• 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:
    The invention relates to a glove made of a covalently crosslinked elastomeric film, wherein at least one layered silicate is contained in the elastomeric film.
    公开号:AT511292A1
    申请号:T858/2010
    申请日:2010-05-26
    公开日:2012-10-15
    发明作者:
    申请人:Semperit Ag Holding；
    IPC主号:
    专利说明:

    - 1 - • * ·
    The invention relates to a glove made of a covalently crosslinked elastomeric film, wherein in the elastomeric film at least one filler is contained, and a method for producing this glove by dipping a glove shape in a dipping bath, in which a latex is presented, wherein in the latex at least one filler is included.
    The trend especially in the examination glove sector - examination gloves are used, for example, in industry, in the laboratory or even in medicine - is due to the increased raw material price in the direction of thinner wall thickness. Due to the lower wall thickness but especially the protective function of the glove is affected. As the requirements for chemical protection have also increased in recent years, this trend is contrary to the needs of users.
    In order to get a grip on the costs of producing such gloves, the gloves are filled with fillers. For this purpose, mainly chalk is currently used. Chalk has the property to reduce the strength of the elastomer glove both immediately after production and after aging, and in addition, the chemical resistance is also massively negatively affected. In addition, such gloves have the disadvantage that they tend to gray color after sterilization.
    To improve the chemical resistance of such gloves, it is known from the prior art to use so-called laminates, ie to select multilayer glove constructions. For example, US 2005/0044609 A1 describes a glove made of a PVC substrate on which a barrier layer comprising an acrylic polymer having a glass transition temperature between -30 ° C. and + 30 ° C. is disposed in order to improve the chemical permeation coefficient. A disadvantage of N2008 / 29900 on such multilayered structures is that, in turn, higher production costs are associated with frequent dipping of the gloves.
    It is therefore an object of the invention to provide a thin-walled examination glove, which is inexpensive to produce.
    This object of the invention is achieved in the glove mentioned above in that the filler is a phyllosilicate, regardless of the method for producing this glove, in which a phyllosilicate is used as filler and the filler prior to addition to the latex in an aqueous Dispersion, and further by the use of a filler comprising a layered silicate, in particular of kaolin, for producing a glove of an elastomeric film. It has surprisingly been found that a significant improvement in the permeation resistance, at least for some chemicals, can be achieved by replacing the filler usually formed by chalk with a layered silicate. The reason for this probably lies in the fact that through the layer silicate, that is, the individual layers, a kind of "Barriere11 in the glove material! itself, that is to say in the elastomeric film, so that chemicals which penetrate into the glove material can be retained better or for a longer period of time between these layers, in particular due to the Van der Waals interactions between the layer atoms and the Atoms of the Chemicals The penetration of the chemicals between the layers may result in a slight swelling of the layered silicate, so that a slight pressure is introduced into the surrounding elastomeric material and thus also the permeation of these chemicals through the glove material itself is delayed. It is advantageous if the e-lastomermoleküle covalently crosslinked with each other so as to prevent the Aufquillen the e-lastomerfilms itself at least largely, otherwise the permeation would be reduced by this increased swelling of the elastomer in turn. It is thus possible with the glove according to the invention to produce these with smaller wall thicknesses, compared with those gloves which are filled with chalk, the mechanical properties being at least approximately comparable to those filled with chalk. On the other hand, it is possible to realize higher permeation times with the same wall thickness as in the case of gloves according to the prior art. It is also advantageous that the sterilization of the gloves, for example by means of electromagnetic radiation such as electron radiation or gamma radiation, does not result in any discoloration of gray. Preferably, the filler, that is the phyllosilicate, is converted into an aqueous dispersion before addition to the latex in order to achieve a more homogeneous distribution of this filler within the elastomer, in particular to prevent agglomerate formation.
    It is preferred if the elastomer film at a layer thickness of 1 mm has a permeation resistance according to DIN EN 374-3 of at least 14 minutes, in particular at least 16 minutes, preferably at least 18 minutes until the breakthrough of the solvent isopropanol.
