Aqueous polyester resin dispersion composition and method for producing the same

By mixing specific concentrations of polyvinyl alcohol with a melt-kneaded polyester and polyvinyl alcohol mixture, the method achieves stable dispersion and excellent adhesiveness in polyester resin compositions, addressing the challenges of existing technologies.

JP7760505B2Active Publication Date: 2025-10-27SUMITOMO SEIKA CHEM CO LTD
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Patent Information

Application Number
JP2022536365
Authority / Receiving Office
JP · JP
Patent Type
Patents
Current Assignee / Owner
Priority Date
2020-07-14
Filing Date
2021-07-13
Publication Date
2025-10-27
Estimated Expiration
2041-07-13

AI Technical Summary

Technical Problem

Existing polyester resin aqueous dispersion compositions face challenges in achieving stable dispersion, good emulsification, and excellent adhesiveness, which are not adequately addressed by existing production methods.

Method used

A method involving the mixing of a specific concentration of an aqueous polyvinyl alcohol solution with a melt-kneaded mixture of polyester and polyvinyl alcohol, with a total content of 78 to 88% by mass, and subsequent processing using a twin-screw extruder to achieve a well-emulsified state with excellent adhesive properties.

Benefits of technology

The method efficiently produces an aqueous polyester resin dispersion that is well-emulsified and exhibits excellent adhesive properties, overcoming the limitations of previous methods.

✦ Generated by Eureka AI based on patent content.

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Abstract

Provided is a method that enables efficient production of a polyester aqueous dispersion composition having a fine emulsified state and excellent adhesive properties. More specifically, provided is a method for producing a polyester resin aqueous dispersion composition, the method comprising additionally mixing, to a melt kneaded product of a polyester and a polyvinyl alcohol, 3-10 mass% of a polyvinyl alcohol aqueous solution such that the total contained amount of the polyester and the polyvinyl alcohol in the resultant mixture becomes 78-88 mass%.
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Description

[Technical Field]

[0001] The present disclosure relates to a method for producing an aqueous polyester resin dispersion composition, etc. The contents of all documents described in this specification are incorporated herein by reference. [Background technology]

[0002] BACKGROUND ART Polyester resin aqueous dispersion compositions are used in a variety of applications, such as binders and fiber treatment agents. [Prior art documents] [Patent documents]

[0003] [Patent Document 1] Japanese Patent Application Laid-Open No. 2001-310944 [Patent Document 2] Japanese Patent Application Publication No. 10-139884 [Patent Document 3] Special Publication No. 2004-500466 [Patent Document 4] Japanese Patent Application Laid-Open No. 2011-032471 Summary of the Invention [Problem to be solved by the invention]

[0004] Considering these applications, it is preferable that the polyester resin aqueous dispersion composition is one in which the polyester resin is stably dispersed in an aqueous medium, has a good emulsified state, and has excellent adhesiveness.

[0005] The present inventors have conducted research to find a method for efficiently producing the preferred aqueous polyester dispersion composition. [Means for solving the problem]

[0006] The present inventors have found that it is possible to produce the preferred aqueous polyester resin dispersion composition by further mixing a specific concentration of aqueous polyvinyl alcohol solution with a melt-kneaded mixture of polyester and polyvinyl alcohol so that the total content of polyester and polyvinyl alcohol in the resulting mixture becomes a specific concentration, and have made further improvements.

