DE2137048A1 - Method and device for the production of a leather substitute product - Google Patents

Description

DR. BERG DIPL.-ING. STAPF

PATENTANWÄLTE 8 MÜNCHEN SO, MAUERKIRCHERSTR. 45

• Dr. Borg Dipl.-Infl. Stopf, 8 Munich 80, MouerkircharaftgBe 45

Your sign Your writing « Our sign

date

«3,

Attorney file 21 354

Etablissements Hutchinson Compagnie Nationale Du Caoutchouc Paris / France

Method and device for the production of a leather substitute product

2098U / U01

The invention relates to a method and a device for producing a soft and durable, air-permeable and water vapor permeable material, especially such a material as a substitute for leather can be used.

It is already known to have such a material in the form of a material which is permeable to water vapor and air and which is liquid To produce water-impermeable product. This product is commonly referred to as "Poromeres" and it consists generally from:

1. a nonwoven, needled nonwoven fabric, which is essentially consists of synthetic fibers, in particular polyester fibers *, which with a binder with a low Modulus of elasticity are impregnated, this fleece of the back of the material, for. B. the "flesh side" of the leather is equivalent to;

2. a surface coating, which is the glossy side or corresponds to the "grain side" of the leather and which consists of a microporous layer of a polymer material with

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low modulus of elasticity, generally made of polyurethane * exists and is applied to the fiber fleece by gluing or covering;

3. one between the non-woven fleece and the cover layer inserted woven carrier to achieve sufficient tensile strength.

The microporous layer is obtained when starting from a polymer solution to which a liquid is added, which is a nonsolvent for the polymer, but which is the same as that used to prepare the solution Solvent is miscible. An essentially colloidal dispersion of the polymer is obtained which is applied in a thin layer either to an auxiliary carrier or to the substrate, which is through the Nonwoven fabric and the woven carrier structure formed is formed. After partial gelling, this The layer is subjected to various treatments, in particular it is immersed in liquids that have a specific Contain quantitative proportion of a product which is a non-solvent for the polymer, but which is with is miscible with the solvent of the solution. By impact

■ 2098 U / UO 1

kung of several successive baths, which are increasingly richer in the nonsolvent maintained at appropriate temperatures is obtained from the Extraction of the solvent by the non-solvent creates a microporous layer.

The so-called deep-frying process (sintering process) is already known for producing a surface coating. in which one has a continuous layerj & us a fine Powder of a linear polymer, in particular of polyurethane, which is generally a blocked isocyanate fraction contains ^ forms. This layer is pressurized and heated without the polymer melting. The blocked isocyanate fraction is released and ensures the formation of molecular bonds, which improve the cohesion of the material.

For the production of the microporous surface layer applied to a substrate, a so-called one is already used "Fibridation process" known in which the techniques used in the manufacture of paper. So-called "fibrids" are made from a polyurethane prepolymer whose radial propagation speed

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The speed is about 1 to 40 cm / second "A polyurethane film _{9 is formed} by" sugjfbtj the prepolymerization solution to an amine solution which does not contain solvent for the prepolymer the Prepolymerisatfilmes to form a PoI] TUrethan = 'polymers with recurring Polyurethaneinhaiten _s can form fibrids ₀ After Uras®tsung d © r to represent non-solvent Äminlösuag spread film with the help of flights! stirrer cut to form fibrids _£ Man filters the fibrids from the pulp using techniques such as those used in papermaking and obtains microporous poromeric films that can be attached to a non-woven or other substrate for the production of a substitute product for leather _e

These various processes are complicated and require considerable manufacturing devices _s resulting in increased manufacturing costs.

The invention now relates to ain ^ method that has relative to the known method has the advantage that the Beschieh ₉ = tung in solution or Dispgrsionsphase avoided °

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In doing so, the ₂ technically too complicated deep-frying mediums FibEidioffFerfehren siirüeksugrsifen, with the sending out © rlsiabtg suf a daat-jieeliea inserted carrier in the production of the more porous material to dispense with the hoirstcslliiKig koatiimisriida.

