Art
[1]The present application relates to a novel adhesive composition, and methods for their preparation.
BACKGROUND
[2]Pressure-sensitive adhesive is generally used, and the monomer and the oil-based solvents derived from petroleum as a raw material. Pressure-sensitive adhesive made from monomers, and which are made as a raw material derived from petroleum has a yield reduction, and environmental hormones, problems of toxic waste generated during the manufacture of the limited oil resources. In particular, the organic solvent is a petroleum-derived using the manufacturing process in order to improve the adhesion in the manufacture of conventional pressure-sensitive adhesive has a problem of environmental pollution in the inhibition of worker health and environmental protection. In addition, most of the pressure-sensitive adhesive is difficult to biodegrade got a monomer unit consisting of a covalent bond, an environmental pollution problem is becoming even by non-decomposed polymer so. Due to this, there have been developed various techniques for ionizing water pressure-sensitive adhesive to remove the adhesive from the adherend efficiently. In the conventional water ionizing adhesive requires a high temperature and an alkaline condition to remove the pressure-sensitive adhesive attached to the adherend and the substrate effectively and there is a need additional energy consumption. In addition, when discharged to the adherend or the pressure-sensitive adhesive material as the molecular environment when removing the adhesive material can be separated from the adhering substrate may result in additional secondary environmental pollution problem.
Detailed Description of the Invention
SUMMARY
[3]
Aspect of the present application is to provide a pressure-sensitive adhesive composition.
[4]
Another aspect of the present application is to provide a method for producing the adhesive composition.
Problem solving means
[5]
It will be described in more detail with respect to the pressure-sensitive adhesive composition and a method of manufacturing the same according to the following, one implementation.
[6]
Include lysine, itaconic acid and water, in the presence of lysine and itaconic acid salt type aqueous solution (salt solution) and is provided with a pressure-sensitive adhesive composition does not form a precipitate (precipitates) in an aqueous solution.
[7]
In the present application the term "adhesiveness (adhesion)" is 2 and the developing means of the object, which requires a (where gas is excluded), and a close-up, after naeneunde pulling them off any power (or days). In some cases, some material having a tackiness (adhesion) may involve, the irreversible destruction of the physical phenomena to be separated from the case after a certain time this can be passed when solidified, such a pressure-sensitive adhesive base material of the substrate coated. In addition, may be one containing the "tackiness (adhesion)", the "Viscoelastic (viscoelasticity)" that requires a certain degree of force in Viscoelastic (viscoelastic) deformation when do separate the adhesive material from the substrate. Adhesive compositions with a Viscoelastic properties (viscoelastic) is via a common machining shape prior to application to a substrate storage and distribution, and can be maintained even when the adhesive force a certain time. Adhesive article with such a pressure-sensitive adhesive composition obtained by coating and drying on a substrate is a label, for example, oriented polypropylene: and the like (Oriented PolyPropylene OPP) tape. With the pressure-sensitive adhesive property is reversible and can be attached and detached when the adhesive composition is applied to a substrate and drying the pressure-sensitive adhesive layer containing a viscoelastic substance is formed on the substrate.
[8]
On the other hand, a viscosity (viscosity) refers to the property that you want to interrupt the flow of certain substances as derived from the inner friction between the molecules. At this time, friction force is generated to stop the distribution of a difference in flow rate. Stickiness and viscosity is a distinct nature, and almost no stickiness even in the composition has a high viscosity and may have a high tackiness any composition that has a low viscosity.
[9]
Precipitate (precipitates) In the present application is to be obtained this scheme lysine aqueous solution (A (aq)), as shown in 1 and itaconic acid aqueous solution of water-insoluble salt (AB (s)) by a chemical change in the (B (aq)), to have not precipitated or insoluble in lysine or itaconic acid solids (a (s)), the solvent lysine or itaconic acid solids (a (s)) from lysine or itaconic acid aqueous solution (a (aq)) as shown in Scheme 2, the insoluble It may include all of the cases that remain in the state. [Reaction Scheme 1]
[10]
A(aq)+B(aq)->AB(s)
[11]
[Reaction Scheme 2]
[12]
A(aq)->A(s)
[13]
The "precipitate" in the present application can be a precipitate that was generated in the substrate or adhesive is applied around the blood, storage and distribution.
[14]
Term in this application, "lysine" is one of the basic amino acid α-, the lysine may be one or a biosynthesis through the lysine biosynthetic pathway from oxalic acid, or chemically synthesized.
[15]
Lysine may include lysine or a mixture of more than one kind of one species lysine.
[16]
Lysine may be at least one selected from D- lysine and a salt thereof represented by L- lysine, the following Formula 2 represented by the following general formula (1).
[17]
Formula 1
[18]
[19]
[Formula 2]
[20]
[21]
The Rai nephritis, for example, there may be mentioned lysine sulfate, lysine acetate, lysine monohydrochloride, lysine dihydrochloride, lysine monohydrate, lysine acetyl salicylate, lysine phosphate, lysine diphosphate, and mixtures or combinations thereof . This Rye nephritis can be converted into preform Lysine (free form).
[22]
According to the present invention is to convert the lysine to Lai nephritis preform are known to those of ordinary skill in the art. You can also use the raw material lysine is available commercially. For example, the lysine may be in D- lysine, L- lysine, and / or DL- lysine, because their physical and chemical characteristics are the same as or similar to, the characteristics of adhesive compositions containing them also the same or similar, the present invention It may belong to the category.
[23]
Itaconic acid as one of the organic acid to be represented by the formula (3).
[24]
[Formula 3]
[25]
[26]
In the adhesive composition may be in the form of lysine, and itaconic acid salt aqueous solution (salt solution). Specifically, lysine, even if mixing the itaconic acid and water, lysine and itaconic acid, without forming a covalent compound or an insoluble salt thereof, may be present in aqueous form. Itaconic acid is not present in the form of insoluble material that is not soluble in water in the adhesive composition of the present application.
[27]
Lysine, itaconic acid and the water content in the adhesive composition according to one embodiment can be controlled so as lysine and itaconic acid, or precipitated as crystal precipitation is not formed. In this way the adhesive is excellent, and when the adhesive composition without forming crystals or precipitates to keep the liquid phase, it is easy to uniformly applied to a substrate.
[28]
Mixing molar ratio of the lysine and itaconic acid is 2.3: 1 to 1: 1 may be 1.5 days. Specifically, the mixing molar ratio of the lysine and itaconic acid is 2.3: 1 to 1: 1.5, 2: 1 to 1: 1.5, from 1.5: 1 to 1: 1.5 or 1.5: 1 to 1: 1. If greater than a content of lysine of the above-mentioned range, or itaconic acid are present, the precipitate in the composition formed may be degraded, or the adhesive, the storage stability or storage stability of the adhesive composition may be degraded.
[29]
The content of solid matter in the adhesive composition may be an a composition of 100 parts by weight based on 70 parts by weight or less, e.g., 0.1 to 70 parts by weight, 1 to 70 parts by weight, 10 to 70 wt. And the content of solids is easier to apply an adhesive on the substrate when the above-mentioned range, when the content of solid matter more than 70 parts by weight, the formed precipitate may be difficult to use as a pressure-sensitive adhesive composition. Even if a less amount of the solid content is not lost in the adhesive strength to precipitate or composition, the content of solid matter in accordance with the field to be applied can also be adjusted to 0.1 to 10 parts by weight level.