[0007] The present disclosure includes, for example, the subject matter described in the following sections: Section 1. (2) Mixing the melt-kneaded mixture of polyester and polyvinyl alcohol with 3 to 10% by mass of an aqueous solution of polyvinyl alcohol so that the total content of polyester and polyvinyl alcohol in the resulting mixture is 78 to 88% by mass. A method for producing an aqueous polyester resin dispersion composition, comprising: Section 2. Before step (2), (1) Melt-kneading polyester and polyvinyl alcohol The method according to item 1, comprising: Section 3. Item 3. The method according to Item 2, wherein in step (1), 0.1 to 5 parts by mass of polyvinyl alcohol is melt-kneaded with respect to 100 parts by mass of polyester. Section 4. After step (2), (3) Adding water to the resulting mixture Item 4. The method according to any one of Items 1 to 3, comprising: Section 5. In step (3), water is added so that the polyester resin content in the composition after the addition of water is 40 to 70 mass%. The method described in item 4. Section 6. 6. The method according to any one of items 1 to 5, wherein the melt-kneaded mixture of polyester and polyvinyl alcohol in step (2) is a mixture obtained by melt-kneading them at a temperature equal to or higher than the melting point of the polyester and lower than the melting point of the polyvinyl alcohol. Section 7. Item 7. The method according to any one of Items 1 to 6, wherein the mixing in step (2) is carried out at a temperature equal to or higher than the melting point of the polyester and lower than the melting point of the polyvinyl alcohol, and lower than the temperature at which the melt-kneading for preparing the melt-kneaded product is carried out. Section 8. Item 8. The method according to any one of Items 1 to 7, wherein the amount of polyvinyl alcohol used in melt-kneading the polyester and polyvinyl alcohol and the amount of polyvinyl alcohol contained in the 3 to 10 mass% aqueous polyvinyl alcohol solution are 0.8 to 6 parts by mass relative to 1 part by mass of the former. Section 9. In a twin-screw extruder having a first feed port and a second feed port from the upstream side, introducing polyester and polyvinyl alcohol through a first supply port and melt-kneading the mixture; and supplying a 3 to 10 mass% aqueous polyvinyl alcohol solution through a second supply port and mixing the mixture so that the total content of polyester and polyvinyl alcohol in the mixture is 78 to 88 mass%; Including, A method for producing an aqueous polyester resin dispersion composition. Section 10. A twin-screw extruder having a first supply port, a second supply port, and a third supply port from the upstream side, A method for producing a mixture of polyester and polyvinyl alcohol, the method comprising: feeding a polyester and polyvinyl alcohol through a first supply port and melt-kneading the mixture; supplying a 3 to 10 mass% aqueous polyvinyl alcohol solution through a second supply port and mixing the resulting mixture so that the total content of the polyester and polyvinyl alcohol in the mixture is 78 to 88 mass%; and Supplying water from a third supply port; Including, A method for producing an aqueous polyester resin dispersion composition. Section A. 11. An aqueous polyester resin dispersion composition obtained by the production method according to any one of items 1 to 10. [Effects of the Invention]

[0008] A method is provided for efficiently producing an aqueous polyester dispersion composition that is in a well-emulsified state and has excellent adhesive properties. DETAILED DESCRIPTION OF THE INVENTION

[0009]

[0033] Each embodiment of the present disclosure will be described in more detail below. The present disclosure preferably includes a method for producing an aqueous polyester dispersion composition, but is not limited thereto. The present disclosure includes all of the disclosures herein that would be recognized by a person skilled in the art.

[0010] A method for producing an aqueous polyester dispersion composition included in the present disclosure includes (2) mixing a molten mixture of polyester and polyvinyl alcohol with 3 to 10 mass% of an aqueous polyvinyl alcohol solution so that the total content of polyester and polyvinyl alcohol in the resulting mixture is 78 to 88 mass%. In this specification, this production method included in the present disclosure may be referred to as the "production method of the present disclosure."

[0011] The polyester used in the manufacturing method of the present disclosure is preferably a copolymer of a dicarboxylic acid and a glycol. The copolymer can be obtained by condensation polymerization of a dicarboxylic acid and a glycol. The condensation polymerization can be carried out by, for example, a known method or a method that can be easily derived from a known method.

[0012] The polyester preferably has a melting point of about 50 to 200° C. The upper or lower limit of the melting point may be, for example, 60, 70, 80, 90, 100, 110, 120, 130, 140, 150, 160, 170, 180, or 190° C. For example, the melting point may be 60 to 190° C. The polyester preferably has a weight average molecular weight of about 5,000 to 60,000. The upper or lower limit of the range is, for example, 6000, 7000, 8000, 9000, 10000, 11000, 12000, 13000, 14000, 15000, 16000, 17000, 18000, 19000, 20000, 21000, 22000, 23000, 24000, 25000, 26000, 27000, 28000, 29000, 30000, 31000, 3200 It may be 0, 33000, 34000, 35000, 36000, 37000, 38000, 39000, 40000, 41000, 42000, 43000, 44000, 45000, 46000, 47000, 48000, 49000, 50000, 51000, 52000, 53000, 54000, 55000, 56000, 57000, 58000, or 59000. The range may be, for example, 6000 to 59000.

