• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    1515727 Copolyester adhesives DYNAMIT NOBEL AG 23 July 1975 [25 July 1974] 30886/75 Heading C3R A copolyester, useful as an adhesive, is derived from terephthalic acid/ester and a glycol mixture comprising 1,4-butanediol and 1,6- hexanediol in a molar ratio of from 9 : 1 to 1 : 9. The copolyester preferably has a melting point of from 100‹ to 130‹ C. and a glass transition temperature of from - 10‹ to + 30‹ C. The copolyesters prepared in the examples also contain isophthalic acid, adipic acid or sebacic acid. The copolyesters may be applied as a melt or as a powder.
    公开号:SU843764A3
    申请号:SU752151509
    申请日:1975-07-04
    公开日:1981-06-30
    发明作者:Брюнинг Клаус；Гюнтер Штурм Карл
    申请人:Динамит Нобель Аг (Фирма)；
    IPC主号:
    专利说明:

    (54) MELT ADHESIVE FOR GLUING
    THERMAL SENSITIVE MATERIALS
    OR by transesterification at a temperature from 150 ° C to 2700 ° C, if necessary in the presence of a catalyst, for example, in a stirred autoclave dimethyl terephthalate and dimethyl eophthalate in a 90:10 molar ratio, are subjected to transesterification with butaidi 1.4-hexane, hexane-1-1, 6 (for example, in a molar ratio of 35:65) in the presence of a transesterification catalyst, for example, tetra-n-butyl titanium and, if necessary, zinc acetate dihydrate. Acid and diol component can be applied in equimolar amounts, preferably take an excess amount of diol component
    Methanol is distilled off at an internal temperature of 150-220 ° C and under normal pressure. After infusion of triphenyl phosphite with a small amount of diol (with the aim of slowing down the transesterification catalyst), air is removed and the internal temperature is raised to 270 ° C. After about an hour, the pressure is reduced to less than one Torr and after a further 3-4 hours of mixing with nitrogen, the vacuum is removed and the product contained in the autoclave is discharged through the BOTTOM valve and then granulated.
    The proposed hot melt adhesive as a target additive contains a means for improving the filling, for example Modaflow (30% alkyl acrylate and 70% 2-ethyl hexyl acrylate) and / or filler, for example, aluminum silicate, talc, silica gel, calcium carbonate, calcium sulfate with a grain size less than 5 microns
    Hot melt adhesive is prepared by mixing the polyester with the target additive, followed by homogenization, for example, in an extruder. Extruded hot melt glue is ground to a powder with a grain size of 50-500 micm.
    The polyester contained in the glue melt has a logarithmic decrement of vibration damping of 0.6-1.3 at the glass transition temperature and a viscosity of 0.5-1.5, determined using 1 weight% solution containing 60 weight parts. phenol and 40 weight.h. 1,1,2,2-tetrachloroethane, at 25 s according to the following equation
    W 1 DL / g, s.
    moreover, t, means solution expiration time — solvent expiration time, and c — concentration in g / ml.
    It is advisable to take the components of the polyester in the following ratio, mol.%: Terephthalic acid: isophthalic acid 50-95: 50-50, terephthalic acid: isophthalic acid:: saturated aliphatic dicarboxylic acid 45-80: 10-25: 10-30, terephthalic Schlote : saturated aliphatic dicarboxylic acid 10-90: 10-90.
    The invention is illustrated by the following examples.
    Example 1. 99.9 wt.% Of a powdered copolyester with a grain size of 60-200 microns based on a mixture of Torephthalic acid and isophthalic acid in a molar ratio of 50:50 and a mixture of butanediol-1.4 with hexanediol-1.6
    Q in a molar ratio of 50:50, having a viscosity of 0.72, a glass transition temperature of 13 ° C and a melting point of 565 ° C, is mixed with 0.1% by weight of Modaflow. The resulting mixture is heated before and by means of a roller machine is applied
    } on the reverse side of the polyvinyl chloride-containing synthetic material for the Thorog shoe lining. After daily storage, the surface of the adhesive is completely non-sticky due to
    0 can do without layer paper. The shoe lining thus coated is glued to the shoe upper by means of a presser, for
    5 10 sec without damaging the thermosensitive polyvinyl chloride surface. The adhesive strength of the bonded materials is determined in a tensile machine on samples 5 cm wide. It is 2.4 N / MM.
