JP2001261913A - Aqueous emulsion composition and woodworking adhesive - Google Patents

Abstract

(57) [Problem] To provide an aqueous emulsion and a woodworking adhesive having high viscosity, excellent water resistance, and excellent adhesion to wood. SOLUTION: A polymer having a vinyl ester monomer unit is used as a dispersoid, and an ethylene unit is contained in an amount of 0.5 to 10 mol%.
A water-soluble polymer (B) mixed with an aqueous emulsion (A) containing a vinyl alcohol-based polymer having a degree of saponification of 95 mol% or more as a dispersant;
An aqueous emulsion composition wherein (B) is a water-soluble polyvinyl alcohol having a viscosity average degree of polymerization of 1,000 to 8,000 and a saponification degree of 70 to 95 mol%, or a water-soluble cellulose derivative having a 2% aqueous viscosity of 1,000 to 8,000 mPa · s.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an aqueous emulsion composition having high viscosity, excellent adhesiveness to wood, and excellent water resistance, and an adhesive for woodwork using the aqueous emulsion composition.

[0002]

2. Description of the Related Art Conventionally, polyvinyl alcohol (hereinafter, referred to as polyvinyl alcohol) has been used.
PVA) is widely used as a protective colloid for emulsion polymerization of ethylenically unsaturated monomers, especially vinyl ester monomers such as vinyl acetate. Vinyl ester aqueous emulsion obtained by emulsion polymerization is used for various adhesives for paper, woodworking and plastics, various binders for impregnated paper and non-woven products, admixtures, jointing materials, paints, paper processing And widely used in fields such as fiber processing. By adjusting the degree of saponification of the PVA-based polymer, such an aqueous emulsion generally has a low viscosity, has a viscosity close to a Newtonian flow, and has a relatively good water resistance. Since it has a high viscosity and relatively low temperature dependence of emulsion viscosity, it has been awarded for various uses. As the woodworking adhesive, a higher viscosity emulsion is preferable, and a vinyl ester aqueous emulsion using so-called partially saponified PVA as a protective colloid is widely used. Partialization
A vinyl ester-based aqueous emulsion using PVA as a protective colloid is excellent in low-temperature stability and easy to obtain a high-viscosity one, but has a problem of poor water resistance. On the other hand, vinyl ester-based aqueous emulsions using completely saponified PVA as a protective colloid have a problem that they are excellent in water resistance, but are inferior in low-temperature stability. Under such circumstances, vinyl alcohol-based polymers containing ethylene units have been proposed (JP-A-11-21529, JP-A-11-21380, JP-A-10-226774, etc.), and have improved water resistance and low-temperature storage stability. Significantly improved. However, the viscosity of the obtained emulsion is generally lower than that of an emulsion using partially saponified PVA as a protective colloid, and at present, it is insufficient as an adhesive for woodworking.

[0003]

SUMMARY OF THE INVENTION Under such circumstances, the present invention provides an aqueous emulsion composition having excellent low-temperature stability and water resistance, and further having a high viscosity and a woodworking composition using the aqueous emulsion composition. It is intended to provide an adhesive.

[0004]

Means for Solving the Problems The present inventors have conducted intensive studies to develop an aqueous emulsion composition and a woodworking adhesive having the above-mentioned preferable properties, and as a result, they have a vinyl ester monomer unit. The polymer is a dispersoid, contains 0.5 to 10 mol% of ethylene units, and has a saponification degree of 95
A water-soluble polymer (B) is blended with an aqueous emulsion (A) having a vinyl alcohol polymer as a dispersant of at least mol%, and the water-soluble polymer (B) has a viscosity average degree of polymerization of 1000. Water-soluble polyvinyl alcohol with a saponification degree of 70 to 95 mol% or a 2% aqueous solution viscosity of 100 to 8000
It has been found that an aqueous emulsion composition that is a water-soluble cellulose derivative of 0 to 8000 mPa · s satisfies the above object. Further, they have found that a woodworking adhesive comprising the aqueous emulsion composition satisfies the above object, and have completed the present invention.

