JPS592476B2 - hot melt adhesive - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention provides a hot melt for textiles that has excellent adhesion to fabrics made of polyester and/or cotton, and has excellent flexibility, hot water washing resistance, and dry cleaning resistance. It concerns adhesives.

In recent years, various hot melt adhesives have been developed that take advantage of advantages such as non-pollution, high adhesive performance, and instant adhesive properties.

In particular, as the proportion of polyester fibers in textile fabrics increases, various polyester hot melt adhesives with excellent adhesive properties have been proposed. For example, Japanese Patent Publication No. 47-18357 and Japanese Patent Application Laid-Open No. 51-125431 lack texture, which is a performance strongly desired as a hot melt adhesive for textiles, and improvements are strongly needed especially for interlining applications. It was wanted. On the other hand, adhesives with excellent texture include those made by copolymerizing polyalkylene ether with polyester, such as those disclosed in Japanese Patent Publication Nos. 10513-1982, 16146-1970, and 16055-1980.
No. 2 has been proposed, but the dry cleaning resistance is insufficient.

It has also been proposed, for example, in JP-A-51-125431, to copolymerize polyester with a small amount of polytetramethylene glycol to improve its texture and hot water washing resistance. is not sufficient.

Copolymer polyamides have traditionally been used as hot-melt adhesives for textiles for permanent adhesive applications, and have been highly evaluated for their adhesion to textiles such as cotton rayon and wool, and their dry cleaning resistance. However, it has serious drawbacks such as yellowing due to the tips and a decrease in hot water washability due to water absorption.Moreover, as polyester fabrics began to be used, the decrease in adhesive strength especially after hot water washing became a major problem. It's coming. On the other hand, polyester hot-melt adhesives have high adhesion to polyester woven fabrics and high hot water washing resistance due to low water absorption, but they have poor dry cleaning resistance and For example, it has not been used much as a textile adhesive because it has insufficient adhesion to woven fabrics such as cotton, wool, and rayon.

The inventors of the present invention have continued intensive research to improve the shortcomings of hot melt adhesives for textiles, and have found that they have excellent texture at the bonded area, excellent dry cleaning resistance and hot water washing resistance, and are also suitable for use on cotton fabrics. The inventors have discovered a polyester hot melt adhesive having excellent adhesive properties and have arrived at the present invention.

That is, the present invention provides a polyester resin consisting of a dicarboxylic acid component, an alkylene glycol component, and a polytetramethylene glycol component, in which the dicarboxylic acid component is 70 to 40 mol% of terephthalic acid, 0 to 55 mol% of isophthalic acid, and 45 to 5 mol% of adipic acid. %, the alkylene glycol component is 1,4L butanediol 50-1
00 mol%, ethylene glycol 50-0 mol%, and further contains 0.1 to 5 mol% of polytetramethylene glycol with a molecular weight of 600 to 4,000 based on the total dicarboxylic acid component. ~1.8, melting point 9'C~
100 parts of polyester resin at 140℃, particle size 200P
The hot melt adhesive part is made by melt-mixing 0.05 to 10 parts of the following inorganic powder particles. The hot melt adhesive of the present invention is a polyester resin having the above composition and a particle size of 200.
By blending 0.05 to 10% by weight of inorganic particles of P or less, it exhibits excellent adhesion to polyester and/or cotton fabrics, as well as excellent flexibility, hot water washing resistance, and dry cleaning resistance. A polyester resin having the above composition alone exhibits relatively excellent adhesion to polyester fabrics, but has poor hot water washing resistance and dry cleaning resistance, and extremely poor adhesion to cotton fabrics. The dicarboxylic acid component used in the present invention is 75 to 40 mol% of terephthalic acid and 0 to 55 mol% of isophthalic acid.
and adipic acid (45 to 5 mol%); however, if terephthalic acid exceeds 70 mol%, the melting point of the polyester becomes too high and cannot be bonded under normal adhesive processing conditions.
Forcibly raising the bonding temperature is undesirable because it causes shrinkage of the polyester fabric.