    Example 2. 99.9% by weight of powder copolyester (grain size 60-220 micm) based on a mixture of terephthalic acid with isophthalic acid in a 70:30 molar ratio and mixture
    butanediol-1,4 with hexanediol-1,6
    in a molar ratio of 50:50, having a viscosity of 0.76, a glass transition temperature of 19 s, a melting point of 83 ° C, and a logarithmic decrement
    0 decay of oscillations 1.15, mix CO, 1 wt.% ModafI OW. The resulting mixture is applied to glued paper, used in the manufacture of shoes for hard socks, with. Coverage through
    “About 5 minutes completely loses stickiness, i.e. Hard socks can be stacked without using lamination paper. Hard socks stick with top material
     shoes at 130C for 5 seconds. In this case, the adhesive strength of the glued. materials is 2.3 N / MM.
    .Primerz. 50% by weight of powder copolyester with a grain size of 60-200 microns based on a mixture of thermal acid and isophthalic acid in a molar ratio of 85:15 and a mixture of 1.4 butanediol and hexandanol 1, 6 in a molar ratio of 50: 50 having a viscosity of 0., 95, temperature
    0 glass transition .29 ° C, melting point and logarithmic decrement of vibration attenuation 0779, mixed with 50 wt.% Aluminum silicate. The resulting mixture is applied by
    5 grooved roll on cotton cloth, on which it is sintered in a drop of hot melt glue. The fabric thus treated is glued to another cotton cloth at 1400 s for 10 s. The initial adhesive strength of the two-ply textile material is 1.8 N / MM. After dry cleaning three times, the adhesive strength is 1.6 M / mm, and after washing three times at 60 ° C - 1, 9 N / Example 4. An example is repeated with the difference that 75% by weight of nopoic copolyester (grain size 60-220 micm) based on a mixture of tereph of the left acid with isophthalic acid and adipic acid in a molar ratio of 80-10: 10 and a mixture of butanediol-1, 4 with hexanediol-1.6 in a molar ratio of 60: 4-0, having a viscosity of 1.03, a glass transition temperature of 20 ° C, a melting point, and a log-1.05 logarithmic damping decrement mixed with 24.5 wt. aluminum silicate and 0.5 weight. % Modaf I pw In this case, the initial adhesive strength of a two-layer textile material is 2.1 N / MM. After three dry cleaning, the adhesive strength is 1.9 N / MM, after washing three times at 2, 2 N / MM. Example 5. The c-TOY example is repeated, with a difference of 99.5% by weight of a powder of a copolymer based on a mixture of terephthalic acid and isophthalic acid in a molar ratio of 50: 5 and a mixture of butanediol-1.4 with hexanediol -1.6 at a molar ratio of 90:10, having a viscosity of 0.85, a glass transition temperature, a melting point of 130 ° C, and a logarithmic decrement of vibration attenuation of 1.25, is mixed with 0.5 wt.% silk gel. Here, the initial adhesive strength of the two-ply textile material is 1.9 N / MM. After dry cleaning three times, it is 1.6 N / MM, and after washing three times at –2.1 .N / MM. Example 6. The example is repeated with the difference that 99.5% by weight of powdered co-ester based on a mixture of terephthalic acid with isophthalic acid in a molar ratio of 85:15 and a mixture of butanediol-1,4 with hexanediol-1.6 in a molar a ratio of 10:90, having a viscosity of 0.82, a glass transition temperature, a melting point of 108 ° C, and an oscillation damping decrement of 0.72, is mixed with 0.5 wt.% talc. Here, the initial adhesive strength of a two-ply textile material is 2.2 N / MM. After a three-time dry cleaning, it is 1.9 N / MM, and after a three-fold wash at borsa, it is 2.1 N / ml. Example 7. The example is repeated with the difference that 99.5% by weight of the powder copolyester based on a mixture of terephthalic acid with isophthalic and sebacic acids in a molar ratio of 45:25:30 and a mixture of butanediol-1, 4. with hexanediol-1,6 in a 50:50 molar ratio, having an viscosity of If 13, a glass transition temperature of -lOOc, a melting point of 40 ° C, and a logarithmic decrement of 1.3 decay of vibrations are mixed with 0.5 wt.