CN106929611A - A kind of ox-hide processing method - Google Patents
A kind of ox-hide processing method Download PDFInfo
- Publication number
- CN106929611A CN106929611A CN201710287247.XA CN201710287247A CN106929611A CN 106929611 A CN106929611 A CN 106929611A CN 201710287247 A CN201710287247 A CN 201710287247A CN 106929611 A CN106929611 A CN 106929611A
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- Prior art keywords
- hide
- reference mass
- processing method
- polyurethane
- treatment
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- Granted
Links
- 238000003672 processing method Methods 0.000 title claims abstract description 25
- 229920002635 polyurethane Polymers 0.000 claims abstract description 70
- 239000004814 polyurethane Substances 0.000 claims abstract description 70
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 69
- 238000010409 ironing Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 230000010358 mechanical oscillation Effects 0.000 claims abstract description 8
- 230000004048 modification Effects 0.000 claims abstract description 8
- 238000012986 modification Methods 0.000 claims abstract description 8
- 239000000049 pigment Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000004519 grease Substances 0.000 claims abstract description 5
- 229920001864 tannin Polymers 0.000 claims description 20
- 235000018553 tannin Nutrition 0.000 claims description 20
- 239000001648 tannin Substances 0.000 claims description 20
- 229920001730 Moisture cure polyurethane Polymers 0.000 claims description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 229920005989 resin Polymers 0.000 claims description 11
- 239000011347 resin Substances 0.000 claims description 11
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 10
- 125000005442 diisocyanate group Chemical group 0.000 claims description 10
- 229920005862 polyol Polymers 0.000 claims description 9
- 150000003077 polyols Chemical class 0.000 claims description 9
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 9
- 239000012948 isocyanate Substances 0.000 claims description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 7
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 6
- 229920000642 polymer Polymers 0.000 claims description 6
- 229940079827 sodium hydrogen sulfite Drugs 0.000 claims description 6
- 239000004925 Acrylic resin Substances 0.000 claims description 5
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical group CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 5
- 238000006386 neutralization reaction Methods 0.000 claims description 5
- 150000001298 alcohols Chemical class 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 239000002023 wood Substances 0.000 claims description 4
- 125000002768 hydroxyalkyl group Chemical group 0.000 claims description 3
- 229920002545 silicone oil Polymers 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 239000003153 chemical reaction reagent Substances 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 claims 1
- 239000004721 Polyphenylene oxide Substances 0.000 claims 1
- 229920000570 polyether Polymers 0.000 claims 1
- 238000005507 spraying Methods 0.000 claims 1
- 239000010985 leather Substances 0.000 abstract description 21
- 108010035532 Collagen Proteins 0.000 abstract description 18
- 102000008186 Collagen Human genes 0.000 abstract description 18
- 229920001436 collagen Polymers 0.000 abstract description 18
- 239000004744 fabric Substances 0.000 abstract description 15
- 239000007921 spray Substances 0.000 abstract description 8
- 238000010276 construction Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 11
- 238000011084 recovery Methods 0.000 description 11
- 239000000243 solution Substances 0.000 description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 7
- 238000004132 cross linking Methods 0.000 description 7
- 238000010586 diagram Methods 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 239000000376 reactant Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- 150000002513 isocyanates Chemical class 0.000 description 5
- 229920001451 polypropylene glycol Polymers 0.000 description 5
- 150000005846 sugar alcohols Polymers 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 238000001764 infiltration Methods 0.000 description 3
- 230000008595 infiltration Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 108010077465 Tropocollagen Proteins 0.000 description 2
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- AYOHIQLKSOJJQH-UHFFFAOYSA-N dibutyltin Chemical compound CCCC[Sn]CCCC AYOHIQLKSOJJQH-UHFFFAOYSA-N 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 239000002759 woven fabric Substances 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- 101000598921 Homo sapiens Orexin Proteins 0.000 description 1
- 101001123245 Homo sapiens Protoporphyrinogen oxidase Proteins 0.000 description 1
- 102100029028 Protoporphyrinogen oxidase Human genes 0.000 description 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 206010061592 cardiac fibrillation Diseases 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012975 dibutyltin dilaurate Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002600 fibrillogenic effect Effects 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 244000309465 heifer Species 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000002655 kraft paper Substances 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 239000012974 tin catalyst Substances 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
