EP1511865B1 - Verfahren zur entfernung von hornsubstanzen aus häuten, pelzen oder pelzfellen - Google Patents

Verfahren zur entfernung von hornsubstanzen aus häuten, pelzen oder pelzfellen Download PDF

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Publication number
EP1511865B1
EP1511865B1 EP03752667A EP03752667A EP1511865B1 EP 1511865 B1 EP1511865 B1 EP 1511865B1 EP 03752667 A EP03752667 A EP 03752667A EP 03752667 A EP03752667 A EP 03752667A EP 1511865 B1 EP1511865 B1 EP 1511865B1
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EP
European Patent Office
Prior art keywords
skins
weight
pelts
alkyl
butyl
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
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EP03752667A
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German (de)
English (en)
French (fr)
Other versions
EP1511865A1 (de
Inventor
Tilman Lüdecke TAEGER
Gunther Pabst
Philippe Lamalle
Stephan Hüffer
Stefan Schroeder
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BASF SE
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BASF SE
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Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • C14C1/06—Facilitating unhairing, e.g. by painting, by liming

Definitions

  • 1,4-Dimercaptobutandiol-containing formulations for the removal of horny substances, in particular hair, from living tissue is known, for example in unwanted beard growth.
  • DE 21 31 630 shows DE 21 31 630 in that it is possible to apply agents consisting of at least 0.25% by weight of dimercaptobutanediol and about 0.01 to 40% by weight of a water-soluble guanidine compound and a pH of less than 12 to guinea pigs to depilate them, or human cornea to eliminate calluses, without causing skin irritation in guinea pigs or even erythremia (malignant growths of the red blood cell formation system).
  • the epidermis remains at the in DE 21 31 630 received treatment described.
  • EP-A 0 095 916 For example, the use of formulations containing aminoethanethiol and 1,4-dimercaptobutanediol and an aminoguanidine or diguanide compound is known to eliminate unwanted human body and facial hair. On page 2, line 1 it is taught that small thiol molecules are preferred to induce rapid depilation because they penetrate the skin more quickly. The epidermis remains at the in EP-A 0 095 916 received treatment described.
  • EP-A 0 096 521 For example, the use of formulations containing, for example, 1,4-dimercaptobutanediol and an aminoguanidine or diguanide compound is known to eliminate unwanted human body and facial hair. The epidermis remains at the EP-A 0 096 521 received treatment described.
  • horny substances are calluses, feathers, nails and claw parts, and in particular hair of animals.
  • the skins, epidermis may still contain remnants of meat of the relevant dead animals.
  • Essential to the invention is that they contain horny substances.
  • the amount of horny substance, based on the total weight of the skin or the fur or the fur coat, is not critical.
  • the inventive method is suitable both for the removal of large amounts of horny substance as well as for the removal of small hair residues.
  • dead animals are understood not only to be slaughtered, hunted or otherwise deliberately killed by humans, but also to animals that have been due to accidents, for example traffic accidents, or fights with other animals or natural causes as age or disease have died.
  • the hides, furs or furskins of the animals are usually skins, furs or fur skins of cattle, calves, pigs, goats, sheep, lambs, elks, game such as deer or deer, and birds such as ostriches, fish or reptiles such as snakes.
  • the procedure is advantageously as follows.
  • R 1 contains at least one sulfur atom
  • at least one radical X 1 to X 4 denotes an SH group
  • at least two radicals X 1 to X 4 Group in the event that R 1 contains no sulfur atom, at least two radicals X 1 to X 4 Group.
  • At least one, more preferably at least two X 1 to X 4 hydroxyl groups are preferred.
  • alkali and alkaline earth metal salts are in particular the mono- and disodium salts, mono- and dipotassium salts and potassium sodium salts of the compounds of general formula I, furthermore the corresponding calcium and magnesium salts.
  • ammonium salts or primary, secondary, tertiary and in particular quaternary mono- and diammonium salts and phosphonium salts are also used.
  • mixtures of compounds of general formula I and their corresponding alkali or alkaline earth metal salts or ammonium or phosphonium salts can be used.