[30]
Itaconic acid and lysine in the pressure-sensitive adhesive composition may contain, as an active ingredient. Specifically, the sum of the pressure-sensitive adhesive composition of solid content based on 100 parts by weight of itaconic acid and lysine content can be 60 to 100 parts by weight, 70 to 99 parts by weight, 80 to 98 parts by weight, or 85 to 97 parts by weight.
[31]
According to another aspect, itaconic acid and lysine according to the present invention may contain a condensate form to the itaconic acid and lysine as units. For example, the condensate is, dimers, trimers, or may be an oligomer, the content of the condensate
[32]
And lysine, and the sum of 100 parts by weight of itaconic acid content portion, based on 20 parts by weight or less, 10 parts by weight or less, can be less than 1 part by weight, and may include zero. When containing the condensation product into the range above can cause poor adhesion of the adhesive composition or not the liquid state is not maintained.
[33]
It will be described with respect to operations and effects showing the same tack as a pressure sensitive adhesive composition described above according to one embodiment as follows. Only the details will be described later in this action and effect is not meant to be interpreted as limiting, it may be described by a different function and effect to the extent there is no scientific contradiction.
[34]
Lysine has 2 amino groups, and itaconic acid has a two carbonyl groups. Hydrogen in the itaconic acid group of the oxygen lone pair and the lysine amino group may be an ionic interaction through hydrogen bonding (ionic hydrogen bond).
[35]
Thus, the adhesive composition of the present invention to analyze the components, such as liquid chromatography, it is possible to determine the lysine and itaconic acid as a raw material. From which is coupled via a lysine in the itaconic acid is ionic hydrogen bonding the adhesive composition, these are found to be present in a salt solution (salt solution) form. In the adhesive composition of the present invention acids lysine and itaconic without precipitation at room temperature (25 ℃) in crystalline form (solid state) or precipitate form is possible to exhibit excellent adhesive properties, while maintaining the liquid state.
[36]
Adhesive composition of the present invention has a water ionizing. Therefore, in the case of using the adhesive composition of the present invention as the adhesive, it is easy to remove, so the substrate or deposition from zero separation, dissociation by the removal of water upon which the adhesive is applied. Specifically, the pressure-sensitive adhesive coated on the base material or adherend may be one that is dissociated within using water of room temperature (25 ℃), stirring or washing with water through a step within 12 hours, in particular within 6 hours, 2 hours and more specifically . The adhesive composition of the present invention, so are easily dissociated with water harmless to the environment and living things dissociated components also is environment-friendly.
[37]
Adhesive composition of the present invention may further include at least one alcohol solvent selected from the group consisting of a primary alcohol, a polyhydric alcohol, a diol (diol) and triols (triol). When further adding a solvent to the adhesive composition to increase the drying rate of the adhesive composition and can improve the workability.
[38]
Day, the weight ratio of the mixed adhesive composition naetal water and alcohol according to the embodiments from 1: can be 0: 1 to 10. More specifically, the mixing weight ratio of alcohol in deionized water and the adhesive composition is from 1: 1 to 10: 1, 1: 1 to 5: 1 or from 1: 1 to 3: 2 days. As the content of the alcohol is increased and the adhesive composition is dried well, it is possible to increase the coating property turns out that the peel strength. However, if the content of the alcohol in the adhesive composition at least 1.5 times compared to deionized water, phase separation can occur within the adhesive composition.
[39]
The alcohol solvent may be a monohydric alcohols (monohydric alcohol), polyhydric alcohols (Polyhydric alcohols), an unsaturated aliphatic alcohol (Unsaturated aliphatic alcohols), alicyclic alcohol (Alicyclic alcohols) or a mixture thereof. The monohydric alcohols may be at least one selected from methanol, ethanol, propan-2-ol, butane-1-ol, pentanol -1-ol and hexadecane-1-ol (hexadecan-1-ol). To the polyhydric alcohol is ethane-1,2-diol (ethane-1,2-diol), 1,2-diol (propane-1,2-diol), propane-1,2,3-triol ( propane-1,2,3-triol), butane-1,3-diol (butane-1,3-diol), butane-1, & all (butane-1,2,3,4 -tetraol), pentane -1,2,3,4,5- phentolamine (pentane-1,2,3,4,5-pentol), hexane -1,2,3,4,5,6- heksol (hexane -1,2,3,4,5,6-hexol), heptane -1,2,3,4,5,6,7- heptol (heptane-1,2,3,4,5,6,7- heptol) it may be at least one selected from the.
[40]
Unsaturated aliphatic alcohols, for example pro-2-en-1-ol (Prop-2-ene-1-ol), 3,7- dimethyl-octa-2,6-diene-1-ol (3,7-Dimethylocta- 2,6-dien-1-ol), Pro-yn-1- ol -2 (Prop-2-yn-1-ol), cyclohexane -1,2,3,4,5,6- heksol (cyclohexane -1,2,3,4,5,6-hexol), 2- (2- propyl) -5-methyl-cyclohexane-1-ol (2- (2-propyl) -5-methyl-cyclohexane-1- It may be at least one selected from ol).
[41]
The pH of the adhesive composition is from 2 to 11, in particular 2 to 9.5, more specifically from 2 to 8.5. Adhesive composition having such a pH range, excellent storage stability and storage stability, and can be no change in the formulation, or even long-term storage quality. The adhesive composition, even after use as well as when used as soon as produced by a long storage period, but the adhesive is excellent not form a precipitate.
[42]
Specifically, the adhesive composition may be one that does not form a precipitate after a storage or distribution at least 14 days. For example more than 14 days, e.g., for 12 months or more, for example, can retain the physical properties by more than 24 months, even when the composition is kept stable. Further, the temperature of the environment in which the adhesive composition may be stored -18 ℃ to 80 ℃, specifically -18 ℃ to 45 ℃, 0 ℃ to 60 ℃, or 20 ℃ to 40 ℃. Even when stored at a low temperature or high temperature environment, if the temperature is ambient temperature of the environment wherein the pressure-sensitive adhesive composition used may be no effect on the formulation and quality. For example, when the storage at low temperature, can be used after a certain period of time allowed to stand at room temperature prior to use.
[43]
According to another aspect of the invention provides a method of mixing a lysine, itaconic acid and water to prepare the above-mentioned adhesive composition comprising the step of stirring below 80 ℃.
[44]
In some cases, when subjected to the steps of mixing said lysine, itaconic acid and water, and stirred at below 80 ℃ outside the above temperature range and the like, a side reaction substances, impurities may be formed, is to obtain the desired pressure-sensitive adhesive composition in which an adhesive that It can be difficult.
[45]
The step of stirring at 80 ℃ or less, for example, may be carried out at 0 ℃ to 80 ℃. More specifically, the step may be carried out at 0 to 75 ℃ ℃, 0 ℃ to 70 ℃, 0 ℃ to 65 ℃, 0 ℃ to 60 ℃.
[46]
The step of stirring in the 80 ℃ or less, for example, i) 0 ℃ to 80 ℃, comprising: a first step of stirring a mixture of from 0 ℃ to 75 ℃, 0 ℃ to 70 ℃, or 0 to 60 ℃ and ii) a room temperature ( It may include a second step of cooling to 20 to 30 ℃).
[47]
The lysine, and itaconic acid can be carried out according to the procedure for adding or mixing a lysine, itaconic acid and water at the same time, the itaconic acid in an aqueous solution of lysine during water mixture.
[48]
The adhesive composition may further include the step of removing the water and the solvent was concentrated under reduced pressure so as to control a solid content to a desired range.