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
- C14C3/00—Tanning; Compositions for tanning
- C14C3/02—Chemical tanning
- C14C3/08—Chemical tanning by organic agents
- C14C3/22—Chemical tanning by organic agents using polymerisation products
-
- C—CHEMISTRY; METALLURGY
- C14—SKINS; HIDES; PELTS; LEATHER
- C14B—MECHANICAL TREATMENT OR PROCESSING OF SKINS, HIDES OR LEATHER IN GENERAL; PELT-SHEARING MACHINES; INTESTINE-SPLITTING MACHINES
- C14B1/00—Manufacture of leather; Machines or devices therefor
- C14B1/02—Fleshing, unhairing, samming, stretching-out, setting-out, shaving, splitting, or skiving skins, hides, or leather
- C14B1/04—Fleshing, unhairing, samming, stretching-out, setting-out, shaving, splitting, or skiving skins, hides, or leather using slicking, scraping, or smoothing-out cylinders or blades fixed on supports, e.g. cylinders, in a plane substantially at right angles to the working surface
-
- 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
- C14C11/00—Surface finishing of leather
-
- 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
- C14C3/08—Chemical tanning by organic agents
- C14C3/14—Fat tanning; Oil tanning
-
- C—CHEMISTRY; METALLURGY
- C14—SKINS; HIDES; PELTS; LEATHER
- C14B—MECHANICAL TREATMENT OR PROCESSING OF SKINS, HIDES OR LEATHER IN GENERAL; PELT-SHEARING MACHINES; INTESTINE-SPLITTING MACHINES
- C14B2700/00—Mechanical treatment or processing of skins, hides or leather in general; Pelt-shearing machines; Making driving belts; Machines for splitting intestines
- C14B2700/14—Processes or apparatus for setting-out, smoothing, ironing or polishing leather or hides
-
- C—CHEMISTRY; METALLURGY
- C14—SKINS; HIDES; PELTS; LEATHER
- C14B—MECHANICAL TREATMENT OR PROCESSING OF SKINS, HIDES OR LEATHER IN GENERAL; PELT-SHEARING MACHINES; INTESTINE-SPLITTING MACHINES
- C14B2700/00—Mechanical treatment or processing of skins, hides or leather in general; Pelt-shearing machines; Making driving belts; Machines for splitting intestines
- C14B2700/27—Rotating drums for treating leather
Abstract
The invention discloses a kind of ox-hide processing method, comprise the following steps：When tanning is arranged, it is put into rotary drum as raw material using ox-hide wet blue, the quality on the basis of the quality of ox-hide wet blue, first adds the water of 100%~200% Reference mass, adds the polyurethane finishing agent treatment of 6%~16% Reference mass；The pigment of 1% Reference mass is added, is processed 1~2 hour；Draining, adds the grease of 8%~15% Reference mass, is processed 1~1.5 hour at 50 DEG C；Ox-hide after taking-up treatment, using vacuum ironing machine, presses the ox-hide 3~4 minutes at 40 DEG C, then takes out ox-hide, hang airing；Moisture is sprayed at the ox-hide inner surface after drying again, the moisture of ox-hide is reached 10%~15%；Buff is drawn using mechanical oscillation, modification ox-hide surface by ox-hide surface rubbing, then carries out/color spray treatment of tinting, after flatiron, obtains the ox-hide of this method treatment.The ox-hide processing method that the present invention is provided can make to form elastic construction in the collagen fabric of the ox-hide after treatment, improve leather elasticity.
Description
Technical field
The present invention relates to a kind of leather finishing agent preparation method, especially a kind of ox-hide processing method.
Background technology
In leather manufacture, especially handbag product manufacturing industry, the elastic recovery of ox-hide is particularly significant, the property
The outward appearance of product can not only be influenceed more influences the function of product.
In existing leather processing, using organic silicone finishing agent or wax, grease-filled leather, it is set to soften, and
Improve its elastic recovery.But the elastic recovery of the leather that these processing methods are obtained can not be lasting.As shown in figure 1, ox
Skin is by after the filling of existing leather processing, being full of filler 12 between the collagen fabric 11 of ox-hide；However, making
During, ox-hide is caused the filler 12 between collagen fabric 11 to be extruded by different degrees of by external force F extruding, while
New chemical bond 13 is formed between collagen fabric 11, causes ox-hide thinning and elastic recovery reduction.Therefore, how
The elasticity and elastic stability for improving ox-hide turn into study hotspot.
Polyurethane correlation finishing agent early has record, for example, a kind of Publication No. CN102070759A " aqueous polyurethane skins
The preparation method of leather retanning agent ", Publication No. CN103030769A " a kind of polyurethane retanning agent ", notification number
CN104073575B " fur tanning agent and preparation method thereof based on isocyanates " disclose polyurethane finishing agent have it is good
Filling effect, however, fillibility polyurethane does not crosslink reaction with ox-hide, after long-time use, ox-hide impaired performance.In addition
In preparation process, it is related to the use of toxic organic solvent, such as tetrahydrofuran, benzene, toluene, is unfavorable for industrialized production.