[0005]

BEST MODE FOR CARRYING OUT THE INVENTION The method for producing a vinyl alcohol-based polymer containing 0.5 to 10 mol% of ethylene units and having a degree of saponification of 95 mol% or more is not particularly limited. By saponifying a copolymer of vinyl ester and ethylene by the method described in (1).

[0006] Here, as the vinyl ester,
Examples thereof include vinyl formate, vinyl acetate, vinyl propionate, and vinyl pivalate. In general, vinyl acetate is preferably used.

[0007] The dispersant may be a copolymer of an ethylenically unsaturated monomer copolymerizable within a range not to impair the effects of the present invention. Such ethylenically unsaturated monomers include, for example, acrylic acid, methacrylic acid, fumaric acid, (anhydride) maleic acid, itaconic acid, acrylonitrile, methacrylonitrile, acrylamide, methacrylamide, trimethyl- (3-acrylamide -3-dimethylpropyl) -ammonium chloride, acrylamido-2-methylpropanesulfonic acid and its sodium salt, ethyl vinyl ether, butyl vinyl ether,
N-vinylpyrrolidone, vinyl chloride, vinyl bromide, vinyl fluoride, vinylidene chloride, vinylidene fluoride, tetrafluoroethylene, sodium vinyl sulfonate, sodium allyl sulfonate, N-vinyl pyrrolidone, N
N-vinylamides such as -vinylformamide and N-vinylacetamide. Further, in the presence of a thiol compound such as thiolacetic acid and mercaptopropionic acid, a vinyl ester monomer such as vinyl acetate is
A terminal-modified product obtained by copolymerizing with ethylene and saponifying it can also be used.

The ethylene unit used in the present invention is 0.5 to 1
The saponification degree of the vinyl alcohol-based polymer containing 0 mol% and having a degree of saponification of 95 mol% or more needs to be 95 mol% or more, preferably 96 mol% or more, more preferably 97 mol% or more. If the saponification degree is less than 95 mol%, there is a concern that the water resistance of the obtained aqueous emulsion composition is reduced. The degree of polymerization of the vinyl alcohol-based polymer is not particularly limited, but is usually in the range of 100 to 8000,
000 is more preferably used. When the degree of polymerization is less than 100, the characteristics of the vinyl alcohol polymer as a protective colloid are not exhibited, and when it exceeds 8,000, there is a problem in industrial production of the vinyl alcohol polymer. If the content of ethylene units is less than 0.5 mol%, the resulting aqueous emulsion composition may have poor storage stability at low temperatures, and if it exceeds 10 mol%, it is an intrinsic property of the vinyl alcohol polymer. Water solubility may decrease.

The vinyl ester monomer constituting the dispersoid of the aqueous emulsion of the present invention includes vinyl formate, vinyl acetate, vinyl propionate, vinyl pivalate, and the like. In general, vinyl acetate is preferably used.

