CN103060483B - Double waterproof chromium-free tanned sheep fur and its making method - Google Patents
Double waterproof chromium-free tanned sheep fur and its making method Download PDFInfo
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Abstract
The invention discloses a double waterproof chromium-free tanned sheep fur and its making method. The preparation method is characterized in that a fur skin water proofing and fur fleece proofing combination process is adopted, a waterproof fatting agent is added in the fatting process, and the surface water proofing treatment is carried out after fixing to make the fur skin reach a depth water proofing effect; and then the water proofing treatment of the fur fleece is carried out in the dry finishing phase. According to the invention, the industrial-production double waterproof chromium-free tanned sheep fur has a shrinkage temperature reaching above 85DEG C, can be permanently stored without detanning and does not contain chromium; the static water absorbing capacity of the fur skin is about 20%, and the deflection frequency is 4000-8000 or more; the zero water absorbing property, the zero water penetration property and the zero surface wetting performance of the fur fleece make water roll on the sheep fur fleece in sphere shape and the fur fleecy not wet, so the sheep fur has an obviously waterproof property; and the tensile strength is not less than 10N/mm<2>, the fracture elongation rate is not less than 50%, and the formaldehyde content is not more than 360mg/kg.
Description
Technical field
The invention belongs to function hides/skins technical field.
Background technology
Fur is also known as fur coat, Mao Ge, and be a member in leather " extended family ", fur goods is always the synonym of fashion elegance, have the title of " soft gold ".Along with the phychology gone back to nature with the mankind that improves constantly of living standards of the people constantly strengthens, the favorable rating of people to leather, fur and goods thereof also grows with each passing day.In order to meet consumption grade that people constantly promote and the pursuit to green consumption, leather and fur product are towards the future development of ecology, personalization, functionalization, fashion-orientation and best quality.With regard to the functionalization of fur and goods thereof and the feature of environmental protection, Zirconium-aluminum-titanium coordinates tanning agent to tan two waterproof type sheep skin deeply by concern and the favor of consumers in general.Especially the fur cap needed for naval, ground force, air force and People's Armed Police, industry uniform, extraordinary labor protection clothing and high-performance business wear.According to the market requirement, process hides cleaning technique national engineering laboratory of Sichuan University organizes research staff to develop Zirconium-aluminum-titanium to coordinate tanning agent to tan two waterproof type sheep skin, through repetition test contrast, produce the sheep skin that can meet waterproof requirement.
Summary of the invention
One of technical scheme of the present invention describes the manufacture method of a kind of pair of waterproof type without chrome tanning sheep skin, and the method comprises the steps:
(1) choose fine, soft fur sheep raw material skin, carry out classification batching according to " lamb skin classification batching standard ";
(2) cut clearly: prescind the discommodities such as head, pawl, tail;
(3) split, weigh: correct amount, as the meter material foundation of following operation;
(4) wash: equipment is 2 tons of paddle-tumbles (lower same), liquor ratio 25, and temperature is room temperature, and the time is 2 hours; Middle slight paddling, draining after two hours, washes away mud, bloodstain and other impurity;
(5) soak in advance: liquor ratio is 20, and interior temperature is 23 DEG C, washing powder 0.2g/L, sterilant FMN0.5 g/L, and mix up liquor ratio, interior temperature by regulation, add washing powder and sterilant, paddling 20min, stops 2h, later interval paddling, the every 60min of paddling 5min/.Totally 4 times, turn 10min, stop, spending the night; Next day paddling 20min, discharge opeing;
(6) water dumping: whizzer water dumping;
(7) cropping: wet cropping is about 20mm;
(8) fleshing: oil film, meat slag are removed;
(9) weigh: correct amount, as the meter material foundation of following operation;
(10) degreasing: liquor ratio is 20, interior temperature 38 DEG C, nonionic grease-removing agent FG-B(reaches prestige billows FG-B nonionic grease-removing agent, Sichuan Dowell Technology Co., Ltd., lot identification mark: 2012-05-29) 2.0 g/L, mix up liquor ratio, interior temperature by regulation, add the FG-B of specified amount, paddling 10min, stop 5min, paddling 10min, stops 10min, paddling 10min, discharge opeing;
(11) wash: liquor ratio is 25, and interior temperature is 35 DEG C, paddling 10min, discharge opeing;
(12) main immersion: liquor ratio is 20, interior temperature is 23 DEG C, sterilant FMN(Da Weilite FMN fungicidal preservative, Sichuan Dowell Technology Co., Ltd.) 0.3g/L, soda ash 0.5g/L, mixes up liquor ratio by regulation, interior temperature, add FG-B, FMN and the soda ash of specified amount, paddling 120min, later interval paddling, paddling 5min ~ 30min, totally 6 times, immersion is spent the night; Next day paddling 10min, discharge opeing;
(13) water dumping: utilize centrifugal hydro-extracting cage water dumping, requires that water content controls below 55%;
(14) scrape hair: the bur sticked on fleece, blood stains and ight soil are scraped off, knot hair scrapes off, ensures to hinder skin phenomenon without scraping hair;
