JPH0525459A - Hot melt joint compound and method for filling therewith - Google Patents

Abstract

PURPOSE:To form a joint of excellent antimildew properties in a labor-reducing manner. CONSTITUTION:The objective hot melt joint compound to be used as a resinous joint compound for filling a joint on a panel or between panels comprising 99.9-10wt.% total of a thermoplastic composition comprising 10-50wt.% ionomer resin and 90-50wt.% wax and 0.1-90wt.% inorganic and/or organic filling pigments, and a method for filling a gap therewith.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a hot-melt joint material for gap filling and a gap filling processing method thereof.

[0002]

2. Description of the Related Art In the field of building material panels, tiles made of decorative ceramics have been attached to panels typified by slate boards and concrete panel boards to produce interior decorative panels for bathrooms and the like. . As a joint material for ceramic tiles, cement joint material has been best known from the past, but the problem of work life limitation, the problem that curing is slow, and long-term aging is necessary. There was a problem in productivity due to the high skill required and the problem of securing human resources. In addition, in cement joints, mold is remarkably generated under high temperature and high humidity after construction, and mold that has been once generated has problems such as it is difficult to remove, and joint products without mold have been strongly demanded in recent years. ing. On the other hand, as the resin joint material, a moisture-curing silicone caulking material,
Moisture-curable urethane caulks, solvent butyl rubber caulks, emulsion type acrylic caulks and other resin joint materials are known, but these are soft joints and are relatively expensive, and they are hard to cure or dry. As with cement jointing materials, productivity and mildew resistance are major problems such as the time required.

[0003]

Problems to be Solved by the Invention The following problems are also solved as main problems of joint materials such as ceramic tile panels for building materials and gap filling seals between assembling inorganic building material panels. Things can be given. The first
Is the development of a joint material that causes extremely little mold in a hot and humid environment such as a bathroom. Secondly, we propose a joint material that can be applied and filled and solidified easily and in a short time, and is suitable for a labor-saving construction method, and a filling processing method for the joint material. Third,
Providing a joint material that forms a finished surface with a smooth appearance, rich towability and scratch resistance, and an aesthetically pleasing appearance after construction, and proposes a construction processing method.

[0004]

As a result of earnest research, the present inventor has found that the specified hot-melt joint material is optimum as a means for solving the above-mentioned problems, and at the same time, the optimum filling thereof is performed. The present invention has been accomplished by finding a processing method.
That is, the present invention relates to ionomer resins (A) 10 to 5
0% by weight and a total of 99.9 to 10% by weight of a thermoplastic composition consisting of 90 to 50% by weight of wax (B), and 0.1 to 90% of an inorganic and / or organic filler (C).
% Of hot melt joint material.
As the wax (B), natural waxes such as natural carnauba wax and montan wax having a crystallinity of at least 20% and a softening point temperature or a melting point of 65 ° C. or higher, paraffin wax, and microcrystalline wax are preferable. Petroleum wax, polyethylene wax,
1 of synthetic waxes such as polypropylene wax, amide wax derived from higher fatty acid, ester wax derived from higher fatty acid, amide ester wax derived from higher fatty acid, and polyester oligo wax
It is a hot melt joint material using one or more waxes. The present invention also provides a gap filling process for a hot melt joint material, in which an adherend is preheated to 10 ° C. or less at a temperature higher than the softening point temperature of the hot melt joint material, and the molten hot melt joint material is pressurized or vacuum-fill molded. Method and / or filling the gap of the adherend with a hot melt applicator gun, then reheating the whole until the softening point temperature of the hot melt joint is close to and removing or repairing the coating joint, filling the gap of the hot melt joint It is a processing method. In particular, the above gap filling processing method in which the hot melt joint material is used for joint filling of a tile panel for a unit bath is highly preferable.