The above dispersoid may be copolymerized with a copolymerizable ethylenically unsaturated monomer as long as the effects of the present invention are not impaired. As at least one monomer unit selected from ethylenically unsaturated monomers and diene monomers, ethylene, propylene, olefins such as isobutylene, vinyl chloride, vinyl fluoride, vinylidene chloride, vinylidene fluoride and the like Halogenated olefins, vinyl formate, vinyl acetate, vinyl propionate,
Vinyl esters such as vinyl versatate, acrylates such as acrylic acid, methacrylic acid, methyl acrylate, ethyl acrylate, butyl acrylate, 2-ethylhexyl acrylate, dodecyl acrylate, 2-hydroxyethyl acrylate, and methacrylic acid Methyl,
Ethyl methacrylate, butyl methacrylate, 2-ethylhexyl methacrylate, dodecyl methacrylate, methacrylates such as 2-hydroxyethyl methacrylate, dimethylaminoethyl acrylate, dimethylaminoethyl methacrylate and quaternized products thereof, and , Acrylamide, methacrylamide, N-methylolacrylamide, N, N-dimethylacrylamide,
Acrylamide monomers such as acrylamide-2-methylpropanesulfonic acid and its sodium salt, styrene monomers such as styrene, α-methylstyrene, p-styrenesulfonic acid, and sodium and potassium salts;
Others such as N-vinylpyrrolidone, butadiene,
Diene monomers such as isoprene and chloroprene, as well as divinylbenzene, tetraallyloxyethane, N, N '
-Methylenebis-acrylamide, 2,2'-bis (4-acryloxypolyethoxyphenyl) propane, 1,3-butylene glycol diacrylate, 1,5-pentanediol diacrylate, neopentyl glycol diacrylate, 1,6- Hexanediol diacrylate, diethylene glycol diacrylate, triethylene glycol diacrylate, tetraethylene glycol diacrylate, polyethylene glycol diacrylate, polypropylene glycol diacrylate, pentaerythritol triacrylate, trimethylolpropane triacrylate, pentaerythritol tetraacrylate, allyl methacrylate, 1,4-butanediol diacrylate, ethylene glycol dimethacrylate,
1,3-butylene glycol dimethacrylate, neopentyl glycol dimethacrylate, 1,6-hexanediol dimethacrylate, diethylene glycol dimethacrylate, triethylene glycol dimethacrylate,
Polyethylene glycol dimethacrylate, dipropylene glycol dimethacrylate, polypropylene glycol dimethacrylate, trimethylolethane trimethacrylate, trimethylolpropane trimethacrylate, 2,2-bis (4-methacryloxypolyethoxyphenyl) propane, aluminum methacrylate, methacrylic acid Zinc, calcium methacrylate, magnesium methacrylate, N, N'-m-phenylenebismaleimide, diallyl phthalate, triallyl cyanurate, triallyl isocyanurate, triallyl trimellitate, diallyl chlorendate, ethylene glycol diglycidyl ether Examples thereof include polyfunctional monomers such as acrylates, which may be used alone or as a mixture of two or more. As a monomer copolymerizable with these vinyl esters, ethylene is preferred.

The method for producing the aqueous emulsion used in the present invention is not particularly limited.
An aqueous solution of a vinyl alcohol polymer containing 0 mol% and having a degree of saponification of 95 mol% or more is used as a dispersant, and a vinyl ester monomer is added temporarily or continuously, and an azo polymerization initiator, A method of adding a polymerization initiator such as hydrogen peroxide, a peroxide-based polymerization initiator such as ammonium persulfate and potassium persulfate, and carrying out emulsion polymerization may be mentioned.

The amount of the vinyl alcohol polymer containing 0.5 to 10 mol% of ethylene units and having a degree of saponification of 95 mol% or more is not particularly limited. 3 to 20 parts by weight, more preferably 5 to 20 parts by weight, based on 100 parts by weight of the polymer
It is in the range of 15 parts by weight. If the amount is less than 3 parts by weight, the polymerization stability may decrease. If the amount exceeds 20 parts by weight, the storage stability of the obtained emulsion may decrease.

In the present invention, the water-soluble polymer (B) to be added to the aqueous emulsion (A) has a viscosity average degree of polymerization of 1000.
-8000, water-soluble polyvinyl alcohol having a degree of saponification of 70-95 mol%, or 2% aqueous solution viscosity of 1,000-80.
It is a water-soluble cellulose derivative of 00 mPa · s, and one or more of these are used. It is important that the degree of saponification of the water-soluble polyvinyl alcohol is at least 70%, preferably at least 80 mol%, more preferably at least 85 mol%. When the saponification degree is less than 70 mol%, the water solubility, which is an intrinsic property of polyvinyl alcohol, may be reduced. On the other hand, if it exceeds 95% by mole, the resulting aqueous emulsion composition may have poor storage stability at low temperatures. It is important that the viscosity average polymerization degree of polyvinyl alcohol is 1000 or more, preferably 1200 or more, and more preferably 1 or more.
500 or more. Further, it is more preferably 4000 or less. When the viscosity average degree of polymerization is less than 1,000, the water-based adhesive property of the obtained aqueous emulsion composition may be reduced. If the viscosity-average degree of polymerization exceeds 8000, the storage stability of the aqueous emulsion composition when left may be reduced.