  • Preferred mono- and di-ammonium salts have as cations those of the formula N (R 3 ) (R 4 ) (R 5 ) (R 6 ) + , wherein R 3 to R 6 are each the same or different and selected from hydrogen, C 1 -C 12 -alkyl, phenyl or CH 2 -CH 2 -OH.
  • R 3 to R 6 are each the same or different and selected from hydrogen, C 1 -C 12 -alkyl, phenyl or CH 2 -CH 2 -OH.
  • Preferred mono- and diphosphonium salts have as cations those of the formula P (R 3 ) (R 4 ) (R 5 ) (R 6 ) + , where R 3 to R 6 are as defined above.
  • I a, I a 'and I b one or their corresponding alkali or alkaline earth metal salts.
  • I b is also called dithioerythrol.
  • racemic dithiothreitol is virtually odorless, easy to dose and readily soluble in water compounds.
  • the compounds I a or I a 'and I b are known and commercially available, for example, from Aldrich or AGROS Chemicals.
  • the synthesis of further compounds of general formula I succeeds as in US 4,472,569 or J. Chem. Soc. 1949, 248 described or by analogous reactions.
  • the treatment according to the invention of the hides, furs or fur skins with one or more compounds of the general formula I is carried out in liming or in the swede, both under hair-destroying and hair-preserving conditions. It succeeds in the liming or the swath instead of the usual concentration of about 4 wt .-% Na 2 S or NaHS or even slightly more, with a concentration of less than 1 wt .-% Na 2 S or NaHS at have the same effect on the removal of horny substances.
  • one or more compounds of general formula I are used in the liming together with thiols known from tanning, for example mercaptoethanol or thioglycolic acid. Preference is given to using less than 0.5% by weight of mercaptoethanol or thioglycolic acid.
  • the skins are treated according to the invention in an aqueous liquor.
  • the process according to the invention is carried out at pH values from 7 to 14, preferably from 8 to 13 and particularly preferably from 9 to 12.5.
  • lime also hydrated lime
  • the use of lime is dispensed with.
  • one or more inorganic alkali metal compounds are added, for example one or more hydroxides or carbonates of alkali metals, preferably sodium or potassium, and most preferably sodium.
  • suitable basic inorganic alkali metal compounds are alkali metal silicates.
  • basic amines for example ammonia, methylamine, dimethylamine, ethylamine or triethylamine, or combinations of alkali metal compound and one or more basic amines.
  • organic solvents may be in the liquor, for example up to 20% by volume of ethanol or isopropanol.
  • the process can be carried out in tannery-standard vessels, which are usually limed.
  • the process according to the invention is carried out in rotatable drums with internals.
  • the speed is usually 0.5 to 100 / min, preferably 1.5 to 10 / min and more preferably to 4.5 / min.
  • the pressure and temperature conditions for carrying out the process according to the invention are generally not critical. As suitable, the implementation has proven at atmospheric pressure; a pressure increased up to 10 bar is also conceivable. Suitable temperatures are 10 to 45 ° C, preferably 15 to 35 ° C and particularly preferably 25 to 30 ° C.
  • the compound or compounds of the general formula I it is possible to dose the compound or compounds of the general formula I at the beginning of the liming process, but initially it is also possible first to soak the skins under basic conditions and to meter one or more compounds of the general formula I after some time.
  • the dosage can be done in one step, ie the total amount of the compound or compounds I used is metered in one step; but I can also dose I in portions or continuously.
  • the process of the invention can be carried out in a period of 10 minutes to 48 hours, preferably 1 to 36 hours and more preferably 3 to 15 hours.
  • phosphines such as. B. triphenylphosphine or tris (2-carboxyethyl) phosphine hydrochloride, furthermore hydroxylamine, urea, guanidine or guanidinium hydrochloride, hydrazine, biocides, enzymes, surfactants and emulsifiers.
  • the method according to the invention can be produced preferably depilated pelts. Surprisingly, it is found that even the epidermis is completely or at least largely detached after a short treatment period.
  • the present invention therefore pats, prepared by the process according to the invention.
  • the pelts according to the invention are very well suited for the production of leather.
  • the pelts according to the invention can be further processed into leather with an improved surface yield and lower swelling damage, compared to leather, the is prepared from pelts, which were depilated with the aid of, for example, Na 2 S, NaHS, thioglycolic acid or aminoethanol.
