Aqueous dispersion of ethylene-carboxylic acid copolymer and method for producing the same
By adding an inorganic salt compound to a mixed solution of ethylene-(meth)acrylic acid copolymer and a basic compound, the method addresses gelation and high viscosity issues, enabling high-concentration, low-viscosity aqueous dispersions for coating and adhesive applications.
Patent Information
- Application Number
- JP2020167382
- Authority / Receiving Office
- JP · JP
- Patent Type
- Patents
- Current Assignee / Owner
- Priority Date
- 2019-11-11
- Filing Date
- 2020-10-02
- Publication Date
- 2025-08-12
- Estimated Expiration
- 2040-10-02
AI Technical Summary
Existing aqueous dispersions of ethylene-carboxylic acid copolymers face issues with gelation and high viscosity, making them unsuitable for applications as coating agents and adhesives, especially at high concentrations.
A method involving mixing ethylene-(meth)acrylic acid copolymer, a basic compound, and water to form a mixed solution, followed by adding an inorganic salt compound, which reduces viscosity and enhances dispersibility, allowing for high concentration dispersions.
The method effectively controls viscosity, inhibits gelation, and maintains high ethylene-carboxylic acid copolymer concentration, improving coatability and application efficiency.
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Abstract
Description
[Technical Field]
[0001] The present invention relates to an aqueous dispersion of an ethylene-carboxylic acid copolymer and a method for producing the same, and more particularly to an aqueous dispersion containing an ethylene-carboxylic acid copolymer and an inorganic additive and a method for producing the same. [Background technology]
[0002] In recent years, ethylene-carboxylic acid copolymers have been used in a variety of applications, such as coating materials, sealing materials, adhesives, packing materials, optical films, etc. Ethylene-carboxylic acid copolymers can be produced by polymerizing ethylene and acrylic acid or methacrylic acid as comonomers in a continuous reactor.
[0003] Ethylene-carboxylic acid copolymers can be dispersed in water and used as coating agents, sealants, adhesives, etc. After the dispersion is applied to the target material, the coating, sealing, adhesion, etc. can be achieved by drying the water.
[0004] When drying the dispersion, the lower the water content (the higher the concentration of ethylene-carboxylic acid copolymer), the more efficiently coating, sealing, bonding, etc. can be performed by evaporating a smaller amount of water.
[0005] Furthermore, the smaller the water content in the dispersion is for the same amount of ethylene-carboxylic acid copolymer, the more advantageous it is in terms of transportation costs.
[0006] However, as the concentration of the ethylene-carboxylic acid copolymer increases, the viscosity of the dispersion increases, which can lead to gelation, significantly deteriorating the coatability of the dispersion and making it unsuitable for use as a coating agent, sealant, adhesive, etc.
[0007] For example, U.S. Pat. No. 6,852,792 discloses an aqueous dispersion for a seal containing an ethylene-carboxylic acid copolymer. However, there is still a need for the development of an aqueous dispersion that is inhibited from gelling, has a low viscosity, and contains a high content of an ethylene-carboxylic acid copolymer. [Prior art documents] [Patent documents]
[0008] [Patent Document 1] U.S. Patent No. 6,852,792 Summary of the Invention [Problem to be solved by the invention]
[0009] An object of the present invention is to provide an aqueous dispersion of an ethylene-carboxylic acid copolymer having excellent dispersibility.
[0010] An object of the present invention is to provide a method for producing an aqueous dispersion of an ethylene-carboxylic acid copolymer having excellent dispersibility. [Means for solving the problem]
[0011] A method for producing an aqueous dispersion of an ethylene-carboxylic acid copolymer according to an exemplary embodiment of the present invention includes the steps of mixing 30 wt % or more of an ethylene-(meth)acrylic acid copolymer, a basic compound, and water to form a mixed solution, and adding an inorganic salt compound to the mixed solution.
[0012] In an exemplary embodiment, the step of forming the mixed solution can include stirring at a temperature of 80° C. or higher.
[0013] In an exemplary embodiment, the step of adding the inorganic salt compound can include adding an aqueous solution of the inorganic salt compound.
[0014] In an exemplary embodiment, the step of adding the inorganic salt compound can include stirring at a temperature of 60-80°C.