On the other hand, if the terephthalic acid content is less than 40 mol%, the melting point of the polyester will be low, the adhesiveness at high temperatures will be reduced, and the hot water washability will be greatly reduced. When the content of isophthalic acid exceeds 50 mol%, the crystallinity of the polyester decreases, the solidification rate slows down, and at the same time the polyester tends to stick. In particular, when used in powder form, it becomes difficult to crush, or even if it can be crushed, it may cause blockage during storage, making it impossible to apply. If the adipic acid content exceeds 45 mol %, the dry cleaning resistance will decrease and the crystal solidification rate will also become slow, which is not preferable. The most desirable ranges for the dicarboxylic acid component are 45 to 60 mol% of terephthalic acid, 45 to 0 mol% of isophthalic acid, and 10 to 40 mol% of adipic acid. The alkylene glycol component used in the present invention consists of 50 to 100 mol% of 1,4-butanediol and 50 to 0 mol% of ethylene glycol.
When 4-butanediol is less than 50 mol% and ethylene glycol exceeds 50 mol%, the crystal solidification rate becomes slow;
Blocking occurs when a powdered hot melt adhesive is applied onto a fabric and then rolled up.

Also, the adhesion to cotton fabrics is reduced, especially after dry cleaning. In the present invention,
Polytetramethylene glycol with a molecular weight of 600 to 4,000 is copolymerized in an amount of 0.1 to 5 mol% based on the total dicarboxylic acid components, but if it is less than 0.1 mol%, the desired texture cannot be obtained. If the amount exceeds 5 mol %, the dry cleaning resistance will be greatly reduced.

The hot melt adhesive of the present invention is prepared by melt-mixing 0.1 to 10 parts by weight of inorganic powder particles with a particle size of 200 P or less to 100 parts by weight of polyester. Adhesion to cotton fabrics is low, and conversely, if it exceeds 10 parts by weight, the adhesion to fabrics decreases, which is undesirable.

The most desirable addition amount is 0.5 to 5 parts by weight. 200
Examples of inorganic powder particles having a particle size of P or less include talc, silica, kaolin, titanium oxide, magnesium oxide, calcium oxide, alumina, calcium carbonate, and shirasu, but the most desirable compound is talc.

The reduced viscosity of the polyester resin of the present invention is 0.5 to 1.8
and is preferably 0.7 to 1.2.

If the reduced viscosity is less than 0.5, the adhesion will not be sufficient and oozing to the back of the fabric will occur. On the other hand, if it exceeds 1.8, the melt viscosity becomes too high, and even if the polyester is melted, sufficient adhesion to the fabric cannot be obtained.

In addition, it is necessary to consider the combination of ingredients so that the melting point is from 90°C to 140°C, but if the melting point is less than 90'C, it will not be possible to obtain excellent hot water washing resistance or dry cleaning resistance, and conversely, If the temperature exceeds ℃, the adhesive force will not be sufficient under normal processing conditions. The polyester hot melt adhesive of the present invention exhibits excellent performance particularly on polyester fiber fabrics, but also exhibits performance on other fabrics, especially cotton fabrics, that cannot be obtained with conventional polyesters.

In addition to textiles, it also has excellent adhesion to adhesives that require flexibility, such as vinyl chloride film, vinyl chloride or polyurethane-based artificial leather, leather, and rubber, and can be adjusted to suit the adhesive conditions. Can be used by selecting. Hereinafter, the present invention will be explained in more detail with reference to Examples.