It is important that the viscosity of a 2% aqueous solution of the water-soluble cellulose derivative is 1000 mPa · s or more, preferably 1500 mPa · s or more, more preferably 20 mPa · s or more.
00 mPa · s or more. 2% aqueous solution viscosity is 1000mPa · s
If it is less than 1, the water-resistant adhesive property of the obtained aqueous emulsion composition may be reduced. Also, it is preferably 7000 mPa · s or less. Preferred examples of the water-soluble cellulose derivative include hydroxyethyl cellulose, methyl cellulose, and carboxymethyl cellulose. One or more of these are used.

The mixing ratio of the aqueous emulsion (A) and the water-soluble polymer (B) is not particularly limited, but is usually (A) /
(B) = 100 / 0.01-100 / 50, preferably 100 / 0.05-100 / 30,
More preferably, it is blended at a ratio of 100 / 0.1 to 100/20.
When the mixing ratio is less than (A) / (B) = 100 / 0.01, the viscosity of the obtained aqueous emulsion composition may be low, and (A) / (B) = 10
If it exceeds 0/50, there is a concern that the water resistance of the obtained aqueous emulsion composition is reduced.

The mixing of the water-soluble polymer (B) with the aqueous emulsion (A) (post-addition method) is not particularly limited. For example, a method of adding a water-soluble polymer powder to an emulsion, stirring and dissolving, preparing an aqueous solution in advance and blending the same,
After the emulsion polymerization, a method in which a water-soluble polymer is subsequently charged and dissolved is exemplified.

As the aqueous emulsion composition and the woodworking adhesive of the present invention, the aqueous emulsion composition obtained by the above-mentioned method can be used as it is, but if necessary, within the range not impairing the effects of the present invention. Conventionally known various emulsions can be added and used.

As the dispersant in the aqueous emulsion of the present invention, a vinyl alcohol polymer containing 0.5 to 10 mol% of the above-mentioned ethylene unit and having a degree of saponification of 95 mol% or more is used. If necessary, a conventionally known anionic, nonionic or cationic surfactant or hydroxyethyl cellulose can be used in combination, and the ethylene unit is 0.5 to 10 as long as the object of the present invention is not impaired. Mol%, saponification degree 9
A vinyl alcohol-based polymer other than the vinyl alcohol-based polymer of 5 mol% or more may be used in combination.

The aqueous emulsion composition and the woodworking adhesive of the present invention have high viscosity, excellent water resistance and excellent low-temperature stability, and are used for flash panel, laminated wood, wood board, plywood processing, and plywood secondary processing. (Kneading), adhesives for woodworking such as general woodworking, various adhesives, binders for impregnated paper, non-woven products, admixtures, jointing materials, paints, paper processing, fiber processing, etc. .

[0020]

Next, the present invention will be described in more detail with reference to Examples and Comparative Examples. In the following Examples and Comparative Examples, “parts” and “%” mean on a weight basis unless otherwise specified. In addition, the water resistance and storage stability of the obtained emulsion were evaluated in the following manner.

(Evaluation of Emulsion) (1) Emulsion Viscosity Using a BH type viscometer (manufactured by Tokimec Co., Ltd.), the viscosity of the obtained aqueous emulsion and aqueous emulsion composition was measured at 30 ° C. at a rotation speed of 20 rpm. It was measured. (2) Wood adhesive strength The obtained aqueous emulsion composition was added to birch wood (straight grain) for 1 hour.
50 g / m2 was applied, and the pieces were pressed together with a load of 7 kg / m2 for 16 hours. After that, the pressure is released and the temperature is reduced to
After curing under H for 5 days, the compressive shear strength was measured (normal adhesive strength). Further, after curing, it was immersed in warm water at 60 ° C. for 3 hours, and the compressive shear strength was measured in a wet state (adhesion resistance to hot water). Low-temperature stability The viscosity change after 14 days when the emulsion was left at 0 ° C. was observed. ○ Little change, slightly thickening, × thickening / gelation

Emulsion Production Example 1 A 1-liter glass polymerization vessel equipped with a reflux condenser, a dropping funnel, a thermometer and a nitrogen inlet was charged with 300 ion-exchanged water.
95 g of PVA-1 (polymerization degree 1000, saponification degree 99.2 mol%, ethylene unit content 6 mol%) was charged 95
Dissolved completely at ° C. Next, this PVA aqueous solution is cooled,
After nitrogen replacement, the temperature was raised to 60 ° C. while stirring at 200 rpm, and then 4.4 g and 5% of a 10% aqueous solution of tartaric acid were added.
3 g of hydrogen peroxide solution (0.04 mol ratio to vinyl acetate
After 15) was added, 26 g of vinyl acetate was charged to initiate polymerization. 30 minutes after the start of the polymerization, completion of the initial polymerization was confirmed. After adding 0.9 g of a 10% aqueous solution of tartaric acid and 3 g of a 5% aqueous hydrogen peroxide solution by shot, 234 g of vinyl acetate was continuously added over 2 hours to complete the polymerization (Em-1).