  • Another object of the present invention are leather, made of the pelts according to the invention. They are characterized by overall advantageous performance properties.
  • wastewaters produced in the process according to the invention in particular effluents from ashes processes, in which no Na 2 S, NaSH or mercaptans such as aminoethanol or thioglycolic acid are used, can be worked up particularly well.
  • the resulting pelts are separated from the liquor, for example by simply removing the pelts or by draining the liquor.
  • the liquor contains inter alia unused (reacted) compound of general formula I, from a few ppm up to 4 wt .-%, besides basic alkali metal compound or basic amines or lime and in particular residues of horns separated from the pelts and the epidermis.
  • the separated liquor containing unused (reacted) compound of the general formula I, furthermore base and residues of the horn materials separated from the pelts and the epidermis is also referred to below as the remainder liquor.
  • Another object of the present invention are therefore residual liquors containing neither Na 2 S nor NaHS and containing as organic sulfur compounds only those of the general formula I, as well as their reaction and secondary products from the removal of horny substances from hides, furs or fur skins of dead animals, and organic sulfur compounds derived from the skins, furs or furskins of the dead animals.
  • residual liquors which contain neither Na 2 S nor NaSH are to be understood as meaning those residual liquors which contain up to 100 ppm, preferably up to 75 ppm, of sulphide.
  • the sulfide determination is carried out as hydrogen sulfide after acidification with concentrated hydrochloric acid, heating to 90 ° C and stripping.
  • the residual liquors according to the invention are obtainable by the process according to the invention. They are almost odorless and particularly easy to work up compared to the known from the prior art residual liquors of tanneries.
  • reaction and secondary products of compounds of general formula I which result from the removal of horny substances from the hides, furs and fur skins of dead animals, are mainly hydrolysis and oxidation products of compounds of general formula I call.
  • Another object of the present invention is therefore a process for the processing of residual liquors.
  • the method according to the invention comprises several steps.
  • the pelts according to the invention are separated from the lime.
  • this step is only necessary if lime has been used in the treatment of animal skins, otherwise it is not necessary.
  • the separation is carried out by settling, flotation, decantation, filtration or centrifugation, wherein for large amounts of residual liquors according to the invention, the separation of the lime by decantation, settling or filtration is preferred.
  • the first step described above makes lime-free residual liquors accessible.
  • the lime-free residual liquors are then neutralized with an acid until a pH of 2 to 8, preferably 3 to 7, particularly preferably 4 to 5 is reached.
  • hydrochloric acid, phosphoric acid, formic acid, sulfuric acid, acetic acid, citric acid, carbonic acid (CO 2 ), adipic acid and dicarboxylic acid mixtures of adipic acid, glutaric acid and succinic acid may be mentioned by way of example.
  • acidification it is possible to work without special measures with respect to evolving hydrogen sulfide.
  • the proteins removed from the nakedness in the liming or swelling precipitate or float, so that they are separated mechanically in a further step, for example by filtration or flotation.
  • the skin of a Southern German cattle was first pre-soaked at 28 ° C with 200 wt .-% water and 0.2 wt .-% of Eusapon® W 120 minutes in a barrel at 1-3 rpm. The liquor was drained and then soaked with 100 wt .-% water, 0.2 wt .-% Eusapon® W and 0.5 wt .-% soda in automatic mode (5 '/ h) 19 hours. Then the fleet was drained.
  • the soaked skins of South German cattle were fleshed green (thickness about 4 mm) and the croupons of the skins cut into pieces of skin weighing 2.5 kg each.
  • dithiothreitol 60 1.0 Aqueous sodium hydroxide solution (50% by weight) 30 1.0 Aqueous sodium hydroxide solution (50% by weight) 30 50 water 0.4 Aqueous sodium hydroxide solution (50% by weight) 60 50 water 30 1.5 1.0 Basyzyme L10 0.5 Rac. dithiothreitol 60 1.0 Aqueous sodium hydroxide solution (50% by weight) 30 1.0 Aqueous sodium hydroxide solution (50% by weight) 30 Aqueous sodium hydroxide solution (50% by weight) 60 0.4 50 water 1.6 1.0 Rac. dithiothreitol 60 1.0 Aqueous sodium hydroxide solution. (50% by weight) 30 1.0 Aqueous sodium hydroxide solution. (50% by weight) 30 50 water 0.4 Aqueous sodium hydroxide solution. (50% by weight) 60 50 water 30