(15) cut edge: prescind below leg knee, the part between the ribs and the hips nest requires to prescind half the part between the ribs and the hips, and nipple, tail are sharp, chest is sharp and the rotten meat of periphery, palpus limit etc. all slice off;
(16) secondary degreasing: liquor ratio is 20, interior temperature is 40 DEG C, nonionic grease-removing agent FG-B 2.5g/L; Mix up liquor ratio and interior temperature by regulation, add the FG-B of specified amount, paddling 10min, stops 10min, totally 3 times, discharge opeing;
(17) secondary washing: liquor ratio 25, interior temperature is room temperature, paddling 10min, discharge opeing;
(18) enzyme bating: liquor ratio is 20, interior temperature is 30 DEG C, sodium carbonate 0.2g/L, macerating enzyme NG 1.0g/L, nonionic grease-removing agent FG-B 0.5g/L.Mix up liquor ratio, interior temperature by regulation, slowly add sodium carbonate, regulate pH to 7.8-8.5.Add NG, FG-B, paddling moves 5min, stops 15min, totally 4 times, stops, discharge opeing, water dumping;
(19) three washings: liquor ratio 25, interior temperature is room temperature, paddling 10-15min, discharge opeing;
(20) pickling, enzyme bating: liquor ratio 20, interior temperature 35 DEG C, salt 60g/L, proteolytic enzyme (537) 10u/ml, formic acid (85%) 3g/L, sulfuric acid (98%) 0.3 ~ 0.5g/L; Prozyme F(proteolysis prozyme F, Chengdu Bailejin Biological Scinece & Technology Co., Ltd., lot identification mark: 2012-06-16) 1.5g/L.Mix up liquor ratio and interior temperature by regulation, first add the salt of specified amount, paddling 15min, survey the concentration of salt in body lotion, require to reach 6.5Be
.above, formic acid diluted by 10 times of normal-temperature water is in advance added, 15min × 3.Survey pH and reach 3.0, temperature 37 DEG C, then add the proteolytic enzyme dissolved, paddling 15min, stop 45min, with post gap paddling, 16-20h, softened after reaching effect and added sulfuric acid diluted with 20 times of water in advance again action time, 15min × 3, more continuous paddling 60min, stop, spending the night.Secondary daily inspection pH, pH control 2.3, are warming up to 28 DEG C, add prozyme F paddling 120min after reaching requirement, leave standstill 24h;
(21) tanning: liquor ratio is 20; Temperature is 35 ~ 38 DEG C; Fatting agent GLH 1.0 g/L, fatting agent GLS 0.5 g/L, DMT-II coordinates tanning agent 12 g/L, alum 4g/L; Carry out in pickling waste liquid, require to reach 6.5Be, less than, regulate with salt; Add the red GLH fatting agent of fatting agent GLH(Ace card, Baume Chemical Co., Ltd. of Germany, lot identification mark: 2012-02-15) and the red GLS fatting agent of fatting agent GLS(Ace card, German Baume Chemical Co., Ltd., lot identification mark: 2012-02-15)), after rotating 60min; Add DMT-II and coordinate tanning agent (zirconium aluminium titanium coordinates tanning agent DMT-II, Chengdu Bailejin Biological Scinece & Technology Co., Ltd., lot identification mark: 2012-05-08) alum, turn 30min, stop drum and spend the night; Next day, paddling 10min, was warmed up to 38 DEG C, and add sodium bicarbonate 1g/L, sodium formiate 1g/L turns 30min; After paddling 30min, sodium bicarbonate 1g/L, turns 30min; Add sodium bicarbonate 1.5g/L, rotate 30min, turn 5min, stop 30min, totally twice, add 1.2 g/L sodium bicarbonate, rotate 30min, require that pH is 4.0, hold over night, is warming up to 35 DEG C, and next day, paddling 30min, required crust leather shrinkage temperature >=85 DEG C;
(22) four washings: liquor ratio is 25, and interior temperature is room temperature, paddling 15min, discharge opeing;
(23) leave standstill: 2 days;
(24) secondary weighing: correct amount, as the meter material foundation of following operation;
(25) five washings: liquor ratio is 25, and interior temperature is room temperature, paddling 15min, discharge opeing;
(26) retanning: liquor ratio is 20, interior temperature is 32 ~ 35 DEG C; Formic acid 1.0g/L, DMT-II coordinates tanning agent, and (zirconium aluminium titanium coordinates tanning agent DMT-II, Chengdu Bailejin Biological Scinece & Technology Co., Ltd., lot identification mark: 2012-05-08) 1.5g/L, ART-1(ART-1 acrylic resin retanning agent, Chengdu Zhong Ke macromolecular material limited-liability company, lot identification mark: 2012-03-18) 0.8g/L, ART-2(ART-2 acrylic resin retanning agent, Chengdu Zhong Ke macromolecular material limited-liability company, lot identification mark: 2012-03-18) 0.8g/L, sodium bicarbonate 0.2 ~ 0.5g/L.Mix up liquor ratio, interior temperature by regulation, first add the formic acid of specified amount, paddling 30min; Add DMT-II and coordinate tanning agent (zirconium aluminium titanium coordinates tanning agent DMT-II, Chengdu Bailejin Biological Scinece & Technology Co., Ltd., lot identification mark: 2012-05-08), paddling 90min; Add ART-1(ART-1 acrylic resin retanning agent, Chengdu Zhong Ke macromolecular material limited-liability company, lot identification mark: 2012-03-18), paddling 30min; Add ART-2(ART-2 acrylic resin retanning agent, Chengdu Zhong Ke macromolecular material limited-liability company, lot identification mark: 2012-03-18), paddling 40min; Gradation adds sodium bicarbonate, regulates pH to 4.0, paddling 60min, hold over night;
(27) six washings: liquor ratio is 25, and interior temperature is room temperature, paddling 15min, discharge opeing;
(28) neutralize: liquor ratio 20, interior temperature is 28 ~ 32 DEG C, hypo 1.0g/L, sodium bicarbonate 0.2 ~ 1.0g/L; Hypo is added, paddling 30min after mixing up liquor ratio, temperature; Add sodium bicarbonate, paddling 120min, regulate pH to be 6.0;