[0015] In an exemplary embodiment, the inorganic salt compound may be added in an amount of 0.01 to 0.3% by weight based on the total weight of the aqueous dispersion.
[0016] In an exemplary embodiment, the inorganic salt compound can include at least one selected from the group consisting of sodium chloride (NaCl), calcium chloride (CaCl), sodium sulfite (NaSO), sodium sulfate (NaSO), sodium carbonate (NaCO), potassium chloride (KCl), trisodium phosphate (NaPO), and ammonium chloride (NHCl).
[0017] In an exemplary embodiment, the ethylene-(meth)acrylic acid copolymer can include 70 to 85 weight percent units derived from ethylene and 15 to 30 weight percent units derived from (meth)acrylic acid.
[0018] In an exemplary embodiment, the ethylene-(meth)acrylic acid copolymer may have a weight average molecular weight (Mw) of 10,000 to 60,000.
[0019] In an exemplary embodiment, the basic compound can be mixed in an amount of 1 to 12% by weight based on the total weight of the mixed solution.
[0020] In an exemplary embodiment, the viscosity of the mixed solution before adding the inorganic salt compound may be 6,000 cP or more, and the viscosity of the aqueous dispersion after adding the inorganic salt compound may be 5,000 cP or less.
[0021] In an exemplary embodiment, the viscosity of the aqueous dispersion containing the ethylene-(meth)acrylic acid copolymer and the inorganic salt compound may be 60% or less of the viscosity of the mixed solution containing the ethylene-(meth)acrylic acid copolymer.
[0022] The aqueous ethylene-carboxylic acid copolymer dispersion according to an exemplary embodiment of the present invention contains 30% by weight or more of an ethylene-(meth)acrylic acid copolymer, a basic compound, an inorganic salt compound, and the balance of water.
[0023] In an exemplary embodiment, the inorganic salt compound may be included in an amount of 0.01 to 0.3% by weight based on the total weight of the aqueous dispersion.
[0024] In an exemplary embodiment, the inorganic salt compound can include at least one selected from the group consisting of sodium chloride (NaCl), calcium chloride (CaCl), sodium sulfite (NaSO), sodium sulfate (NaSO), sodium carbonate (NaCO), potassium chloride (KCl), trisodium phosphate (NaPO), and ammonium chloride (NHCl).
[0025] In an exemplary embodiment, the ethylene-(meth)acrylic acid copolymer can include 70 to 85 weight percent units derived from ethylene and 15 to 30 weight percent units derived from (meth)acrylic acid.
[0026] In an exemplary embodiment, the basic compound can be included in an amount of 1 to 12% by weight based on the total weight of the aqueous dispersion.
[0027] The coated film according to an exemplary embodiment of the present invention contains 30% by weight or more of an ethylene-(meth)acrylic acid copolymer, a basic compound, and an inorganic salt compound.
[0028] A multilayer film according to an exemplary embodiment of the present invention comprises the coated film.
[0029] In an exemplary embodiment, the multilayer film may include the coated film, a polyolefin layer adhered to one side of the coated film, and an aluminum layer adhered to the other side of the coated film. [Effects of the Invention]
[0030] According to an exemplary embodiment of the present invention, the ethylene-(meth)acrylic acid copolymer can be effectively dispersed in an aqueous dispersion by adding an inorganic salt compound to the aqueous dispersion, thereby easily adjusting the viscosity of the aqueous dispersion and providing an aqueous dispersion of the ethylene-(meth)acrylic acid copolymer having a high concentration and low viscosity.