[0013] Preferred examples of the dicarboxylic acid include terephthalic acid, isophthalic acid, and orthophthalic acid. The dicarboxylic acid may be used alone or in combination of two or more.

[0014] Preferred examples of the glycol include ethylene glycol, diethylene glycol, polyethylene glycol, 1,3-propanediol, 1,4-butanediol, 1,6-hexanediol, etc. The glycols may be used alone or in combination of two or more.

[0015] The polyvinyl alcohol used in the production method of the present disclosure is preferably polyvinyl alcohol having a weight-average molecular weight of about 500 to 2500. The upper or lower limit of the weight-average molecular weight range may be, for example, 600, 700, 800, 900, 1000, 1100, 1200, 1300, 1400, 1500, 1600, 1700, 1800, 1900, 2000, 2100, 2200, 2300, or 2400. For example, the weight-average molecular weight may be 600 to 2400. Furthermore, polyvinyl alcohol having a saponification degree of 70 to 99 mol% is preferred. That is, polyvinyl alcohol is produced by saponifying polyvinyl acetate, and the saponification degree is preferably 70 to 99 mol%. The upper or lower limit of the degree of saponification may be, for example, 71, 72, 73, 74, 75, 76, 77, 78, 79, 80, 81, 82, 83, 84, 85, 86, 87, 88, 89, 90, 91, 92, 93, 94, 95, 96, 97, or 98 mol%. For example, the degree of saponification may be 71 to 98 mol%.

[0016] The melt-kneaded mixture of polyester and polyvinyl alcohol can be prepared using, for example, an extruder (particularly, a twin-screw extruder). The production method of the present disclosure may further include (1) melt-kneading polyester and polyvinyl alcohol before the above step (2).

[0017] In this specification, a resin obtained by melt-kneading a polyester and a polyvinyl alcohol is also referred to as a polyester resin. More specifically, the polyester resin in this specification can be referred to as a resin containing a polyester contained in a melt-kneaded mixture of a polyester and a polyvinyl alcohol.

[0018] The polyester resin is not particularly limited as long as it is a resin containing polyester. For example, it may be a resin consisting essentially of polyester alone, or a resin consisting essentially of polyester and polyvinyl alcohol. When the melt-kneading is performed at a temperature equal to or higher than the melting point of the polyester used and lower than the melting point of the polyvinyl alcohol used, the resulting polyester resin may be a resin consisting essentially of polyester alone. When a resin consisting essentially of polyester alone is obtained, the melt-kneading temperature varies depending on the melting point of the polyester used, but is exemplified by a temperature of about 100 to 180°C. The upper or lower limit of the range may be, for example, 101, 102, 103, 104, 105, 106, 107, 108, 109, 110, 111, 112, 113, 114, 115, 116, 117, 118, 119, 120, 121, 122, 123, 124, 125, 126, 127, 128, 129, 130, 131, 132, 133, 134, 135, 136, 137, 138, 139 , 140, 141, 142, 143, 144, 145, 146, 147, 148, 149, 150, 151, 152, 153, 154, 155, 156, 157, 158, 159, 160, 161, 162, 163, 164, 165, 166, 167, 168, 169, 170, 171, 172, 173, 174, 175, 176, 177, 178, or 179°C. For example, the range may be 110 to 170°C or 120 to 160°C.

[0019] When the polyester resin is a resin containing polyester and polyvinyl alcohol, the polyvinyl alcohol is preferably contained in an amount of, for example, 0.5 to 20 parts by mass per 100 parts by mass of the polyester resin. The upper or lower limit of this range may be, for example, 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, or 19 parts by mass. For example, this range may be 1 to 19 parts by mass. Furthermore, the ratio of the polyester to the polyvinyl alcohol is preferably 0.1 to 5 parts by mass of polyvinyl alcohol per 100 parts by mass of polyester. The upper or lower limit of the range may be 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1, 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, 1.9, 2, 2.1, 2.2, 2.3, 2.4, 2.5, 2.6, 2.7, 2.8, 2.9, 3, 3.1, 3.2, 3.3, 3.4, 3.5, 3.6, 3.7, 3.8, 3.9, 4, 4.1, 4.2, 4.3, 4.4, 4.5, 4.6, 4.7, 4.8, or 4.9 parts by mass. For example, the range may be 0.2 to 4 parts by mass.