(29) seven washings: liquor ratio is 25, and interior temperature is room temperature, paddling 15min, discharge opeing;
(30) stuffing: liquor ratio is 20, interior temperature is 55 DEG C, silicone based waterproof currying agent 6.0g/L, aluminium tannin or DMT-I (zirconium aluminium titanium coordinates tanning agent DMT-I, Chengdu Bailejin Biological Scinece & Technology Co., Ltd., lot identification mark: 2012-06-01) 3.0g/L; After mixing up liquor ratio, temperature, gradation adds silicone based waterproof currying agent Densodrin CD(waterproof currying agent Densodrin CD, BASF stock company of Germany, lot identification mark: 2012-04-21) and Densodrin OF(waterproof currying agent Densodrin OF, BASF stock company of Germany, lot identification mark: 2012-04-21), paddling 90min; Add aluminium tannin or DMT-I(zirconium aluminium titanium cooperation tanning agent DMT-I, Chengdu Bailejin Biological Scinece & Technology Co., Ltd., lot identification mark: 2012-06-01) be fixed, paddling 90min;
(31) eight washings: liquor ratio is 25, and interior temperature is room temperature, paddling 15min, discharge opeing;
(32) surface treatment: liquor ratio is 20, interior temperature is 55 DEG C, silicone based waterproof currying agent Densodrin OF(waterproof currying agent Densodrin OF, BASF stock company of Germany, lot identification mark: 2012-04-21) the anti-treatment agent PM4700 of 1.0g/L, organic fluorine class water-resisting agent PM4700(tri-, Minnesota Mining and Manufacturing Company, lot identification mark: 2012-05-23) 1.5g/L, formic acid 0.2 ~ 1.0g/L; After mixing up liquor ratio, temperature, add silicone based waterproof currying agent, paddling 60min; Add the anti-treatment agent PM4700 of organic fluorine class water-resisting agent PM4700(tri-, Minnesota Mining and Manufacturing Company, lot identification mark: 2012-05-23), paddling 60min; Add formic acid, paddling 30 ~ 60min, regulate pH to 4.0;
(33) nine washings: liquor ratio is 25, and interior temperature is room temperature, paddling 15min, discharge opeing;
(34) technique is carried out water dumping, drying, moisture regain, stretching, extension, toggling, placement, brush alcohol, is scalded hair, cropping, dry boiling hot hair and cropping routinely;
(35) dermatotome WATER REPELLENT: organic fluorine class water-resisting agent PM4800(oiliness concentrates spill resistant agent PM-4800, Minnesota Mining and Manufacturing Company, lot identification mark: 2012-05-18) 500g/kg, ethyl acetate or butylacetate 500g/kg; Evenly be sprayed with machine fluoro water proofing agent PM4800(oiliness and concentrate spill resistant agent PM-4800, Minnesota Mining and Manufacturing Company, lot identification mark: 2012-05-18) and ethyl acetate or butylacetate mixed solution (1:4 mixing) on dermatotome, on average often open spray 150g;
(36) naturally dry;
(37) plate: at temperature is 100 DEG C, pave one by one, plate with through type natural lustre finishing machine; A full skin plates, without extremely rolling over;
(38) fleece WATER REPELLENT: organic fluorine class water-resisting agent PM 4800(oiliness concentrates anti-dryingagent PM-4800, Minnesota Mining and Manufacturing Company, lot identification mark: 2012-05-18) 500g/kg, ethyl acetate or butylacetate 500g/kg; Evenly be sprayed with machine fluoro water proofing agent PM4800(oiliness and concentrate anti-dryingagent PM-4800, Minnesota Mining and Manufacturing Company, lot identification mark: 2012-05-18) and ethyl acetate or butylacetate mixed solution (1:4 mixing) on fleece, on average often open spray 150g.
(39) naturally dry;
(40) dry boiling hot hair: at 150 DEG C, scald hair with through type ironing machine;
(41) cropping: carry out cropping with reshear;
(42) dry boiling hot hair: at 150 DEG C, carry out boiling hot hair with through type ironing machine;
(43) dedusting, namely two waterproof type is obtained without chrome tanning sheep skin;
Another technical scheme of the present invention be a kind of two waterproof types obtained by aforesaid method without chrome tanning sheep skin, it is characterized in that its meet index as follows:
(1) according to People's Republic of China (PRC) light industry standard QB/T 1271-1991 " mensuration of fur product-shrinkage temperature ", measure shrinkage temperature and can reach more than 85 DEG C, not tempering stored for a long time;
(2) according to People's Republic of China (PRC) light industry standard QB/T 1275-1991 " mensuration of fur product-chromium sesquioxide ", this fur product is measured not containing chromium;
(3) according to National Standard of the People's Republic of China GB/T 4689.21-2008 " test of leather-physics and mechanical testing-static water absorption ", measure fur static water absorption amount and only have about 20%;
(4) fur dynamic water-proof, measure according to National Standard of the People's Republic of China GB/T 22890-2008 " test of leather-physics and the soft leather water resistance of mechanical testing ", its penetration time is at least 30 minutes.The non-absorbency of fur and watertightness and surperficial nonwetting performance, make water can not be moistening in spherical can rolling on sheep skin fleece, has obvious water-repellancy;
(5) according to People's Republic of China (PRC) light industry standard QB/T 1269-1991 " mensuration of fur product-shrinkage temperature ", People's Republic of China (PRC) light industry standard QB/T 1269-1991 " mensuration of fur product-elongation ", measures tensile strength>=10N/mm
2, elongation at break>=50%;
(6) according to National Standard of the People's Republic of China GB/T 19941-2005 " mensuration of leather and fur-chemical test-formaldehyde content ", formaldehyde content≤360mg/kg.