    In particular, the glove may have a layer thickness selected from a range with a lower limit of 0.05 mm and an upper limit of 0.4 mm, or which is selected from a range with a lower limit of 0.1 mm and an upper limit of 0.3 mm.
    According to one embodiment of the invention it is provided that the filler is a clay mineral. Clay minerals offer the advantage that they are available on the one hand in comparison to synthetically produced sheet silicates cost and beyond clay minerals have the advantage that they are already predominantly very fine-grained, especially with particle sizes of less than 5 pm, in particular less than 2 pm. It is thus achievable a correspondingly homogeneous, fine distribution of the filler in the elastomer film.
    Particularly good results with regard to increasing the permeation resistance have been achieved if the clay mineral used is a mineral selected from a group comprising kaolinite, dickite, nacrite, halloysite, allophane or imogolite or mixtures thereof or the clay mineral according to another Embodiment variant is formed by kaolin and / or talc. In particular with kaolin it is also possible to achieve an improvement in the mechanical properties of the elastomeric glove, in particular with regard to the tear resistance or the tear propagation resistance of the glove. Furthermore, by using kaolin and / or talc, the gas permeability of the glove can also be reduced.
    It is advantageous if the kaolin has a kaolinite content of at least 70% by weight, the remainder being able to be formed by conventional accompanying substances occurring in clay minerals, such as quartz or mica-like silicates. The kaolin preferably has a kaolinite content of at least 80% by weight, in particular at least 90% by weight. N2008 / 29900 4-
    It is also possible that the clay mineral is hard-calcined to further improve the mechanical properties of the glove.
    In a preferred embodiment, it is provided that the proportion of the filler in the elastomeric film is selected from a range with a lower limit of 5 phr and an upper limit of 30 phr (phr: particles per 100 parts rubber). Although below 5 phr, an improvement in permeation resistance was observed, but not to the extent desired for the invention. With a content greater than 30 phr, the tear strength of the glove decreases, so that the advantage of better chemical resistance, that is, greater permeation resistance, does not outweigh the disadvantage of the reduced tear strength of the glove.
    In particular, the filler is contained in a portion selected from a range having a lower limit of 10 phr and an upper limit of 25 phr, preferably having a lower limit of 12 phr and an upper limit of 20 phr.
    It is furthermore advantageous if the filler is particulate, with 50% of the particles having a particle diameter of not more than 10 μm in order to achieve better distribution in the elastomer film.
    In particular, it is advantageous if at least 60% of the particles have a particle diameter of not more than 10 μm, preferably if at least 75% of the particles have a particle diameter of not more than 10 μm.
    According to a further embodiment variant, it is provided that the particle diameter of the largest particles amounts to a maximum of 30 μm. Namely, it has been observed that particles larger than 30 μm in diameter are defects within the elastomer film, and hence the mechanical properties are deteriorated.
    Preferably, the filler is used particulate, wherein the particle diameter of the largest particles is a maximum of 20 pm, in particular a maximum of 10 pm.
    According to another embodiment of the invention, it is provided that the filler has a volume-specific surface area of not more than 40 m2 / cm3, in particular not more than 25 m2 / cm3, preferably not more than 20 m2 / cm3, measured according to the BET method (DIN ISO 9277: 2003-05 ) having. The use of fillers with higher volume-specific surfaces leads to the fact that solvents entering the elastomeric film or N2008 / 29900 solvents are bound to a higher proportion of the filler and thus lead to a higher swelling of the phyllosilicate, which results in higher fractions of filler at the Elastomeric film suffers the mechanical properties, in particular the tear strength.
    The elastomer film is preferably made of a natural rubber latex, since it can not only be produced comparatively inexpensively, but also a special interaction (Van der Waal) between the sheet silicates and the natural rubber latex could be observed.
    As already mentioned above, it is particularly advantageous that the glove can be produced in one layer from a single elastomeric film, whereby a corresponding cost optimization can be achieved.
    According to one embodiment variant of the method, it is provided that the dispersion is added to the dispersion prior to the premixing of the latex, that is, for example, before the maturation of the latex, whereby a better incorporation of the filler into the elastomer film is achieved.