[0020] The polyester resin preferably contains 90 to 100% by mass of polyester. The upper or lower limit of this range may be, for example, 91, 92, 93, 94, 95, 96, 97, 98, or 99% by mass. For example, the range may be 91 to 99% by mass. In addition to polyester and polyvinyl alcohol, the polyester resin may contain other resins as long as the effects of the composition of the present disclosure are not impaired. For example, it may contain a general thermoplastic resin other than polyester (such as polyolefin and its copolymer, polyamide, or polyurethane). It may also contain a polymeric emulsifier other than polyvinyl alcohol (such as ethylene oxide-propylene oxide copolymer, polyvinyl ether, polyacrylamide, or hydroxyethyl cellulose), a preservative, or the like. These components can be mixed into the polyester resin, for example, during the melt-kneading stage.

[0021] Although not particularly limited, the polyester resin is preferably a resin consisting essentially of polyester alone, or a resin consisting essentially of polyester and polyvinyl alcohol alone.

[0022] The median particle size of the polyester resin is preferably about 0.1 to 5 μm. The range may be, for example, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1, 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, 1.9, 2, 2.1, 2.2, 2.3, 2.4, 2.5, 2.6, 2.7, 2.8, 2.9, 3, 3.1, 3.2, 3.3, 3.4, 3.5, 3.6, 3.7, 3.8, 3.9, 4, 4.1, 4.2, 4.3, 4.4, 4.5, 4.6, 4.7, 4.8, or 4.9 μm. For example, the range may be 0.5 to 3 μm.

[0023] The median particle size is a median diameter measured by a laser diffraction particle size distribution analyzer. That is, it is a value obtained when the polyester resin aqueous dispersion composition is measured using a laser diffraction particle size distribution analyzer. An example of such an analyzer is the SALD2300 manufactured by Shimadzu Corporation.

[0024] In the step (2) of the manufacturing method of the present disclosure, a 3 to 10 mass% aqueous polyvinyl alcohol solution is further mixed with the melt-kneaded mixture of polyester and polyvinyl alcohol. The upper or lower limit of this range (3 to 10 mass%) may be, for example, 3.5, 4, 4.5, 5, 5.5, 6, 6.5, 7, 7.5, 8, 8.5, 9, or 9.5 mass%. For example, the range may be 3.5 to 8 mass%.

[0025] The mixing is performed so that the total content of polyester and polyvinyl alcohol in the resulting mixture is 78 to 88 mass%. That is, the total amount of polyester and polyvinyl alcohol present in the melt-kneaded mixture of polyester and polyvinyl alcohol and polyvinyl alcohol present in the 3 to 10 mass% aqueous polyvinyl alcohol solution is 78 to 88 mass% of the resulting mixture. The upper or lower limit of this range (78 to 88 mass%) may be, for example, 78.5, 79, 79.5, 80, 80.5, 81, 81.5, 82, 82.5, 83, 83.5, 84, 84.5, 85, 85.5, 86, 86.5, 87, or 87.5 mass%. The range may be, for example, 78.5 to 87.5 mass%.

[0026] The mixing can be carried out using, for example, an extruder (particularly, a twin-screw extruder).

[0027] The mixing is preferably carried out at a temperature equal to or higher than the melting point of the polyester used and lower than the melting point of the polyvinyl alcohol used. The temperature is preferably lower than the temperature at which the polyester and polyvinyl alcohol are melt-kneaded. Depending on the melting point of the polyester used, the temperature may be, for example, about 100 to 170°C. The upper and lower limits of the range are, for example, 101, 102, 103, 104, 105, 106, 107, 108, 109, 110, 111, 112, 113, 114, 115, 116, 117, 118, 119, 120, 121, 122, 123, 124, 125, 126, 127, 128, 129, 130, 131, 132, 133, 134 , 135, 136, 137, 138, 139, 140, 141, 142, 143, 144, 145, 146, 147, 148, 149, 150, 151, 152, 153, 154, 155, 156, 157, 158, 159, 160, 161, 162, 163, 164, 165, 166, 167, 168, or 169°C. For example, the range may be 110 to 165°C or 120 to 160°C.