[49]
The pressure sensitive adhesive product comprising a pressure-sensitive adhesive composition described above on the substrate is provided according to another aspect of the invention. The adhesive product described; And a pressure sensitive adhesive product is provided comprising a pressure sensitive adhesive layer obtained by coating and drying the pressure-sensitive adhesive composition described above on the substrate. Through the dried composition may be a solvent is removed. The drying may be carried out at 25 ℃ to 45 ℃.
[50]
The substrate can be used both if the adhesive composition is applied can adherend in the art. The substrate may be, for example, glass, stainless steel (SUS), polymer film or the like. Polymer film such as polyethylene, polypropylene, ethylene / propylene copolymer, polybutene-1, ethylene / vinyl acetate copolymer, polyethylene / styrene mixture of a butadiene rubber, a polyvinyl chloride film such as a polyolefin-based film or the like is mainly used in can. It may be a thermoplastic elastomer, and mixtures thereof, such as a polyol copolymer Further, polyethylene terephthalate, polycarbonate, poly (methyl methacrylate) or a polyurethane plastic, such as polyamide.
[51]
When using glass as the substrate, the film forming ability is excellent got a coating of pressure-sensitive adhesive composition onto a glass having a hydrophilic property can be performed more uniformly. When using a SUS as a base material, itaconic acid in the adhesive composition to cause the SUS and interaction is excellent in the adhesion of the pressure-sensitive adhesive layer formed from the base material and the adhesive composition.
[52]
The more the content of the solid matter increases in the pressure-sensitive adhesive composition is applied to the above-described base material is reduced the contact angle of the substrate and the adhesive composition. When thus reducing the contact angle of the substrate and the adhesive composition may be a pressure-sensitive adhesive layer formed by applying and drying the base material and the adhesive composition is uniformly formed to improve the adhesive strength of the adhesive layer to the substrate. The contact angle can be measured by a static method (Sessile Drop method) by using a contact angle meter. For example, Phoenix (phoenix)'s products (such as: Phoenix-150, Phoenix-MT, Phoenix-Alpha, Phoenix-Smart, Phoenix 300 Touch, or Phoenix-multi) may be used, the drop volume (drop volume) 5 the contact angle can be measured by ㎕.
[53]
According to another aspect of the invention the step of combining the adhesive composition to a first substrate by applying the adhesive composition to a first substrate; And attaching to each other the composition is bound by contacting the first substrate and the second substrate a first substrate and a second substrate; a first method for attaching the substrate and the second substrate comprising a are provided.
[54]
The first base and second base may be selected from one or more independently of each other, glass, stainless steel, polymer, metal, plastic, selected from the group consisting of paper, textile and the soil, but is not limited thereto. . Wherein the first substrate and the second substrate may be the same material, for example.
[55]
One pressure-sensitive adhesive composition or adhesive according to the embodiment, the product can be used as a pressure-sensitive adhesive tape, a sheet of labels, a spray-type adhesive, the dust remover, such as a water ionizing pressure-sensitive adhesive, it can be easily removed without damaging the adherend by using the water and the recycling of packaging is easy. And the case of applying the composition to the agricultural chemical and seed fields, there is an advantage that can easily be removed with water after the use of the pressure-sensitive adhesive-containing composition can be more diverse widen the application range. In addition, water ionizing plaster of the present disclosure as compared to conventional organic solvent-based pressure-sensitive adhesive cost savings as well as ease the handling workability is improved and it is possible that cleaning of the working environment.
[56]
Adhesive compositions according to the present application it is possible to select a monomer by a bio-derived as a starting material for use in the manufacture, since the monomer that may be utilized in a living body when the pressure-sensitive adhesive are removed, they are by the water of the petroleum-derived monomers, polymers or it is possible to prevent environmental contamination due to the oligomer in advance. Adhesive tape, sheet or the like for the labeling of structures formed of the composition of the present application using the water ionizing pressure-sensitive adhesive is improved in mechanical strength such as tensile shear strength, peel strength.
[57]
According to another embodiment, adhesive composition or the adhesive material of the present application is a reactive diluent if necessary, emulsifying agent, tackifier (tackifier), plasticizers, fillers, antioxidants, cure accelerators, flame retardants, flocculants, surfactants, thickeners, sunscreen, an elastomer, a pigment, a dye, (scented), fillers, UV filters, anti-static agents, anti-blocking agent, slip agent, inorganic filler, a mixing agent, a stabilizer, a modifier resin, a coupling agent, a leveling agent, a fluorescent whitening agent, a dispersant, a heat stabilizer from, light stabilizers, UV absorbers, waxes, wetting agents, flame retardants, antioxidants, preservatives, and the group consisting of lubricants may include a selected one or more additives. The total content of these additives does not particularly restricted, and may include various additives in accordance with the Where Used in various weight ranges. The content of each of the additives listed above may be used at a level commonly used in the art.
[58]
The reactive diluent as a diluent to help the components of the composition are to be evenly applied to the object to which the composition is applied, for example, n- butyl glycidyl ether, Ali patik glycidyl ether, 2-ethylhexyl glycidyl ether, phenyl glycidyl ether, O- cresyl glycidyl ether, nonylphenyl glycidyl ether, p- tert-butylphenyl glycidyl ether, 1,4-butanediol diglycidyl ether, hexanediol diglycidyl 1.6- ether, neopentyl diglycidyl ether, 1,4-dimethyl cyclohexane oldi diglycidyl ether, polypropylene glycol diglycidyl ether, ethylene glycol diglycidyl ether, polyethylene glycol diglycidyl ether, diethylene glycol glycidyl ether, resorcinol air between noldi glycidyl ether, hydrogen carbonate to bisphenol Eagle receiver ether, a trimethylolpropane triglycidyl procedure pen Tyr, glycerol polyglycidyl ether, di Glycerol polyglycidyl ether, pen Terry tree toll polyglycidyl ether, Kane stall glycidyl ether, tolyl service polyglycidyl ether, neopentyl Cannock Acid glycidyl ether, diglycidyl cyclohexane dicarboxylic -1.2- carboxylate, diglycidyl phthalate -O-, N, N- diglycidyl amine, N, N- diglycidyl -O- toll rudien, triglycidyl -p- aminophenol, tetraglycidyl- diaminodiphenyl methane, triglycidyl-diisocyanate, 1,4-butanediol diglycidyl ether, 1.6- hexanediol diglycidyl ether, polypropylene glycidyl dildi glycidyl ether and triethyl Rolf pen triglycidyl ether least one member selected from the group consisting of a can.
[59]
The emulsifier, may be mentioned, for example, polyoxyethylene, copolymers of polyoxypropylene, polyoxyethylene and copolymers of octyl phenyl ether, and at least one selected from the group consisting of sodium dodecyl benzene sulfide.
[60]
The tackifier, for example, rosin and their modified products (Rosin and its modified products) (for example: rosin, hydrogenated rosin, polymerized rosin, male rosin, rosin glycerin, rosin modified phenolic resin, etc.), terpene-based resins ( terpene-based resin) (example: terpene resin, terpene-phenol resin, terpene-styrene resin, terpene-phenolic resin), petroleum resin (petroleum resin) (for example: C5 petroleum resin, C9 resin, bicyclic ronadiene petroleum resin, hydrogenated petroleum resin, styrene-terpene resin), phenolic resin (phenolic resin), polymethyl styrene resin, ketone formaldehyde resin, xylene formaldehyde resin, cashew oil modified phenol resin (cashew oil modified phenolic resin), tall oil-modified phenol resin (tall there may be mentioned a rosin emulsion, TPR water based resin, 2402 resin emulsion, petroleum resin emulsion), coumarone-indene resin, and the like: oil modified phenolic resin), rubber (rubber), a resin emulsion (resin emulsion) (eg.