  • the cask was operated for another 45 minutes at 5 revolutions / minute. Subsequently, a further 40 wt .-% of water were metered. After 10 hours at 23 to 27 ° C with periodic operation at 3 revolutions / minute for 5 minutes each hour, the experiments were terminated by draining the liquor and washing the sheets twice for 15 minutes each with 150 wt% water ,
  • the pelts treated according to the examples according to the invention were only slightly superior to the skins treated according to Comparative Example C1 with respect to the swelling, but were characterized by a smoother and flatter scar, in particular the pelts of Examples 1.4 to 1.6 according to the invention.
  • the epidermis and hair with hair roots in the pelts 1.1 to 1.3 were largely destroyed in the pelts 1.4 to 1.6.
  • the deliming or neutralization was carried out in each case with a mixture consisting of two parts by weight of formic acid and three parts by weight of adipic acid.
  • the liquor was brought to pH 7.5-8.5 in two dosing steps. Penetration of the acid mixture across the skin cross section was compared with phenolphthalein as In checked. The time required for this was noted.
  • the leathers thus obtained were washed with water and dried and stretched and folded by conventional methods.
  • The. Folding thickness of the leather was 2.0-2.2 mm.
  • the data in% by weight refers to the dried leather, unless stated otherwise.
  • the "wet white” cowhides thus obtained were placed in 100% by weight of water and adjusted to a pH of ⁇ 3.0 by addition of sodium formate and sodium bicarbonate.
  • the leather was tumbled at 30 ° C for 60 minutes and then washed with 200% by weight of water.
  • Relugan® GTP 4% by weight was added and tumbled for 60 minutes.
  • 2 wt .-% Tamol® NA commercially available from BASF Aktiengesellschaft
  • Lipoderm â licker A1 commercially available from BASF Aktiengesellschaft
  • wt .-% wt .-%
  • 1 wt .-% Lipoderm® Likker LA
  • Crust leather 2.1 was obtained. to 2.6. with very good coloring and good grain tightness at the same time very good body and excellent softness with elegant grip.
  • the crust leather 2.4 to 2.6 had a smoother and finer scars than V2. Further performance properties are shown in Table 2.
  • Table 2 crust leather Out of nakedness hair decomposition Scar Resistance Wet white leather Puncture pull-out force according to DIN 53331 [N] V2 V1 2 2 140 2.1 1.1 2 2 176 2.2 1.2 1.5 2 173 2.3 1.3 1 2 178 2.4 1.4 1 1 185 2.5 1.5 1 1 1 190 2.6 1.6 1.5 1 188
  • the hair decomposition and the scar resistance were assessed visually and haptically by 2 propands (1: very good, 6: insufficient).
  • the skin of a Southern German bovine was first pre-soaked at 28 ° C with 150 wt .-% water and 0.2 wt .-% Eusapon® W 120 minutes in a barrel at 1-3 rpm. The liquor was drained and then with 150 wt .-% water, 0.2 wt .-% Eusapon® W and 0.5 wt .-% Soda soaked with occasional stirring for 19 hours. Then the fleet would be drained.
  • the soaked skins of South German cattle were fleshed green (thickness about 4 mm) and the croupons of the skins cut into pieces of skin of 2.5 kg each.
  • the keg was operated for another 45 minutes at 15 revolutions / minute. Subsequently, an additional 40 parts by weight of water were metered. After 10 hours at 23 to 27 ° C with periodic operation at 3 revolutions / minute for 5 minutes each hour, the experiments were terminated by draining the liquor and washing the sheets twice for 15 minutes each with 150 wt% water ,
  • the pelts treated according to the examples according to the invention were only slightly superior to the skins treated according to Comparative Example C3 with regard to swelling, but were characterized by a smoother and flatter scar, in particular the pelts of Examples 3.2 and 3.3 according to the invention.
  • the epidermis and the hair with hair root in pelage 3.1 was largely destroyed in the pelts 3.2 to 3.3.
  • Crust leather 4.1 was obtained. to 4.2. with very good coloring and good grain tightness at the same time very good body and excellent softness with elegant grip.
  • the crust leathers 4.2 to 4.3 had smoother and finer scars than V4. Further performance properties are shown in Table 4. crust leather Out of nakedness hair removal grain tightness Puncture pull-out force according to DIN 53331 [N] V4 V3 2 2 140 4.1 3.1 2 2 176 4.2 3.2 1.5 1 185