% calcium carbonate. In this case, the adhesive strength of the bonded materials is 2.1 N / MM. Example 8 Example 1 is repeated, with the difference that 99.5% by weight of terephthalic acid-based copolyester powder and 1-butanediol-4 mixture with hexanediol-1.6 in a molar ratio of 50:50, having a viscosity of 0.6, a glass transition temperature of 29 ° C, a melting point of 123 ° C, and a logarithmic decrement of vibration damping of 0.63, is mixed with O, .5 weight. calcium sulfate. In this case, the adhesive strength of the bonded materials is 2 N / MM. Etc. and measure 9. Repeat example 1 with the difference that 99.5% by weight of the powder copolyester specified in the table are mixed with 0.5 weight. % Modaflow. In tab. Table 1 shows the physical properties of copolymers of terephthalic acid with ethylene glycol. 2 copolymers of terephthalic acid with butanediol-1,4. In tab. Figure 3 shows the physical properties of terephthalic acid copolyesters with mixtures of isobutanediol-1,4 and hexanediol-1.6. Data on the adhesive strength of bonded materials are summarized in Table. 4. As follows from the table and examples, the proposed glue provides increased adhesive strength. Example 10 (comparative). Example 1 is repeated, with the difference that 99.9 wt.% Powdered polyester is based on a mixture of 70 mol.% Terephthalic acid with 30 mol.% Isophthalic acid and ethylene glycol having a melting point, glass transition temperature, a viscosity of 0.72 and logarithmic the damping decrement of vibrations 1,2, is mixed with 0.1 wt.% Modaflow. In order to avoid serious damage to the PVC surface, bonding is carried out for 3 seconds. In this case, the adhesive strength of the deposited materials is 1.2 N / No. i. Example 11 (comparative) Comparative Example 1 was repeated with the difference that 50% by weight of powdered polyester was mixed with 50% by weight of aluminum silicate. The resulting melt is used to glue cotton fabrics together for 4 seconds in the same way as in the example. The initial adhesive strength of the two-layer textile material is 1.0 N / MM. After three dry cleaning, it is 0.6 N / MM, and after three times washing at –1.0 N / MM. EXAMPLE 12 (comparative), Example 1 is repeated, with the difference that. 99.9 wt.% Powdered polyester based on a mixture of 85 mol.% Terephthalic acid with 15 mol.% Adipic acid and amesi 50 mol.% Ethylene glycol with 50 butanediol-1,4, having a melting point of 182 ° C, a glass transition temperature of 65 ° C, viscosity .0 / 74 and a logarithmic damping factor of 0.85, mixed with O.jl wt.% Modaflow. In order to avoid serious damage to the polyvinyl chloride surface, bonding is carried out during 3 sec. Thereby, the adhesive strength of the adhered materials is 1.3 N / MM. PRI me R 13 (comparative). Comparative Example 3 is repeated with the difference that 50% by weight of the powdered polyester is mixed with 50% by weight. Alkynini silicate and the resulting melt adhesive are used to glue cotton fabrics for 4 seconds in the same way as in the example. For STONj, the initial adhesive strength of the two-layer textile material is 1.1 N / MM. After dry cleaning three times, it is 0.8 N / MM, and after washing three times at –1.2 N / MM. PRI me R 14 (comparative), (known glue). Example 1 is repeated, with the difference that a) 99.9 is the weight of the P1 of terephthalic acid-based skim polyester and a mixture of 80 mol. 1.4-butanediol with 20 mol.% hexanediol-1, 6 having a melting point, glass transition temperature, a viscosity of 0.76, and a logarithmic decrement of vibration attenuation 0.44, mixed with 0.1 wt.% Modaflow or b) 99 , 9 wt.% Powdered polyester based on a mixture of 90 mol.% Terephthalic acid with 10 mol.% Isophthalic acid and a mixture of 90 mol.% Butanediol-1,4 with 10 mol.% Hexanediol-1,6, having a melting point, temperature a glass transition 450e, a viscosity of 0.71 and a logarithmic damping decrement of 0.49, is mixed with 0.1 wt.