In the examples, parts indicate parts by weight. The intrinsic viscosity of the polyester was measured at 30° C. in a mixed solvent of phenol/tetrachloroethane 6/4 (weight ratio). The melting point was measured with a fully automatic melting point measuring device (Mettler, MODELFP-1). For hot water washing, place the adhesive cloth in the home washing machine at 70°C.
I did laundry for 2 hours. As a dry cleaning test, the adhesive cloth was immersed in perchloren at 50° C. for 1 hour. The adhesive strength was evaluated using a T-type peel tester, and the retention rate was determined from the ratio of the peel adhesive strength immediately after hot water washing and immediately after the dry cleaning test to the normal peel adhesive strength. Example 1 Stirrer,
In a stainless steel autoclave equipped with a thermometer and cooling tube, add 970 parts of dimethyl terephthalate, 6 parts of dimethyl isophthalate J and V, and 19 parts of 1,4-butanediol.
80 parts, polytetramethylene glycol (molecular weight -10
50) Prepare 210 parts of potassium oxalate titanate, 1.40 parts of potassium titanate oxalate, and 0.85 parts of antimony trioxide, and heat at 170°C to 220°C.
After carrying out the transesterification reaction at ℃ for 3 hours, 1.92 parts of triphenyl phosphorite, 146 parts of adipic acid, and talc with a particle size of 2 to 5P (Micron White≠5 manufactured by Hayashi Kasei Kogyo Co., Ltd.) were added.
000) was added thereto, and an esterification reaction was carried out at 220'C to 260C for 1 hour.

Next, the pressure was gradually reduced at 260°C to remove excess glycol, and then a polycondensation reaction was carried out at 260°C for 2.5 hours under a reduced pressure of 0.1 to 0.3 m7fLH9. The resulting depolymerized polyester (A) had a reduced viscosity of 0.88 and a melting point of 122.
It was warm at ℃. As a result of compositional analysis by NMR, the composition of the depolymerized polyester (4) was 50 mol% of terephthalic acid, 40 mol% of isophthalic acid, 10 mol% of adipic acid, and 1,4-
The amount of polytetramethylene glycol was 2 mol per 100 mol % of butanediol and 100 mol of total dicarboxylic acids. As a result of elemental analysis, the amount of talc contained in polyester (4) was 3%. An 80P film made by dissolving this polyester in chloroform was sandwiched between polyester-based proof cloths and heated at 180°C and 200°C.
Adhesion was carried out for 5 seconds under a gr/Cll load. The obtained adhesive fabric has excellent texture and T-peel adhesion strength of 2.05K'/
CTfL, peel adhesion strength after immersion in Parkren is 1.85K
'/Cm, retention rate is 900t), peeling adhesive strength after hot water washing is 200K'/CT! L. The retention rate was 98%.
In addition, an 80P film made of the same polyester material was sandwiched between the cotton yarn plaid cloth, and bonding was performed under the same conditions. The obtained adhesive fabric has an excellent texture and a T-peel adhesive strength of 1.90K'/
Peel adhesion strength after soaking in Cml percrene is 1.45K'/
CTn, retention rate 76%, peel adhesion strength after washing with hot water is 1.
The 65K2/CTrLl retention rate was 87%. Example 2
~3 Comparative Examples 1 to 7 Polyesters (B) to (J) were obtained in the same manner as in Example 1.

Claims (1)

[Claims] 1 In a polyester resin consisting of a dicarboxylic acid component, an alkylene glycol component and a polytetramethylene glycol component, the dicarboxylic acid component is terephthalic acid 7
0-40 mol%, isophthalic acid 0-55 mol% and adipic acid 45-5 mol%, alkylene glycol component 1,4-butanediol 50-100 mol%,
Consisting of 50 to 0 mol% of ethylene glycol, and further 0.1 to 5 mol% of molecular weight 600 based on the total dicarboxylic acid.
0.05 to 10 parts by weight of inorganic powder particles with a particle size of 200μ or less are melt-mixed to 100 parts by weight of a polyester resin containing polytetramethylene glycol of ~4000 and having a reduced viscosity of 0.5 to 1.8 and a melting point of 90 to 140°C. Hot melt adhesive.