[61]
The plasticizer is contained in the composition may serve to improve the processing flow and stretching. And a plasticizer may improve features such as electric insulation, adhesion, cold resistance, light resistance, oil resistance, within the soap properties, flame retarding flame resistance, heat stability, Iga-porous (intramolecular active) of the composition, activity (inter-molecular active), non-toxic.
[62]
A plasticizer for improving function, such as cold resistance may be such as dioctyl adipate (DOA), DOZ (dioctyl azelate), DOS (dioctyl sebacate), Flexol TOF (UCC Co.), polyethylene glycol esters. It may be a heat-resistant (non-volatile), and a non-plasticizer for the planet enhancements are polyester, NBR (nitrile butadiene rubber), such as polymer blends, trimellitic acid esters, pentaerythritol esters and the like. A plasticizer for improving the light fastness properties, DOP, DOA, DOS, polyesters, epoxidized soybean oil: can be a (epoxidized soybean oil ESBO) and the like.
[63]
A plasticizer for the oil resistance improvement force flex aromatic phosphoric acid ester (trade name: TPP, TCP, 112 (CDP), 179A (TXP)) may be, polyester, NBR or the like, a plasticizer for in-soap properties are TCP, ESBO , may be a polyester-based.
[64]
A plasticizer for the flame resistance flame retardant may be a TCP, TXP such as phosphate, may be a chlorinated paraffin, chlorinated alkyl stearate, NBR or the like, a plasticizer for the thermal stability is ESBO, DOZ, DOS, DOP, such as polyethylene glycol.
[65]
Iga plasticizer for the microporous is DOA. May be such as BBP, TOF, TCP, octanoic tildi diphenyl phosphate, a plasticizer for the activity DOZ, DOS, dibasic phosphites: may be a (dibasic lead phosphate DLP), ESBO, polyethylene glycol ester and the like.
[66]
A plasticizer for the non-toxic may be such BPBG, octanoic tildi phenyl phosphate, ESBO, citric acid esters, NBR.
[67]
The plasticizer is specifically dibutyl phthalate (DBP), dihexyl phthalate (DHP), di-2-ethylhexyl phthalate (DOP), di -n- octyl phthalate (DnOP), diisooctyl phthalate (DIOP), dideoxy silt de-rate (DDP), diisobutyl to silt de-rate (DIDP), C8 ~ C10 mixed higher alcohol phthalate, butyl benzyl phthalate (BBP), dioctyl adipate (DOA), dioctyl azelate (DOZ), dioctyl sebacic Kate (DOS), tree Crescent quality force page (TCP), tree key silane carbonyl phosphate (TXP), mono-oxide tildi phenyl phosphate (Santicizer141), monobutyltin-Dickie silane carbonyl phosphate, trioctyl phosphate (TOF), aromatic oil, the poly beuden, paraffin or the like can be used.
[68]
Thickening agents herein include, for example, arginine (alginin), alginate (alginic acid), see sodium carbonate (sodium alginate), guar gum (guar gum), xanthan gum (xanthan gum), collagen (collagen), alginate (alginate ), gelatin (gelatin), greener Cellar is (Furcellaran), agarose (agar), color last (carrageenan), casein (casein), locust bean gum (locust bean gum), pectin (pectin), polyethylene oxide, polyethylene glycol, such as polyvinyl alcohol, polyvinylpyrrolidone, it may be used.
[69]
The surfactant may be used are all so long as it is conventionally used in the art. For example, C8 to C18 chain alkyl having length sulfate, alkyl ether sulfate or alkyl aryl ethers having 8 to 18 C atoms and the ethylene oxide or propylene oxide units of less than 40 in the hydrophobic group of the sulfates, C8 to C18 a may be an alkyl sulfonate, alkylaryl sulfonates, alkyl polyglycol ethers or alkylaryl polyglycol ethers 1 has a ethylene oxide units of esters and semi-esters, C8 to 40 of sulfosuccinic acid with alcohols or alkyl phenols. For example, sodium dodecyl sulfate (sodium dodecyl sulfate: SDS), sodium - and the like silicate (Na-silicate) can be used.
[70]
The filler as the addition in order to improve the strength, durability and workability of the composition of example, calcium carbonate, talc, stop, ceramic, silica, dolomite, clay, titanium white, zinc white, talc, carbon (to prevent shrinkage, blocking prevention) , it may be a potassium carbonate, titanium oxide, a liquid polysulfide polymer, a volatile diluent (volatile diluents), magnesium oxide, step five days (processing oil) and the like.
[71]
The curing accelerator may, for example, such as dibutyltin dilaurate, JCS-50 (jyoho kuka Kagaku Kogyo, Ltd.), formate TK-1 (Mitsui Kagaku Polyurethane Co., Ltd.). And anti-oxidation agent, for example, dibutyl hydroxy toluene (BHT), Irganox (R) 1010, Irganox (R) 1035FF, Irganox (R) 565 (both, Ciba Specialty Chemicals According to literature may be available).
[72]
The antistatic agent is not particularly limited, and specifically, 1-hexyl-4-methyl-pyridinium hexafluorophosphate, dodecyl silpi bipyridinium hexafluorophosphate, fluorinated organic metal compound (for example, 3M's HQ-115), an alkali metal salt (e. g., NaPF 6 , NaSbF 6 , KPF 6 , KSbF 6 and the like), conductive polymers (e.g., poly-thiophene (Bayer Corporation PEDOT), polyaniline, polypyrrole and the like), metal oxides (e.g., indium doped tin oxide (ITO), antimony-doped tin oxide (ATO), tin oxide, zinc oxide, antimony oxide, indium oxide, etc.), quaternary ammonium salts (e. g., Sigma-Aldrich's poly (acrylamide -co- diallyl dimethyl ammonium chloride) solution), 1 butyl-3-methyl imidazolium hexafluoro phosphate microporous [BMIM] [PF 6 ], 3-butyl-1- (2-hydroxyethyl) (methanesulfonyl trifluoromethyl) imidazolium bis imide [BHEIM] [NTf 2 ], (methanesulfonyl-trifluoromethyl) methyl tetrabutyl ammonium bis already De [TBMA] [NTf 2 may be, etc.], and these may be used alone or as a mixture of two or more.
[73]
The elastomer refers to a polymer having the properties of rubber or elastomer, such as ethylene-vinyl acetate copolymer, acrylic rubber, natural rubber, isoprene rubber, styrene butadiene rubber, chloroprene rubber, butyl rubber, ethylene propylene rubber, styrene-ethylene -butylene-copolymer and the like can be used butadiene-styrene copolymer, acrylonitrile.
[74]
The stabilizer serves to stabilize the adhesive strength or the like of the composition, and examples thereof include alcohol and the like, polyhydric amine can be approached. For example, alkylene glycol, dialkylene glycol, benzene diols, benzene triols, di-alcohol amine, tri-alcohol amine, arabitol, mannitol, iso malteu, glycerol, xylitol, sorbitol, maltitol, erythritol, ribitol, dulsi tolyl, lactitol, tray tolyl, Heidi sorbitol, polyglycidyl tolyl, alkylenediamines, diamines selected from alkenylene, phenylene diamine and the amino-n- group consisting of an alkyl alkane diamine may be at least.
[75]
The fluorescent whitening agent may be such as benzoxazole (benzooxazole) compounds, benzothiazole (benzothiazole) compounds or benzoimidazole (benzoimidazole) compound.