The aim of the Erfiadraig is a fmisSahxen for the production of a weiclifsa mad Mf t ° and water vapor permeable material, which is characterized in that a water vapor permeable fleece is produced under a tape applicator in the same running direction and at the same speed as it passes while on the Fleece above the tape a crosslinkable coating mass of a microporous product is spread out, the tape being of sufficient length to keep the mass under pressure for at least part of the duration of the crosslinking »

The invention is particularly suitable for the production of a material ₉ which can be used as a substitute for leather and according to the invention a method 3Hr production © ines such material is proposed, which is characterized in that a fleece with a

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Permeability to water vapor of at least 40 g per

2
m per hour _s makes it under © imer Bandauftragsein "direction in the running direction and at the same speed as the same vorbeibewe'gt while propagating on the nonwoven above the belt a removable coating composition of a microporous _product? which has 40 to 90% open cells and of which a 6 mm thick sample has a remanent deformation of 15 to 35 % at 20 C with an elongation of 300% at a speed of 21 cm per minute, the tape being of sufficient length to the mass during at least part of the network to keep under pressure "

The invention relates in particular to a substitute product for leather, which consists of a fleece with a covering of a microporous polyurethane layer, which is characterized in that the fleece has a water vapor permeable

2
speed of at least 40 g / m / hour and that the layer has 40 to 90% open cells, with a 6 mm thick sample of the same at 20 ° C for an elongation of 300 % at a speed of 21 cm per minute a remanent deformation from 15 to 35 % .

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The product obtained according to the invention has in particular the following qualities:

-The grain of natural leather can be faithfully reproduced become what is not possible with the previous procedures;

-The "grip" or the "touch" of the product obtained is better than that of the comparable known products; -it has a permanent deformability, which is the important application for the production of shoes on the one hand enables the shoe to be given the desired shape during manufacture and, on the other hand, during use of the shoe ensures an adaptation to the shape of the foot and thus best the valued properties of natural leather and gives the user the desired Convenience there.

The invention also relates to a device for carrying out the method according to the invention. Below will be more in detail the details of the implementation of this process and the properties of those obtained thereby Products with reference to the accompanying drawing

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explained.

Fig. 1 of the accompanying drawings represents a schematic Longitudinal section through a device for the continuous production of a leather substitute material;

FIG. 2 is a schematic cross-section along line 2-2 of FIG.

The first stage of the process according to the invention consists of " in producing a fleece that is permeable to water vapor. To produce a quality material, the Water vapor permeability of the fleece preferably min-

2
at least 40 g / m / hour as measured by the method of Kanagy and Vickers as described in "Journal of the Leather Chemists Association", 45, 211-242 (April 19, 1950).

For most purposes, especially as a leather substitute, porous nonwovens are used. In such Nonwovens are, for example, woven fabrics, tricot fabrics, such as. B. Jersey, felts, porous, with rubber or synthetic resins, such as. B. vinyl halide polymers, impregnated nonwovens and re-produced

2098 U / UO 1

(reinforced) leather itself. The choice of fibers is not critical; these fleeces can be made of polyamides, polyesters, Polyester amides, rayon viscose, wool, cotton, glass and mixtures thereof. You can also use elastomers Use fibers and elastic fabrics. Particularly preferred as leather substitutes are the porous, non-woven, preferably heat-shrunk nonwovens made of polyethylene terephthalate fibers, which are impregnated with the above-mentioned polymers. If you don't - woven fibers is used, it is useful to interweave by needling (tying) for example on a loom "Hunter No. 9" and by 5 to 25% shrinkage in the Promote warmth. You can also use a non-woven fiber fleece use as such, but it can also be mixed with 10 to 60% by weight of a binding polymer dissolved in impregnate in an amount of 20 to 30% in a suitable solvent; depending on the type of polymer the solvent used is in particular ethyl acetate, methyl ethyl ketone, dimethylformamide, dimethyl sulfoxide, tetrahydrofuran, Use chlorinated solvents, etc. The impregnation polymer can also be in the form of an aqueous Emulsion, in the form of a dispersion or a latex. Preferably the binding polymer has

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2 a modulus of elasticity below 5 kg / mm.

You can use a polyester polymer with urethane segments or a urethane polyether or polyurea, a polyamide, a polyvinyl chloride or, in conjunction with a polyurethane, an elastomeric butadiene acrylonitrile in Use the form of an emulsion, an elastomeric latex, etc. The impregnation product can be immersed, can be applied to the non-woven fleece with the help of a squeegee, with the help of a roller or by dusting.