[0028] By this mixing, the resulting mixed liquid can be preferably emulsified.

[0029] In the melt-kneading of polyester and polyvinyl alcohol, it is preferable to melt-knead, for example, about 0.1 to 5 parts by mass of polyvinyl alcohol to 100 parts by mass of polyester. The upper or lower limit of this range (0.1 to 5 parts by mass) may be 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1, 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, 1.9, 2, 2.1, 2.2, 2.3, 2.4, 2.5, 2.6, 2.7, 2.8, 2.9, 3, 3.1, 3.2, 3.3, 3.4, 3.5, 3.6, 3.7, 3.8, 3.9, 4, 4.1, 4.2, 4.3, 4.4, 4.5, 4.6, 4.7, 4.8, or 4.9 parts by mass. For example, the range may be 0.2 to 4 parts by mass.

[0030] Furthermore, the amount of polyvinyl alcohol used in melt-kneading the polyester and polyvinyl alcohol and the amount of polyvinyl alcohol contained in the 3 to 10 mass % aqueous polyvinyl alcohol solution used in step (2) are preferably, for example, about 0.2 to 50 mass parts of the latter relative to 1 mass part of the former. The upper or lower limit of this range (0.2 to 50 parts by mass) may be 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, or 49 parts by mass. For example, the range may be 0.6 to 6.5 parts by mass. The range is more preferably, for example, 0.8 to 6 parts by mass or 1 to 5 parts by mass.

[0031] The mixture obtained by the mixing in step (2) can be preferably used as the polyester resin aqueous dispersion composition of the present disclosure.

[0032] Furthermore, the production method of the present disclosure may further include (3) adding water to the resulting mixture after step (2) as needed (e.g., to reduce the viscosity or polyester resin concentration of the polyester resin aqueous dispersion composition). The water addition is preferably carried out so that the polyester resin content of the composition after water addition is 40 to 70% by mass. The upper or lower limit of this range may be, for example, 41, 42, 43, 44, 45, 46, 47, 48, 49, 50, 51, 52, 53, 54, 55, 56, 57, 58, 59, 60, 61, 62, 63, 64, 65, 66, 67, 68, or 69% by mass. For example, the range may be 45 to 65% by mass.

[0033] Steps (1) and (2) can be carried out more efficiently by using, for example, a twin-screw extruder equipped with a first supply port and a second supply port from the upstream side, and steps (1) to (3) can be carried out more efficiently by using, for example, a twin-screw extruder equipped with a first supply port, a second supply port, and a third supply port from the upstream side.

[0034] For example, from the first supply port, Steps (1) and (2) can be carried out by adding polyester and polyvinyl alcohol, melting and kneading them, and then supplying and mixing a 3 to 10 mass% aqueous polyvinyl alcohol solution from the second supply port so that the total content of polyester and polyvinyl alcohol in the resulting mixture is 78 to 88 mass%.

[0035] Alternatively, for example, step (3) can be carried out by further supplying water from a third supply port.

[0036] In this specification, the term "comprising" includes "consisting essentially of" and "consisting of." Furthermore, the present disclosure encompasses all arbitrary combinations of the constituent elements described in this specification.

[0037] Furthermore, the various characteristics (properties, structures, functions, etc.) described in each embodiment of the present disclosure above may be combined in any way to specify the subject matter encompassed by the present disclosure, i.e., the present disclosure encompasses all subject matter consisting of any combination of the combinable characteristics described herein. [Example]

[0038] Hereinafter, the embodiments of the present disclosure will be described more specifically with reference to examples, but the embodiments of the present disclosure are not limited to the following examples.

[0039] In the following studies, the polyvinyl alcohol used was "Poval 40-80E" (saponification degree 79 to 81 mol%), a product name of Kuraray Co., Ltd.

