0g and methacryloxypropyl three isopropoxy silane 4.5g are mixed.With N hydroxymethyl acrylamide 9.0g, Sodium dodecylbenzene sulfonate 1.0g, Nonyl pheno (20) ether 2.0g is dissolved in the 100.0g deionized water, slowly adds above-mentioned monomer mixture again and forms pre-emulsion.Add earlier about 1/10 pre-emulsion to four-hole bottle, reacted 0.5 hour at 70 ℃, be dissolved in KPS 1.6g in the 40g deionized water then and pre-emulsion drips synchronously, the time is 4.5 hours.Be warming up to 90 ℃ at last, reacted 1.5 hours.Be cooled to below 50 ℃, regulate pH to 7.0 with ammoniacal liquor, add sulfo-succinic acid di-isooctyl sodium 1.2g and non-silicone mineral oil antifoam agent 0.6g then, product filters with 250 mesh filter screens.The solid content of gained emulsion adhesive is 50%, and viscosity is 230mPaS, freeze-thaw stability: qualified, and stability in storage:＞6 months.
Embodiment 4:
In the 1000ml four-hole bottle of agitator, prolong, nitrogen protection and feeding device is housed; add deionized water 160g, Sodium dodecylbenzene sulfonate 1.0g, Nonyl pheno (20) ether 2.0g; with sodium bicarbonate 1.5g, Potassium Persulphate (KPS) 0.8g also heats up.Vinylbenzene 70.0g, ethyl propenoate 45.0g, butyl acrylate 168.5g, vinylformic acid 6.0g and glycidyl acrylate 4.5g are mixed.With N hydroxymethyl acrylamide 9.0g, Sodium dodecylbenzene sulfonate 1.0g, Nonyl pheno (20) ether 2.0g is dissolved in the 100.0g deionized water, slowly adds above-mentioned monomer mixture again and forms pre-emulsion.Add earlier about 1/10 pre-emulsion to four-hole bottle, reacted 0.5 hour at 70 ℃, be dissolved in KPS 1.6g in the 40g deionized water then and pre-emulsion drips synchronously, the time is 4.5 hours.Be warming up to 90 ℃ at last, reacted 1.5 hours.Be cooled to below 50 ℃, regulate pH to 7.0 with ammoniacal liquor, add sulfo-succinic acid di-isooctyl sodium 1.2g and non-silicone mineral oil antifoam agent 0.6g then, product filters with 250 mesh filter screens.The solid content of gained emulsion adhesive is 50%, and viscosity is 220mPaS, freeze-thaw stability: qualified, and stability in storage:＞6 months.
Embodiment 5:
In the 1000ml four-hole bottle of agitator, prolong, nitrogen protection and feeding device is housed; add deionized water 160g, disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate 1.0g, Nonyl pheno (20) ether 2.0g; with sodium bicarbonate 1.5g, Potassium Persulphate (KPS) 0.8g also heats up.Vinylbenzene 70.0g, ethyl propenoate 45.0g, butyl acrylate 168.5g, vinylformic acid 6.0g and glycidyl methacrylate 4.5g are mixed.With N hydroxymethyl acrylamide 9.0g, disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate 1.0g, Nonyl pheno (20) ether 2.0g is dissolved in the 100.0g deionized water, slowly adds above-mentioned monomer mixture again and forms pre-emulsion.Add earlier about 1/10 pre-emulsion to four-hole bottle, reacted 0.5 hour at 70 ℃, be dissolved in KPS 1.6g in the 40g deionized water then and pre-emulsion drips synchronously, the time is 4.5 hours.Be warming up to 90 ℃ at last, reacted 1.5 hours.Be cooled to below 50 ℃, regulate pH to 7.0 with ammoniacal liquor, add sulfo-succinic acid di-isooctyl sodium 1.2g and non-silicone mineral oil antifoam agent 0.6g then, product filters with 250 mesh filter screens.The solid content of gained emulsion adhesive is 50%, and viscosity is 210mPaS, freeze-thaw stability: qualified, and stability in storage:＞6 months.