[0031] This can improve the coatability of the aqueous dispersion and inhibit gelation. [Brief explanation of the drawings]
[0032] [Figure 1] FIG. 1 is a schematic flow chart illustrating a method for producing an aqueous dispersion of an ethylene-carboxylic acid copolymer according to an exemplary embodiment of the present invention. [Figure 2] FIG. 2 is a graph showing the viscosity of aqueous dispersions depending on the concentration of copolymer and the concentration of basic compound according to an exemplary embodiment. [Figure 3] FIG. 3 is a schematic cross-sectional view showing a coated film and a multilayer film including the coated film according to an exemplary embodiment of the present invention. [Figure 4] FIG. 4 is a graph showing the change in viscosity of an aqueous dispersion when an inorganic salt compound is added according to an exemplary embodiment of the present invention. [Figure 5] FIG. 5 is a graph showing the change in viscosity of an aqueous dispersion in the copolymer concentration range of 35 to 41 wt % due to the addition of an inorganic salt compound. [Figure 6] FIG. 6 is a graph showing the relationship between the type and concentration of inorganic salt compounds and the viscosity of the aqueous dispersion according to an exemplary embodiment. DETAILED DESCRIPTION OF THE INVENTION
[0033] In an exemplary embodiment of the present invention, a method for producing an aqueous dispersion of an ethylene-carboxylic acid copolymer includes mixing 30% by weight or more of an ethylene-(meth)acrylic acid copolymer, a basic compound, and water to form a mixed solution, and then adding an inorganic salt compound to the mixed solution, thereby easily producing an aqueous dispersion of an ethylene-carboxylic acid copolymer having a high concentration and low viscosity.
[0034] An exemplary embodiment of the present invention also provides an aqueous dispersion of an ethylene-carboxylic acid copolymer.
[0035] As used herein, the term "(meth)acrylic acid" includes both acrylic acid and methacrylic acid.
[0036] FIG. 1 is a schematic flow chart illustrating a method for producing an aqueous dispersion of an ethylene-carboxylic acid copolymer according to an exemplary embodiment of the present invention.
[0037] According to an exemplary embodiment, an ethylene-(meth)acrylic acid copolymer, a basic compound, and water may be mixed to prepare a mixed solution (eg, step S10).
[0038] The ethylene-(meth)acrylic acid copolymer may be mixed in an amount of 30 wt % or more based on the total weight of the mixed solution. Thus, the aqueous dispersion prepared according to an exemplary embodiment of the present invention may contain the ethylene-(meth)acrylic acid copolymer at a high concentration. Preferably, the ethylene-(meth)acrylic acid copolymer may be mixed in an amount of 40 wt % or more, more preferably 42 wt % or 45 wt % or more.
[0039] In an exemplary embodiment, the ethylene-(meth)acrylic acid copolymer may be mixed in an amount of 49 wt% or less based on the total weight of the mixed solution. If the content exceeds this amount, gelation of the ethylene-(meth)acrylic acid copolymer is promoted, and it may be substantially difficult to adjust the viscosity of the ethylene-carboxylic acid copolymer aqueous dispersion to a range suitable for use as a coating agent.
[0040] In an exemplary embodiment, the weight average molecular weight (Mw) of the ethylene-(meth)acrylic acid copolymer may be 10,000 to 60,000. The weight average molecular weight may be preferably 10,000 to 40,000, and more preferably 20,000 to 40,000.
[0041] For example, the weight-average molecular weight of the ethylene-(meth)acrylic acid copolymer may be 15,000 to 25,000 (first copolymer). By adding an inorganic salt compound to the aqueous dispersion of the first copolymer, the viscosity of the aqueous dispersion can be effectively reduced.
[0042] The weight-average molecular weight of the ethylene-(meth)acrylic acid copolymer may be 25,000 to 35,000 (second copolymer). In the case of the second copolymer, the degree of viscosity increase may be greater even at the same copolymer concentration. Therefore, generally, if the concentration of the second copolymer exceeds 30% relative to the aqueous dispersion, the viscosity may increase too much. However, as described below, the viscosity of an aqueous dispersion of a high molecular weight copolymer can be effectively controlled by adding an inorganic salt compound.
[0043] In some embodiments, the ethylene-(meth)acrylic acid copolymer may have a polydispersity index of 2 to 5, preferably 2.5 to 4.
[0044] In an exemplary embodiment, the ethylene-(meth)acrylic acid copolymer can contain 70 to 85 wt% of units derived from ethylene and 15 to 30 wt% of units derived from (meth)acrylic acid. If the units derived from (meth)acrylic acid are less than 15 wt%, the ethylene-(meth)acrylic acid copolymer may not be dispersed in an aqueous solution. Preferably, the copolymer contains 75 to 80 wt% of units derived from ethylene and 20 to 25 wt% of units derived from (meth)acrylic acid.
[0045] In some embodiments, the melting point (Tm) of the ethylene-(meth)acrylic acid copolymer may be 50 to 100°C. This allows the aqueous dispersion to be applied at low temperatures as a coating agent, sealant, adhesive, etc. The melting point may be preferably 60 to 95°C, and more preferably 70 to 80°C.