[0040] Example 1 Two hoppers were installed at the first feed port located 80 mm from the upstream tip of a twin-screw extruder (PCM-30, manufactured by Ikegai Corporation, L / D = 4 1.5, cylinder length 1260 mm), and polyester (melting point 95°C) and polyvinyl alcohol were fed into each hoppers at a rate of 40 kg / h and 0.48 kg / h, respectively.

[0041] The materials were melt-kneaded at a cylinder temperature of 140°C and a rotation speed of 450 rpm up to a second supply port located 480 mm from the upstream tip of the twin-screw extruder, and then an aqueous polyvinyl alcohol solution with a concentration of 8% by mass was supplied from the second supply port at a rate of 9.2 kg / hour using a plunger pump.

[0042] The mixture was mixed and emulsified from the second feed port to the third feed port, located 1000 mm from the upstream end of the twin-screw extruder, at a cylinder temperature of 120°C, a rotation speed of 450 rpm, and a solids concentration (total of polyester and polyvinyl alcohol) of 83% by mass. Then, 29.5 kg / h of pure water was fed into the third feed port using a plunger pump. Mixing was continued from the third feed port to the twin-screw extruder outlet at a cylinder temperature of 90°C and a rotation speed of 450 rpm. The mixture was then discharged from the twin-screw extruder. This operation was continued for 10 minutes until operation stabilized. The switch valve was then opened, and the aqueous polyester resin dispersion was placed in a 5-L stirring vessel equipped with a propeller-type stirring rod (propeller diameter 58 mm, three blades) and stirred at 500 rpm.

[0043] The dispersion stirred in the stirring tank was poured into the inlet of a cooling tube and cooled at a cooling temperature of 40°C. After that, the dispersion was discharged from the outlet of the cooling tube, which was located 10,800 mm from the inlet of the cooling tube, to obtain an aqueous dispersion of polyester resin.

[0044] Example 2 An aqueous dispersion of a polyester resin was obtained by the same operation as in Example 1, except that polyvinyl alcohol was supplied from the first supply port at 0.4 kg / hour, an aqueous polyvinyl alcohol solution having a concentration of 8% by mass was supplied from the second supply port at 10.3 kg / hour, and pure water was supplied from the third supply port at 28.6 kg / hour, so that the solid content concentration from the second supply port to the third supply port would be 81.3%.

[0045] Example 3 An aqueous dispersion of a polyester resin was obtained by the same operation as in Example 1, except that polyvinyl alcohol was supplied from the first supply port at 0.6 kg / hour, an aqueous polyvinyl alcohol solution having a concentration of 8% by mass was supplied from the second supply port at 7.7 kg / hour, and pure water was supplied from the third supply port at 30.9 kg / hour, so that the solid content concentration from the second supply port to the third supply port would be 85.3%.

[0046] Example 4 An aqueous dispersion of polyester resin was obtained in the same manner as in Example 1, except that the pure water supplied from the third supply port was changed to 19.0 kg / hour.

[0047] Example 5 An aqueous dispersion of polyester resin was obtained in the same manner as in Example 1, except that the polyester resin and polyvinyl alcohol were supplied from the first supply port at 30 kg / h, 0.4 kg / h, an aqueous polyvinyl alcohol solution having a concentration of 8% by mass was supplied from the second supply port at 6.9 kg / h, and pure water was supplied from the third supply port at 22.1 kg / h.

[0048] Comparative Example 1 An aqueous dispersion of a polyester resin was obtained by the same operation as in Example 1, except that polyvinyl alcohol was supplied from the first supply port at 0.20 kg / hour, an aqueous polyvinyl alcohol solution having a concentration of 8% by mass was supplied from the second supply port at 17.5 kg / hour, and pure water was supplied from the third supply port at 22.3 kg / hour, so that the solid content concentration from the second supply port to the third supply port would be 72.1%.

[0049] Comparative Example 2 The same operation as in Example 1 was performed, except that polyvinyl alcohol was supplied from the first supply port at 0.8 kg / h, an aqueous polyvinyl alcohol solution having a concentration of 8% by mass was supplied from the second supply port at 5.0 kg / h, and pure water was supplied from the third supply port at 33.4 kg / h so that the solids concentration from the second supply port to the third supply port would be 90.0%. However, the inside of the twin-screw extruder was clogged with unemulsified polyester resin, and an aqueous dispersion of polyester resin could not be obtained.