[76]
The pigment may be a natural pigment or synthetic pigment, which may be an inorganic pigment or an organic pigment as a different category. ,
[77]
The perfume, for example, but are not limited thereto may be used alone or in combination such as peppermint oil, mint seupeah oil, carboxylic or menthol.
[78]
The flame retardant may be a melamine cyanide rate (melamine cyanurate), magnesium hydroxide, pyrophyllite, zeolite, sodium silicate, aluminum hydroxide, antimony (antimony trioxide). And water resistance improving additive may be glyoxal (glyoxal).
[79]
Examples of the modified resins include polyol resins, phenol resins, acrylic resins, polyester resins, polyolefin resins, epoxy resins, epoxidized polybutadiene resins.
[80]
The coupling agents can improve adhesion and bonding reliability between the adhesive composition and the packaging material. When such a coupling agent is added the composition under high temperature and / or high humidity conditions, it is possible to improve adhesion reliability when a long-term stand. Examples of the coupling agent, γ- glycidoxypropyltrimethoxysilane doksi the profile triethoxysilane, γ- glycidoxypropyltrimethoxysilane doksi trimethoxysilane, γ- glycidoxypropyltrimethoxysilane doksi propyl methyl diethoxy silane, γ- glycidyl silane on doksi propyltriethoxysilane , 3-mercaptopropyl trimethoxysilane, vinyl trimethoxysilane, vinyl triethoxysilane, γ- methacryloxypropyltrimethoxysilane trimethoxysilane, γ- methacryloxypropyltrimethoxysilane propyl triethoxysilane, γ- aminopropyl in trimethoxysilane, γ- aminopropyl a silane, 3-isocyanato propyl triethoxy silane in, γ- acetoacetate propyl trimethoxy silane, γ- acetoacetate in profile triethoxysilane, β- cyanoacetyl tree can be used a silane compound such as silane, β- cyanoacetyl tree on silane, acetoxy acetonitrile trimethoxysilane.
[81]
The mixing agent may be an aromatic hydrocarbon resin.
[82]
The anti-aging agent may be N- (1,3- dimethylbutyl) -N'- phenyl -p- phenylene diamine.
[83]
The wetting agents are, for example, may be alone or a mixture of sugar, glycerin, sorbitol solution, or non-crystalline sorbitol solution.
[84]
The ultraviolet absorber is ethylhexyl methoxycinnamate (for example, 2-Ethylhexyl 4-methoxycinnamate), ethylhexyl silsal florisil acrylate, 4-methyl benzylidene camphor, isoamyl p- methoxycinnamate, loam methacrylic alkylene, phenyl may be such as salicylate, papba (pABA), ethyl hexyl dimethyl paba, paba glyceryl-benzimidazole sulfonic acid, homo-year-old rate, sinok glyphosate, ethylhexyl triazol zone, polysilicon -15, T yieyi. These may be used alone or two or more in combination.
[85]
The adhesive composition of the adhesive application or product, in addition to the aforementioned additives, US4959412, CA1278132, US6777465, WO2007-120653, US2003-0064178, US7306844, US 7939145, WO 2011-136568, WO 2010-071298, Republic of Korea Patent Application Publication 2016-0095132, the additive disclosed in Japanese Patent Publication 5959867, Korea Patent 989 942 which are incorporated by reference as a whole.
[86]
An adhesive composition or a pressure sensitive adhesive product, according to one embodiment may be used to attach a label, such as a variety of packaging materials, including metal, glass and plastic. The packaging may for example be a container for food, drink or household goods, and these containers may be made of glass, metal or plastic.
[87]
The pressure-sensitive adhesive composition or the pressure-sensitive adhesive products can be used in applications such as adhesives, coating agents, carriers, or food additive according to its composition and properties.
[88]
For if the adhesive composition or a pressure sensitive adhesive product of the present application is used in adhesive applications, for for the labeling, sealing, paper, cigarette paper, for self-adhesive block toys, sand piece, bathroom / kitchen cleaners for, food for animal ointment spray , exfoliation, body hair, hair gel for fixing. Is applicable soil stabilizer (soil stabilizer), waterweeds and strength agents, cardboard, or the like for the adhesive zones. The soil stabilizer means for removing the dust generated in the plant, such as fine dust and sandstorm.
[89]
When the adhesive composition or a pressure sensitive adhesive product of the present application is used as a coating, may be used for fire control, fruit vegetables, stem jeolhwaryu cut surface, it can be used for hair dye, antifouling coating pretreatment. Here antifouling coating pre-treatment, after the coating media is easy to contaminate the composition, may be used in the process of simply cleaned when the contaminated water.
[90]
When the adhesive composition or a pressure sensitive adhesive product of the present application is used as a transport agent, a disinfectant is applicable for forestry, for fire control, bath perfume, disinfectant, farm materials, such as household goods and toys. Forest disinfectant can enter the forest disinfectant, such as the pine nematodes, for example, disinfectants, and the like for example, bird flu, antiseptics, disinfectants foot-and-mouth disease. And farm materials include fertilizers, taping, seed coatings.
[91]
When the pressure-sensitive adhesive composition or a pressure sensitive adhesive product of the present application applied to a farm materials, may be used for seed coating, the plant taping, insecticides additives, excipients fertilizers, natural pesticides. And there is a composition of the present application can be used in the manufacture of edible coloring well butge or by the addition of citric infant is used without the paper drip is added, the paint when it is applied to dairy products. When the composition of the present application cleaning as another example to be applied to dairy products, there may be used a zero decontamination pretreatment To elaborate than this, sprinkled on the polluted medium, such as the composition of the present application as a screen door or window frames, cars with water It can be quickly decontaminated.
[92]
When performing the pressure-sensitive adhesive composition or the pressure-sensitive adhesive product is carrying the features of this application, the oxygen barrier properties, moisture barrier properties, the use of oil and it is possible to implement the heat silring function it eco-friendly food packaging coating layer suppressing the external moisture from penetrating while an effect to prevent and delay the decay and oxidation of foods. Also, if the pressure-sensitive adhesive composition or a pressure sensitive adhesive product of the present application is used as a food additive when used refers to, for example material for the wheat gluten substitute, jelly, syrup, drug, dye, cream, or the like freezing agent.
Effects of the Invention
[93]
Adhesive composition according to one embodiment has a water ionizing adhesive, coating and carrier functions. When using the adhesive composition as a water ionizing adhesive from the adherend or the substrate according to one embodiment is dissociated by the water can be easily removed from the adherend or a substrate. Therefore, this pressure-sensitive adhesive is environmentally friendly as water ionizing material.
Brief Description of the Drawings
[94]
Figure 1 is a photograph to confirm the image after drying at room temperature (25 ℃) after applying the pressure-sensitive adhesive composition according to the embodiment 3 on the substrate.
[95]
2 are the pictures for the image check performed after the after coating the adhesive composition on the base material oven (40 ℃) drying according to the third embodiment.
Mode for the Invention
[96]
Hereinafter, the embodiments, but to be described in detail example, not meant to be limited to the following examples.
[97]
[Example 1] lysine and stability evaluation of the compositions containing various organic acids
[98]
When the composition prepared by mixing a basic amino acid, lysine and various organic acids were evaluated in the stability of each composition (whether precipitation).