In the U.S. Patent application of United States Patent (USP) US2923594, US2523326 and Publication No. 20060080784A1
Disclose isocyanates and its related polymer is used as the relevant information of tanning finishing agent.The wherein molecular mass of isocyanates
It is relatively low, and effectively can be crosslinked with collagen molecules, so as to improve the shrinkage temperature of leather, but leather cannot be improved
Elasticity.
The content of the invention
In order to overcome the defect of prior art, the present invention to propose a kind of ox-hide processing method that can improve leather elasticity.
It is a kind of ox-hide processing method provided up to this purpose, the present invention, comprises the following steps：
A1：When tanning is arranged, it is put into rotary drum as raw material using ox-hide wet blue, the quality with ox-hide wet blue is
Reference mass, first adds the water of 100%~200% Reference mass, adds the polyurethane finishing agent of 6%~16% Reference mass
Treatment；
A2：The pigment of 1% Reference mass is added, is processed 1~2 hour；
A3：Draining, adds the grease of 8%~15% Reference mass, is processed 1~1.5 hour at 50 DEG C；
A4：Ox-hide after taking-up treatment, using vacuum ironing machine, presses the ox-hide 3~4 minutes at 40 DEG C, with
After take out ox-hide, by ox-hide hang airing；
A5：Moisture is sprayed at the ox-hide inner surface after drying again, the moisture for making the ox-hide reaches 10%~
15%；
A6：The soft ox-hide is drawn using mechanical oscillation, modification ox-hide surface, by ox-hide surface rubbing, applies to ox-hide
Color/color spray treatment, after flatiron, obtains the ox-hide of this method treatment.
Preferably, in the step A1, the polyurethane finishing agent is added in three times, every minor tick 15 minutes.
Preferably, in the step A1, before being additionally included in the addition polyurethane finishing agent, 8% benchmark matter is added
The step of acrylate resin tanning agent of amount.
Preferably, in the step A1,3%~9% benchmark is additionally added while the polyurethane finishing agent is added
The resin retaning agent of quality.
Preferably, in the step A1, also including adding the resin tannin of 2% Reference mass, 5.5% Reference mass
Synthesize composite filled tannin, the neutralization tannin of 5.5% Reference mass, the polymer tannin and 4% Reference mass of 2% Reference mass
Grain wood.
Preferably, the polyurethane finishing agent includes：Alcohols solvent and polyurethane solute, wherein the polyurethane is by low
Polyurethane prepolymer that polymers polyalcohol is formed with diisocyanate and sodium hydrogensulfite end-capping reagent for raw material is prepared from, institute
The mol ratio for stating oligomer polyol, diisocyanate and sodium hydrogensulfite is 1：2~3：2~3.
Preferably, the molecular weight of the oligomer polyol is 1000~8000, and degree of functionality is 2~3.
Preferably, the oligomer polyol is selected from one or more of PPG or hydroxyalkyl silicone oil.
Preferably, described diisocyanate is selected from IPDI, the isocyanide of 4,4- dicyclohexyl methyl hydrides two
Acid esters, cyclohexanedimethyl diisocyanate or toluene di-isocyanate(TDI).
Preferably, described alcohols solvent is ethanol or isopropanol.
Beneficial effects of the present invention are：The polyurethane finishing agent used in ox-hide processing method in the present invention has many officials
The flexible strand that can be rolled into a ball, can occur many sites and be crosslinked with the collagenous fibres in leather.The polyurethane finishing agent have two to
Three active function groups, can be bonded from different collagenous fibres simultaneously, similar to " bridge " is costed between tropocollagen molecule, rise
To effective crosslinked action；Meanwhile, will not be excessive because of crosslinking points, it is unfavorable on the contrary so as to cause collagenous fibres is too bonded
In the enhancing of leather elasticity.In addition, isocyanates hard section assigns strand in polyurethane molecular chain in the polyurethane finishing agent
Rigidity, polyalcohol soft section assigns Chain Flexibility, and it is the polyalcohol of macromolecular that soft section is chosen in the polyurethane, makes polyurethane integral
Reason agent has compared with high-flexibility.After the polyurethane finishing agent prepared using the present invention is applied to leather arrangement, when leather is subject to curved
During folding external force, the polyurethane molecular chain between collagen plays a part of support, and after external force is removed, polyurethane molecular chain can be sent out
The effect of " spring " is waved, its resilience is helped, the elasticity of leather is improved.