Preferably, its fur shrinkage temperature can reach more than 85 DEG C, not tempering stored for a long time.
Preferably, this fur, by what measure after ashing, is as the criterion with dry weight, and the Zr content of described fur is 1 ~ 6 % by weight, Al content be 1 ~ 5 % by weight, Ti content is 1 ~ 3 % by weight.
Preferably, this fur, by what measure after ashing, is as the criterion with dry weight, and the Si content of described fur is 0.05 ~ 0.3%.
Preferably, the static water absorption amount of this fur only has 20% ± 3%.
Preferably, measure according to National Standard of the People's Republic of China GB/T 22890-2008 " test of leather-physics and mechanical testing-soft leather water resistance ", its penetration time is at least 30 minutes; Described fur water vapour permeability is greater than 0.5mg/cm
2h; Its fur water vapour permeability preferred is greater than 1.5mg/cm2h; The non-absorbency of fur and watertightness and surperficial nonwetting performance, make water can not be moistening in spherical can rolling on sheep skin fleece, has obvious water-repellancy.
Another technical scheme of the present invention is that siliceous water-resisting agent is as the application without chrome tanning sheep skin water-resisting agent.
Another technical scheme of the present invention is that fluorine-containing water repellent is as the application without chrome tanning sheep skin water-resisting agent.
Embodiment
Below by enforcement, the present invention is specifically described; what be necessary to herein means out is that the present embodiment is only used to further illustrate the present invention; and limiting the scope of the invention can not be interpreted as, the person skilled in the art in this field can make some nonessential improvement and adjustment according to the content of foregoing invention.
embodiment 1
The fine-wool sheepskin choosing more than the improvement three generations on the ground such as Xinjiang, the Inner Mongol, Gansu and Qinghai, as raw material skin, prepares two waterproof type without chrome tanning sheep skin through following steps.
(1) choose fine, soft fur sheep raw material skin, carry out classification batching according to " lamb skin classification batching standard ";
(2) cut clearly: prescind the discommodities such as head, pawl, tail;
(3) split, weigh: correct amount, as the meter material foundation of following operation;
(4) wash: equipment is 2 tons of paddle-tumbles (lower same), liquor ratio 25, and temperature is room temperature, and the time is 2 hours; Middle slight paddling, draining after two hours, washes away mud, bloodstain and other impurity;
(5) soak in advance: liquor ratio is 20, and interior temperature is 23 DEG C, washing powder 0.2g/L, sterilant FMN0.5 g/L.Mix up liquor ratio, interior temperature by regulation, add washing powder and sterilant, paddling 20min, stops 2h, later interval paddling, the every 60min of paddling 5min/.Totally 4 times, turn 10min, stop, spending the night; Next day paddling 20min, discharge opeing;
(6) water dumping: whizzer water dumping;
(7) cropping: wet cropping is about 20mm;
(8) fleshing: oil film, meat slag are removed;
(9) weigh: correct amount, as the meter material foundation of following operation;
(10) degreasing: liquor ratio is 20, interior temperature 38 DEG C, nonionic grease-removing agent FG-B(reaches prestige billows FG-B nonionic grease-removing agent, Sichuan Dowell Technology Co., Ltd., lot identification mark: 2012-05-29) 2.0 g/L, mix up liquor ratio, interior temperature by regulation, add the FG-B of specified amount, paddling 10min, stop 5min, paddling 10min, stops 10min, paddling 10min, discharge opeing;
(11) wash: liquor ratio is 25, and interior temperature is 35 DEG C, paddling 10min, discharge opeing;
(12) main immersion: liquor ratio is 20, interior temperature is 23 DEG C, sterilant FMN(Da Weilite FMN fungicidal preservative, Sichuan Dowell Technology Co., Ltd.) 0.3g/L, soda ash 0.5g/L, mixes up liquor ratio by regulation, interior temperature, add FG-B, FMN and the soda ash of specified amount, paddling 120min, later interval paddling, paddling 5min ~ 30min, totally 6 times, immersion is spent the night; Next day paddling 10min, discharge opeing;
(13) water dumping: utilize centrifugal hydro-extracting cage water dumping, requires that water content controls below 55%;
(14) scrape hair: the bur sticked on fleece, blood stains and ight soil are scraped off, knot hair scrapes off, ensures to hinder skin phenomenon without scraping hair;
(15) cut edge: prescind below leg knee, the part between the ribs and the hips nest requires to prescind half the part between the ribs and the hips, and nipple, tail are sharp, chest is sharp and the rotten meat of periphery, palpus limit etc. all slice off;
