CN105624339B - A kind of method for shortening process hides soaking time - Google Patents

A kind of method for shortening process hides soaking time Download PDF

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Publication number
CN105624339B
CN105624339B CN201510991013.4A CN201510991013A CN105624339B CN 105624339 B CN105624339 B CN 105624339B CN 201510991013 A CN201510991013 A CN 201510991013A CN 105624339 B CN105624339 B CN 105624339B
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China
Prior art keywords
cgmcc
lipase
protease
soaking
water
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CN201510991013.4A
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Chinese (zh)
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CN105624339A (en
Inventor
路福平
李玉
曹珊
程宝箴
薛斌
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Tianjin University of Science and Technology
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Tianjin University of Science and Technology
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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
    • C14C1/04—Soaking
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/44—Resins; rubber; leather
    • G01N33/447—Leather

Abstract

The present invention relates to a kind of methods for shortening process hides soaking time, are using Na+With Ca2+When carrying out leather soaking, addition protease and lipase are as auxiliary agent, to Na in soaking process+With Ca2+Concentration be adjusted, the protease produces protease by bacillus amyloliquefaciens CGMCC No.11218 and Alkaliphilic bacillus superior strain CGMCC No.6537.The processing time of traditional soaking process is shortened, and reduces the vulcanized sodium usage amount in follow-up epilation process.