The present invention will be described in more detail below. The ionomer resin (A) of the present invention is a generic term for polymers having a structure in which the molecular chain of the polymer has a side chain of a carboxyl group and a part of the carboxyl group is crosslinked between the molecular chains by a metal cation. is there. As a representative example, ethylene-methacrylic acid copolymer or ethylene-acrylic acid copolymer developed by DuPont is cross-linked with a metal cation such as sodium or zinc between the molecular chains, trade name Surlyn. is there. A similar resin is commercially available from Mitsui Polychemical under the trade name of Himilan and can be preferably used. In the hot melt joint material of the present invention, the ionomer resin is preferably contained in an amount of 10 to 50% by weight with respect to the thermoplastic component in the joint material.
Particularly preferably, it is 15 to 35% by weight. 10% by weight
Below, the joint material is extremely brittle and lacks impact resistance and durable adhesion. When it is 50% by weight or more, the work melt viscosity of the joint material becomes abnormally high and workability is insufficient. In the present invention,
As a reason for using the ionomer resin, it is possible to improve the toughness as a hot melt joint material and improve the adhesion to tiles by using it, and a joint material rich in chemical resistance, hard and crack resistant is used. This is because it is essential for getting it.

The wax (B) of the present invention means a vegetable natural wax, an animal natural wax, a mineral natural wax,
One or more kinds of mixed wax selected from petroleum wax, synthetic hydrocarbon wax, synthetic ester wax, synthetic amide wax, higher fatty acid salt and the like can be preferably used, and the following are representative. Nozawa,
Examples of plant-based natural waxes include carnauba wax, wood wax, Onokyurirou, esbaltrou, candelilla wax, and examples of animal-based natural waxes include whale wax, wool wax, shellac wax, insect wax, and beeswax.
Examples of mineral type natural waxes include montan wax, ozokerite, ceresin and the like, and examples of petroleum type waxes include paraffin wax, microcrystalline wax and modified derivatives thereof. Examples of synthetic hydrocarbon waxes are Fischer-Tropsch wax,
Examples thereof include polyethylene wax, polypropylene wax and derivatives thereof. Examples of synthetic ester waxes include synthetic ester waxes derived from bis (2-hydroxyethyl) terephthalate and fatty acids having 13 or more carbon atoms, synthetic ester waxes derived from terephthalic acid and diol components, isophthalic acid and diols. Examples thereof include synthetic ester waxes derived from components, synthetic ester waxes derived from tris (2-hydroxyethyl) isocyanurate and higher fatty acids having 13 or more carbon atoms. Examples of the synthetic amide wax include methylene bis stearamide wax, methylol stearamide wax, stearic acid amide wax, higher fatty acid amide ester wax derived from monoethanolamine and higher fatty acid having 13 or more carbon atoms, and the like. Examples of higher fatty acid salts include zinc stearate and calcium stearate. Among the above waxes, natural waxes such as natural carnauba wax and montan wax, petroleum waxes such as paraffin wax and microcrystalline wax, polyethylene wax, polypropylene wax, amide wax derived from higher fatty acid having 13 or more carbon atoms, and 13 carbon atoms. It is a particularly preferable example to use one or more waxes of synthetic waxes such as ester wax derived from higher fatty acid, amide ester wax derived from higher fatty acid having 13 or more carbon atoms, and polyester oligo wax. is there.

In the present invention, the ionomer resin (A) is used.
It is important to select and use a wax (B) having good compatibility with, but it is not particularly limited. When used alone, it is preferable to use the wax whose compatibility is insufficient and the like in the minimum necessary amount, and to use it together with other compatible wax. It is also possible to use the wax by compatibilizing it by a method such as partial graft modification with a heat radical generating catalyst. In the present invention, the optimum wax amount of the wax (B) is 90 to 50% by weight, and particularly preferably 85 to 65% by weight, as a blending ratio with respect to the thermoplastic component in the hot melt joint material. When it is 90% by weight or more, the joint material is extremely brittle and lacks impact resistance and durable adhesion. If it is less than 50% by weight, the work melt viscosity of the joint material becomes abnormally high and workability is insufficient. In the present invention,
Wax (B) having a crystallinity of at least 20% and a softening point temperature or a melting point of 65 ° C. or higher is good because it is a hot-melt joint material considering heat resistance, stain resistance and chemical resistance. It is highly preferable to Further, in the present invention, as a means for enhancing the compatibility between the ionomer resin and the wax, there is no problem even if a small amount of the already known tackifiers described below is used in combination. Known tackifiers include (hydrogenated) rosin and (hydrogenated) rosin ester derivative, (hydrogenated) terpene resin, (hydrogenated)
Examples thereof include terpene-phenol resin, (hydrogenated) dicyclopentadiene resin, and petroleum fraction copolymer resin having 5 to 9 carbon atoms.