(16) secondary degreasing: liquor ratio is 20, interior temperature is 40 DEG C, nonionic grease-removing agent FG-B 2.5g/L; Mix up liquor ratio and interior temperature by regulation, add the FG-B of specified amount, paddling 10min, stops 10min, totally 3 times, discharge opeing;
(17) secondary washing: liquor ratio 25, interior temperature is room temperature, paddling 10min, discharge opeing;
(18) enzyme bating: liquor ratio is 20, interior temperature is 30 DEG C, sodium carbonate 0.2g/L, macerating enzyme NG 1.0g/L, nonionic grease-removing agent FG-B 0.5g/L.Mix up liquor ratio, interior temperature by regulation, slowly add sodium carbonate, regulate pH to 7.8-8.5, add NG, FG-B, paddling moves 5min, stops 15min, totally 4 times, stops, discharge opeing, water dumping;
(19) three washings: liquor ratio 25, interior temperature is room temperature, paddling 10-15min, discharge opeing;
(20) pickling, enzyme bating: liquor ratio 20, interior temperature 35 DEG C, salt 60g/L, proteolytic enzyme (537) 10u/ml, formic acid (85%) 3g/L, sulfuric acid (98%) 0.3 ~ 0.5g/L; Prozyme F(proteolysis prozyme F, Chengdu Bailejin Biological Scinece & Technology Co., Ltd., lot identification mark: 2012-06-16) 1.5g/L.Mix up liquor ratio and interior temperature by regulation, first add the salt of specified amount, paddling 15min, survey the concentration of salt in body lotion, require to reach 6.5Be
.above, formic acid diluted by 10 times of normal-temperature water is in advance added, 15min × 3.Survey pH and reach 3.0, temperature 37 DEG C, then add the proteolytic enzyme dissolved, paddling 15min, stop 45min, with post gap paddling, 16-20h, softened after reaching effect and added sulfuric acid diluted with 20 times of water in advance again action time, 15min × 3, more continuous paddling 60min, stop, spending the night.Secondary daily inspection pH, pH control 2.3, are warming up to 28 DEG C, add prozyme F paddling 120min after reaching requirement, leave standstill 24h;
(21) tanning: liquor ratio is 20; Temperature is 35 ~ 38 DEG C; Fatting agent GLH 1.0 g/L, fatting agent GLS 0.5 g/L, DMT-II coordinates tanning agent 12 g/L, alum 4g/L; Carry out in pickling waste liquid, require reach 6.5Be, less than words use salt regulate; Add the red GLH fatting agent of fatting agent GLH(Ace card, Baume Chemical Co., Ltd. of Germany, lot identification mark: 2012-02-15) and the red GLS fatting agent of fatting agent GLS(Ace card, German Baume Chemical Co., Ltd., lot identification mark: 2012-02-15)), after rotating 60min; Add DMT-II and coordinate tanning agent (zirconium aluminium titanium coordinates tanning agent DMT-II, Chengdu Bailejin Biological Scinece & Technology Co., Ltd., lot identification mark: 2012-05-08) alum, turn 30min, stop drum and spend the night; Next day, paddling 10min, was warmed up to 38 DEG C, and add sodium bicarbonate 1g/L, sodium formiate 1g/L turns 30min; After paddling 30min, sodium bicarbonate 1g/L, turns 30min; Add sodium bicarbonate 1.5g/L, rotate 30min, turn 5min, stop 30min, totally twice, add 1.2 g/L sodium bicarbonate, rotate 30min, require that pH is 4.0, hold over night, is warming up to 35 DEG C, and next day, paddling 30min, required crust leather shrinkage temperature >=85 DEG C;
(22) four washings: liquor ratio is 25, and interior temperature is room temperature, paddling 15min, discharge opeing;
(23) leave standstill: 2 days;
(24) secondary weighing: correct amount, as the meter material foundation of following operation;
(25) five washings: liquor ratio is 25, and interior temperature is room temperature, paddling 15min, discharge opeing;
(26) retanning: liquor ratio is 20, interior temperature is 32 ~ 35 DEG C; Formic acid 1.0g/L, DMT-II coordinates tanning agent, and (zirconium aluminium titanium coordinates tanning agent DMT-II, Chengdu Bailejin Biological Scinece & Technology Co., Ltd., lot identification mark: 2012-05-08) 1.5g/L, ART-1(ART-1 acrylic resin retanning agent, Chengdu Zhong Ke macromolecular material limited-liability company, lot identification mark: 2012-03-18) 0.8g/L, ART-2(ART-2 acrylic resin retanning agent, Chengdu Zhong Ke macromolecular material limited-liability company, lot identification mark: 2012-03-18) 0.8g/L, sodium bicarbonate 0.2 ~ 0.5g/L.Mix up liquor ratio, interior temperature by regulation, first add the formic acid of specified amount, paddling 30min; Add DMT-II and coordinate tanning agent (zirconium aluminium titanium coordinates tanning agent DMT-II, Chengdu Bailejin Biological Scinece & Technology Co., Ltd., lot identification mark: 2012-05-08), paddling 90min; Add ART-1(ART-1 acrylic resin retanning agent, Chengdu Zhong Ke macromolecular material limited-liability company, lot identification mark: 2012-03-18), paddling 30min; Add ART-2(ART-2 acrylic resin retanning agent, Chengdu Zhong Ke macromolecular material limited-liability company, lot identification mark: 2012-03-18), paddling 40min; Gradation adds sodium bicarbonate, regulates pH to 4.0, paddling 60min, hold over night;
