EP2956558B1 - Procédé pour la fabrication de cuir - Google Patents

Procédé pour la fabrication de cuir Download PDF

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Publication number
EP2956558B1
EP2956558B1 EP14703867.3A EP14703867A EP2956558B1 EP 2956558 B1 EP2956558 B1 EP 2956558B1 EP 14703867 A EP14703867 A EP 14703867A EP 2956558 B1 EP2956558 B1 EP 2956558B1
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EP
European Patent Office
Prior art keywords
leather
acid
methanesulfonic acid
deliming
salts
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EP14703867.3A
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German (de)
English (en)
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EP2956558A1 (fr
Inventor
Robert Orth
Yu Mei
Walter Bertkau
Thomas Schneider
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BASF SE
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BASF SE
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Priority to EP14703867.3A priority Critical patent/EP2956558B1/fr
Publication of EP2956558A1 publication Critical patent/EP2956558A1/fr
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C14—SKINS; HIDES; PELTS; LEATHER
    • C14C—CHEMICAL TREATMENT OF HIDES, SKINS OR LEATHER, e.g. TANNING, IMPREGNATING, FINISHING; APPARATUS THEREFOR; COMPOSITIONS FOR TANNING
    • C14C1/00—Chemical treatment prior to tanning
    • C14C1/08—Deliming; Bating; Pickling; Degreasing
    • C—CHEMISTRY; METALLURGY
    • C14—SKINS; HIDES; PELTS; LEATHER
    • C14C—CHEMICAL TREATMENT OF HIDES, SKINS OR LEATHER, e.g. TANNING, IMPREGNATING, FINISHING; APPARATUS THEREFOR; COMPOSITIONS FOR TANNING
    • C14C3/00—Tanning; Compositions for tanning
    • C14C3/02—Chemical tanning
    • C14C3/04—Mineral tanning
    • C14C3/06—Mineral tanning using chromium compounds
    • C—CHEMISTRY; METALLURGY
    • C14—SKINS; HIDES; PELTS; LEATHER
    • C14C—CHEMICAL TREATMENT OF HIDES, SKINS OR LEATHER, e.g. TANNING, IMPREGNATING, FINISHING; APPARATUS THEREFOR; COMPOSITIONS FOR TANNING
    • C14C9/00—Impregnating leather for preserving, waterproofing, making resistant to heat or similar purposes
    • C14C9/02—Impregnating leather for preserving, waterproofing, making resistant to heat or similar purposes using fatty or oily materials, e.g. fat liquoring