Brief description of the drawings
The schematic diagram that Fig. 1 is deformed in use for the collagen fabric structure of prior art heifer；
Fig. 2 is the chemical reaction schematic diagram of step S12 in embodiment 1；
Fig. 3 is the chemical reaction schematic diagram of step S14 in embodiment 1；
Fig. 4 is the cross-linking reaction schematic diagram of step A11 in embodiment 1；
The schematic diagram of the ox-hide wet blue that Fig. 5 is used for step A11 in embodiment 1；
Fig. 6 is to use the collagen fabric structure change signal before and after the disposal methods ox-hide that provides of the present invention
Figure；
The schematic diagram that Fig. 7 is deformed in use for the collagen fabric structure of the ox-hide after being processed in Fig. 6.
Specific embodiment
Technical scheme is further illustrated below by specific embodiment.
Embodiment one
A kind of polyurethane finishing agent S1 and preparation method thereof and use the polyurethane finishing agent that the present embodiment is provided
Ox-hide processing method.
The preparation method of the polyurethane finishing agent S1 is comprised the following steps：
S11：By 0.1mol degrees of functionality Fn=3, the PPOX triol (abbreviation of number-average molecular weight Mn=1000g/mol
Be PPG) and 0.3mol IPDI (english abbreviation is IPDI) composition reactant and 20ppm two bays
Sour dibutyl tin (english abbreviation DBTDL) catalyst is added in a there-necked flask of 1000ml；
S12：Under conditions of 85 DEG C of oil baths, mechanical agitation is carried out to the reactant in the there-necked flask, reacted 2 hours
Afterwards, the polyurethane prepolymer for being formed will be reacted and is down to room temperature, its chemical reaction schematic diagram is as shown in Fig. 2 the polyurethane prepolymer
PPG and IPDI interconnections in thing, form the chain-like molecular structure of PPG-IPDI-PPG-IPDI ...；
S13：The polyurethane prepolymer is diluted to the solution that solidification amount is 50% using ethanol；
S14：Use quality percentage is 30% sodium hydrogensulfite (NaHSO3) aqueous solution in the solution add
0.3mol sodium hydrogensulfites carry out end capping reaction to the polyurethane prepolymer, react 1 hour at room temperature, and its chemical reaction shows
It is intended to as shown in Figure 3；
S15：Use quality percentage is 20% dilute sulfuric acid (H2SO4) adjust to 5 the pH value of the solution, that is, formed
Solid content is about 45% polyurethane finishing agent S1.
Comprised the following steps using the ox-hide processing method of polyurethane finishing agent S1：
A11：Referring to Fig. 5, when tanning is arranged, it is put into rotary drum as raw material using ox-hide wet blue 50, it is blue with ox-hide
Quality on the basis of the quality of wet skin 50, first adds the water of 100% Reference mass, then adds 6%, 5% and 5% benchmark matter in three times
Weight polyurethane finishing agent S1, every minor tick 15 minutes, as shown in figure 4, after the polyurethane finishing agent S1 is soluble in water, polyurethane
Sodium hydrogensulfite end-blocking depart from, expose the NH of the collagen fabric in the NCO group 21 of end and the ox-hide2Group 31
It is bonded, crosslinking points 35 is formed, by the elastic connection of strand 30 of the polyurethane between each crosslinking points 35, wherein poly- ammonia
The NCO group 21 of ester end and the NH of the collagen fabric2The reaction equation of the crosslinking of group 31 is as follows：
-NCO+-NH2→-NH-CO-NH-；
A12：The pigment of 1% Reference mass is added, is processed 1 hour；
A13：Draining, adds the Synthetic Oil of 8% Reference mass, is processed 1 hour at 50 DEG C；
A14：Ox-hide after taking-up treatment, using vacuum ironing machine, presses the ox-hide 3~4 minutes at 40 DEG C, with
After take out ox-hide, by ox-hide hang airing 2~3 days；
A15：Moisture is sprayed at the ox-hide inner surface after drying again, the moisture for making the ox-hide reaches 10%~
15%；
A16：The soft ox-hide is drawn using mechanical oscillation, modification ox-hide surface, by ox-hide surface rubbing, applies to ox-hide
Color/color spray treatment, the ox-hide is pressed by rotary ironing machine, and ironing temperature is 100~150 DEG C, and this implementation is obtained after flatiron
The ox-hide A1 of example ox-hide disposal methods.