In the present invention, the total blending ratio of the thermoplastic composition comprising the ionomer resin (A) and the wax (B) may be 99.9 to 10% by weight in the hot melt joint material. Particularly preferably 95 to 30
The range of weight% is good. This is because it is impossible to adjust the hue of the joint at 100% by weight (as it is), and at 10% by weight or less, the resin component is insufficient, the joint material lacks toughness, and the workability is extremely difficult. Is. The following are typical examples of the inorganic and / or organic filling material (C) of the present invention. Examples of inorganic fillers include titanium white, clay, talc, calcium carbonate, silica, colloidal silica, alumina, glass powder, fine sand powder, carbon black, metal powder, iron oxide,
Lead white, red lead, ultramarine, dark blue, cobalt oxide, titanium black, strontium chromate, zinc chromate, iron black, molybdenum red, molybdenum white, emerald green, etc. Preferably the powder particle size is 100μ
In the following, a fine powder of 35 μm or less is particularly preferable. For white joint materials, titanium white and silica,
It is particularly preferable to use talc, calcium carbonate or the like.
As an organic filling material, polymer beads such as polyacrylic acid ester and polystyrene obtained by an emulsion polymerization method or a suspension polymerization method and having a particle size of 5 μm or less, an azo dye, a phthalocyanine dye, an isoindolinone dye Examples thereof include dyes and aniline dyes. Particularly preferable examples include polymer crosslinked beads. It is preferable that 0.1 to 90% by weight of the filler is blended in the hot melt joint material, preferably 5 to 80% by weight, and particularly preferably 50 to 80% by weight. When 0, the hue cannot be adjusted. If it exceeds 90% by weight, there is a problem in workability and joint toughness.

In the present invention, the reason why the inorganic and / or organic filler (C) is used as a main component of the hot-melt joint material is that it is essential for the relaxation of the solidification shrinkage ratio of the joint material or the hue adjustment. is there. The hot-melt joint material of the present invention is not particularly limited in handling form, and may be in the form of pellets, blocks, sticks, powders, films, pail cans, or the like. The melt viscosity is not particularly limited, but it is preferable that the melt viscosity at 200 ° C. is at most 2.5 million centipoise or less, preferably 200,000 centipoise or less in view of the low temperature joint filling property. In the hot melt joint material of the present invention, the following already known,
Anti-aging agent, UV absorber, UV stabilizer, silane coupling agent, organic titanate coupling agent, softening agent (plasticizer), antifungal agent, thixotropic agent, organic gelling agent, crystallization accelerator, etc. There is no problem in using the various additives together. In the case of performing joint filling processing of a building material panel such as filling the gaps of a tile panel or the like with the hot melt joint material of the present invention to form a tile joint, the filling processing method of the present invention described below is preferable. It is customary to prepare a device capable of heating and melting the joint material with a known hot melt applicator at a melting temperature of about 140 to 220 ° C. and supplying the required amount instantaneously or quantitatively. As the known hot melt applicator, in the examples classified by the discharge mechanism type, a gear pump type, a kneader / ruder type, an air pump type, a normal pressure tank type, a suction type, etc. can be adopted. In addition, a simple manual handgun or a vacuum type (defoaming type) applicator may be used.