Emulsion Production Example 2 In place of using PVA-1 used in Emulsion Production Example 1, PVA-2 (polymerization degree 1700, saponification degree 98.1 mol%, ethylene unit content 4 mol%) was used. Em-2 was obtained in the same manner as in Emulsion Production Example 1.

Comparative Emulsion Production Example 1 Instead of using PVA-1 used in Emulsion Production Example 1, PVA-3 (polymerization degree 1700, saponification degree 98.5 mol%; PVA-117 manufactured by Kuraray Co., Ltd.) was used. Otherwise, Em-3 was obtained in the same manner as in Emulsion Production Example 1.

Emulsion Comparative Production Example 2 In place of using PVA-1 used in Emulsion Production Example 1, PVA-4 (polymerization degree: 1700, saponification degree: 88 mol%; PVA-217 manufactured by Kuraray Co., Ltd.) was used. Em-4 was obtained in the same manner as in Emulsion Production Example 1.

Example 1 While stirring 100 parts by weight of Em-1 obtained in Emulsion Production Example 1 at 80 ° C., hydroxylethyl cellulose (manufactured by Daicel Chemical Industries, Ltd .; HEC SP-900; 2% aqueous solution viscosity 5000 mPa · s). s) 0.3 part by weight was charged, dissolved over 2 hours, and then cooled. Thereafter, the mixture was filtered using a 60-mesh stainless steel wire mesh. As a result, a polyvinyl acetate emulsion having a solid content (TSC) of 48.3% was obtained. 5 parts of dibutyl phthalate was added to and mixed with 100 parts by weight of this emulsion. The physical properties of this emulsion were measured by the methods described above. Table 1 shows the results.

Example 2 Example 1 was repeated except that Em-2 obtained in Emulsion Production Example 2 was used instead of Em-1 used in Example 1.
An emulsion was obtained in the same manner as described above, and the physical properties were measured. Table 1 also shows the results.

Comparative Example 1 An emulsion was obtained in the same manner as in Example 1 except that Em-3 obtained in Emulsion Comparative Production Example 1 was used instead of Em-1 used in Example 1, and physical properties were obtained. It was measured.
Table 1 also shows the results.

Comparative Example 2 Em-4 100 obtained in Comparative Emulsion Production Example 2
5 parts by weight of dibutyl phthalate was added to and mixed with parts by weight. The physical properties of this emulsion were measured by the methods described above. The results are shown in Table 1.

Example 3 While stirring 100 parts by weight of Em-2 obtained in Emulsion Production Example 2 at 80 ° C., PVA-4 (polymerization degree 17
00, saponification degree: 88 mol%; PVA-217 manufactured by Kuraray Co., Ltd.)
One part by weight was charged, dissolved over 2 hours, and then cooled. Thereafter, the mixture was filtered using a 60-mesh stainless steel wire mesh. As a result, a polyvinyl acetate emulsion having a solid content of 48.5% was obtained. 5 parts of dibutyl phthalate was added to and mixed with 100 parts by weight of this emulsion. The physical properties of this emulsion were measured by the methods described above. The results are shown in Table 1.

Comparative Example 3 An emulsion was obtained in the same manner as in Example 1 except that Em-3 obtained in Emulsion Comparative Production Example 1 was used instead of Em-2 used in Example 3, and physical properties were obtained. It was measured.
Table 1 also shows the results.