    In order to achieve the highest possible proportion of filler in the elastomer film and thus a correspondingly high increase in the permeation resistance, it is advantageous if the pre-crosslinking is carried out up to a degree of crosslinking of not more than 96% (toluene swelling, 20 ° C., ISO 1817),
    In particular, the pre-crosslinking can be carried out up to a degree of crosslinking of not more than 85%, preferably up to a degree of crosslinking of not more than 80%, since the filler is better integrated or embedded in the elastomer matrix.
    It is also possible to covalently attach the filler to the matrix, e.g. over silanes or the like.
    For a better understanding of the invention, this will be explained in more detail with reference to the following examples. All statements on ranges of values in the description of the present invention should be understood to include any and all sub-ranges thereof, e.g. is the statement 1 to 10 to be understood that all sub-areas, starting from the lower limit 1 and the upper limit 10 are included, ie. all sections begin N2006 / 29900 ··· # * * * * * I · * »« · * * # · · · l I · · # - «» • * I «· * * * * ·· * ·« · · * · «* · -6-with a lower limit of 1 or greater and end with an upper limit of 10 or less, eg 1 to 1.7, or 3.2 to 8.1 or 5.5 to 10.
    The preparation of the gloves is done with the exception of the use of a phyllosilicate filler as the prior art accordingly. Such a glove can thus be produced, for example, by the following dipping method.
    In a compounding step, if necessary, the chemicals required for a preliminary vulcanization step are added to the latex and, if appropriate, a homogenization of the latex is carried out. Subsequently, the optionally of / vulcanized latex is transferred to a chain dipping plant, where it passes through the steps of dipping, margins, wet leaching, drying, optionally dry leaching, if necessary, powdering, stripping, packaging, quality control and optionally sterilization. The dipping forms are subjected to cleaning, coagulant dipping and drying before re-dipping in latex.
    The forms are usually made of porcelain, but can also be made of glass, stainless steel or plastic. A clean surface of this dip form is a criterion for a homogeneous deposition of the latex film in the subsequent dipping process. Both basic and acidic solutions, oxidizing compounds, surfactants or often a combination of these cleaning chemicals is used for the degreasing and cleaning of the dipping forms.
    The composition of the coagulation bath is, inter alia, a parameter for the thickness of the deposited latex film. The coagulation bath is usually composed of the coagulant (usually CaNO 3, optionally also CaCl 2), the release agent (CaCO 3) and the wetting agent (cationic surfactants). The release agent facilitates the removal of the glove from the dip mold, wherein in some powder-free processes other inorganic salts and partly also polymers can be used, as is known from the prior art.
    The deposited positive metal ions on the surface of the dip form cause a discharge and subsequently the coagulation of the negatively stabilized latex as soon as the mold dips into the precrosslinked latex. Depending on the immersion time and the concentration of the metal ions, different film thicknesses are obtained. N2008 / 29900 7 -
    Gloves can be made with a rolled edge at the bottom of the shaft. For this purpose, a part of the deposited film is mechanically rolled together at the edge by rotating brushes. Due to the stickiness of the film, the rolled bead remains over the entire manufacturing process.
    The wet latex film is given mechanical strength by brief drying before wet leaching. By dipping the latex films in a warm (~ 50 °) water bath proteins are at least partially washed out in addition to the coagulant.
    To prepare powder-free gloves, instead of powdering, a surface treatment, e.g. by chlorination, to improve the on and extendability of the gloves. But there are also sliding coatings possible.
    Since immersion methods for gloves are known per se from the prior art, the person skilled in the art is for example referred to EP 0 856 294 A, in particular FIGS. 4 and 5 of this EP-A and the associated explanations in column 14, line 38 to column 18 , Line 51, in particular with regard to the comments on coagulation, diving in latex, various washes, various post-treatments, such as Chlorination or halogenation of the surface of the gloves or of the latex, the production of surface roughness or the provision of powder-free gloves, etc. It is to be dispensed with unnecessary repetitions of the prior art in the context of the present invention and therefore forms the EP 0 856 294 A1 at least to the extent mentioned part of the disclosure of this application.