[99]
Adhesive composition production process comprising a lysine and itaconic acid:
[100]
Was 54 wt% L- lysine preform (Lysine free form) adding DIW (deionized water) aqueous solution of 56.1g in 100g, and simultaneously diluted and stirred for 30 minutes at room temperature (25 ℃). Itaconic acid added slowly at room temperature to 48.06g (25 ℃) in the diluted lysine and the mixture was stirred for 1 hour at 60 ℃ and then stirred for 1 hour. Then, the reaction mixture was terminated after reaching room temperature (25 ℃) reaction to give the adhesive composition 204.11g. The content of the solid content in the composition is from about 50 parts by weight based on 100 parts by weight of the composition, the mixing molar ratio of lysine and itaconic acid is 1: 1 and the solvent is deionized water.
[101]
In the same manner as in the method, a composition was prepared by changing only the type of organic acid. To the same manner as in Example 1, except for using each of the organic acids shown in Table 1 to prepare a composition.
[102]
TABLE 1
[103]
According to Table 1 it was evaluated whether or not precipitation of the resulting composition. Specifically, each of the compositions using a bar coater group (bar coater) on top of the OPP film thickness 50㎛ (Sam Young Chemical Co.) was coated to a thickness of about 50㎛. After the composition is allowed to stand for 14day the applied film at room temperature (25 ℃), relative humidity 60 ± 10% condition, to determine the change in the surface of the adhesive composition present on the OPP film was evaluated for shape change. The evaluation results are shown in Table 2 below.
[104]
TABLE 2
[105]
Referring to the results of Table 2, the composition comprising a lysine and itaconic acid has a composition comprising the other hand, other organic acids and precipitation of lysine is not formed could not be formed a precipitate to evaluate the adhesion. That is, when a composition prepared by mixing a lysine and various organic acids, it was confirmed that all the composition is not intended to represent the adhesive without forming a precipitate.
[106]
Example 2 Solubility evaluation of the solvent of the composition
[107]
According to the method described in Example 1 to prepare a pressure-sensitive adhesive composition comprising a lysine, and itaconic acid. (Molar ratio = 1 of lysine and itaconic acid: 50 parts by weight of 1, solid content) In an additional 25g of solvent for the preparation of adhesive compositions in Table 3, respectively 50g and stirred for 1 hour. After performing the stirring was confirmed that the solubility of each solvent in the adhesive composition. To evaluate the solubility of the adhesive composition results in accordance with each type, and the solvent of the added solvent shown in Table 3 below.
[108]
TABLE 3
[109]
Referring to Table 3, the adhesive composition of the present application has been dissolved in the case of using an alcohol such as methanol as solvent, did not dissolve for other organic solvents.
[110]
[111]
[ Example 3] Lysine and the itaconic acid to the mixing molar ratio of the shape of the pressure-sensitive adhesive composition according to, viscosity, and the initial adhesive strength analysis
[112]
The composition of the stability, viscosity, and the initial adhesive strength of the adhesive composition in lysine and the molar ratio of itaconic acid of the present application were analyzed.
[113]
According to the method described in Example 1 to prepare a pressure-sensitive adhesive composition comprising a lysine, and itaconic acid. However, each of the third molar ratios of lysine and itaconic: 1. 2.5: 1, 2: 1, 1.5: 1, 1: 1, 1: 1.5, 1: 2, 1: 2.5 and 1: the pressure-sensitive adhesive composition was prepared in three. (50 parts by weight of solid content)
[114]
(1) Stability Evaluation
[115]
Specific methods for the Safety of each of the adhesive compositions of the various having a molar ratio as follows: To about 1g was determined for each of the pressure-sensitive adhesive composition in an aluminum dish (dish) having a diameter of 5cm. In dry conditions, since it was confirmed whether or not the crystallization of the adhesive composition.
[116]
i) Drying Condition 1
[117]
At room temperature (25 ℃), relative humidity 60 ± 10% conditions for 14day was confirmed whether the adhesive composition within a precipitate formed and the surface changes.
[118]
ii) Drying Condition 2
[119]
In the oven (oven) to control 40 ℃ was confirmed whether the adhesive composition within a precipitate formed and the surface changes over 48hr.
[120]
(2) viscosity rating
[121]
The viscosity is a rotary viscometer (a manufacturer: LAMYRHEOLOGY) to measure the viscosity at 25 ± 1 ℃, LV-1 one form of a Spindle, conditions of 60rpm using.
[122]
(3) Initial adhesion
[123]
In the reliability evaluation were evaluated for initial adhesive force with respect to the composition is not formed is precipitated. Initial adhesion was measured using a Rheometer equipment of Anton Paar 社, compared to the initial adhesion of the pressure-sensitive adhesive composition through the equipment. Contact for one minute the probe (Probe) of a SUS material having a 25mm diameter in the adhesive composition by measuring the force generated sikimyeo peeling off the probe to the same speed after maintaining the Negev 0.01mm (gap) for the initial adhesive force moment consisting of It was the quantitative evaluation.
[124]
The evaluation results are shown in Table 4 below.
[125]
TABLE 4
[126]
* In Table 4, room temperature denotes a drying oven conditions 1 shows the drying conditions 2.
[127]
Referring to Table 4, the lysine and itaconic acid molar ratio is 3: 1 to 2.5: 1 when the pressure-sensitive adhesive composition was formed a precipitate.
[128]
The molar ratio of lysine with itaconic acid of 2.5: 1, when the other hand, the molar ratio of lysine and itaconic acid 2 precipitate is formed: there was not formed a precipitate; 1. To confirm that the more specific the critical point, the molar ratio of lysine with itaconic acid of 2.5: 1, 2.4: 1, 2.3: 1, 2.2: 1, 2.1: 1, 2: After preparing a pressure-sensitive adhesive composition by broken down at 1 (solid content: content of 50 parts by weight) was evaluated in the same manner as the stability, the viscosity, and the initial adhesive strength.
[129]
The evaluation results are shown in Table 5 below.
[130]
Table 5
[131]
Referring to Table 5, the mole ratio of lysine with itaconic acid of 2.5: 1 to 2.4: case 1, whereas precipitate is formed, the molar ratio of lysine and itaconic acid 2.3: 1 to 2: The precipitate is formed when the first It did not.
[132]
[ Example 4] The shape of the adhesive composition, the viscosity and solids content of the initial adhesive strength analysis
[133]
A composition shape, viscosity, and the initial adhesive strength of the adhesive composition according to the solids content of the present application were analyzed.
[134]
1) a molar ratio of lysine and itaconic acid 1: 1, the evaluation according to the solids content
[135]
According to the method described in Example 1 to prepare a pressure-sensitive adhesive composition comprising a lysine, and itaconic acid. However, the pressure-sensitive adhesive composition was prepared so that the adhesive composition in solid content to 10% by weight, respectively, 20%, 30%, 40%, 50%, 60%, 70%, 75% by weight. (Molar ratio of lysine and itaconic acid is 1: 1) The solid content was adjusted in the water content.
[136]
Shaped embodiment of the composition according to the same method as described in Example 3, was evaluated for the viscosity and the initial adhesive strength. The evaluation results are shown in Table 6 below.
[137]
TABLE 6
[138]
Referring to Table 6, when the pressure-sensitive adhesive of the content of solids 75% by weight of the composition, and it was confirmed the formation of a precipitate is not dissolved.
[139]
If the content of solids in the composition is 75% by weight, it did not form a precipitate when the precipitate is formed, whereas, the solids content of the composition 60% by weight and 70% by weight. In order to confirm more specific threshold, the composition 60% by weight of the solids content, respectively, 61 wt%, 62 wt%, 63 wt%, 64 wt%, 65 parts by weight, 66% by weight, 67% by weight, 68% by weight, 69 wt%, 70 wt%, 71 wt.%, and 72 after producing the pressure-sensitive adhesive composition by more granular than a% by weight (molar ratio of lysine and itaconic acid is 1: 1), in the same manner as stability, viscosity, and the initial adhesive strength It was evaluated.