Comparative Example 4 PVA-4 used in Example 3 (PVA-21 manufactured by Kuraray Co., Ltd.)
Instead of using 7), PVA-3 (degree of polymerization 1700,
An emulsion was obtained in the same manner as in Example 3 except that a saponification degree of 98.5 mol%; PVA-117 manufactured by Kuraray Co., Ltd. was used, and physical properties were measured. Table 1 also shows the results.

Comparative Example 5 An emulsion was obtained in the same manner as in Example 4 except that Em-3 obtained in Emulsion Comparative Production Example 1 was used instead of Em-2 used in Example 4, and physical properties were obtained. It was measured.
Table 1 also shows the results.

Example 4 While stirring 100 parts by weight of Em-2 obtained in Emulsion Production Example 2 at 80 ° C., methyl cellulose (Metroze 90SH-4000 manufactured by Shin-Etsu Chemical Co., Ltd., 2%
0.3 part by weight of aqueous solution viscosity 4000 mPa · s) was added, dissolved over 2 hours, and then cooled. Thereafter, the mixture was filtered using a 60-mesh stainless steel wire mesh. As a result, a polyvinyl acetate emulsion having a solid content of 48.1% was obtained. 5 parts of dibutyl phthalate was added to and mixed with 100 parts by weight of this emulsion. The physical properties of this emulsion were measured by the methods described above. The results are shown in Table 1.

Example 5 While stirring 100 parts by weight of Em-2 obtained in Emulsion Production Example 2 at 80 ° C., sodium carboxymethylcellulose (CMC-22002 manufactured by Daicel Chemical Industries, Ltd.) was used.
% Aqueous solution viscosity 6000 mPa · s) 0.3 parts by weight
After dissolving over time, it was cooled. Thereafter, the mixture was filtered using a 60-mesh stainless steel wire mesh. As a result,
A polyvinyl acetate emulsion having a solid content of 48.1% was obtained. 5 parts of dibutyl phthalate was added to and mixed with 100 parts by weight of this emulsion. The physical properties of this emulsion were measured by the methods described above. The results are shown in Table 1.

Comparative Example 6 100 of the emulsion obtained in Emulsion Production Example 1
5 parts by weight of dibutyl phthalate was added to and mixed with parts by weight. The physical properties of this emulsion were measured by the methods described above. The results are shown in Table 1.

[0037]

[Table 1]

PVA-1; polymerization degree 1000, saponification degree 99.2 mol%, ethylene unit content 6 mol% PVA-2; polymerization degree 1700, saponification degree 98.1 mol%, ethylene unit content 4 mol% PVA-3; polymerization Degree 1700, saponification degree 98.5 mol% ｛manufactured by Kuraray Co., Ltd.
PVA-117｝ PVA-4; polymerization degree 1700, saponification degree 88mol%, manufactured by Kuraray Co., Ltd.
PVA-217｝

[0039]

The aqueous emulsion and adhesive for woodworking of the present invention have high viscosity, excellent water resistance and excellent adhesion to wood materials, and are used for flash panel, laminated wood, wood board, plywood processing, Suitable for the following processing (kneading), adhesives for woodworking such as general woodworking, various adhesives, binders for impregnated paper, nonwoven products, admixtures, jointing materials, paints, paper processing and textile processing. Used for

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Claims (4)

[Claims] 1. A polymer having a vinyl ester monomer unit is used as a dispersoid, and an ethylene unit is contained in an amount of 0.5 to 10 mol%.
A water-soluble polymer (B) mixed with an aqueous emulsion (A) containing a vinyl alcohol-based polymer having a degree of saponification of 95 mol% or more as a dispersant;
An aqueous emulsion composition wherein (B) is a water-soluble polyvinyl alcohol having a viscosity average degree of polymerization of 1,000 to 8,000 and a saponification degree of 70 to 95 mol%, or a water-soluble cellulose derivative having a 2% aqueous viscosity of 1,000 to 8,000 mPa · s. 2. The aqueous emulsion composition according to claim 1, wherein the water-soluble cellulose derivative is at least one selected from hydroxyethyl cellulose, methyl cellulose, and carboxymethyl cellulose. 3. The aqueous emulsion composition according to claim 1, wherein the dispersoid is a polymer having a vinyl ester monomer and an ethylene unit. 4. A woodworking adhesive comprising the aqueous emulsion composition according to claim 1.