Definitions

  • the present invention relates to a process for the production of leather comprising a plurality of steps, characterized in that methanesulfonic acid is used in at least one step selected from deliming and fatliquoring.
  • Processes for making leather typically involve a variety of steps. Many leather making steps are carried out in the aqueous medium at a certain pH. The adjustment of the optimum pH is of great importance and influences the properties of the produced leather.
  • the choice of a suitable acid to neutralize the leather has a significant influence on the quality of the leather produced. This is the case, for example, in the deliming step. For example, using too much acid can negatively affect the optical and physical properties of the leather, possibly because the raw hides swell too much. If one chooses a too weak acid, this can mean that the adjustment of the pH is slow or the acid or other substances needed for the production of the leather do not completely penetrate the rawhide. In addition to the pH, the properties of the leather are often influenced by the materials used and the manufacturing process in a way that is not always predictable.
  • conventional leather production methods in the deliming step remove the lime residues adhering to the liming, for example with about 1% lactic acid, dilute acetic acid, formic acid or other organic acids.
  • suitable acids are, for example, ammonium salts such as ammonium sulfate or ammonium chloride, boric acid, phosphoric acid or carbonic acid.
  • hydrochloric acid or sulfuric acid is also possible.
  • the use of these acids in leather production has long been known to the person skilled in the art and is described, for example, in Römpp's Chemie Lexikon under the heading "Tannery”. For a subsequent Mineralgerbung the nakedness is adjusted sour by pimples, whereby as pimples usually inorganic acids and common salt, if necessary also with additions of organic acids serve.
  • EP 563,139 describes the use of methanesulfonic acid for pimpling leather.
  • the object of the present invention was to provide a process for producing leather which does not have the disadvantages of the prior art which gives soft and attractive leather and is efficient to perform.
  • the object has been achieved by a process for producing leather comprising a plurality of steps, characterized in that methanesulfonic acid is used in at least one step selected from deliming and fatliquoring.
  • Animal skins are the skins of any dead animals such as beef, veal, pork, goat, sheep, kangaroo, fish, ostrich or game. It is irrelevant to the present invention whether the animals whose hides one wishes to treat were slaughtered, were huntmännisch killed or have died from natural causes.
  • Processes for making leather typically involve a variety of steps.
  • the hair is removed from the animal skin.
  • This step is also referred to as a shearing step.
  • the animal skin is usually treated with basic substances such as lime. Frequently, sodium hydroxide, sodium carbonate, sulfides or organic sulfur compounds are also added.
  • the deboning step for example, meat remnants and subcutaneous connective tissue are mechanically removed from the animal skin.
  • the deliming step also: descaling, English: deliming
  • the basic components from the depilatory step are partially or completely neutralized.
  • the animal skin is loosened and prepared for the absorption of tannin and thus on the actual tanning.
  • Suitable tanning methods include the use of mineral salts (chromium III, aluminum, zirconium or iron salts), vegetable tanning with vegetable tannins (tannins in leaves, barks, woods and fruits), tanning (synonymously tanning) with fish and marine oils (Trane) or with fats of the brain, synthetic tanning with synthetically produced tannins (syntans, resin tanning agents, polymer tanning agents, polyphosphates, paraffinsulfochloride), aldehyde tanning (formerly formaldehyde, today mainly glutaraldehyde). It is also possible to combine different tanning procedures.
  • the leather After tanning, the leather is usually mechanically dehydrated (withering) and brought to a uniform thickness with folding machines.
  • the final leather properties become such as softness, color, fullness, texture, ductility, water absorption, etc., determined by the wet finish. Further steps are often the retannage, deacidification or neutralization, dyeing, fatliquoring and fixation of dyes and fatty substances.
  • all tanning agent groups which have been described in the main tanning can be used for retanning.
  • synthetic tanning agents, vegetable tanning agents and resin and polymer tanning agents are of particular importance in the retanning, since they often have a particularly favorable influence on the fullness and structure of the leather.
  • the acid residues of strong acids are often neutralized, as a result of which, as a rule, a better resistance of the leather is obtained.
  • the coloring is often done with dyes that form a chemical bond with the leather fiber.
  • Advantageous dyes are distinguished not only by the good dyeing properties (for example, tacking properties on the leather, combinability, large color palette) and fastness properties, but also by low environmental impact.
  • the natural leather color depends, among other things, on the tanning agent used. Chrome tannins often give a light, greyish-green intrinsic color, vegetable oils can, for example, yellow-brown - reddish brown.
  • Aluminum salts and synthetic tannins often yield white to light beige leather. Glutaraldehyde and fatty tanning agents usually color the leathers yellowish.
  • a pH of 4 to 6.5 is usually set, preferably from 4.5 to 6.
  • a more acidic pH is set to ensure uniform fixation of the fatliquoring agent through the leather cross section to reach.
  • a pH of from 2 to 6, preferably from 2.5 to 5, particularly preferably from 3 to 4 and especially preferably from 3.2 to 3.5 is set towards the end of the fatliquoring step.
  • steps are often carried out in the order given for preparation. However, within limits, it is also possible to execute them in other orders or to execute and combine steps together. Not all of the above steps need to be performed to produce leather. In addition, processes for producing leather may include other steps in addition to the aforementioned steps.
  • methanesulfonic acid is used in the deliming step or in the fatliquoring step for the production of leather.
  • Methanesulfonic acid serves primarily to adjust the pH.
  • Methanesulfonic acid is preferably added to the animal skin at the beginning of the actual working step.
  • the operation consists essentially of the neutralization of basic components with acids, which according to the invention methanesulfonic acid include.
  • the use of methanesulfonic acid in a particular step is also understood to mean the addition of methanesulfonic acid before the actual working step or after the preceding working step, if this serves to prepare the actual working step.
  • methanesulfonic acid is used at least in the deliming step.
  • methanesulfonic acid is used at least in the fatliquoring step.
  • Methanesulfonic acid is used according to the invention usually as an aqueous solution.
  • methanesulfonic acid is used as 0.05 to 0.5% strength by weight aqueous solution, preferably 0.07 to 0.2% by weight and particularly preferably 0.08 to 0.15% by weight.
  • methanesulfonic acid is used together with salts and / or other acids and / or acid derivatives. Suitable acid derivatives are, for example, esters or acid anhydrides.
  • methanesulfonic acid is used with salts of methanesulfonic acid.