The nonwoven fabric 2 forming the substrate, which is unwound from a spool 1, is in contact with the upper thread (hair side) of a conveyor belt 4, which is formed by a pressed and flat endless metal fabric which runs around two pulling drums 5 and 6 of which the second is subjected to the action of a tensioning device, not shown, which maintains the tension of the belt 4, displaced horizontally. The upper thread with which the substrate 2 is drawn in contact is guided by sliding on the top of a table 7, the heating devices 8, 9 and 11 onwei ζ,,

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After it is under a pressure roller. 12, which is arranged perpendicular to the first drum 5, the substrate 2 is located under a mixer head 13 which is carried by a carriage (carriage) 14 which moves back and forth transversely on the crossbeam 16 of a frame 17 emotional. A crosslinkable coating compound made of a microporous product is fed through this head in the form of a pasty liquid 18. It is useful if the coating composition, once crosslinked, contains 40 to 90 % open cells. Excellent results are obtained if the coating material is one in which a 6 mm thick sample of the crosslinked material which has not been applied to the substrate is applied at 20 ° C. for an elongation of 30 % at a rate of 21 cm per minute exhibits remanent deformation of 15 to 35%. Such results can be obtained if a linear polyether or polyester with a molecular weight between 1000 and 5000 and at least two terminal hydroxyl groups is selected as the basic component of the coating material and this component is allowed to react with a polyisocyanate, especially a diisocyanate. This then results in a chain lengthening with the formation of urethane groups. At-

2098U / U01

Games for suitable polyethers are, in particular, the polyalkylene ethers of diols, in particular of glycol, for example a glycol polyethylene ether, a glycol polypropylene ether, a glycol polytetramethylene ether, a glycol polytetramethylene ether, a glycol polyhexamethylene ether, a glycol polyoctamethylene ether and a glycolamethylene ether and mixtures thereof, a glycol polynonamethylene ether, mixtures thereof. You can also use polyglycols that contain several different radicals in the molecular chain, such as. B. the compound HO (CH ₂ —OC ₂ H ₄ O) _n H, in which η is an integer above 1.

Polyesters, which can be used as a substitute or together with the above polyethers, are z ^v . B. those that are formed when carboxylic acids, carboxylic acid esters or hydrazides can react with mono- or polyglycols, for example the dicarboxylic acid condensation products z. B. azelaic, suberic, adipic, sebacic acid and alkylene glycols, e.g. B. of ethylene glycol, propylene glycol or tetramethylene glycol.

As diisocyanates, aromatic, aliphatic, cycloaliphatic Diisocyanates or their mixtures are used

209814/1401

will. Examples of such diisocyanates are e.g. B. tolylene-2,4-diisocyanate, tolylene-2,6-diisocyanate, m-phenylene diisocyanate, Biphenylene-4,4 * -diisocyanate, methylenebis- (4-phenylisocyanate), 4-chlorophenylene-1,3-diisocyanate, naphthalene-1,5-diisocyanate, tetramethylene-1,4-diisocyanate, Decamethylene-1,10-diisocyanate, cyclohexylene-1,4-diisocyanate etc.

In general, 0.5 to 2 moles of diisocyanate are used per mole of the basic ingredient. The polyaddition of the polyether or polyester and the diisocyanate can be carried out prior to the operations described below (working with the prepolymer) or be carried out simultaneously with it. The crosslinking is done with the help of a diol, in particular of a glycol of the type mentioned above. In general, 0.5 to 2 moles of dialcohol are used per Moles of polyether (or polyester) diisocyanate addition product,

To form cells in the final material, crosslinking is carried out in the presence of water. This is used in an amount of 1.8 to 2.2 moles per mole of diisocyanate in excess in the reaction mixture; h _e that. did not take part in the polyaddition reaction ·. That

2098H / U01

Water reacts with these isocyanate groups and carbon dioxide is released. This leads to the achievement from 40 to 90% open cells, paying particular attention to the rate of formation of the CO ^, the elongation the chain and its crosslinking acts, for example by introducing the catalysts in a suitable amount, which promote these different reactions and by regulating the working conditions, especially the temperature.