[0050] The polyester resin aqueous dispersions obtained in each of the Examples and Comparative Examples were evaluated for median particle size and emulsion state by the following methods.

[0051] <Median particle size> The median particle size of the dispersed particles in the obtained polyester resin aqueous dispersion was measured using a laser diffraction particle size distribution measuring device (trade name "SALD-2300" manufactured by Shimadzu Corporation).

[0052] <Emulsified state> The emulsified state of the resulting polyester resin aqueous dispersion was visually evaluated according to the following criteria. ○: No unemulsified matter ×: Unemulsified matter present

[0053] [Table 1]

[0054] The polyester resin aqueous dispersion of Example 1 was evaluated for adhesiveness by the following method, and the evaluation was good.

[0055] <Adhesiveness> The polyester resin aqueous dispersion obtained in Example 1 was applied to an aluminum foil (width: 25 mm, thickness: 30 μm) using a coating machine (Bar Coater No. 4, manufactured by Nippon Cedars Service Co., Ltd.) so that the thickness of the film after drying would be approximately 4 μm. The aluminum foil coated with the dispersion was dried by heating in an oven at 100° C. for 1 minute to form a film.

[0056] Next, a PVC (polyvinyl chloride) (width: 25 mm) adherend was bonded to the obtained film using a heat sealing machine (product name "TP-701" manufactured by Tester Sangyo Co., Ltd.). The heat sealing conditions were a sealing temperature of 140°C and a sealing pressure of 2 kg / cm. 2 The sealing time was 3 seconds, and the resulting heat-sealable substrate (PVC / dispersion coating / aluminum foil) (width: 25 mm) was used as a test piece. After cooling the test piece, a T-peel test was performed using a tensile tester (Shimadzu Corporation, trade name "Autograph AGS-J") at a tension speed of 50 mm / min. This allowed the peel strength of the coating to be measured and the adhesiveness to be evaluated. The evaluation criteria were as follows: ○: Peel strength 15N / 25mm or more ×: Peel strength less than 15N / 25mm

[0057] In addition, evaluation was impossible for all of the comparative examples due to poor emulsification. The results are shown in the table below.

[0058] [Table 2]

Claims

1. (2) Mixing the melt-kneaded mixture of polyester and polyvinyl alcohol with 3 to 10% by mass of an aqueous solution of polyvinyl alcohol so that the total content of polyester and polyvinyl alcohol in the resulting mixture is 78 to 88% by mass. A method for producing an aqueous polyester resin dispersion composition, comprising:

2. Before step (2), (1) Melting and kneading polyester and polyvinyl alcohol The method of claim 1 , comprising:

3. The method according to claim 2, wherein in the step (1), 0.1 to 5 parts by mass of polyvinyl alcohol is melt-kneaded with respect to 100 parts by mass of polyester.

4. After step (2), (3) adding water to the resulting mixture; The method according to any one of claims 1 to 3, comprising:

5. In step (3), water is added so that the polyester resin content in the composition after the addition of water is 40 to 70 mass%. The method of claim 4.

6. The method according to any one of claims 1 to 5, wherein the melt-kneaded mixture of the polyester and the polyvinyl alcohol in step (2) is a mixture obtained by melt-kneading the polyester and the polyvinyl alcohol at a temperature equal to or higher than the melting point of the polyester and lower than the melting point of the polyvinyl alcohol.

7. The method according to any one of claims 1 to 6, wherein the mixing in step (2) is carried out at a temperature that is equal to or higher than the melting point of the polyester and lower than the melting point of the polyvinyl alcohol, and is equal to or lower than the temperature at which melt-kneading for preparing the melt-kneaded product is carried out.

8. The method according to any one of claims 1 to 7, wherein the amount of polyvinyl alcohol used in melt-kneading the polyester and polyvinyl alcohol and the amount of polyvinyl alcohol contained in the 3 to 10 mass% aqueous polyvinyl alcohol solution are 0.8 to 6 parts by mass per 1 part by mass of the former.

Citation Information

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