(27) six washings: liquor ratio is 25, and interior temperature is room temperature, paddling 15min, discharge opeing;
(28) neutralize: liquor ratio 20, interior temperature is 28 ~ 32 DEG C, hypo 1.0g/L, sodium bicarbonate 0.2 ~ 1.0g/L; Hypo is added, paddling 30min after mixing up liquor ratio, temperature; Add sodium bicarbonate, paddling 120min, regulate pH to be 6.0;
(29) seven washings: liquor ratio is 25, and interior temperature is room temperature, paddling 15min, discharge opeing;
(30) stuffing: liquor ratio is 20, interior temperature is 55 DEG C, silicone based waterproof currying agent 6.0g/L, aluminium tannin or DMT-I (zirconium aluminium titanium coordinates tanning agent DMT-I, Chengdu Bailejin Biological Scinece & Technology Co., Ltd., lot identification mark: 2012-06-01) 3.0g/L; After mixing up liquor ratio, temperature, gradation adds silicone based waterproof currying agent Densodrin CD(waterproof currying agent Densodrin CD, BASF stock company of Germany, lot identification mark: 2012-04-21) and Densodrin OF(waterproof currying agent Densodrin OF, BASF stock company of Germany, lot identification mark: 2012-04-21), paddling 90min; Add aluminium tannin or DMT-I(zirconium aluminium titanium cooperation tanning agent DMT-I, Chengdu Bailejin Biological Scinece & Technology Co., Ltd., lot identification mark: 2012-06-01) be fixed, paddling 90min;
(31) eight washings: liquor ratio is 25, and interior temperature is room temperature, paddling 15min, discharge opeing;
(32) surface treatment: liquor ratio is 20, interior temperature is 55 DEG C, silicone based waterproof currying agent Densodrin OF(waterproof currying agent Densodrin OF, BASF stock company of Germany, lot identification mark: 2012-04-21) the anti-treatment agent PM4700 of 1.0g/L, organic fluorine class water-resisting agent PM4700(tri-, Minnesota Mining and Manufacturing Company, lot identification mark: 2012-05-23) 1.5g/L, formic acid 0.2 ~ 1.0g/L; After mixing up liquor ratio, temperature, add silicone based waterproof currying agent, paddling 60min; Add the anti-treatment agent PM4700 of organic fluorine class water-resisting agent PM4700(tri-, Minnesota Mining and Manufacturing Company, lot identification mark: 2012-05-23), paddling 60min; Add formic acid, paddling 30 ~ 60min, regulate pH to 4.0;
(33) nine washings: liquor ratio is 25, and interior temperature is room temperature, paddling 15min, discharge opeing;
(34) technique is carried out water dumping, drying, moisture regain, stretching, extension, toggling, placement, brush alcohol, is scalded hair, cropping, dry boiling hot hair and cropping routinely;
(35) dermatotome WATER REPELLENT: organic fluorine class water-resisting agent PM4800(oiliness concentrates spill resistant agent PM-4800, Minnesota Mining and Manufacturing Company, lot identification mark: 2012-05-18) 500g/kg, ethyl acetate or butylacetate 500g/kg; Evenly be sprayed with machine fluoro water proofing agent PM4800(oiliness and concentrate spill resistant agent PM-4800, Minnesota Mining and Manufacturing Company, lot identification mark: 2012-05-18) and ethyl acetate or butylacetate mixed solution (1:4 mixing) on dermatotome, on average often open spray 150g;
(36) naturally dry;
(37) plate: at temperature is 100 DEG C, pave one by one, plate with through type natural lustre finishing machine; A full skin plates, without extremely rolling over;
(38) fleece WATER REPELLENT: organic fluorine class water-resisting agent PM 4800(oiliness concentrates anti-dryingagent PM-4800, Minnesota Mining and Manufacturing Company, lot identification mark: 2012-05-18) 500g/kg, ethyl acetate or butylacetate 500g/kg; Evenly be sprayed with machine fluoro water proofing agent PM4800(oiliness and concentrate anti-dryingagent PM-4800, Minnesota Mining and Manufacturing Company, lot identification mark: 2012-05-18) and ethyl acetate or butylacetate mixed solution (1:4 mixing) on fleece, on average often open spray 150g;
(39) naturally dry;
(40) dry boiling hot hair: at 150 DEG C, scald hair with through type ironing machine;
(41) cropping: carry out cropping with reshear;
(42) dry boiling hot hair: at 150 DEG C, carry out boiling hot hair with through type ironing machine;
(43) dedusting, namely two waterproof type is obtained without chrome tanning sheep skin.