    The core of the invention is, as stated above, in the production of gloves with increased resistance to permeation against chemicals, that is, that these gloves oppose the passage of chemicals through the elastomeric film, a higher resistance and thus the permeation time is higher. This is achieved by using a layered silicate. In particular, a clay mineral, preferably from a group comprising kaolinite, dickite, nacrite, haloisitol, allophane, imogilite, is used as sheet silicate. In particular, the clay mineral may be formed by kaolin and / or talc, wherein the proportion of the layered silicate filler may be between 5 phr and 30 phr. If no kaolinite is used, it is advantageous if the kaolin has a kaolinite content of at least 70 wt. -% having. In addition to the improved permeation times, that is to say the higher permeation times, these gloves have an improved swelling behavior against various solvents, that is to say that the swelling is smaller than in comparison with gloves without the filler according to the invention. Furthermore, the gas permeability of such gloves can also be improved.
    It is also possible that the phyllosilicate surface-modified and / or hard-calcined is used. For example, the phyllosilicate can be silanized. By modifying the OH groups with silanes, the interaction with polar rubbers can be influenced. For example, with monofunctional silanes, such as triethyopropylsilane, trimethoxyoctylsilane triethoxyoctylsilane, the hydrophobing can achieve a lower viscosity of the latex and thus better film formation. By using bifunctional Organosiianen, such as 3-chloropropyltriethoxysilane, bis (3-triethoxysilylpropyl) tetrasulfane, triethoxy (3-thiocyanatopropyl) silane, especially of bifunctional Organosiianen with crosslinking active groups (eg vinyl or thiol), a covalent attachment of the phyllosilicate can the rubber can be achieved, whereby, for example, higher tensile strengths, etc. can be achieved.
    The phyllosilicate filler is preferably first converted into an aqueous dispersion, particulate fillers in particular being used and the particle size, ie the particle diameter, being preferably selected so that at least 50% have a particle diameter of not more than 10 μm and further preferably the particle diameter of the largest Particle is a maximum of 30 pm. In the context of the invention, however, fine particulate fillers are preferred, that is to say that the maximum grain or the maximum particle diameter is less than 30 μm and at least 50% of the particles have a particle diameter of not more than 3 μm.
    The filler may further have a volume-specific surface corresponding to the above information.
    Preferably, the filler is dispersed prior to being added to the latex in a solvent, especially water. This filler dispersion is preferably mixed in before the precrosslinking of the latex in these. But it is also possible that the dispersion is buried after maturation, ie after the pre-crosslinking of the mixture.
    It is furthermore advantageous if the crosslinking of the elastomer molecules takes place covalently in a glove according to the invention, for example by means of sulfur, peroxides N2008 / 29900 -9 -I1 * * * ► * * * I · * • tl < · * I or other materials that lead to crosslinking, as this greatly reduces the increased swelling of the film and thus further improves the permeation, ie the permeation times can be increased.
    It is further advantageous if the precrosslinking of the elastomer is not too strong before the glove is dipped to improve film formation at the higher filler levels. In particular, pre-crosslinking levels of not more than 96% or not more than 85%, preferably not more than 80%, are preferred.
    The degree of crosslinking is determined by the swelling, if the filler is mixed after the pre-crosslinking, but if the filler is added before crosslinking, the Vorvernetzungsgrad can be determined, for example, via the module. For the production of a glove according to the invention, for example, the following basic formulation can be used,
    Latex: 100 phr
    Stabilizer: 0.1 phr to 0.5 phr
    ZnO: 0.1 phr to 0.8 phr, preferably 0.3 phr S: 0.4 phr to 1.2 phr, preferably 0.8 phr
    Zinc diethyldithiocarbamate: 0.1 phr to 1 phr, preferably 0.3 phr
    Zinc dibutyldithiocarbamate: 0.1 phr to 1 phr, preferably 0.2 phr
    Zinc 2-mercaptobenzothiazoi: 0 phr to 0.2 phr, preferably 0.05 phr of 1,3-diphenylguanidine: 0 phr to 0.5 phr, depending on the temperature of the pre-crosslinking at room temperature, preferably up to 0.2 phr
    Aging protection: 0.5 phr to 1.5 phr, preferably 0.8 phr
    As the stabilizer, for example, KOH or another stabilizer known in the art may be used. Anti-aging agents can also be used according to the state of the art.