The gap filling processing method of the hot melt joint material of the present invention is to press or vacuum fill the hot melt joint material with the object to be filled preheated to 10 ° C. or less from the softening point temperature. This is the most preferable method, in which case the melt discharge temperature of the hot melt joint material is approximately 140 to 220 ° C, more preferably 180 to 200 ° C.
Is preferred. Therefore, in the above method, it is customary to use a mold that adheres closely to the surface of the material to be filled,
The mold is not particularly limited, but it is preferable to use a mold that does not scratch the tile surface, and it is preferable that the contact surface is made of silicone rubber, urethane rubber, Teflon, polyimide or the like. Among the molds for filling tile panels, a silicon bat mold, which is excellent in heat resistance and releasability, is a particularly preferable example. The pressure filling method is not particularly limited, but the discharge pressure of the hot melt joint material is 10 kg / cm ² or less, preferably 3 kg / c.
m ² or less is preferable. In view of the relationship with the preheating temperature, it is preferable to appropriately select a discharge pressure at which filling is completed in a short time or a discharge pressure that does not cause protrusion and has an excellent finished appearance.
Further, the state of preheating the object to be filled in advance also means a case where the temperature of the mold material used together for molding is also included. The preheating temperature is preferably 10 ° C. or lower, which is higher than the softening point temperature of the hot melt joint material, and may be room temperature. It is preferable to appropriately select a temperature at which the molding cycle can be efficiently performed. Further, it is preferable that rapid cooling or slow cooling can be performed after the completion of filling. In the vacuum filling method, the degree of vacuum is 500 mmHg as measured by the manometer.
The following is preferable, and it is highly preferable that the filling process can be performed at 100 mmHg or less. Further, when molding and filling the jointing agent, there is no problem in adopting a method of applying various known release agents to the molding die in advance in order to facilitate the demolding.

Further, in the present invention, as a method for filling the gap of the hot melt joint material, after filling the gap of the adherend with the hot melt applicator gun, it is heated to near the softening point temperature of the hot melt joint material to form the coating joint. A method of removing or repairing is also preferable. Specifically, a hot-melt joint material is spray-applied to a gap between adherends with a commercially available (known) hot-melt applicator, and then reheated to near the softening point temperature of the hot-melt joint material to This is a method of removing and / or smoothing the protruding portion. A good example is a construction method in which a robot or the like is incorporated and continuous coating is performed by automatic control during coating. There is no particular limitation on the hot melt applicator used, and it is preferably used as long as it is rich in mechanical stability and can be applied quantitatively. There are no particular restrictions on the use of the hot melt joint material of the present invention, and it can be preferably used for joint filling of tile panels for unit baths. The same applies to the application of the gap filling processing method.

[0012]

EXAMPLES The present invention will now be described with reference to Examples and Comparative Examples in order to more specifically describe the present invention, but the present invention is not limited to these Examples. The parts or% described in the examples mean parts by weight and% by weight, respectively.

Example 1 As an ionomer resin, 35 parts of Himilan 1702 manufactured by Mitsui Polychemical Co., and a melting point of 82 to 85 ° C.
55 parts of natural carnauba wax, 10 parts of high wax 2203A manufactured by Mitsui Petrochemical Co., Ltd. as an acid-modified polyethylene wax having a softening point of 107 ° C. and a crystallinity of 65%, 30 parts of titanium white, and 150 parts of calcium carbonate of 200 mesh pass. Was melt-kneaded at a temperature of 180 ° C. to obtain a white hot-melt joint material (A). The hot melt joint material (A) had a melt viscosity at 200 ° C. of 50 to 80,000 centipoise, and the softening point temperature of this composition was 105 ° C. In addition, a 1 m square tiled panel was prepared by bonding white ceramic tiles 5 mm thick and 10 cm wide to a calcium silicate plate so as to have a joint width of 5 mm in advance. A flat plate bat type silicon mold having a rich rubber elasticity was used as a mold having one injection port and one depressurization port, and the mold was placed on the mold so that the surface of the tile surface of the panel was in close contact with the mold. It was fixed in close contact with the mold under a pressure of ² Kg / cm ² . The degree of vacuum in the joint gap was set to about 50 mmHg using a manometer vacuum gauge, and the overall molding preheating temperature was set to 80 ° C. While continuing to reduce the pressure, the hot melt joint material (A) was introduced from the injection port of the mold.
Was injected at a melting temperature of 190 ° C. through a hot melt melting tank. (The time required for injection was about 10 seconds.) 10 seconds after the start of injection, that is, when the jointing material protruded from the pressure reducing opening, the pressure reducing opening was closed and the entire mold was rapidly cooled to 30 ° C.
After cooling the entire mold, the mold was removed. As a result, the joint gaps between the tiles were evenly filled with the hot melt joint material, and no remarkable protrusion to the surface of the tile was observed. After leaving the panel after construction for 5 days at room temperature,
No mold or the like was found in the joints of the panel taken out after being left for one month at 35 ° C./90% humidity. In addition, in the observation after the filling and solidification of the joints, no cracks were found, and the joints formed were extremely white and glossy. The hardness of the joint material showed an instantaneous value of 72 to 74 in Shore D and was a joint material rich in nail scratch resistance.