Description

A kind of method for shortening process hides soaking time
Technical field
The invention belongs to leather industry production fields, and in particular to bacillus amyloliquefaciens CGMCC No.11218 bacterial strains institute Producing enzyme powder and application of the 41649 yielding lipase powder of aspergillus oryzae TCCC in Soaking Process in Leather Manufacture, so as to so that soaking time Shorten, and reduce the vulcanized sodium usage amount in follow-up depilation operation.
Background technology
In leather production process, the first step process carried out required for rawhide obtained by purchase is that immersion makes it fully It eases back.The nonfibrous protein of soil, foul, preservative and solubility can be removed during immersion.But rawhide storage Time is longer, and the amount that soluble protein removes during immersion is fewer.Simple immersion method is the raw material skin that is directly soaked in water, But it needs to spend longer soaking time, and for dry plate skin, water is not easy to permeate.It can soaked in traditional leather industry Some chemical assistants such as alkali, surfactant, neutral salt etc. are added during water.But to strengthen washing after immersion to prevent pair Postorder liming expansion affects.In recent years during immersion, using enzyme as Soaking also increasingly by Everybody is approved, enzyme is most one of material of application potential, and most possible to change chemicals in leather processing procedure dirty Serious present situation is contaminated, can promote to realize that the green in leather making process cleans.Enzyme, which is applied to immersion process, to be effectively removed Intracutaneous non-collagen tissue, caking property reduces to promote the infiltration of water between making hide fiber.With can remove scurf, shorten immersion Time reduces the advantages that uniformity of the grain wrinkle with increasing immersion, and preferable condition is provided for the processing of subsequent handling.
The content of the invention
After a kind of processing time shortening in place of overcome the deficiencies in the prior art, is provided, is reduced The method of the shortening process hides soaking time of vulcanized sodium usage amount in continuous epilation process.
The present invention realizes that the technical solution of purpose is as follows：
A kind of method for shortening process hides soaking time, is using Na+With Ca2+Carry out leather soaking when, addition protease with Lipase is as auxiliary agent, to Na in soaking process+With Ca2+Concentration be adjusted, processing time of traditional soaking process is contracted It is short, and reduce the vulcanized sodium usage amount in follow-up epilation process.
Moreover, the protease is bacillus amyloliquefaciens CGMCC No.11218 and Alkaliphilic bacillus superior strain CGMCC No.6537 produce protease.
Moreover, the bacillus amyloliquefaciens CGMCC No.11218 bacterial strains are laid eggs, white enzyme powder dosage is 0.05- 0.2%, Alkaliphilic bacillus superior strain CGMCC No.6537 lay eggs white enzyme powder dosage as 0.05-0.1%.
Moreover, the lipase is Aspergillus carneus CGMCC No.3.3919 institutes yielding lipase powder.
Moreover, the Aspergillus carneus CGMCC No.3.3919 institutes yielding lipase powder dosage is 0.05-0.8%.
Moreover, bacillus amyloliquefaciens CGMCC No.11218 bacterial strains produce prolease activity as 5000U/g-10000 U/ g；Alkaliphilic bacillus superior strain CGMCC No.6537 produce prolease activity as 3000-10000U/g；Aspergillus carneus CGMCC No.3.3919 institutes yielding lipase vigor is 3000-8000U/g.
Moreover, the technological parameter of immersion：Water：Temperature：25℃；CGMCC No.11218 protease：0.5%；CGMCC No.6537 protease：0.1%；CGMCC No.3.3919 lipase：0.4%；NaCl:0.1%；CaCl2:0.5%.
Moreover, the processing step of immersion is：Water is added in from drum door, lipase, ox-hide, NaCl, rotation 60min stop 20min then four times in 4h, rotates 40min and stops 20min, adds in and turns 20min twice in 2h after two kinds of protease and stop 40min, Cold water is washed three times, each 15min, drain, and surface water-filling is completed.
Beneficial effects of the present invention are as follows：
The present invention is by the use of protease and lipase as auxiliary agent, to Na in soaking process+With Ca2+Concentration be adjusted, The processing time of traditional soaking process is shortened, and reduces the vulcanized sodium usage amount in follow-up epilation process.
The protease that the present invention uses is bacillus amyloliquefaciens CGMCC No.11218 and Alkaliphilic bacillus Producing Strain Strain CGMCC No.6537 produce protease, which has preferable pH stability, can meet leaching in pH5-11 Enzyme activity needed for water, and with certain resistance to heavy metal；Lipase main component is Aspergillus carneus CGMCC No.3.3919 institutes yielding lipase, the protease have preferable temperature stability, there is preferable enzyme activity in 15 DEG C -60 DEG C Power.
Description of the drawings
Fig. 1：CGMCC No.11218 enzyme powders are used for the effect of leather soaking in time-varying process；
Fig. 2：CGMCC No.11218 enzyme powders influence leather soaking be subject to NaCl effects；
Fig. 3：Lipase is used for the effect of leather soaking in time-varying process；
Fig. 4：Lipase influences leather soaking be subject to NaCl effects.
Specific embodiment
The present invention is described below by specific embodiment.Unless stated otherwise, technological means used in the present invention It is method known in those skilled in the art.In addition, embodiment is interpreted as illustrative, it is not intended to limit the present invention Scope, the spirit and scope of the invention are limited only by the claims that follow.To those skilled in the art, without departing substantially from this The various changes carried out to the material component in these embodiments and dosage on the premise of invention spirit and scope or change It belongs to the scope of protection of the present invention.
The bacterium producing multi enzyme preparation of the protease used in the present invention is bacillus amyloliquefaciens (Bacillus Amyloliquefaciens), deposit number is CGMCC No.11218 and Alkaliphilic bacillus (Bacillus Alcalophilus), bacterial strain deposit number is CGMCC No.6537；The bacterium producing multi enzyme preparation of lipase in the present invention is yellowish pink bent Mould (Aspergillus carneus), deposit number are CGMCC No.3.3919.
Prolease activity in the present invention is measured by GBT 23527-2009 methods, the lipase activity in the present invention Power is measured by GBT 23535-2009 methods.