[140]
The evaluation results are shown in Table 7.
[141]
Table 7
[142]
Referring to Table 7, when the adhesive is the amount of solids in the composition, 70% by weight in the case where the one hand, the adhesive composition is in a solid content of more than 71% by weight, maintaining the liquid phase, it was confirmed the formation of a precipitate.
[143]
2) the molar ratio of lysine and itaconic acid 2: 1, 1: 1.5 or 2.5: 1 if the evaluation according to the solids content
[144]
If the molar ratio of lysine and itaconic acid are changed, and evaluate whether precipitation of the solid content.
[145]
According to the method described in Example 1 to prepare a pressure-sensitive adhesive composition comprising a lysine, and itaconic acid. However, the molar ratio of lysine and itaconic acid, respectively 2: To a mixture of lysine and itaconic acid such that: 1, 1: 1.5 and 2.5. With respect to the composition having the molar ratio, the solids content of the composition was adjusted to a water content such that the respective 10%, 20%, 30%, 40%, 50%, 60%, 70% by weight . It was evaluated in the method and the stability of the composition in the same manner described in Example 1. For each composition. The evaluation results are shown in Table 8.
[146]
Table 8
[147]
Referring to Table 8, the molar ratio of lysine and itaconic acid 2: 1 and 1: 1.5 in this case, do not form precipitates to change to a solids content of 10% to 70% by weight. On the other hand, the molar ratio of lysine with itaconic acid of 2.5: 1, when the precipitate was formed at any solids content.
[148]
That is, the stability and adhesive strength of the adhesive composition of the present application is determining the effect of the mole ratio of lysine and itaconic acid is large, when the molar ratio of lysine and itaconic acid are the same, it was confirmed that the content of solids hitting the impact .
[149]
Example 5 Comparative The initial adhesive strength and water-ionizing
[150]
It was compared to the conventional pressure-sensitive adhesive and the adhesive strength and the water ionizing the adhesive composition of the present application.
[151]
According to the method described in Example 1 to prepare a pressure-sensitive adhesive composition comprising a lysine, and itaconic acid. However, the amount of solids in the pressure-sensitive adhesive composition was adjusted such that the content of the 10% by weight. (Molar ratio of lysine and itaconic acid = 1: 1)
[152]
Available commercial polyvinyl alcohol-based adhesive to the (polyvinyl alcohol based adhesive:. PVA 088-50, Qingdao Sanhuan Colorchem CO, LTD) and then prepared, by adjusting the water content so that the solid content is 10% by weight adhesive composition (hereinafter, the control group 1) was prepared.
[153]
Carried out using the same method as that described for Example 3, it was evaluated for initial viscosity and adhesion of the pressure-sensitive adhesive composition (10 wt% solid content) and the control group of the present application one.
[154]
In addition, to evaluate the water ionizing of the adhesive composition of the present application (10 wt% solid content) and the first control group. Method for evaluating the water ionizing is as follows: after coating the adhesive composition of the present application to a thickness of 50 ~ 60㎛ to the upper PET film and dried at 40 ℃ for 30 minutes. By cutting the dried resultant was 25mmX25mm size attached to a stainless steel (SUS304), and was prepared by adhering the specimen to five times at a pressure of 2kgf compression using a hand roller. PVA adhesive is to prepare a specimen and attached to a stainless steel (SUS304), and squeezed 5 times at a pressure of 2kgf using a hand roller, the adhesive was cut into a size of 25mmX25mm was coated to a thickness of 50 ~ 60㎛ to the upper PET film .
[155]
After each of the specimens by 200rpm using a stirrer and then fully immersed in a normal temperature and normal pressure, distilled water (DIW) in the neutral pH conditions i) has elapsed 1 hour, or ii) after 24 hours, it was confirmed the sample state. The time elapsed before the pressure-sensitive adhesive composition or the pressure-sensitive adhesive from the specimen after it is fully removed from the base material was measured to evaluate the water ionizing the specimen.
[156]
The evaluation results are shown in Table 9 below.
[157]
Table 9
[158]
Referring to Table 9, the adhesive composition according to the present application is compared with the polyvinyl alcohol-based adhesive composition (Control 1) shows the initial adhesive force equivalent, was isolated in a short time in the water. On the other hand, the polyvinyl alcohol-based adhesive composition 24 hours after immersion in water, but soluble in water after 1 hour was only partially soluble in water.
[159]
That is, the pressure-sensitive adhesive composition according to the present invention has the above as compared with the conventional pressure-sensitive adhesive adhesive force is equal to the water level or ionizing very excellent, This is expected to use in a variety of fields.
[160]
[Example 6] Evaluation of the water ionizing solvent
[161]
Carried out according to the production method described in Example 1 to prepare a pressure-sensitive adhesive composition comprising a lysine, and itaconic acid (6-1 to 6-3 below). However, the molar ratio of lysine and itaconic acid, respectively 1.5: 1, 1: 1, and 1: 1.5 to prepare a pressure-sensitive adhesive composition. (50 parts by weight of solid content)
[162]
Further, in accordance with the production method described in Example 1 to prepare a pressure-sensitive adhesive composition comprising a lysine, and itaconic acid (6-4 to 6-6 below). However, the molar ratio of lysine and itaconic acid, respectively 1.5: 1, 1: 1, and 1: 1.5 were prepared adhesive composition, the solvent is 1: was used as the deionized water and a mixture of methanol of 1 weight ratio. (50 parts by weight of solid content)
[163]
As a control group, we were prepared using a commercially commercially available acrylic pressure sensitive adhesive (K901, ㈜ HA P & I) (hereinafter, control group 2). (Solid content 59% by weight) was evaluated according to the following method with respect to ionizing the water pressure-sensitive adhesive composition of the respective evaluation results are shown in Table 10.
[164]
1) water ionizing
[165]
It was applied to a thickness of the composition of the prepared adhesive composition, the control group and 2 ~ 50 60㎛ the upper PET film were each dried at 40 ℃ for 30 minutes.
[166]
By cutting the dried resultant was 25mmX25mm size attached to a stainless steel (SUS304), and was prepared by adhering the specimen to five times at a pressure of 2kgf compression using a hand roller.
[167]
After each of the specimens by 200rpm using a stirrer and then fully immersed in a normal temperature and normal pressure, distilled water (DIW) in the neutral pH conditions i) has elapsed 1 hour, or ii) after 24 hours, it was confirmed the sample state.
[168]
[Table 10]
[169]
Referring to Table 10, the adhesive product obtained using a pressure-sensitive adhesive composition according to the present application was isolated from the water within one hour after dipping in water. However, acrylic pressure-sensitive adhesive is not soluble in water after 24 hours.
[170]
In the above, but one implementation example described with reference to drawings and embodiments, it be understood that it is only and are possible various modifications and equivalent other implement those skilled therefrom in the art that the exemplary will be. Accordingly, the scope of protection of the present application should be defined by the appended claims.

Claims

[Claim 1]Lysine, itaconic acid, and includes water, wherein the lysine and itaconic acid salt aqueous solution (salt solution) in the form, and would not form a precipitate (precipitates) in the aqueous adhesive composition.