In step A11, the polyurethane finishing agent S1 is spaced addition in three times, is conducive to slow infiltration, it is to avoid once
Property add excessive concentration to react too fast on the ox-hide surface, hinder the further infiltration of the polyurethane finishing agent S1 and anti-
Should.In step A14, pressed using vacuum ironing machine, increased the adhesion of pigment, grease and ox-hide, dye ox-hide
Firmly, the hydrophobicity and elasticity of ox-hide are improved.The pliability of soft adjustable ox-hide is drawn in mechanical oscillation in step A16, makes ox-hide fine
It is loose that dimension becomes, so that the softness that ox-hide becomes；Modification is carried out to ox-hide surface can cover the flaw on ox-hide surface；Tint/spray
Color can protect ox-hide surface property and make the uniform of ox-hide surface color change；Ox-hide is pressed by rotary ironing machine, reduces ox-hide
Moisture, makes the smooth of ox-hide change.In various embodiments, can according to the demand of ox-hide product, repeat it is described draw it is soft, apply
Color/color spray, flatiron operation.
In order to contrast the ox-hide A1 of prior art tannin ox-hide and the ox-hide disposal methods using the present embodiment, use
Common tanning agent is processed same batch with the ox-hide wet blue at position, makes conventional kraft B1, is comprised the following steps：
B11：When tanning is arranged, it is put into rotary drum as raw material using ox-hide wet blue 50, with ox-hide wet blue 50
Quality on the basis of quality, first adds the water of 100% Reference mass, then (english abbreviation is by the resin tannin of 2% Reference mass
Relugan D) and the composite filled tannin of synthesis (english abbreviation the be Basyntan HL) mixing of 5.5% Reference mass after points three
Secondary addition, adds 2.5% Reference mass, every minor tick 10~15 minutes every time；
B12：By the neutralization tannin (english abbreviation is NTL) and the acrylate resin tanning of 8% Reference mass of 4% Reference mass
Added in three times after agent mixing, 4% Reference mass, every minor tick 10~15 minutes are added every time；
B13：By the resin retaning agent (english abbreviation is Retingan R7) of 3% Reference mass, the grain of 4% Reference mass
Wood, the neutralization tannin (english abbreviation is Tamol M) of 1.5% Reference mass, polymer tannin (the English contracting of 2% Reference mass
Be written as Relugan FR-RV) and 1% Reference mass pigment add after, process 2 hours；
B14：Draining, adds the Synthetic Oil of 8% Reference mass, is processed 1 hour at 50 DEG C；
B15：Ox-hide after taking-up treatment, using vacuum ironing machine, presses the ox-hide 3~4 minutes at 40 DEG C, with
After take out ox-hide, by ox-hide hang airing 2~3 days；
B16：Moisture is sprayed at the ox-hide inner surface after drying again, the moisture for making the ox-hide reaches 10%~
15%；
B17：The soft ox-hide is drawn using mechanical oscillation, modification ox-hide surface, by ox-hide surface rubbing, applies to ox-hide
Color/color spray treatment, after flatiron, obtains the ox-hide B1 of common tanning agent treatment.
It is Y-direction along the direction of the ridge line 51 of ox-hide wet blue 50 referring to Fig. 5, is X perpendicular to the direction of ridge line 51
To.Using AATCC 66-2008Wrinkle Recovery of Woven Fabrics:RecoveryAngle(AATCC 66-
2008 woven fabric wrinkle recoveries：Recovery angle is tested) testing standard carries out recovery angle test to ox-hide A1 and ox-hide B1, folds 15 points
Recovery angle testing result after clock is as shown in table 1.
Table 1
Embodiment two
A kind of polyurethane finishing agent S2 and preparation method thereof and use the polyurethane finishing agent that the present embodiment is provided
Ox-hide processing method.
The preparation method of the polyurethane finishing agent S2 is comprised the following steps：
S21：By 0.1mol degrees of functionality Fn=3, the APEO trihydroxylic alcohol of number-average molecular weight Mn=4000g/mol and
The reactant of cyclohexanedimethyl diisocyanate composition and the dibutyltin dilaurate catalyst of 50ppm of 0.3mol are added
To in a there-necked flask of 1000ml；
S22：Under conditions of 90 DEG C of oil baths, mechanical agitation is carried out to the reactant in the there-necked flask, reacted 3 hours
Afterwards, the polyurethane prepolymer for being formed will be reacted and is down to room temperature, APEO trihydroxylic alcohol and ring in the polyurethane prepolymer
Hexane diformazan group diisocyanate interconnection；
S23：The polyurethane prepolymer is diluted to the solution that solidification amount is 50% using ethanol；
S24：Use quality percentage be 30% aqueous solution of sodium bisulfite in the solution add 0.2mol sulfurous
Sour hydrogen sodium carries out end capping reaction to the polyurethane prepolymer, reacts 1.5 hours at room temperature；
S25：Use quality percentage is that 20% dilute sulfuric acid adjusts to 3 the pH value of the solution, that is, form solid content
About 48.5% polyurethane finishing agent S2.