You can also use an auxiliary pore former, for example a halogenated hydrocarbon such as monofluorotrichloromethane or methylene chloride. The auxiliary pore former allows cell bursting in the desired one to be facilitated by regulating the belt temperatures Moment of the networking phase. The proportion of this auxiliary pore-forming agent is 0.03 to 0.8%, based on the total weight of the other components, so that macro-cell formation is avoided. The main entrainer, participating in the crosslinking reaction enables a cell density gradient to be achieved without the formation of a compact surface skin due to the fact that its

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Effect is relatively independent of the temperature of the surface of the tape application device.

The swelling agents, the effect of which is caused solely by thermal dissociation, either lead to a compact skin ₉ if the walls of the mold are below the critical temperature, or to a visible porous structure. The effects of the two pore-forming systems can also be combined with advantage will.

The coating compound 18 can be made by any suitable method. Man can do this in particular Coating compound according to the production process for prepolymers or according to the so-called "one shot" production process produce. After the coating compound 18 has been applied to the substrate in the manner that a layer is formed, the thickness of which is essentially determined by the speed of the carriage 14, the feed of the components feeding the various tubes 15 of the head 13 and the linear speed of the Belt 4 is defined, the coating compound 18 is in contact with the upper thread / an endless belt +) (Hair side)

20981 4 / UCM

Application and printing _device 19 ΰ which is almost parallel to the last ® ® aagaord «net above the conveyor belt 4 and with the help of two drums 21 and 22 _s dis can be adjusted in height independently of each other and which are provided by devices for compliance with the The tension of the belt 19 is completed _{s is} driven ο The second drum 22 is normally set at a height slightly above that of the first Troisa.sl 21 the first belt 23 _9, which is in direct contact with the drums 21 and 22 ;, a metal mesh like the conveyor belt 4 is _s while the second belt 24 preferably consists of a silicone elastomer © n ₀ The outer side of this second belt has a motif _g may be the just any motive ,, but which in the illustrated example th represents the grain of _leather's the one on the outer superficiality © of the coating of the out-of-the-way synthetic leather strip wants to apply ₀

The speed of the bsiden lower and upper band or 19 is synchronized by a differential Gesehwindigbsits ° converter in the way ₉ that the two with

213704

ύΦ.τ IMtergeits the substrate 2 tsad u <se Olbergsit® der Besefe-Ielitosg 18 each lsi contact steksadsa threads (brims) © is © speed safefsiscia,) dia gmusM is the same and that so is Fsrlssif © the V @ Ha © ts "ang _s di @ nedh. des releases of Trcasasl 21 Bad wälirsadi der ämeiifolgsE-deii Frsisetzuag i / on üö * Bad dlsr Esspassloa dar Mssss Tbsgiaatg that on BsEid 24 befiadlida © Moti ^ y constantly nssatss: Sraek and

H on the "coating 18 atifgsbif-aeiiTü sssd sir ^ asidfrei is printed on it, _o the pasty © mass two endless belts 18 may duvch DEA edges of the substrate 2 26 zuxückgeteLtes x ^ erdaa ^ di © ^übegi? ÜlisiHigsroIlen 27 and 28 with a vertical axis lamfea ₉ by. deaea the first one that drives you men symeliron ait that both Baaders 4 nnü 19 drives.

Di® Heigsiarielatiaiigoa S ₅ 9 iaad 11 are completed by a via de® Baad 19 Taefsstigtsn shaft 2 <S, which traliltmg with plates 29 with infrared tr aliltmg sur activating the opening and closing time tiiiEg d © s S. © aktionsgl © i ₉ ■ ^ elshas stsr formation of the gaiiHaselifeeri leads to open cells, wmτ see isfc _o

Öfi, S SnIoSdTS-C CiI (S jM'tt.iic ^ naive ^ i, biujjio viiü i, iöiiifaii, -:. _; ^

201814/1401

the cellular Polymerisatüberzug to 80/90% crosslinked The end of the cross-linking is achieved in a Heisüchacht 31st The final product _ΰ which a © water vapor permeable has ⁰ ness 35 to 70 g / m / Stund®, is wound onto © ine winding device 32 »The Läng © of the conveyor 'belt is, for example, 8 m for a Baadauftrags" means v © n 4 m _o Instead of the endless belt 19 may also be a strip of paper ODSR other suitable material which does v © n a coil unwinds and winds on a lower mounted © D rn, be used "