  • Suitable salts of methanesulfonic acid include, for example, alkali metal or alkaline earth metal salts such as sodium, potassium, magnesium or calcium salts of methanesulfonic acid.
  • methanesulfonic acid is used together with inorganic salts.
  • Suitable inorganic salts are, for example, salts of sulfuric acid, hydrohalic acids, phosphoric acid, boric acid, carbonic acid, nitric acid.
  • suitable inorganic salts are, for example, ammonium sulfate, sodium sulfate, sodium chloride, ammonium chloride.
  • methanesulfonic acid is used together with salts of organic acids.
  • Suitable salts of organic acids are, for example, ammonium, alkali metal or alkaline earth metal salts of organic acids, such as ammonium, sodium, potassium or magnesium salts of organic acids.
  • Suitable salts of organic acids are, for example, salts of monocarboxylic acids or dicarboxylic acids. Examples of suitable salts of organic acids are, for example, salts of formic acid, acetic acid, propionic acid, oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, tartaric acid, lactic acid, phthalic acid, terephthalic acid, maleic acid, fumaric acid.
  • methanesulfonic acid is used together with other acids.
  • Suitable other acids may be inorganic acids or organic acids.
  • Suitable inorganic acids are, for example, sulfuric acid, hydrochloric acid, boric acid, carbonic acid, phosphoric acid.
  • Suitable organic acids are, for example, monocarboxylic acids or dicarboxylic acids. Examples of suitable organic acids are formic, acetic, lactic, formic, propionic, oxalic, malonic, succinic, glutaric, adipic, tartaric, lactic, phthalic, terephthalic, maleic and fumaric acids.
  • methanesulfonic acid is used in combination with ammonium sulfate. In another embodiment, methanesulfonic acid is used in combination with formic acid. In another embodiment, methanesulfonic acid is used in combination with one or more ammonium salts of dicarboxylic acids. In another embodiment, methanesulfonic acid is used in combination with one or more aliphatic dicarboxylic acids. In another preferred embodiment, methanesulfonic acid is used in combination with one or more carboxylic acid esters.
  • the amount of Saizen, other acids or acid derivatives can vary widely.
  • an aqueous solution containing 0.05 to 0.2% by weight of methanesulfonic acid and 0.5 to 2% by weight of ammonium sulfate is used.
  • a pH of 4 to 9, preferably 6 to 8.5 and particularly preferably 7.5 to 8.5 is set.
  • the deliming step lasts from 30 minutes to 4 hours, in exceptional cases shorter or longer.
  • the deliming step is completed in 45 to 90 minutes.
  • Processes according to the invention are characterized in that they are simple to carry out and permit an efficient and rapid adjustment of the pH in the individual process steps. Furthermore, inventive methods allow the production of leather, which are characterized by advantageous optical and haptic properties. In particular, they are characterized by pleasant softness and do not swell so much, do not swell so much as leather, which are produced by conventional methods.
  • the leathers produced according to the invention are characterized by a good softness and have a pleasant, appealing, fine and clean grain. In addition, they have good dyeing properties such as high uniformity and color brilliance.
  • the physical properties such as tensile strength, tear strength, elongation at break or scar extensibility of the leather produced by the process according to the invention are comparable or better than those of leather, which have been prepared according to the prior art.
  • leather produced according to the invention which has been produced using methanesulfonic acid in the deliming step, is distinguished, in addition to the advantages described above, by the fact that calcium ions can be removed from the leather very efficiently. As a result, in particular the softness and tear strength of the leather is advantageously influenced.
  • Another object of the present invention is leather, which has been produced by the process according to the invention.
  • a rawhide of beef was depilated and fleshed. The depilation took place with the addition of quick lime and sodium sulfide.
  • the leathers were treated with decalcifier according to Example I.1 to I.6 to adjust a pH of 8. The skins were first treated at room temperature for 20 minutes with a mixture A and then for 60 minutes with a mixture B. Subsequently, the skins were subjected to tanning and retanning with identical chromium-tanning formulations.
  • methanesulfonic acid made it possible to adjust the pH in a shorter time and gave clean and flat raw skins which were not so much swollen as skins which were subjected to deliming without methanesulfonic acid.
  • the leathers made using methanesulfonic acid in the deleting step are softer than leathers made according to the prior art and have them nice, fine and clean scars.
  • the physical properties are comparable to or better than those of leathers made according to the prior art.
  • cowhide rawhide Four pieces of cowhide rawhide were depilated and fleshed. The depilation took place with the addition of quick lime and sodium sulfide. For deliming, the skins were first washed at room temperature for 20 minutes with water and then first treated with a 1.2 wt% solution of ammonium sulfate and then with a 3.5 wt% solution of ammonium sulfate and allowed to act for 10 minutes to a pH from 8.3 to 8.5.
  • the pH of the deliming solutions for Examples II.1 and II.2 was between 8.3 and 8.43 in both cases and was very similar.
  • the content of free calcium ions in the decalcification solution to Example II.1 and II.2 was significantly higher with the addition of methanesulfonic acid than without the addition of methanesulfonic acid.
  • the following procedure was performed on different pieces before the start of the deliming process and after completion of the deliming process.
  • the leathers of Examples II.1 and II.2 were dried before or after completion of the deliming. 0.15 g of leather was placed in a 50 ml Erlenmeyer flask and 4 ml of a mixture of nitric acid and hydrochloric acid (mass ratio 1.3) were added. As soon as the mixture was cooled back to room temperature, to this was added 1 ml of hydrogen peroxide (32 wt% in water). The mixture was heated to 120 ° C for 180 min. The mixture was cooled to room temperature and made up to 50 ml volume with water. The content of calcium ions in the leather was determined by determining the concentration of calcium ions in the solution by atomic absorption spectrometry.
  • the leathers of Examples II.1 and II.2 were washed twice with water for 10 minutes. Subsequently, the skins were subjected to tanning and retanning with identical chromium-tanning formulations.
  • the leathers of Example II.2 (with the addition of methanesulfonic acid) were less swollen and softer than the leathers of Example II.1 (without methanesulfonic acid).
  • Chromium-tanned wet-blue leather (beef) was cut into 1-by-1 cm pieces and 25 g each was placed in a 250-ml glass flask.
  • 25 g each was placed in a 250-ml glass flask.
  • 5 g of fatliquoring agent according to Table 2 were given and in each case so much fully desalted (VE) water that the amount of liquid in the flask including fatliquoring agent was 75 ml.
  • the flasks were heated to 40 ° C for three hours.
  • Table 2 Chromium content of the wastewater of various wet-blue leathers with addition of formic acid or MSA in the fatliquoring step; fatliquoring agents used: SS: sulfonated rapeseed oil, SIM: sulfite fish oil, OSL: sulfite fish oil, SXL / N: composite fatliquor, sulfate castor oil; Quantities of acid in% by weight relative to the leather used.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Treatment And Processing Of Natural Fur Or Leather (AREA)