Table 1 lists Mianyang fur prepared by the embodiment of the present invention 1 and the shrinkage temperature of Mianyang fur under identical testing standard, chromium content, static water absorption amount, dynamic water-proof, tensile strength, elongation at break and the isoparametric correlation data of formaldehyde content obtained by prior art, and the two waterproof types further illustrated prepared by preparation method of the present invention all achieve significant progressive and effect without chrome tanning sheep skin in water-repellancy, the feature of environmental protection etc.
two waterproof types of table 1 embodiment of the present invention 1 contrast without chrome tanning sheep skin and existing sheep skin performance perameter
| Performance perameter | Sheep skin obtained by embodiment 1 | The sheep skin that art methods is obtained |
| Shrinkage temperature/DEG C | ≥85 | ≥85 |
| Chromic oxide content/% | 0 | 2-3 |
| Static water absorption amount/% | ≤20 | ＞50 |
| Dynamic water-proof/min | ≥30 | ＜5 |
| Tensile strength/(N/mm 2) | ≥10 | ≥10 |
| Elongation at break/% | ≥50 | ≥50 |
| Formaldehyde content/(mg/kg) | ≤100 | ≤360 |
Claims (8)
1. two waterproof type is without a chrome tanning sheep skin, it is characterized in that:
(1) shrinkage temperature can reach more than 85 DEG C, not tempering stored for a long time;
(2) not containing chromium;
(3) fur static water absorption amount only has 20%;
(4) penetration time of fur dynamic water-proof test is at least 30 minutes;
(5) tensile strength>=10N/mm
2, elongation at break>=50%;
(6) formaldehyde content≤360mg/kg.
2. waterproof type as claimed in claim 1 two is without chrome tanning sheep skin, it is characterized in that, by what measure after ashing, is as the criterion with dry weight, and the Zr content of described fur is 1 ~ 6 % by weight, Al content be 1 ~ 5 % by weight, Ti content is 1 ~ 3 % by weight.
3. the two waterproof type as described in as arbitrary in claim 1-2 is without chrome tanning sheep skin, and it is characterized in that, by what measure after ashing, be as the criterion with dry weight, the Si content of described fur is 0.05 ~ 0.3%.
4. two waterproof type as claimed in claim 1 or 2 is without chrome tanning sheep skin, and it is characterized in that, penetration time is at least 30 minutes; Described fur water vapour permeability is greater than 0.5mg/cm
2h.
5. two waterproof type as claimed in claim 4 is without chrome tanning sheep skin, and it is characterized in that its penetration time is at least 30 minutes, fur water vapour permeability is greater than 1.5mg/cm
2h.
6. waterproof type as claimed in claim 1 two is without chrome tanning sheep skin, it is characterized in that, adopts siliceous water-resisting agent to carry out WATER REPELLENT and prepares pair waterproof type without chrome tanning sheep skin with bating method without chrome coordinated.
7. two waterproof type as claimed in claim 1 is without chrome tanning sheep skin, it is characterized in that, employing fluorine-containing water repellent carries out WATER REPELLENT and bating method without chrome coordinated prepares two waterproof type without chrome tanning sheep skin.
8. manufacture as arbitrary in Claims 1 to 5 as described in two waterproof type without the preparation method of chrome tanning sheep skin, it is characterized in that the method comprises the steps:
(1) choose fine, soft fur sheep raw material skin, carry out classification batching according to " lamb skin classification batching standard ";
(2) cut clearly: prescind head, pawl, tail;
(3) split, weigh: correct amount, as the meter material foundation of following operation;
(4) wash: equipment is 2 tons of paddle-tumbles, and liquor ratio is 25, and temperature is room temperature, and the time is 2 hours; Middle slight paddling, draining after two hours, washes away mud, bloodstain and other impurity;
(5) soak in advance: liquor ratio is 20, and interior temperature is 23 DEG C, washing powder 0.2g/L, sterilant 0.5g/L, mixes up liquor ratio, interior temperature by regulation, add washing powder and sterilant, paddling 20min, stops 2h, later interval paddling, the every 60min of paddling 5min/, totally 4 times, turn 10min, stop, spending the night; Next day paddling 20min, discharge opeing;
(6) water dumping: whizzer water dumping;
(7) cropping: wet cropping is 20mm;
(8) fleshing: oil film, meat slag are removed;
(9) weigh: correct amount, as the meter material foundation of following operation;
(10) degreasing: liquor ratio is 20, interior temperature 38 DEG C, nonionic grease-removing agent 2.0g/L, mix up liquor ratio, interior temperature by regulation, add nonionic grease-removing agent, paddling 10min, stops 5min, and paddling 10min, stops 10min, paddling 10min, discharge opeing;
(11) wash: liquor ratio is 25, and interior temperature is 35 DEG C, paddling 10min, discharge opeing;
(12) main immersion: liquor ratio is 20, interior temperature is 23 DEG C, sterilant 0.3g/L, soda ash 0.5g/L; Mix up liquor ratio and interior temperature by regulation, add sterilant and soda ash, paddling 120min, later interval paddling, paddling 5min ~ 30min, totally 6 times, immersion is spent the night; Next day paddling 10min, discharge opeing;
(13) water dumping: utilize centrifugal hydro-extracting cage water dumping, requires that moisture content controls below 55%;