The following examples are intended to illustrate the invention without, however, restricting it thereto.

example 1

Working procedure ^ for the_Pregolvmerisat

First of all, a prepolymer is produced by 13,000 g of ethylene glycol polyadipate with a hydroxyl number of 1.76 and a molecular weight of 2000 (viscosity 500 cP), which has been dehydrated for 8 hours at 5 mm of mercury between 120 and 130 ° C, with 5450 g of diphenylmethane-4,4'-diisocyanate lets react, whereby one six

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Works for hours with stirring at 50 ° C. The prepolymer obtained in this way contains a certain number of free isocyanate groups which were determined by titration against dibutylamine (content of free HCO ~ 16).

The following mixture is prepared separately from this

Gram

1,4-butanediol 1300

Tin octoate 14

Triethylenediamine (Dabco) 36

Surface active agent (silicone DG 193) Houndry Process IO

Emulsifier W M (Bayer) 10

Additive SM-Dow Corning, 5% in water 40 monofluorotrichloromethane 05

This crosslinking mixture and the prepolymer are set at a temperature between 30 and 60.degree can be, by pumping, which a given ratio between the crosslinking agent and the prepolymer deliver, introduced into the mixer head 13. The mixing is carried out in the mixer head, including one Mixing screw rotates at a speed of 5 to 20 rpm. The dyes (metal oxide or an organic Dye in butyl dioctyl phthalate or in a plastic

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ornamental polymer) are © ntw © d @ r directly gu siaer of the compounds added or by a third pump with the Hiifsquellsitt ©! in dan misehisr head

guided

As a variant of Example 1 was gur Ergieltaag kaaa a · Viskositätρ approximately that of the Fropolyraeriiats nad of the crosslinking agent-corresponds to _a total weight Erleicliteruag d © r homogenization of the hybrid of ¥ © rs © tg ⁱ ffing8 © is © kösg © in © a polyester of the same Art siigsTboiaj, ^ fie © r for the Prep © ° lymerisat is used. In this case it is advisable to add the isocyanate excess in the prepolymer in an amount corresponding to the stoichiometric ratio with the polyester added to the crosslinking agent = höheng which can be the ratio of Prepolymerssat to Ver »netsungsmittel so 2s 1 to I ₅ IgIy expressed in MoleSj brought" obtained in the Miseherkopf

is evenly distributed on the substrate <

• Example 1 is repeated _s w © b © i this time the linear one

20ISH / UÖ1

2 1 "97Π / Q i J / U HQ

giykoied-ipatpQlysstsr <3xsi: Qh, sia Adipat voa Butane l ussffi Jltfc? lssglyk®l eit © iiscsir tfydrassylzali.! from I ₉ 76, Μΐ m.ittlQ '£ <mt MolilmalMfgstfisfet v-ea 2500 and eiasr Vis

krtifcat tfoiit 900 sP replaces w

The following polyols are prepared Best parts

Polyester (ethylene glycol butaiidiol adipate,

middle Molektilai-gewielit 2000)

Triethylendlamine

EmilgatQT

Mditif SM (5 % la water) Mono! ! nor tr χ elilona © tSiam

Weight in g

11000

112

32

15th

This is at the same time with 4700 g diphenylmethane-4,4 * - t with the help of © d © s K © pfes 13 distributed on the tape,

Sefcst m & n the units as in example 1

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Example 4

Example 3 is repeated, this time the polyester being replaced by a polyoxyalkylene glycol-polypropylene glycol a molecular weight between 1500 and 3000 is replaced.

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Claims (1)