Claims (10)

  1. Procédé de fabrication de cuir, comprenant plusieurs étapes, caractérisé en ce que dans au moins une étape sélectionnée parmi le déchaulage et le graissage, on utilise de l'acide méthanesulfonique.
  2. Procédé selon au moins l'une quelconque des revendications précédentes, dans lequel on utilise de l'acide méthanesulfonique au moins dans l'étape de déchaulage.
  3. Procédé selon au moins l'une quelconque des revendications précédentes, dans lequel on utilise de l'acide méthanesulfonique au moins dans l'étape de graissage.
  4. Procédé selon au moins l'une quelconque des revendications précédentes, dans lequel on utilise de l'acide méthanesulfonique en tant que mélange avec des sels et/ou d'autres acides et/ou des dérivés d'acides.
  5. Procédé selon au moins l'une quelconque des revendications précédentes, dans lequel on utilise de l'acide méthanesulfonique sous forme de solution aqueuse à 0,05 à 0,5 % en poids.
  6. Procédé selon au moins l'une quelconque des revendications précédentes, dans lequel le cuir est du cuir tanné au chrome.
  7. Utilisation d'acide méthanesulfonique pour fabriquer du cuir, l'acide méthanesulfonique étant utilisé dans une étape de déchaulage ou dans une étape de graissage.
  8. Utilisation selon la revendication 7, dans laquelle l'acide méthanesulfonique est utilisé dans l'étape de déchaulage.
  9. Utilisation selon la revendication 7 ou 8, dans laquelle l'acide méthanesulfonique est utilisé dans l'étape de graissage.
  10. Utilisation selon les revendications 7 à 9, dans laquelle l'acide méthanesulfonique est utilisé en combinaison avec des sels et/ou d'autres acides et/ou des dérivés d'acides.
EP14703867.3A 2013-02-14 2014-02-12 Procédé pour la fabrication de cuir Active EP2956558B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP14703867.3A EP2956558B1 (fr) 2013-02-14 2014-02-12 Procédé pour la fabrication de cuir