Comprised the following steps using the ox-hide processing method of polyurethane finishing agent S2：
A21：When tanning is arranged, it is put into rotary drum as raw material using ox-hide wet blue, with the quality of ox-hide wet blue
On the basis of quality, first add the water of 150% Reference mass, then in three times by the acrylic resin of 3%, 3%, 2% Reference mass
Tanning agent is added, every minor tick 10~15 minutes；
A22：By the resin retaning agent of 9% Reference mass, three are divided after the polyurethane finishing agent S2 mixing of 15% Reference mass
Secondary addition, adds 8% Reference mass, every minor tick 15 minutes every time；
A23：The pigment of 1% Reference mass is added, is processed 1.5 hours；
A24：Draining, adds the natural oil of 15% Reference mass, is processed 1.5 hours at 50 DEG C；
A25：Ox-hide after taking-up treatment, using vacuum ironing machine, presses the ox-hide 3~4 minutes at 40 DEG C, with
After take out ox-hide, by ox-hide hang airing 2~3 days；
A26：Moisture is sprayed at the ox-hide inner surface after drying again, the moisture for making the ox-hide reaches 10%~
15%；
A27：The soft ox-hide is drawn using mechanical oscillation, modification ox-hide surface, by ox-hide surface rubbing, applies to ox-hide
Color/color spray treatment, the ox-hide is pressed by rotary ironing machine, and ironing temperature is 100~150 DEG C, and this implementation is obtained after flatiron
The ox-hide A2 of example ox-hide disposal methods.
In step A22, interval adds in three times after the polyurethane finishing agent S2 and resin retaning agent mixing, has
Slowly permeated beneficial to the polyurethane finishing agent S2, it is to avoid disposable to add excessive concentration to react too fast on the ox-hide surface,
Hinder the further infiltration and reaction of the polyurethane finishing agent S2.In alternative embodiments, in step A22 resin is answered
Tanning agent consumption can also be the 6% of Reference mass.
In order to contrast the ox-hide A2 of prior art tannin ox-hide and the ox-hide disposal methods of the present embodiment, by embodiment
Step B11 to B17 in one, the ox-hide wet blue used step A21 is processed with batch with the ox-hide wet blue at position,
Wherein the amount of water of step B11 is consistent with step A21, step B14 with and step A24 it is consistent, ox-hide B2 is obtained after treatment.
Ox-hide A2 and ox-hide B2 are carried out to be tested with the identical recovery angle of embodiment one, test data is as shown in table 2.
Table 2
Embodiment three
A kind of polyurethane finishing agent S3 and preparation method thereof and use the polyurethane finishing agent that the present embodiment is provided
Ox-hide processing method.
The preparation method of the polyurethane finishing agent S3 is comprised the following steps：
S31：By 0.1mol degrees of functionality Fn=2, the polyoxypropyleneglycol (English of number-average molecular weight Mn=8000g/mol
Be abbreviated as PEG) and 0.2mol toluene di-isocyanate(TDI) (english abbreviation is TDI) composition reactant and 100ppm two bays
Sour dibutyl tin catalyst is added in a there-necked flask of 1000ml；
S32：Under conditions of 90 DEG C of oil baths, mechanical agitation is carried out to the reactant in the there-necked flask, reacted 4 hours
Afterwards, the polyurethane prepolymer for being formed will be reacted and is down to room temperature, PEG the and TDI interconnections in the polyurethane prepolymer；
S33：The polyurethane prepolymer is diluted to the solution that solidification amount is 50% using isopropanol；
S34：Use quality percentage be 30% aqueous solution of sodium bisulfite in the solution add 0.3mol sulfurous
Sour hydrogen sodium carries out end capping reaction to the polyurethane prepolymer, reacts 2 hours at room temperature；
S35：Use quality percentage is that 10% dilute sulfuric acid adjusts to 3 the pH value of the solution, that is, form solid content
About 49% polyurethane finishing agent S3.