Leather water imbibition in the present invention measures by the following method：
(1) it is sampled by QB/T 2706, carries out air adjustment by QB/T2707, the quality of sample is measured, essence Really to 0.0001g.
(2) by Ku Baier ware balls end under, the deionized water at 20 DEG C ± 2 DEG C is added in, makes liquid level jewel in scale 0mL records the scale number of degrees between 1mL.Sample is put into Ku Baier ware post ends, inclination makes distilled water be flowed into from spheric end Post ends make sample all submerge, using fresh-keeping membrane closure post ends to prevent moisture evaporation.
(3) post ends are lifted in defined time point, move the water to flow into spheric end, after all having flowed 1min, read the quarter of water Degree calculates the uptake of water.The uptake of water absorbs the milliliter number of water for unit quality leather sample, is represented with %.
Chloride ion content in the present invention measures by the following method：
(1) 17g silver nitrates constant volume in 1L volumetric flasks is weighed.It weighs 10g potassium chromates to be dissolved in 100mL water, stirs lower be added dropwise Then silver nitrate solution is filtered to there is red-brown precipitation.
(2) by sodium chloride, calcination 3h to constant weight, claims standard to 0.0001g in Muffle furnace, the constant volume in 1000mL volumetric flasks, Calculate its concentration.Then the silver nitrate solution in (1) is demarcated using chlorination sodium standard solution, obtains silver nitrate standardized titration Solution.
(3) the sample solution of certain volume (below chloride ion-containing 85mg) is taken in 150mL conical flasks, adds in 4 drop potassium chromates Indicator is titrated using silver nitrate standard titration solution, until there is stable Chinese red as terminal in suspension, is done simultaneously Blank test.The absolute difference of parallel result is not more than 1%.
Embodiment 1
Observe influence of the CGMCC No.11218 enzyme powders to leather soaking
As shown in table 1, the CGMCC No.11218 enzyme powders of corresponding mass is taken to be placed in Ku Baier wares, add in deionization Water makes liquid level be maintained at scale 0mL, then inserts skin sample into different Ku Baier wares, and lifting Ku Baier ware spheric ends makes liquid Total reflux is made skin sample be completely immersed in liquid, then post ends is sealed using preservative film, so as to prevent to post ends Moisture evaporation.Then in 15min, 30min, 60min, 120min and for 24 hours when, lifting post ends makes liquid fully flow into spherical shape End, 1min reads scale and calculates water absorption rate after all having flowed, and the results are shown in Figure 1.It can be seen that CGMCC No.11218 Enzyme powder significantly improves water absorption rate of the rawhide during immersion.
Table 1：CGMCC No.11218 enzyme powder dosages during leather soaking
Embodiment 2
NaCl is acted on and GMCC No.11218 enzyme powders are on the relation between leather soaking influence
The chlorination sodium standard solution configured with the sodium chloride of calcination to constant weight demarcates silver nitrate solution, according to meter The concentration of silver nitrate standard solution can be obtained by calculating draws the immersion liquid reacted in 1ml embodiments 2 for 24 hours for 0.1012mol/L., will It is placed in 150ml conical flasks, is then added in 40 μ L potassium chromates indicator and 10mL deionized waters, is used silver nitrate standard solution It is titrated to and apparent and stable salmon pink occurs as terminal, each sample carries out two groups of parallel tests.Chloride ion content Calculating visible 2..It is mg/L that chloride ion content, which calculates gained unit,.The visible Fig. 2 of its result.It can be seen that sodium chloride is to enzyme Act on leather soaking has obvious influence in the process, and the sodium chloride of high concentration acts on GMCC No.11218 enzyme powders There is certain negative effect in leather soaking process.
——②
V1--- the dosage (mL) of silver nitrate standard titration solution
V0--- the dosage (mL) of blank test silver nitrate standard solution
C(AgNO3) --- the dosage (mol/L) of silver nitrate standard titration solution
35.453 --- the molal weight (g/mol) of chlorion
V --- solution sampling volume (mL) to be measured
Embodiment 3
Observe influence of the lipase to leather soaking
As shown in table 2, the fatty enzyme powder of corresponding mass is taken to be placed in Ku Baier wares, deionized water is added in, protects liquid level It holds in scale 0mL, then inserts skin sample into different Ku Baier wares, lifting Ku Baier ware spheric ends makes liquid total reflux to column Shape end makes skin sample be completely immersed in liquid, and then post ends are sealed using preservative film, so as to prevent moisture evaporation.So After 15min, 30min, 60min, 120min and for 24 hours when, lifting post ends makes liquid fully flow into spheric end, after all having flowed 1min reads scale and calculates water absorption rate, and the results are shown in Figure 3.It can be seen that fatty enzyme powder can significantly improve rawhide and exist Water absorption rate during immersion, also, the lipase of low concentration is still significantly improved for the water absorption rate of leather.
Table 2：Leather soaking process fat enzyme dosage
Embodiment 4
NaCl effects and lipase are observed on the relation between leather soaking influence
The immersion liquid that fatty enzyme for 24 hours has been reacted in 1ml embodiments 3 is drawn, is placed it in 150ml conical flasks, so After add in 40 μ L potassium chromates indicator and 10mL deionized waters, it is titrated to using silver nitrate standard solution occur it is apparent and steady Fixed salmon pink, each sample carry out two groups of parallel tests.2. chloride ion content is calculated according to formula.The visible Fig. 4 of its result.
Embodiment 5
Use NaCl and CaCl2Adjust Na+、Ca2+The enzyme immersion technique of concentration
Technological parameter：Water：200%；Temperature：25℃；CGMCC No.11218 protease：0.5%；CGMCC No.6537 Protease：0.1%；CGMCC No.3.3919 lipase：0.4%；NaCl:0.1%；CaCl2:0.5%, NaOH.
From drum door add in water, lipase, ox-hide, NaCl, rotate 60min, stop 20min, then in 4h rotate 40min stop 20min (four times) is added in and is turned 20min in 2h after two kinds of protease and stop 40min (twice).Cold water is washed three times, each 15min, row Liquid, surface water-filling are completed.