    This mixture is preferably ripened, this ripening being carried out at 30 ° C. for, for example, 24 hours or at 60 ° C. for 2 to 4 hours,
    Preferably, the latex used is a natural rubber latex. However, other elastomers may also be used, e.g. Styrene-butadiene rubbers, butadiene rubbers, isobutylene-isoprene rubbers, ethylene-propylene-diene monomers, nitrile N2008 / 29900.
    Butadiene rubbers, chloroprene rubbers, fluoro rubbers, or mixtures thereof.
    Subsequently, the aqueous kaolin dispersion can be added.
    As can be seen from the following tables, an extension of the permeation times could be achieved by using a layered silicate, in particular kaolin.
    Table 1: Glove made of natural rubber latex, solvent isopropanol, wall thickness of the glove and breakthrough of the solvent in each case as an average of ten measurement results, measured according to DIN EN 374-3, proportion of the filler in each case 20 phr. Filler wall thickness [mm] Breakthrough time [min] Normalized to 1 mm wall thickness [min] Kaolin1 0.210 3.8 17.99 (kaolin content 85%) talc 0.171 2.15 12.58 chalk 0.250 2.7 10.8 1: without kaolin the breakthrough time normalized to 1mm wall thickness is 9.8 minutes Similar results have been obtained with the minerals Dickit, Nakrit, Halloysite, Allophane, Imogolite, it being noted that generally not natural substances have to be used, but also substances with this corresponding composition, N2008 / 29900 •••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••
    Table 2: Influence of the filler content (kaolin):
    Percentage [hr] Breakthrough time [min] at 1 mm wall thickness 500 modulus [N] 0 9.8 2.2 15 14.76 20 17.99 4.7 30 18.25 8.3 40 19.32 12.3
    The embodiments describe possible embodiments of the glove, it being noted at this point that the invention is not limited to the specifically illustrated embodiments thereof, but also various combinations of the individual embodiments are possible with each other and this possibility of variation due to the teaching of technical action by representational Invention in the skill of those skilled in this technical field. N2Q08 / 29900
    权利要求:
    Claims (17)
    [1]
    1. A glove of a covalently cross-linked elastomeric film, wherein in the e-lastomer film at least a filler is included, characterized in that the filler is a layered silicate.
    [2]
    2. Glove according to claim 1, characterized in that the elastomeric film at a layer thickness of 1 mm has a permeation resistance according to DIN EN 374-3 of at least 14 minutes until the breakthrough of the solvent isopropanol,
    [3]
    3. Glove according to claim 1 or 2, characterized in that the at least one filler is a clay mineral.
    [4]
    4. Glove according to claim 3, characterized in that the clay mineral is selected from a group comprising kaolinite, dickite, nacrite, halloysite, allophane, imogolite.
    [5]
    5. Glove according to claim 3, characterized in that the clay mineral is kaolin and / or talc.
    [6]
    6. Glove according to claim 5, characterized in that the kaolin contains at least 70 wt .-% kaolinite.
    [7]
    7. Glove according to one of claims 3 to 6, characterized in that the clay mineral is hard-calcined.
    [8]
    A glove according to any one of claims 1 to 7, characterized in that the filler is contained in an amount selected from a range with a lower limit of 5 phr and an upper limit of 30 phr. N2008 / 29900

    φ * * ·; · F # ♦ t «4 I ♦ k · · · · ·« · * · * »* ♦ · -2-
    [9]
    9. glove according to one of claims 1 to 8, characterized in that the filler is particulate, wherein 50% of the particles have a particle diameter of not more than 10 pm.