Comprised the following steps using the ox-hide processing method of polyurethane finishing agent S3：
A31：When tanning is arranged, it is put into rotary drum as raw material using ox-hide wet blue, with the quality of ox-hide wet blue
On the basis of quality, first add the water of 200% Reference mass, then by the resin tannin of 2% Reference mass, 5.5% Reference mass
Added in three times after synthesizing composite filled tannin mixing, 2.5% Reference mass, every minor tick 10~15 minutes are added every time；
A32：By after the acrylate resin tanning agent mixing for neutralizing tannin and 8% Reference mass of 4% Reference mass points three
Secondary addition, adds 4% Reference mass, every minor tick 10~15 minutes every time；
A33：By the resin retaning agent of 3% Reference mass, the grain wood of 4% Reference mass, the neutralization list of 1.5% Reference mass
Rather, the pigment mixing of the polymer tannin of 2% Reference mass, 6% Reference mass polyurethane finishing agent S3 and 1% Reference mass
Add, process 2 hours；
A34：Draining, adds the Synthetic Oil of 6% Reference mass and the natural oil of 4% Reference mass, locates at 50 DEG C
Reason 1.2 hours；
A35：Ox-hide after taking-up treatment, using vacuum ironing machine, presses the ox-hide 3~4 minutes at 40 DEG C, with
After take out ox-hide, by ox-hide hang airing 2~3 days；
A36：Moisture is sprayed at the ox-hide inner surface after drying again, the moisture for making the ox-hide reaches 10%~
15%；
A37：The soft ox-hide is drawn using mechanical oscillation, modification ox-hide surface, by ox-hide surface rubbing, applies to ox-hide
Color/color spray treatment, the ox-hide is pressed by rotary ironing machine, and ironing temperature is 100~150 DEG C, and this implementation is obtained after flatiron
The ox-hide A3 of example ox-hide disposal methods.
In order to contrast the ox-hide A3 of prior art tannin ox-hide and the ox-hide disposal methods of the present embodiment, by embodiment
Step B11 to B17 in one, the ox-hide wet blue used step A31 is processed with batch with the ox-hide wet blue at position,
Wherein the amount of water of step B11 is consistent with step A31, step B14 with and step A34 it is consistent, ox-hide B3 is obtained after treatment.
Ox-hide A3 and ox-hide B3 are carried out to be tested with the identical recovery angle of embodiment one, test data is as shown in table 3.
Table 3
Certainly, in the polyurethane finishing agent preparation method that other alternate embodiments of the invention are provided, form described
In the reactant of polyurethane prepolymer, the oligomer polyol can also be the one of other PPGs or hydroxyalkyl silicone oil
Plant or various, the diisocyanate can also select 4,4- dicyclohexyl methyl hydride diisocyanates.In alternate embodiment
In, pH value regulation can also be carried out to the solution using acid solutions such as hydrochloric acid, acetic acid or formic acid in step S15, S25 or S25.It is comprehensive
On, the polyurethane finishing agent preparation method that the present invention is provided without using toxic organic solvent, to environment and operating personnel without
Evil, is conducive to industrialized production.
Referring to Fig. 6, constituted in original collagen fabric 41 using the ox-hide of ox-hide disposal methods of the invention
In structure, it is crosslinked with collagen fabric 41 by polyurethane, collagen fabric 41 is passed through into resilient polyurethane molecular
Chain 42 connection it is more firm while, filler 43 is more fully filled in the collagen fabric 41 and polyurethane
In the space that strand 42 is formed.After being processed through polyurethane finishing agent of the invention, shape between the collagen fabric of the ox-hide
Into elastic construction, the elasticity of the ox-hide can be effectively improved.Referring to Fig. 7, when the ox-hide by external force when being acted on, the glue
Although former azelon 41 deforms, new molecular link will not be formed.Therefore, after external force effect is lost, polyurethane point
The elastic construction that subchain 42 and the collagen fabric 41 are formed can make the ox-hide be returned to original shape as far as possible
State.
In sum, the polyurethane in the present invention is the strand with multi-functional flexibility, can be with the glue in leather
There are many site crosslinkings in fibrillation.Polyurethane finishing agent of the invention have two to three active function groups, can simultaneously with difference
Collagenous fibres be bonded, similar to " bridge " is costed between tropocollagen molecule, play effective crosslinked action；Meanwhile, will not
Because crosslinking points are excessive, so as to cause collagenous fibres is too bonded, the enhancing of leather elasticity is unfavorable on the contrary.In addition, described
Isocyanates hard section assigns molecule chain rigidity in polyurethane molecular chain in polyurethane finishing agent, and it is soft that polyalcohol soft section assigns strand
Property, soft section is chosen in the polyurethane for the polyalcohol of macromolecular, polyurethane finishing agent is had compared with high-flexibility.Using this hair
After bright polyurethane finishing agent is applied to leather arrangement, when leather is subject to bending external force, the polyurethane molecular chain between collagen rises
To the effect of support, after external force is removed, polyurethane molecular chain can play the effect of " spring ", help its resilience, improve skin
The elasticity of leather.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be in other specific forms realized.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires to be limited rather than described above, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.Any reference in claim should not be considered as the claim involved by limitation.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each implementation method is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that for clarity, those skilled in the art should
Specification an as entirety, the technical scheme in each embodiment can also be formed into those skilled in the art through appropriately combined
May be appreciated other embodiment.