Claims (2)

  1. A kind of 1. method for shortening process hides soaking time, it is characterised in that：When Na+ and Ca2+ is used to carry out leather soaking, add Protease is added, as auxiliary agent, the concentration of Na+ in soaking process and Ca2+ to be adjusted, by traditional soaking process with lipase Processing time shortens, and reduces the vulcanized sodium usage amount in follow-up epilation process；The protease is solution starch gemma bar Bacterium CGMCC No.11218 and Alkaliphilic bacillus superior strain CGMCC No.6537 produce protease；The solution starch gemma Bacillus CGMCC No.11218 bacterial strains lay eggs white enzyme powder dosage as 0.05-0.2%, Alkaliphilic bacillus superior strain CGMCC No.6537 lays eggs white enzyme powder dosage as 0.05-0.1%；The lipase produces fat by Aspergillus carneus CGMCC No.3.3919 Fat enzyme powder；The Aspergillus carneus CGMCC No.3.3919 institutes yielding lipase powder dosage is 0.05-0.8%；Bacillus amyloliquefaciens CGMCC No.11218 bacterial strains produce prolease activity as 5000U/g-10000U/g；Alkaliphilic bacillus superior strain CGMCC No.6537 produces prolease activity as 3000-10000U/g；Aspergillus carneus CGMCC No.3.3919 institutes yielding lipase vigor is 3000-8000U/g；
    The technological parameter of immersion：Water：Temperature：25℃；CGMCC No.11218 protease：0.5%；CGMCC No.6537 albumen Enzyme：0.1%；CGMCC No.3.3919 lipase：0.4%；NaCl:0.1%；CaCl2:0.5%.
  2. 2. shorten the method for process hides soaking time according to claim 1, it is characterised in that：The processing step of immersion is：From Drum door adds in water, and lipase, ox-hide, NaCl rotates 60min, stops 20min, then four times in 4h, rotates 40min and stops 20min is added in and is turned 20min twice in 2h after two kinds of protease and stop 40min, and cold water is washed three times, each 15min, drain, and surface fills Water is completed.
CN201510991013.4A 2015-12-23 2015-12-23 A kind of method for shortening process hides soaking time Expired - Fee Related CN105624339B (en)

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Families Citing this family (3)

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Publication number Priority date Publication date Assignee Title
CN106350619B (en) * 2016-09-29 2019-04-09 天津科技大学 The method of few chromium combination tanning after a kind of immersion of complex enzyme formulation
CN107699553B (en) * 2017-11-03 2021-04-09 天津科技大学 Alkaline keratinase KerT from bacillus amyloliquefaciens and unhairing application thereof
CN109295263A (en) * 2018-10-10 2019-02-01 赞宇科技集团股份有限公司 A kind of process hides soaking enzyme preparation, application and process hides immersion technique

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Publication number Priority date Publication date Assignee Title
CN101235421A (en) * 2008-02-02 2008-08-06 四川大学 Animal fur clean depilation and fur fiber loosing method for preparing leather and application thereof
CN101525609A (en) * 2009-03-23 2009-09-09 陕西科技大学 Composite soaking enzyme preparation
CN101760569A (en) * 2008-12-25 2010-06-30 峰安皮业股份有限公司 Leather making bio-pretreatment method
CN103243182A (en) * 2013-04-26 2013-08-14 四川大学 Tanning method free of lime, sulfide, chloride ion and heavy metal chromium pollution
CN105039606A (en) * 2015-08-28 2015-11-11 焦作隆丰皮草企业有限公司 Quick soaking method of shorn sheepskin

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Publication number Priority date Publication date Assignee Title
WO2010043709A1 (en) * 2008-10-17 2010-04-22 Novozymes A/S Enzymatic treatment for the leather process

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101235421A (en) * 2008-02-02 2008-08-06 四川大学 Animal fur clean depilation and fur fiber loosing method for preparing leather and application thereof
CN101760569A (en) * 2008-12-25 2010-06-30 峰安皮业股份有限公司 Leather making bio-pretreatment method
CN101525609A (en) * 2009-03-23 2009-09-09 陕西科技大学 Composite soaking enzyme preparation
CN103243182A (en) * 2013-04-26 2013-08-14 四川大学 Tanning method free of lime, sulfide, chloride ion and heavy metal chromium pollution
CN105039606A (en) * 2015-08-28 2015-11-11 焦作隆丰皮草企业有限公司 Quick soaking method of shorn sheepskin

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