    [10]
    10. Glove according to claim 9, characterized in that the particle diameter of the largest particles is a maximum of 30 pm.
    [11]
    11. Glove according to one of claims 1 to 10, characterized in that the filler has a volume-specific surface area of not more than 40 m2 / cm3, measured by the BET method.
    [12]
    12. Glove according to one of claims 1 to 11, characterized in that the elastomeric film is made of natural rubber latex.
    [13]
    13. Glove according to one of claims 1 to 12, characterized in that the elastomeric film is monolayered.
    [14]
    14. A method for producing a glove according to any one of claims 1 to 12 by dipping a glove shape in a dip in which a latex is presented, wherein in the latex at least one filler is included, characterized in that a phyllosilicate is used as the filler and the filler is converted to an aqueous dispersion prior to addition to the latex.
    [15]
    15. The method according to claim 14, characterized in that the dispersion is added to the latex before the pre-crosslinking.
    [16]
    16. The method according to claim 14 or 15, characterized in that the pre-crosslinking is carried out to a degree of crosslinking of not more than 96% {toluol swelling). N2008 / 29900 «· ** · * * · 4 * *« 4 ·· '· * * • * «« · 4 II * I * * * * tf 4 »« ft »*** 4 ·· -3-
    [17]
    17. Use of a layered silicate, in particular of kaolin, as a filler for producing a glove made of an elastomeric film. Semperit Aktiengesellschaft Holding by

    Lawyers Butii6T ~ & 1. A glove made of a covalently crosslinked elastomeric film, wherein in the elastomeric film at least one layered silicate, which is a clay mineral, is contained as a filler, characterized in that the clay mineral is selected from a group comprising kaolinite, dickite, nacrite, halloysite, allophane, imogolite or that the clay mineral is kaolin as is known in the art, the kaolin containing at least 70% by weight kaolinite. 2. Glove according to claim 1, characterized in that the layered silicate is silanized for surface modification. 3. Glove according to claim 1, characterized in that the clay mineral is hard-calcined. A glove according to any one of claims 1 to 3, characterized in that the filler is contained in an amount selected from a range with a lower limit of 5 phr (parts per 100 parts of elastomer) and an upper limit of 30 phr , 5. Glove according to one of claims 1 to 4, characterized in that the filler is particulate, wherein 50% of the particles have a particle diameter of not more than 10 pm. 6. Glove according to claim 5, characterized in that the particle diameter of the largest particles is a maximum of 30 pm. 7. Glove according to one of claims 1 to 6, characterized in that the filler has a volume-specific surface area of not more than 40 m2 / cm3, measured by the BET method. FOLLOW-UP A2010 / 00858 t ♦

    : -2

    8. Glove according to one of claims 1 to 7, characterized in that the elastomeric film is made of natural rubber latex. 9. Glove according to one of claims 1 to 8, characterized in that the elastomeric film is a single layer. 10. A method for producing a glove according to any one of claims 1 to 8 by dipping a glove shape in a dip in which a latex is presented, wherein in the latex at least one filler is included, characterized in that a phyllosilicate is used as the filler and the filler is converted to an aqueous dispersion prior to addition to the latex. 11. The method according to claim 10, characterized in that the dispersion is added to the latex before the pre-crosslinking. 12. The method according to claim 10 or 11, characterized in that the pre-crosslinking is carried out to a degree of crosslinking of not more than 96% (Toluolquellung). Semperit Aktiengesellschaft Holding by attorneys Affiliated Attorney at Law GmbH FOLLOW-UP A2010 / 00858
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    引用文献:
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    AT518307B1|2016-03-04|2020-04-15|Semperit Ag Holding|Method of making a prophylactic article|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    ATA858/2010A|AT511292B1|2010-05-26|2010-05-26|GLOVE|ATA858/2010A| AT511292B1|2010-05-26|2010-05-26|GLOVE|
    US13/115,620| US20110289655A1|2010-05-26|2011-05-25|Glove|
    EP11167608A| EP2389820A1|2010-05-26|2011-05-26|Glove|
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