% Modaflow .. To avoid serious damage to The vinyl chloride gluing surface is held at and accordingly for three seconds. Here, the adhesion strength of the adhered materials is 1.5 N / MM and 1.6 N / MM, respectively. PRI me R 15 (comparative). Comparative example is repeated. Example 5 with the difference that 5% by weight of powdered polyester a and b, respectively, are mixed with 50% by weight of alcumini silicate and the resulting hot melt adhesives are used to glue cotton fabrics at 19Ot and, accordingly, for 4 seconds as in example 3. In this case, the initial adhesive. the strength of the bilayer textile material is 1.4 N / MM and. 1.5 N / MM, respectively. After a three-time dry cleaning, it is 1.2 N / MM and 1.3 N / MM, respectively, and after a three-time washing at 60 ° C, it is 1.4 M / mmi 1, .5 N / MM, respectively. Table 1
    Isophthalic acid Adipic acid Isophthalic acid Adipic acid Isophthalic acid Adipic acid Isophthalic acid Adipic acid Adipic acid Azelaic acid
    0.71
    0,69
    0.61
    0.74
    0.81
    0.72
    0.42
    0.65
    0.72
    0.6
    0.38
    Ieophthalic acid /
    20/30 120 / sebacic acid
    Continuation of table 1
    6.70
    1.3
    -8 Isophthalic acid Same
    Continued table. 2 36 carbon atoms aliphatic dibasic acid, commercially available under the name Empol. Ta & faces
    Continued tab. 3
    01
    ъ
    m
    1L VO
    go
    %
    (N
    fS
    yu
    0 VO
    1L 17 8437 invention hot melt adhesive for bonding thermosensitive materials containing a thermoplastic polyester and a target additive, characterized in that, in order to increase adhesive strength, it contains polyester based on terephthalic acid or a mixture of it with isophthalic acid and / or saturated ... aliphatic dicarboxylic acid and a mixture of butanedibl-1,4 with hexanediol-1, 6, which has a temperature of water-. 418 40–130 ° C and the glass transition temperature from and to the target additive, a means for improving bottling and / or inorganic filler in the following ratio of components, weight,%: Polyester -50-99.9 Target additive 0.1–50 Information sources , taken into account during the examination 1. Patent of Germany No. 1103489, cl. 22 i, 12.10,61. 2. Patent of the USSR 605548, cl. C 09 D 3/64, 09/15/73 (prototype).
    权利要求:
    Claims (2)
    [1]
    Claim
    Hot melt adhesive for gluing thermosensitive materials containing a thermoplastic polyester and a target additive, characterized in that, in order to increase adhesion strength, it contains polyester based on terephthalic acid or a mixture of it with Ieophthalic acid and / or saturated aliphatic dicarboxylic acid and a mixture of butanediol-1.4 with hexanediol-1.6, having a melting point.
    40-130 ^ 0 and a glass transition temperature from -10 ° С to + 30 ° С and, as a target additive, a means for improving filling and / or inorganic filler in the following ratio of j components, wt.%:
    Polyester 50-99.9
    Target additive 0.1-50 Sources of information taken into account during the examination of L. 1. Federal patent »1103489, cl. 22 ί α , 10.10.61.
    [2]
    2. USSR patent No. 605548, cl. C 09 D 3/64, September 15, 73 (prototype).
    类似技术:
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    同族专利:
    公开号 | 公开日
    CA1054748A|1979-05-15|
    DE2435863C3|1983-02-24|
    FR2279784A1|1976-02-20|
    GB1515727A|1978-06-28|
    CH618199A5|1980-07-15|
    FR2279784B1|1981-01-02|
    SE414775B|1980-08-18|
    US4094721A|1978-06-13|
    DE2435863A1|1976-02-05|
    SE7508434L|1976-01-26|
    NL180514C|1987-03-02|
    ES439308A1|1977-02-16|
    JPS5137129A|1976-03-29|
    DE2435863B2|1979-08-30|
    JPS5922753B2|1984-05-29|
    BE831588A|1975-11-17|
    NL7508896A|1976-01-27|
    NL180514B|1986-10-01|
    ATA568475A|1978-08-15|
    IT1041006B|1980-01-10|
    AT349213B|1979-03-26|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE2435863A|DE2435863C3|1974-07-25|1974-07-25|Linear, saturated, semi-crystalline copolyesters|
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