Claims Iy method of making a soft and air and Water vapor permeable material, characterized in that a fleece (2) permeable to water vapor is produced, this translationally shifts, on the fleece a crosslinkable coating mass made of a microporous Product (18) spreads and in contact with the spread coating mass over the fleece a tape applicator (19) which translates in the same direction and at the same speed as the fleece is moved, can be painted, the application length of the tape on the mass is sufficient to the mass during at least keep some of the duration of the networking under pressure. 2. A method for producing a leather substitute material, characterized in that a fleece (2) with a 2 produces water vapor permeability of at least 40 g / m / hour, shifts this translationally, on the fleece a crosslinkable coating mass (18) made of a microporous product which has 40 to 90 % open cells 2098U / U01 j and of which a 6 ram thick © sample at 20 C and b <ai © iaer elongation of 300 X at a speed of 21 cm per minute has a remaasate deformation of 15 to 35 % , spreads and in general contact with the spread load = tungssasse over the fleece can paint a® Bandaufseimriefitiing (19), which is driven translationally in the same direction and at the same speed as the fleece ^ where the application length of the tape on the mass is sufficient ^ to the mass for at least its ■ part of the duration the networking mater pressure to lialt®n _o 3 ο A method according to claim 1 or 2 ₉ characterized ₉ characterized in that the surface of the tape applicator device (19) _s having the coating composition comes into contact ₉ is turned "embossed © dsr raised motif which is printed on the coating composition _o 4, method according to claim 3 _9, characterized in that. that the motif carried by the ribbon reproduces the grain of the leather. 5ο method according to one of the preceding claims _s thereby tp that the © Beseliie-lituaragSBiasse a Poly- = atb.SE "© dsif © irass iiEü © area Polyösfecsr old a molecular gc-t'ielät smselias. -1000 now 50CÖ csad ninäesBias two terminal Hjdrο; ψ · §Εΐιιρ .ρ®ϊΐρ © in Diisocjaaat, a dialcohol 5 ₉ ά & ώιτοΐτ marked ₉ that the Diisoeyanat la eiiasr Meiaga ψ & κί I ₅ I to 2 MoI per mole of polyether or polyester ₉ dsr Dialkoli ©! in an amount of 0 ^ 5-2 M © 1 per mole Folyäther (or polyester) -Diisoeyanat ^ adduct mnd the water in an amount of Ij8 to 2 ₉ 2 mol per mol of unreacted diisocyanate A method aaeli Änspnicli 5 ₉ characterized in that the Beseiiicfit-iingsiHasse also eiaen pore former, in particular © inen halogenier ^ th hydrocarbon, in an amount of Q ₁ to Og GEWC S-I, contains ₉ 03. 8 _Θ Lederersatgprodaktg consisting of a übsrsogenen with a microporous nonwoven PolyuretlianseMeht, characterized gekeniise _s lehnst that the fleece has a water vapor permeability 2
of at least 40 g / m / hour and the layer contains 40 to 90 % open cells and that a 6 mm thick 2 0 8 8 14/1401 Sample of which at 20 C and an elongation of 300% at a speed of 21 cm per minute has a remanent deformation of 15 to 35% _o 9 "Apparatus for carrying out the method according to claim or 2, which has a conveyor belt which is able to convey in contact therewith a substrate in the form of a fleece to _{be coated P} characterized by a distribution head (13) j which on one of a Hin ° movement driven carriage is secured _s to produce a layer of the coating material (18) on the substrate a tape applicator device (19) _t which is moved at the same linear speed as the conveyor belt and the same procedure follows as soon as the tape applicator device (19 ) comes into contact with the layer (18) carried by the substrate from a certain point behind the distribution head (13) and that it remains in contact with this layer over a predetermined length, as well as by heating means (8,9,11 and 29) which are provided in the active zone in which the tape applicator (19) is in contact with the layer of the coating material, for a thermal treatment of this coating material. 2098U / U01 21 370A8 10. Apparatus according to claim 9, characterized in that the tape application device (19) is provided with a motif that is to be printed on the coating compound, 11. Apparatus according to claim 9 or 10, characterized in that it has a differential speed converter for Has synchronization of the displacement speed of the two belts (4 and 19). 12. Device according to one of claims 9 to 11, in which the conveyor belt (4) is an endless belt, characterized in that that the tape application device (19) itself is also an endless tape. 13. The apparatus according to claim 12, characterized in that • the drums (21, 22) around which the tape applicator (19) can be adjusted in height independently of each other. 14. Device according to one of claims 9 to 13, characterized in that that two soft belts (26) are provided, which move at the same speed as the belts (4, 19) and move them to the respective edges of the 20981 kl U01 Tape application device (19) in the active zone of the latter are applied for the lateral reception of the coating compound. 15. Device according to one of claims 9 to 11 and 13 and 14, characterized in that the application device (19) consists of a tape of paper or other suitable material which unwinds from a reel and is wound onto a mandrel arranged below . 2098U / 1 Le e SO rs e ite