[0046] The ethylene-(meth)acrylic acid copolymer can have acidity due to the carboxyl groups of the units derived from (meth)acrylic acid, and the basic compound can neutralize the carboxyl groups of the units derived from (meth)acrylic acid.
[0047] In an exemplary embodiment, the basic compound can include at least one selected from the group consisting of ammonium hydroxide (NH4OH), lithium hydroxide (LiOH), sodium hydroxide (NaOH), potassium hydroxide (KOH), cesium hydroxide (CsOH), and an organic amine compound.
[0048] The basic compound can undergo an acid-base neutralization reaction with the carboxyl groups of the (meth)acrylic acid-derived units of the ethylene-(meth)acrylic acid copolymer. In this case, the dispersibility of the ethylene-(meth)acrylic acid copolymer in water can be increased. In an exemplary embodiment, the basic compound can be contained in an amount of 1 to 12 wt % based on the total weight of the mixed solution. If the content of the basic compound is less than 1 wt %, the neutralization reaction of the carboxyl groups of the (meth)acrylic acid-derived units may be insufficient. This may result in a decrease in the water dispersibility of the ethylene-(meth)acrylic acid copolymer. If the content of the basic compound exceeds 12 wt %, the ethylene-(meth)acrylic acid copolymer may be over-neutralized, resulting in an increase in the viscosity of the aqueous dispersion. Preferably, the basic compound can be contained in an amount of 2 to 6 wt % based on the total weight of the mixed solution.
[0049] Water can be provided as a solvent and / or dispersion medium for the ethylene-(meth)acrylic acid copolymer and the basic compound. In some embodiments, the water can include purified water or deionized water.
[0050] In an exemplary embodiment, the mixed solution may contain water as the balance relative to the total content of the ethylene-(meth)acrylic acid copolymer and the basic compound. In one embodiment, the mixed solution may contain no components other than the ethylene-carboxylic acid copolymer, the basic compound, and the balance of water.
[0051] In an exemplary embodiment, the step (S10) of forming the mixed solution can be performed by stirring at a temperature of 80°C or higher. In this case, the neutralization reaction between the ethylene-(meth)acrylic acid copolymer and the basic compound can be promoted, and the at least partially neutralized ethylene-(meth)acrylic acid copolymer and unreacted ethylene-(meth)acrylic acid copolymer can be effectively dissolved in water. Preferably, the mixing can be performed at a temperature of 90°C or higher.
[0052] In an exemplary embodiment, the viscosity of the mixed solution may be 6,000 cP or more. The viscosity may be the viscosity at room temperature (25°C). In this case, the coatability of the aqueous dispersion at room temperature may be insufficient.
[0053] In an exemplary embodiment, an inorganic salt compound can be added to the mixed solution (eg, step S20).
[0054] The inorganic salt compound can be dissolved in the mixed solution to increase the ion concentration in the mixed solution, and the ethylene-(meth)acrylic acid copolymer, which is at least partially ionized by the neutralization reaction, can be effectively dispersed in the mixed solution due to the repulsive forces between the ions, thereby effectively reducing the viscosity of the aqueous dispersion.
[0055] For example, when the inorganic salt compound is mixed with the ethylene-(meth)acrylic acid copolymer, the basic compound, and water in producing the mixed solution (e.g., step S10), the inorganic salt compound dissociated in water may not affect the viscosity reducing effect of the aqueous dispersion.
[0056] In an exemplary embodiment, the inorganic salt compound may be added in an amount of 0.01 to 0.3 wt % based on the total weight of the aqueous dispersion. If the content of the inorganic salt compound is less than 0.01 wt %, the viscosity reducing effect of the aqueous dispersion of the ethylene-(meth)acrylic acid copolymer may be insufficient. If the content of the inorganic salt compound is more than 0.3 wt %, the inorganic salt compound may form a precipitate in the aqueous dispersion of the ethylene-carboxylic acid copolymer. Preferably, the content of the inorganic salt compound is 0.04, 0.07, or 0.1 wt % or more, and may be 0.2 wt % or less.