Example 2 As an ionomer resin, 35 parts of Himilan 1702 manufactured by Mitsui Polychemical Co., 55 parts of ethylene bis stearamide wax having a melting point of 140 ° C. and a softening point temperature of 145 were used.
℃ acid-modified polypropylene wax as Sanyo Kasei product Sazol TS-200 10 parts, carbon black 1
0 parts, 40 parts of talc, and 100 parts of calcium carbonate of 200 mesh pass were melt-kneaded at a temperature of 180 ° C. to obtain a black hot melt joint material (B). The melt viscosity of the hot melt joint material (B) at 200 ° C. was 30,000 to 50,000 centipoise, and the surface hardness was measured with a Shore D hardness meter, and showed an instantaneous value of 70 to 75 at about room temperature. The softening point temperature of this composition was 152 ° C. In addition, width 5 beforehand
5 mm thick and 10 cm wide so as to have a joint width of mm
1m with black corner ceramic tiles attached to a slate board
A corner tiled panel was prepared. A silicon mold having a high rubber elasticity is used as a mold, and the panel is placed downward so that the tile surface of the panel is in close contact with the mold.
The mold was brought into close contact with the mold under a pressure of about cm ² , and the mold was set so that the preheating temperature was 120 ° C. Melt temperature 2 of the hot melt joint material (B) through a gear pump hot melt applicator from the injection port of the molding die under a pressure of 1.5 kg / cm @ 2 in the joint gap.
Poured at 00 ° C. (The time required for injection is about 13
It was seconds. ) 13 seconds after the start of injection, that is, when the jointing material protruded from the air opening, the supply was closed, the entire mold was rapidly cooled to 30 ° C., and then the mold was released. As a result, the joint gaps between the tiles were evenly filled with the hot melt joint material, and no remarkable protrusion to the surface of the tile was observed. The panel after the construction was left at room temperature for 5 days and then left at 35 ° C./80% humidity for 1 month, and no mold was found in the joints of the panel taken out. In addition, in the observation after the filling and solidification of the joint portion, no cracks were found, and the joint was formed with a very excellent scratch resistance and gloss.

Example 3 The hot melt joint material (A) obtained in Example 1 was used as a new type melter 60, which is a manual type applicator manufactured by Hakuko Metal Co., Ltd.
At a melting temperature of 200 ° C., the mixture was discharged in a bead shape to the joint forming groove of the panel to which the white tile similar to that described in Example 1 was applied, and the gap filling coating was performed. After the filling is completed,
The construction panel was heated to about 90 ° C. in a dryer and taken out, and immediately the protruding portion of the softened hot melt joint was cut with a concave chisel. As a result, the appearance of the joint filling part is
It was possible to form a beautiful concave cut surface with a uniform filling film pressure. After the panel after construction was left at room temperature for 5 days and then left at 35 ° C / 80% saturated humidity for 1 month, no mold was found in the joints of the panel taken out. In addition, in the observation after the filling and solidification of the joint portion, no cracks were found, and the joint was formed with a very excellent scratch resistance and gloss.