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP13155256.4A EP2607499A3 (fr) 2013-02-14 2013-02-14 Procédé destiné à la fabrication de cuir
PCT/EP2014/052691 WO2014124951A1 (fr) 2013-02-14 2014-02-12 Procédé de fabrication de cuir
EP14703867.3A EP2956558B1 (fr) 2013-02-14 2014-02-12 Procédé pour la fabrication de cuir

Publications (2)

Publication Number Publication Date
EP2956558A1 EP2956558A1 (fr) 2015-12-23
EP2956558B1 true EP2956558B1 (fr) 2016-11-16

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EP13155256.4A Withdrawn EP2607499A3 (fr) 2013-02-14 2013-02-14 Procédé destiné à la fabrication de cuir
EP14703867.3A Active EP2956558B1 (fr) 2013-02-14 2014-02-12 Procédé pour la fabrication de cuir

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Application Number Title Priority Date Filing Date
EP13155256.4A Withdrawn EP2607499A3 (fr) 2013-02-14 2013-02-14 Procédé destiné à la fabrication de cuir

Country Status (12)

Country Link
US (1) US11001902B2 (fr)
EP (2) EP2607499A3 (fr)
KR (1) KR102230317B1 (fr)
CN (1) CN104981549A (fr)
AR (1) AR094785A1 (fr)
AU (1) AU2014218021B2 (fr)
BR (1) BR112015019537A2 (fr)
ES (1) ES2616043T3 (fr)
MX (1) MX377941B (fr)
TW (1) TWI653341B (fr)
WO (1) WO2014124951A1 (fr)
ZA (1) ZA201506725B (fr)

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US10131831B2 (en) 2014-04-11 2018-11-20 Basf Se Process for acidizing using retarded acid formulations
CN104313199B (zh) * 2014-10-28 2016-03-09 北京泛博化学股份有限公司 小液比制备绵羊皮服装毛革的方法
EP3469104B1 (fr) * 2016-06-14 2022-09-28 Basf Se Procédé de préparation de cuir
CN109485562B (zh) * 2017-09-13 2022-11-25 斯塔尔国际有限公司 脱灰剂及其用途和脱灰方法
WO2020126855A1 (fr) * 2018-12-21 2020-06-25 Basf Se Mélange comprenant de l'acide méthanesulfonique et de l'acide sulfurique
EP3670675A1 (fr) * 2018-12-21 2020-06-24 LANXESS Deutschland GmbH Adjuvants dans la fabrication du cuir pour le travail de rivière
IL286137B2 (en) * 2019-02-13 2025-09-01 DEBx Medical Holding BV Preparations for removing dead or contaminated tissues from body surface injuries and the oral cavity
IT202000017719A1 (it) * 2020-07-22 2022-01-22 Beken Italia S R L Processo a ridotto impatto ambientale per la concia di pelli
NL2027083B1 (en) 2020-12-09 2022-07-07 Stahl Int B V Process for deliming of hides, skins or pelts

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Also Published As

Publication number Publication date
TW201441374A (zh) 2014-11-01
WO2014124951A1 (fr) 2014-08-21
BR112015019537A2 (pt) 2017-07-18
US11001902B2 (en) 2021-05-11
AU2014218021A1 (en) 2015-09-03
ZA201506725B (en) 2017-09-27
MX2015010584A (es) 2016-05-31
CN104981549A (zh) 2015-10-14
EP2607499A3 (fr) 2013-07-10
MX377941B (es) 2025-03-11
KR102230317B1 (ko) 2021-03-19
NZ710857A (en) 2020-09-25
EP2607499A2 (fr) 2013-06-26
EP2956558A1 (fr) 2015-12-23
US20150376726A1 (en) 2015-12-31
AU2014218021B2 (en) 2017-03-16
KR20150119203A (ko) 2015-10-23
TWI653341B (zh) 2019-03-11
ES2616043T3 (es) 2017-06-09
AR094785A1 (es) 2015-08-26

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