[0057] In an exemplary embodiment, the inorganic salt compound may include at least one selected from the group consisting of sodium chloride (NaCl), calcium chloride (CaCl), sodium sulfite (NaSO), sodium sulfate (NaSO), sodium carbonate (NaCO), potassium chloride (KCl), trisodium phosphate (NaPO), and ammonium chloride (NHCl). Preferably, sodium chloride (NaCl) and sodium sulfite (NaSO) can be used, since they can minimize the influence of the packaging film formed from the copolymer aqueous dispersion on the packaged article.
[0058] In an exemplary embodiment, the inorganic salt compound may be added to the mixed solution in the form of an aqueous solution. For example, the inorganic salt compound may be dissolved in water to prepare an aqueous solution of the inorganic salt compound, and the aqueous solution of the inorganic salt compound may then be added to the mixed solution to prepare the aqueous dispersion of the ethylene-carboxylic acid copolymer. In this case, the amount of the inorganic salt compound used may be adjusted based on the total weight of the aqueous dispersion of the ethylene-carboxylic acid copolymer.
[0059] In an exemplary embodiment, the step of adding the inorganic salt compound can be carried out at a temperature of 60 to 80°C. For example, the aqueous solution of the inorganic salt compound can be added to the mixed solution and stirred at a temperature of 60 to 80°C. If the inorganic salt compound is added at a temperature below 60°C, the viscosity of the mixed solution increases as the temperature drops, making it difficult to uniformly stir the aqueous solution of the inorganic salt compound and the mixed solution, and the viscosity-reducing effect of the inorganic salt compound may be reduced. If the inorganic salt compound is added at a temperature above 80°C, the amount of water evaporated from the aqueous dispersion during addition may increase, and the concentration of the ethylene-(meth)acrylic acid copolymer may increase too much. This may make it difficult to adjust the viscosity of the aqueous dispersion to the desired range.
[0060] In an exemplary embodiment, the viscosity of the ethylene-carboxylic acid copolymer aqueous dispersion containing the inorganic salt compound may be 6,000 cP or less. Within this range, the aqueous dispersion can be uniformly applied even at room temperature. The viscosity may be preferably 5,000 cP or less or 3,000 cP or less, and more preferably 1,000 cP or less.
[0061] In an exemplary embodiment, the viscosity of the aqueous dispersion may be 60% or less of the viscosity of the mixed solution. For example, the addition of the inorganic salt compound can reduce the viscosity of the aqueous dispersion to 60% or less. As a result, even if the mixed solution contains a high concentration of ethylene-(meth)acrylic acid copolymer and has a high viscosity, the viscosity can be effectively adjusted using the inorganic salt compound. Preferably, the viscosity of the aqueous dispersion may be 20% or less, 15% or less, or 10% or less of the viscosity of the mixed solution.
[0062] The ethylene-carboxylic acid copolymer aqueous dispersion contains an ethylene-(meth)acrylic acid copolymer aqueous dispersion, a basic compound, an inorganic salt compound, and the remaining amount of water.
[0063] The ethylene-(meth)acrylic acid copolymer is contained in an amount of 30% by weight or more, preferably 40% by weight or more, more preferably 41% by weight or more, or 45% by weight or more, based on the total weight of the aqueous dispersion.
[0064] In an exemplary embodiment, the basic compound can include at least one selected from the group consisting of ammonium hydroxide (NH4OH), lithium hydroxide (LiOH), sodium hydroxide (NaOH), potassium hydroxide (KOH), cesium hydroxide (CsOH), and an organic amine compound.
[0065] The basic compound can undergo an acid-base neutralization reaction with the carboxyl group of the (meth)acrylic acid-derived unit of the ethylene-(meth)acrylic acid copolymer, which increases the dispersibility of the ethylene-(meth)acrylic acid copolymer in water and prevents gelation.
[0066] In an exemplary embodiment, the basic compound may be contained in an amount of 1 to 12 wt % based on the total weight of the ethylene-carboxylic acid copolymer aqueous dispersion. If the content of the basic compound is less than 1 wt %, the neutralization reaction of the carboxyl groups of the (meth)acrylic acid-derived units may be insufficient. This may result in a decrease in the aqueous dispersibility of the ethylene-(meth)acrylic acid copolymer. If the content of the basic compound exceeds 12 wt %, the ethylene-(meth)acrylic acid copolymer may be over-neutralized, resulting in an increase in the viscosity of the aqueous dispersion. Preferably, the basic compound may be contained in an amount of 2 to 6 wt % based on the total weight of the ethylene-carboxylic acid copolymer aqueous dispersion.