[Claim 2]
The method of claim 1, wherein the precipitate is precipitated in the adhesive composition of lysine and itaconic acid.
[Claim 3]
The method of claim 1, wherein the mixing molar ratio of the lysine and itaconic acid is controlled such that the precipitation of lysine and itaconic acid are not formed in the adhesive composition, the adhesive composition.
[Claim 4]
The method of claim 3 wherein the mixing molar ratio of the lysine and itaconic acid is 2.3: 1 to 1: 1.5, the adhesive composition.
[Claim 5]
The method of claim 1 wherein the adhesive composition has solids content of 70 by weight based on the total weight of the composition unit or less, the pressure-sensitive adhesive composition.
[Claim 6]
The method of claim 1, wherein the pressure-sensitive adhesive composition, a primary alcohol, a polyhydric alcohol, a diol (diol) and triols (triol), further comprising at least one solvent selected from the group consisting of a pressure-sensitive adhesive composition.
[Claim 7]
7. The method of claim 6 wherein the alcohol is methanol, ethanol, propan-2-ol, butane-1-ol, pentanol -1-ol and hexadecane-1-ol at least one monovalent alcohol selected from the group consisting of (hexadecan-1-ol) ( monohydric alcohol). Ethane-1,2-diol (ethane-1,2-diol), 1,2-diol (propane-1,2-diol), propane-1,2,3-triol (propane-1,2 , 3-triol), butane-1,3-diol (butane-1,3-diol), butane-1, & all (butane-1,2,3,4-tetraol), pentane -1,2,3,4,5- phentolamine (pentane-1,2,3,4,5-pentol), hexane-1,2,3-hexane -1,2,3,4,5,6- heksol , 4,5,6-hexol), heptane -1,2,3,4,5,6,7- heptol (one or more selected from the group consisting of heptane-1,2,3,4,5,6,7-heptol) polyol (polyhydric alcohols); Pro-2-en-1-ol (Prop-2-ene-1-ol), 3,7- dimethyl-octa-2,6-diene-1-ol (3,7-Dimethylocta-2,6-dien-1 -ol), Pro-yn-1- ol -2 (Prop-2-yn-1-ol unsaturated aliphatic alcohol (unsaturated aliphatic alcohols selected from a)); Cyclohexane -1,2,3,4,5,6- heksol (cyclohexane-1,2,3,4,5,6-hexol), 2- (2- propyl) -5-methyl-1-cyclohexanone ol (2- (2-propyl) -5-methyl-cyclohexane-1-ol) at least one aliphatic alcohol selected from the group consisting of (alicyclic alcohols) or a mixture of pressure-sensitive adhesive composition.
[Claim 8]
The method of claim 1 wherein the adhesive composition is stored at -18 to 45 ℃ if more than 14 days would precipitate that is not formed, the pressure-sensitive adhesive composition.
[Claim 9]
The method comprising mixing a lysine, itaconic acid, and water; And the method comprising, in the adhesive composition of lysine, itaconic acid and the water content is made in the control so that the precipitation of lysine and itaconic acid is not formed, the pressure-sensitive adhesive composition; and stirring the mixture below 80 ℃.
[Claim 10]
10. The method of claim 9, wherein the mixing molar ratio of the lysine and itaconic acid 2.3: 1 to 1: 1.5, for producing a pressure-sensitive adhesive composition.
[Claim 11]
10. The method of claim 9, wherein the mixture is a primary alcohol, a polyhydric alcohol, a diol, further comprising at least one solvent selected from the group consisting of (diol) and triols (triol), process for preparing a pressure-sensitive adhesive composition.
[Claim 12]
A first pressure-sensitive adhesive product comprising a pressure-sensitive adhesive composition of any one of to claim 8.
Claims amendments (under Article 19)
- International Bureau of the date of receipt: 27 August 2018 (27.08.2018)
[1]
Lysine, itaconic acid, and includes water, wherein the lysine and itaconic acid salt aqueous solution (salt solution) in the form, and would not form a precipitate (precipitates) in the aqueous adhesive composition.
[2]
The method of claim 1, wherein the precipitate is precipitated in the adhesive composition of lysine and itaconic acid.
[3]
The method of claim 1, wherein the mixing molar ratio of the lysine and itaconic acid is controlled such that the precipitation of lysine and itaconic acid are not formed in the adhesive composition, the adhesive composition.
[4]
The method of claim 3 wherein the mixing molar ratio of the lysine and itaconic acid is 2.3: 1 to 1: 1.5, the adhesive composition.
[5]
The method of claim 1 wherein the adhesive composition has solids content of 70 by weight based on the total weight of the composition unit or less, the pressure-sensitive adhesive composition.
[6]
The method of claim 1, wherein the pressure-sensitive adhesive composition, a primary alcohol, a polyhydric alcohol, a diol (diol) and triols (triol), further comprising at least one solvent selected from the group consisting of a pressure-sensitive adhesive composition.
[7]
Calibrate　
according to claim 6,
The solvent is methanol, ethanol, propan-2-ol, butane-1-ol, pentanol -1-ol and hexadecane-1-ol (hexadecan-1-ol) one or more monohydric alcohols (monohydric alcohol) selected from. Ethane-1,2-diol (ethane-1,2-diol), 1,2-diol (propane-1,2-diol), propane-1,2,3-triol (propane-1,2 , 3-triol), butane-1,3-diol (butane-1,3-diol), butane-1, & all (butane-1,2,3,4-tetraol), pentane -1,2,3,4,5- phentolamine (pentane-1,2,3,4,5-pentol), hexane-1,2,3-hexane -1,2,3,4,5,6- heksol , 4,5,6-hexol), heptane -1,2,3,4,5,6,7- heptol (one or more selected from the group consisting of heptane-1,2,3,4,5,6,7-heptol) polyol (polyhydric alcohols); Pro-2-en-1-ol (Prop-2-ene-1-ol), 3,7- dimethyl-octa-2,6-diene-1-ol (3,7-Dimethylocta-2,6-dien-1 -ol), Pro-yn-1- ol -2 (Prop-2-yn-1-ol) at least one unsaturated aliphatic alcohol selected from the group consisting of (unsaturated aliphatic alcohols); Cyclohexane -1,2,3,4,5,6- heksol (cyclohexane-1,2,3,4,5,6-hexol), 2- (2- propyl) -5-methyl-1-cyclohexanone ol (2- (2-propyl) -5-methyl-cyclohexane-1-ol) at least one aliphatic alcohol selected from the group consisting of (alicyclic alcohols) or a mixture of pressure-sensitive adhesive composition.
[8]
The method of claim 1 wherein the adhesive composition is stored at -18 to 45 ℃ if more than 14 days would precipitate that is not formed, the pressure-sensitive adhesive composition.
[9]
The method comprising mixing a lysine, itaconic acid, and water; And the method comprising, in the adhesive composition of lysine, itaconic acid and the water content is made in the control so that the precipitation of lysine and itaconic acid is not formed, the pressure-sensitive adhesive composition; and stirring the mixture below 80 ℃.
[10]
10. The method of claim 9, wherein the mixing molar ratio of the lysine and itaconic acid 2.3: 1 to 1: 1.5, for producing a pressure-sensitive adhesive composition.
[11]
10. The method of claim 9, wherein the mixture is a primary alcohol, a polyhydric alcohol, a diol, further comprising at least one solvent selected from the group consisting of (diol) and triols (triol), process for preparing a pressure-sensitive adhesive composition.
[12]
A first pressure-sensitive adhesive product comprising a pressure-sensitive adhesive composition of any one of to claim 8.