Claims (10)
1. a kind of ox-hide processing method, comprises the following steps：
A1：When tanning is arranged, it is put into rotary drum as raw material using ox-hide wet blue, on the basis of the quality of ox-hide wet blue
Quality, first adds the water of 100%~200% Reference mass, adds at the polyurethane finishing agent of 6%~16% Reference mass
Reason；
A2：The pigment of 1% Reference mass is added, is processed 1~2 hour；
A3：Draining, adds the grease of 8%~15% Reference mass, is processed 1~1.5 hour at 50 DEG C；
A4：Ox-hide after taking-up treatment, using vacuum ironing machine, presses the ox-hide 3~4 minutes at 40 DEG C, then takes
Go out ox-hide, by ox-hide hang airing；
A5：Moisture is sprayed at the ox-hide inner surface after drying again, the moisture of the ox-hide is reached 10%~15%；
A6：The soft ox-hide is drawn using mechanical oscillation, modification ox-hide surface, by ox-hide surface rubbing, carries out tinting/spraying to ox-hide
Color treatment, after flatiron, obtains the ox-hide of this method treatment.
2. ox-hide processing method according to claim 1, it is characterised in that：In the step A1, the polyurethane integral
Reason agent is added in three times, every minor tick 15 minutes.
3. ox-hide processing method according to claim 1, it is characterised in that：In the step A1, addition is additionally included in
Before the polyurethane finishing agent, add 8% Reference mass acrylate resin tanning agent the step of.
4. ox-hide processing method according to claim 1, it is characterised in that：It is described poly- adding in the step A1
The resin retaning agent of 3%~9% Reference mass is additionally added while urethane finishing agent.
5. ox-hide processing method according to claim 1, it is characterised in that：In the step A1, also including adding 2%
The resin tannin of Reference mass, the composite filled tannin of synthesis of 5.5% Reference mass, the neutralization tannin of 5.5% Reference mass,
The polymer tannin of 2% Reference mass and the grain wood of 4% Reference mass.
6. ox-hide processing method as claimed in any of claims 1 to 5, it is characterised in that：The polyurethane is arranged
Agent includes：Alcohols solvent and polyurethane solute, wherein what the polyurethane was formed by oligomer polyol and diisocyanate
Polyurethane prepolymer and sodium hydrogensulfite end-capping reagent are prepared from for raw material, the oligomer polyol, diisocyanate with
And the mol ratio of sodium hydrogensulfite is 1：2~3：2~3.
7. ox-hide processing method according to claim 6, it is characterised in that：The molecular weight of the oligomer polyol is
1000~8000, degree of functionality is 2~3.
8. ox-hide processing method according to claim 6, it is characterised in that：The oligomer polyol is selected from polyether polyols
One or more of alcohol or hydroxyalkyl silicone oil.
9. ox-hide processing method according to claim 6, it is characterised in that：Described diisocyanate is selected from isophorone
Diisocyanate, 4,4- dicyclohexyl methyl hydride diisocyanates, cyclohexanedimethyl diisocyanate and toluene di-isocyanate(TDI).
10. ox-hide processing method according to claim 1, it is characterised in that：Described alcohols solvent is ethanol or isopropyl
Alcohol.
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| CN104499319A (en) * | 2014-12-17 | 2015-04-08 | 广东菲安妮皮具股份有限公司 | Cow leather dyeing process |
| CN105154594A (en) * | 2015-08-19 | 2015-12-16 | 际华三五一二皮革服装有限公司 | Manufacturing method for high-strength calfskin for special purpose |
| CN105151594A (en) * | 2015-09-24 | 2015-12-16 | 武汉锦星科技有限公司 | Garbage recycling management system and management method based on internet and garbage can |
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| CN101994254A (en) * | 2009-08-31 | 2011-03-30 | 香港纺织及成衣研发中心 | Wool knitted fabrics shape-remembering finishing agent as well as preparation method and application thereof |
| CN102070759A (en) * | 2010-11-29 | 2011-05-25 | 陕西科技大学 | Method for preparing water-based polyurethane leather retanning agent |
| CN104499319A (en) * | 2014-12-17 | 2015-04-08 | 广东菲安妮皮具股份有限公司 | Cow leather dyeing process |
| CN105154594A (en) * | 2015-08-19 | 2015-12-16 | 际华三五一二皮革服装有限公司 | Manufacturing method for high-strength calfskin for special purpose |
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