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Treatment And Processing Of Natural Fur Or Leather (AREA)
  • Detergent Compositions (AREA)
EP03752667A 2002-05-22 2003-05-19 Verfahren zur entfernung von hornsubstanzen aus häuten, pelzen oder pelzfellen Expired - Lifetime EP1511865B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10223012 2002-05-22
DE10223012 2002-05-22
PCT/EP2003/005231 WO2003097880A1 (de) 2002-05-22 2003-05-19 Verfahren zur entfernung von hornsubstanzen aus häuten, pelzen oder pelzfellen

Publications (2)

Publication Number Publication Date
EP1511865A1 EP1511865A1 (de) 2005-03-09
EP1511865B1 true EP1511865B1 (de) 2009-08-05

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EP03752667A Expired - Lifetime EP1511865B1 (de) 2002-05-22 2003-05-19 Verfahren zur entfernung von hornsubstanzen aus häuten, pelzen oder pelzfellen

Country Status (13)

Country Link
US (1) US7404826B2 (es)
EP (1) EP1511865B1 (es)
JP (1) JP2005531650A (es)
KR (1) KR20050010825A (es)
CN (1) CN100381581C (es)
AR (1) AR039980A1 (es)
AT (1) ATE438742T1 (es)
AU (1) AU2003232797A1 (es)
BR (1) BR0311165A (es)
DE (1) DE50311784D1 (es)
ES (1) ES2329463T3 (es)
PT (1) PT1511865E (es)
WO (1) WO2003097880A1 (es)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AR039980A1 (es) 2002-05-22 2005-03-09 Basf Ag Procedimiento para eliminar sustancias corneas de pieles o pellejos
WO2004038046A1 (de) * 2002-10-21 2004-05-06 Basf Aktiengesellschaft Verfahren zur entfernung von hornsubstanzen aus tierhäuten
DE10353746A1 (de) * 2003-11-17 2005-06-09 Basf Ag Verfahren zum Entfernen von Hornsubstanzen aus Häuten toter Tiere
CN102559948B (zh) * 2010-12-14 2015-05-20 张壮斗 一种循环废液进行浸灰碱或复灰碱的羊皮制革工艺
KR20220092672A (ko) 2020-12-24 2022-07-04 한국신발피혁연구원 피혁 탈회 처리용 암모니아 무발생 탈회제 및 이를 이용한 피혁의 탈회 처리법

Family Cites Families (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1973130A (en) * 1933-07-21 1934-09-11 Rohm & Haas Process of unhairing hides or skins
AT187223B (de) 1954-06-24 1956-10-25 Chemie Linz Ag Verfahren zum Vorbereiten von tierischen Häuten für die Gerbung
US3097912A (en) * 1959-03-30 1963-07-16 Booth Henry Hair and wool depilation method and composition
DE2131630A1 (de) * 1970-06-29 1972-01-05 Avon Prod Inc Mittel zur Entfernung von Hornsubstanzen,insbesondere Haaren
US3865546A (en) * 1970-10-22 1975-02-11 Collaborative Res Inc Depilatory composition and method of use
YU36755B (en) * 1971-11-17 1984-08-31 Basf Ag Process for the elimination of hairs from hides and furs
DE2917376A1 (de) * 1979-04-28 1980-11-13 Roehm Gmbh Enzymatisches verfahren zur haargewinnung und zum gleichzeitigen hautaufschluss
US4618344A (en) * 1982-06-01 1986-10-21 The Procter & Gamble Company Depilatory compositions
EP0095916A3 (en) 1982-06-01 1984-08-08 THE PROCTER & GAMBLE COMPANY Depilatory compositions
EP0096521A3 (en) 1982-06-01 1985-01-23 THE PROCTER & GAMBLE COMPANY Depilatory compositions
DE3224881A1 (de) * 1982-07-03 1984-03-01 Röhm GmbH, 6100 Darmstadt Verfahren zur herstellung von enthaartem, lagerfaehigem hautmaterial
US4472569A (en) * 1983-06-13 1984-09-18 Phillips Petroleum Company Mercaptohydroxy alkanes
DE19933968A1 (de) * 1999-07-20 2001-01-25 Trumpler Gmbh & Co Chem Fab Hilfsmittel für den Hautaufschluß und die Haarlockerung von Tierhäuten
AR039980A1 (es) 2002-05-22 2005-03-09 Basf Ag Procedimiento para eliminar sustancias corneas de pieles o pellejos
DE10249077A1 (de) 2002-10-21 2004-04-29 Basf Ag Verfahren zur Herstellung von Leder
WO2004038046A1 (de) 2002-10-21 2004-05-06 Basf Aktiengesellschaft Verfahren zur entfernung von hornsubstanzen aus tierhäuten
DE10309221A1 (de) 2003-02-28 2004-09-09 Basf Ag Egalisierhilfsmittel für das Färben von Fasern

Also Published As

Publication number Publication date
ATE438742T1 (de) 2009-08-15
BR0311165A (pt) 2005-03-15
AU2003232797A1 (en) 2003-12-02
WO2003097880A1 (de) 2003-11-27
US20050229326A1 (en) 2005-10-20
AR039980A1 (es) 2005-03-09
KR20050010825A (ko) 2005-01-28
EP1511865A1 (de) 2005-03-09
DE50311784D1 (de) 2009-09-17
US7404826B2 (en) 2008-07-29
CN1653195A (zh) 2005-08-10
CN100381581C (zh) 2008-04-16
ES2329463T3 (es) 2009-11-26
PT1511865E (pt) 2009-08-21
JP2005531650A (ja) 2005-10-20

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