Claims (10)
1. single-component self-crosslink emulsion adhesive for dry type composite film is characterized in that: the letex polymerization that its adopts seeded emulsion polymerization and pre-emulsification technology to carry out, and in parts by weight, it comprises the material of following component:
Hard monomer 10～25
Soft monomer 25～40
(methyl) vinylformic acid 0.5～2.0
Cross-linking monomer 0.5～3.0
Composite emulsifier 0.5～2.0
Initiator 0.25～0.5
Sodium bicarbonate 0.1～0.5
Functional agent 0.01～1.0
Water 45～55.
2. single-component self-crosslink emulsion adhesive for dry type composite film according to claim 1 is characterized in that described hard monomer is the mixture of one or both materials in methyl methacrylate and the vinylbenzene.
3. single-component self-crosslink emulsion adhesive for dry type composite film according to claim 1, it is characterized in that described soft monomer is made up of one or both monomers in ethyl propenoate, butyl acrylate, 2-EHA, butyl methacrylate, the Jia Jibingxisuanyizhi, and based on butyl acrylate.
4. single-component self-crosslink emulsion adhesive for dry type composite film according to claim 1 is characterized in that described (methyl) vinylformic acid is acrylic or methacrylic acid.
5. single-component self-crosslink emulsion adhesive for dry type composite film according to claim 1 is characterized in that described initiator is Potassium Persulphate or ammonium persulphate.
6. single-component self-crosslink emulsion adhesive for dry type composite film according to claim 1 is characterized in that described composite emulsifier is made of anionic emulsifier and nonionic emulsifier; Anionic emulsifier is a Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, and disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate, one or more mixtures of ethoxy alcohol sulfonic acid disodium succinate constitute; Nonionic emulsifying agent is Nonyl pheno (10～30) ether and octyl phenol polyoxy ethene (10～30) ether or its mixture; Wherein, the quality proportioning of anionic emulsifier and nonionic emulsifier is 2: 1～1: 2.
7. single-component self-crosslink emulsion adhesive for dry type composite film according to claim 1 is characterized in that described functional agent is sulfo-succinic acid di-isooctyl sodium or non-silicone mineral oil.
8. single-component self-crosslink emulsion adhesive for dry type composite film according to claim 1, it is characterized in that described cross-linking monomer is a N hydroxymethyl acrylamide, glycidyl acrylate, glycidyl methacrylate, vinyltrimethoxy silane, vinyltriethoxysilane, vinyl silane triisopropoxide, in the methacryloxypropyl three isopropoxy silane a kind or 2 kinds.
9. single-component self-crosslink emulsion adhesive for dry type composite film according to claim 1 is characterized in that described glass transition temperature Tg according to the emulsion polymer described in the claim 1 is between-10～-30 ℃.
10. the preparation method of the described single-component self-crosslink emulsion adhesive for dry type composite film of claim 1 comprises following technological step:
(1) takes by weighing the emulsifying agent of composite emulsifier gross weight 50～80% and the water of water inventory 20～40%, place pre-emulsion tank, hard monomer, soft monomer, (methyl) vinylformic acid, cross-linking monomer slowly joins and carries out emulsification in the pre-emulsion tank after mixing, emulsification times 30～60min, standby;
(2) add the water of water inventory 50～70%, the emulsifying agent of composite emulsifier total amount 20～50% in reactor, the initiator of initiator total amount 30～40%, sodium bicarbonate be as kettle base solution, stirs temperature of reaction kettle to 65～80 ℃ of raising simultaneously;
(3) add 10% pre-emulsion, in 65～80 ℃, be incubated then to blue light and occur;
(4) after insulation half an hour, the initiator of initiator total amount 60～70% is dissolved in the water of water inventory 5～20%, and with step (1) in the residue pre-emulsion drip simultaneously, the dropping time is 3～5h;
(5) be warming up to 85 ℃ at last, reaction 1～2h is cooled to room temperature, regulates the pH value, and adds functional agent.
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