[0067] In this specification, the phrase "the ethylene-carboxylic acid copolymer aqueous dispersion contains an inorganic salt compound" can encompass the case where the aqueous dispersion contains ions dissociated from the inorganic salt compound.
[0068] The inorganic salt compound can improve the water dispersibility of the ethylene-(meth)acrylic acid copolymer, for example, by dissolving the inorganic salt compound in water, the inorganic salt compound can increase the ion concentration in the aqueous dispersion.
[0069] In an exemplary embodiment, the inorganic salt compound may be contained in an amount of 0.01 to 0.3 wt % based on the total weight of the aqueous dispersion. If the content of the inorganic salt compound is less than 0.01 wt %, the viscosity of the aqueous dispersion of the ethylene-(meth)acrylic acid copolymer may not be sufficiently reduced. If the content of the inorganic salt compound is more than 0.3 wt %, the inorganic salt compound may cause some of the components of the aqueous dispersion of the ethylene-carboxylic acid copolymer to solidify, forming a precipitate in the dispersion.
[0070] In an exemplary embodiment, the inorganic salt compound may include at least one selected from the group consisting of sodium chloride (NaCl), calcium chloride (CaCl), sodium sulfite (NaSO), sodium sulfate (NaSO), sodium carbonate (NaCO), potassium chloride (KCl), trisodium phosphate (NaPO), and ammonium chloride (NHCl). Preferably, sodium chloride (NaCl) and sodium sulfite (NaSO) can be used, since they can minimize the influence of the packaging film formed from the copolymer aqueous dispersion on the packaged article.
[0071] Water can be provided as a solvent and / or dispersion medium for the ethylene-(meth)acrylic acid copolymer, the basic compound, and the inorganic salt compound. In some embodiments, the water can include pure water or deionized water. For example, the basic compound and the inorganic salt compound can be dissolved in water and exist substantially in an ionic state.
[0072] In an exemplary embodiment, water may be included as the balance relative to the ethylene-carboxylic acid copolymer, the basic compound, and the inorganic salt compound. In one embodiment, the aqueous dispersion may contain no components other than the ethylene-carboxylic acid copolymer, the basic compound, the inorganic salt compound, and the balance of water.
[0073] The aqueous dispersion of the ethylene-carboxylic acid copolymer may have a viscosity of about 6,000 cP or less when the concentration of the copolymer is about 41% by weight. The aqueous dispersion may also have a viscosity of about 1,000 cP or less or about 500 cP or less when the concentration of the copolymer is about 35% by weight. The viscosity may be measured at room temperature (25°C).
[0074] FIG. 2 is a graph showing the viscosity of aqueous dispersions depending on the concentration of copolymer and the concentration of basic compound according to an exemplary embodiment.
[0075] 2, the viscosity of the aqueous dispersion may vary depending on the concentration of the copolymer and the concentration of the basic compound contained in the aqueous dispersion. For example, when the concentration of the basic compound is constant, the viscosity of the aqueous dispersion may change as the concentration of the copolymer contained in the aqueous dispersion increases. In this case, the viscosity of the aqueous dispersion may increase as the concentration of the copolymer increases.
[0076] For example, when the concentration of the copolymer contained in the aqueous dispersion is constant, the viscosity of the aqueous dispersion may increase as the concentration of the basic compound increases.
[0077] In an exemplary embodiment, the aqueous dispersion may satisfy the following relational expression 1 when the content of the ethylene-(meth)acrylic acid copolymer is 35% by weight or more.
[0078] [Equation 1]
number
[0079] In Relational Formula 1, V may be the viscosity (cP) of the aqueous dispersion, and Ce may be the content (wt%) of the copolymer.
[0080] An aqueous dispersion satisfying the above-mentioned relational expression 1 can have a low viscosity even if it contains the copolymer at a high concentration. In this case, the concentration of the aqueous dispersion can be further increased while maintaining coatability.
[0081] In some embodiments, the aqueous dispersion may be free of an organic solvent, which allows the coating layer to be easily formed by evaporating the water after application of the aqueous dispersion.