Comparative Example 1 A water-based cement joint material prepared by mixing white cement and fine alumina powder in a ratio of 1: 2 was used in the joint forming groove of a panel to which the same white tile as in Example 1 was attached. The gap was filled using a coated iron and joint processing was performed. It was left at room temperature and cured for 3 days. 35 this panel
When left at a temperature of 85 ° C./saturation humidity of 85% for one month, black mold and blue mold were considerably generated. Comparative Example 2 As an ionomer resin, 70 parts of Himilan 1702 manufactured by Mitsui Polychemical Co., 30 parts of natural carnauba wax having a melting point of 82 to 85 ° C. crystallinity, and 3 of titanium white.
The white hot-melt joint material prepared by melt-kneading 0 part and 150 parts of 200-mesh pass calcium carbonate at a temperature of 180 ° C. is a highly thixotropic composition whose viscosity cannot be measured at 200 ° C. Therefore, it was not possible to continuously discharge a fixed amount from the lower part of the melting tank of the hot melt applicator at 200 ° C. Comparative Example 3 As an ionomer resin, 5 parts of Himilan 1702 manufactured by Mitsui Polychemical Co., 95 parts of natural carnauba wax having a melting point of 82 to 85 ° C. and titanium white 5 were used.
Part and 50 parts of talc were melt-kneaded at a temperature of 180 ° C. to obtain a white hot-melt joint material (C). The joint filling processed product obtained by using the obtained melt (C) in the same manner as in Example 1 had many cracks formed at the edge portion of the tile or near the bonding interface with the tile portion after cooling at room temperature. Was observed. Further, the bead-like discharged solid matter containing only the hot melt joint material (C) lacks towability and is a brittle joint material, which is a problem.

[0017]

As is apparent from the examples, the hot-melt joint material of the present invention has excellent antifungal properties, and the processing method (joint filling method) of the present invention is excellent in short-time filling. The most distinctive feature is the appearance and durability of finished products. As shown in Comparative Example 1, when the cement joint of the conventional method is used, there is a problem that mold is generated in a considerably short time. We have found that this problem is significantly affected by the water used. Further, as shown in Comparative Examples 2 and 3, a hot melt composition exceeding the range of the present invention was extremely problematic as a joint material. The present invention is considered to be highly practical as a preferable labor-saving joint material and its filling processing method in the decorative tiled panel manufacturing market.

Claims (5)

[Claims] 1. A total of 99.9 to 10% by weight of a thermoplastic composition comprising 10 to 50% by weight of an ionomer resin (A) and 90 to 50% by weight of a wax (B), and an inorganic and / or organic filler. A hot melt joint material containing 0.1 to 90% by weight of the material (C). 2. A wax (B) having a crystallinity of at least 20% and a softening point temperature or a melting point of 65 ° C. or higher, such as natural waxes such as carnauba wax and montan wax, paraffin wax, and microcrystalline wax. Selected from synthetic waxes such as petroleum wax, polyethylene wax, polypropylene wax, amide wax derived from higher fatty acid, ester wax derived from higher fatty acid, amide ester wax derived from higher fatty acid, polyester oligo wax, etc. The hot melt joint material according to claim 1, wherein one or more waxes are used. 3. The hot-melt joint material according to claim 1 or 2 is 10 ° C. higher than the softening point temperature of the hot-melt joint material.
The following is a gap filling processing method for a hot melt joint material, in which the adherend is preheated in advance and the molten hot melt joint material is pressurized or vacuum filled. 4. The hot melt joint material according to claim 1 or 2 is filled in a gap between adherends with a hot melt applicator gun, and then the entire coated article is reheated to near the softening point temperature of the hot melt joint material. A method for filling gaps of hot melt joint materials, which removes or repairs coating joints. 5. A gap filling processing method, which comprises using the hot melt joint material according to claim 1 or 2 for joint filling of a tile panel for a unit bath.