[0082] The aqueous dispersion of the ethylene-carboxylic acid copolymer according to the exemplary embodiment can be used as a coating or bonding agent, for example, to coat the surface of a thin metal film.
[0083] FIG. 3 is a schematic cross-sectional view showing a coated film and a multilayer film including the coated film according to an exemplary embodiment of the present invention.
[0084] In an exemplary embodiment, the aqueous dispersion can be applied onto a substrate and then dried to form a coated film 10 .
[0085] The coated film 10 may have another layer laminated on at least one surface thereof to form a multilayer film 100. For example, an upper layer 20 may be laminated on the top of the coated film 10, and a lower layer 30 may be laminated on the bottom of the coated film 10 to form the multilayer film 100. The other layer may include a polymer film layer and a metal thin film layer.
[0086] For example, a polyolefin layer can be bonded to one side of the coated film 10 and an aluminum layer can be bonded to the other side to form the multilayer film 100.
[0087] The multilayer film 100 can be provided, for example, in food packaging.
[0088] Hereinafter, experimental examples including specific examples and comparative examples will be presented to aid in understanding the present invention, but these examples are merely illustrative of the present invention and do not limit the scope of the appended claims. It will be apparent to those skilled in the art that various changes and modifications can be made to these examples within the scope and technical spirit of the present invention, and it goes without saying that these changes and modifications also fall within the scope of the appended claims.
[0089] Example 1 Approximately 35% by weight of ethylene-carboxylic acid copolymer (weight ratio of ethylene:acrylic acid = 80:20, weight average molecular weight (Mw) = 30,000), approximately 3% by weight of NH4OH, and the remaining amount of distilled water were mixed at approximately 90°C for 1 hour to form a mixed solution. NaCl was dissolved in 3 mL of water to prepare an aqueous NaCl solution. The prepared NaCl aqueous solution was added to the mixed solution and stirred at about 70° C. to prepare an aqueous dispersion of the ethylene-carboxylic acid copolymer of the example. At this time, the content of NaCl was adjusted to 0.1% by weight based on the total weight of the aqueous dispersion of the ethylene-carboxylic acid copolymer.
[0090] Example 2 An aqueous dispersion was produced in the same manner as in Example 1, except that 41 wt % of ethylene-carboxylic acid copolymer was mixed when the mixed solution was formed.
[0091] Experimental Example 1 The viscosity was measured for the aqueous dispersions of Examples 1 and 2, and the mixed solutions of Examples 1 and 2 to which no NaCl aqueous solution was added (mixed solutions of Examples 1 and 2), and the graph shown in Figure 3 below was obtained. The viscosity was measured at room temperature (25°C) using a Brookfield viscometer with a plate spindle.
[0092] 4, the viscosity of the examples with added inorganic salt compounds was significantly reduced compared to the dispersions without added inorganic salt compounds (NaCl) (0 wt%). The viscosity of the aqueous dispersion with a concentration of 35 wt% was measured at approximately 6,848 cP before the addition of the inorganic salt compounds and approximately 463 cP after the addition of the inorganic salt compounds. The viscosity of the aqueous dispersion with a concentration of 41 wt% was measured at approximately 10,500 cP before the addition of the inorganic salt compounds and approximately 5,715 cP after the addition of the inorganic salt compounds.
[0093] The viscosity change trends were calculated based on the viscosities of aqueous dispersions without and with inorganic salt compounds at concentrations of 35% by weight and 41% by weight, and are shown in the graph in Figure 5.
[0094] Referring to FIG. 5, the viscosity (V) of the aqueous dispersion to which the inorganic salt compound is added can satisfy the following relational expression 1 when the content (Ce) of the ethylene-(meth)acrylic acid copolymer is 35% by weight or more.
[0095] [Equation 1]
number
[0096] Example 3 Approximately 35% by weight of ethylene-carboxylic acid copolymer (weight ratio of ethylene:acrylic acid = 80:20, weight average molecular weight (Mw) = 30,000), approximately 3% by weight of NH4OH, and the remaining amount of distilled water were mixed at approximately 90°C for 1 hour to form a mixed solution. Aqueous solutions of NaCl, CaCl2 and Na2SO3 were prepared by dissolving each of NaCl, CaCl2 and Na2SO3 in 3 mL of water. The aqueous solutions of NaCl, CaCl2, and Na2SO3 were added to the mixed solution to prepare an aqueous dispersion of ethylene-carboxylic acid copolymer, where the concentrations of NaCl, CaCl2, and Na2SO3 in the aqueous dispersion were adjusted to 0.04 and 0.07 wt%, respectively.
[0097] Experimental Example 2 The viscosity was measured for the aqueous dispersion of Example 3 and is shown in FIG. Referring to FIG. 6, it was confirmed that the viscosity of the aqueous dispersion can be effectively reduced by adjusting the type and concentration of the inorganic salt compound.
Claims
1. mixing 30% by weight or more of an ethylene-(meth)acrylic acid copolymer, a basic compound, and water to form a mixed solution; adding an inorganic salt compound to the mixed solution; The inorganic salt compound is added in an amount of 0.01 to 0.3% by weight based on the total weight of the aqueous dispersion; The inorganic salt compound is calcium chloride (CaCl 2 ) or sodium sulfite (Na 2 SO 3 ) a method for producing an aqueous dispersion of an ethylene-carboxylic acid copolymer,
2. The method for producing an aqueous dispersion of an ethylene-carboxylic acid copolymer according to claim 1, wherein the step of forming the mixed solution includes stirring at a temperature of 80°C or higher.
3. 2. The method for producing an aqueous dispersion of an ethylene-carboxylic acid copolymer according to claim 1, wherein the step of adding the inorganic salt compound includes adding an aqueous solution of the inorganic salt compound.
4. 2. The method for producing an aqueous dispersion of an ethylene-carboxylic acid copolymer according to claim 1, wherein the step of adding the inorganic salt compound comprises stirring at a temperature of 60 to 80°C.
5. The method for producing an aqueous dispersion of an ethylene-carboxylic acid copolymer according to claim 1, wherein the ethylene-(meth)acrylic acid copolymer contains 70 to 85% by weight of units derived from ethylene and 15 to 30% by weight of units derived from (meth)acrylic acid.
6. The method for producing an aqueous dispersion of an ethylene-carboxylic acid copolymer according to claim 1, wherein the ethylene-(meth)acrylic acid copolymer has a weight average molecular weight (Mw) of 10,000 to 60,000.
7. 2. The method for producing an aqueous dispersion of an ethylene-carboxylic acid copolymer according to claim 1, wherein the basic compound is mixed in an amount of 1 to 12% by weight based on the total weight of the mixed solution.
8. 2. The method for producing an aqueous dispersion of an ethylene-carboxylic acid copolymer according to claim 1, wherein the viscosity of the mixed solution before adding the inorganic salt compound is 6,000 cP or more, and the viscosity of the aqueous dispersion after adding the inorganic salt compound is 5,000 cP or less.
9. 2. The method for producing an aqueous dispersion of an ethylene-carboxylic acid copolymer according to claim 1, wherein the viscosity of the aqueous dispersion containing the ethylene-(meth)acrylic acid copolymer and the inorganic salt compound is 60% or less of the viscosity of the mixed solution containing the ethylene-(meth)acrylic acid copolymer.
10. containing 30% by weight or more of an ethylene-(meth)acrylic acid copolymer, 0.01 to 0.3% by weight of a basic compound, an inorganic salt compound, and the balance being water; The inorganic salt compound is calcium chloride (CaCl 2 ) or sodium sulfite (Na 2 SO 3 ) An aqueous dispersion of an ethylene-carboxylic acid copolymer.
11. The ethylene-carboxylic acid copolymer aqueous dispersion according to claim 10, wherein the ethylene-(meth)acrylic acid copolymer contains 70 to 85% by weight of units derived from ethylene and 15 to 30% by weight of units derived from (meth)acrylic acid.
12. 11. The ethylene-carboxylic acid copolymer aqueous dispersion according to claim 10, wherein the basic compound is contained in an amount of 1 to 12% by weight based on the total weight of the aqueous dispersion.
Citation Information
Patent Citations
Preparation of lowwviscosity aqueous polymer solution
JP1979061249A
Water-base dispersion and its use
JP1996188682A
Coating agent for paper-made container and container produced by using the same
JP2003336191A
Coating composition containing low mfi ethylene acrylic acid copolymer
JP2003529624A
Easily openable sealant film, packaging material and container using the same
JP2005263277A