(14) scrape hair: the bur sticked on fleece, blood stains and ight soil are scraped off, knot hair scrapes off, ensures to hinder skin phenomenon without scraping hair; (15) cut edge: prescind below leg knee, the part between the ribs and the hips nest requires to prescind half the part between the ribs and the hips, nipple, tail point, the sharp and rotten meat of periphery of chest, must all slice off on limit;
(16) secondary degreasing: liquor ratio is 20, interior temperature is 40 DEG C, nonionic grease-removing agent 2.5g/L; Mix up liquor ratio and interior temperature by regulation, add nonionic grease-removing agent, paddling 10min, stops 10min, totally 3 times, discharge opeing;
(17) secondary washing: liquor ratio 25, interior temperature is room temperature, paddling 10min, discharge opeing;
(18) enzyme bating: liquor ratio is 20, interior temperature is 30 DEG C, sodium carbonate 0.2g/L, macerating enzyme 1.0g/L, nonionic grease-removing agent 0.5g/L, mixes up liquor ratio, interior temperature, slowly add sodium carbonate by regulation, regulates pH to 7.8-8.5; Add macerating enzyme, nonionic grease-removing agent, paddling 5min, stops 15min, totally 4 times, stops, discharge opeing, water dumping;
(19) three washings: liquor ratio 25, interior temperature is room temperature, paddling 10-15min, discharge opeing;
(20) pickling, enzyme bating: liquor ratio 20, interior temperature 35 DEG C, salt 60g/L, proteolytic enzyme 10u/ml, the formic acid 3g/L of 85%, the sulfuric acid 0.3 ~ 0.5g/L of 98%; Prozyme 1.5g/L; Mix up liquor ratio and interior temperature by regulation, first add salt, paddling 15min, survey the concentration of salt in body lotion, require to reach more than 6.5Be, add formic acid diluted by 10 times of normal-temperature water in advance, 15min × 3 time, survey pH and reach 3.0, temperature 37 DEG C, add the proteolytic enzyme dissolved again, paddling 15min, stops 45min, with post gap paddling, 16-20h, softened after reaching effect and added sulfuric acid diluted with 20 times of water in advance again action time, 15min × 3 time, more continuous paddling 60min, stop, spending the night; Secondary daily inspection pH, pH control 2.3, are warming up to 28 DEG C, add prozyme paddling 120min after reaching requirement, leave standstill 24h;
(21) tanning: liquor ratio is 20, temperature is 35 ~ 38 DEG C; Fatting agent GLH 1.0g/L, fatting agent GLS0.5g/L, zirconium aluminium titanium coordinates tanning agent 12g/L, alum 4g/L; Carry out in pickling waste liquid, require to reach 6.5Be, less than, regulate with salt; Add fatting agent GLH and fatting agent GLS, after rotating 60min; Add zirconium aluminium titanium and coordinate tanning agent and alum, turn 30min, stop drum and spend the night; Next day, paddling 10min, was warmed up to 38 DEG C, and add sodium bicarbonate 1g/L, sodium formiate 1g/L turns 30min; After paddling 30min, add the sodium bicarbonate of 1g/L, turn 30min; Add the sodium bicarbonate of 1.5g/L, rotate 30min, turn 5min, stop 30min, totally twice, add the sodium bicarbonate of 1.2g/L, rotate 30min, require that pH is 4.0, hold over night, is warming up to 35 DEG C, and next day, paddling 30min, required crust leather shrinkage temperature >=85 DEG C;
(22) four washings: liquor ratio is 25, and interior temperature is room temperature, paddling 15min, discharge opeing;
(23) 2 days are left standstill;
(24) again weigh: correct amount, as the meter material foundation of following operation;
(25) five washings: liquor ratio is 25, and interior temperature is room temperature; Paddling 15min, discharge opeing;
(26) retanning: liquor ratio is 20, interior temperature is 32 ~ 35 DEG C; Formic acid 1.0g/L, zirconium aluminium titanium coordinates tanning agent 1.5g/L, acrylic resin retanning agent ART-1,0.8g/L, acrylic resin retanning agent ART-2,0.8g/L, sodium bicarbonate 0.2 ~ 0.5g/L; Mix up liquor ratio and interior temperature by regulation, first add formic acid, paddling 30min; Add zirconium aluminium titanium and coordinate tanning agent, paddling 90min; Add acrylic resin retanning agent ART-1, paddling 30min, add acrylic resin retanning agent ART-2, paddling 40min; Gradation adds sodium bicarbonate, regulates pH to 4.0, paddling 60min, hold over night;
(27) six washings: liquor ratio is 25, and interior temperature is room temperature, paddling 15min, discharge opeing;
(28) neutralize: liquor ratio 20, interior temperature is 28 ~ 32 DEG C, hypo 1.0g/L, sodium bicarbonate 0.2 ~ 1.0g/L; Hypo is added, paddling 30min after mixing up liquor ratio and temperature; Add sodium bicarbonate, paddling 120min, regulate pH to be 6.0;
(29) seven washings: liquor ratio is 25, and interior temperature is room temperature, paddling 15min, discharge opeing;
(30) stuffing: liquor ratio is 20, interior temperature is 55 DEG C, silicone based waterproof currying agent 6.0g/L, and aluminium tannin or zirconium aluminium titanium coordinate tanning agent 3.0g/L; After mixing up liquor ratio, temperature, gradation adds silicone based waterproof currying agent, paddling 90min; Add aluminium tannin or zirconium aluminium titanium cooperation tanning agent, be fixed, paddling 90min;
(31) eight washings: liquor ratio is 25, and interior temperature is room temperature, paddling 15min, discharge opeing;
(32) surface treatment: liquor ratio is 20, interior temperature is 55 DEG C, silicone based waterproof currying agent 1.0g/L, organic fluorine class water-resisting agent 1.5g/L, formic acid 0.2 ~ 1.0g/L; After mixing up liquor ratio, temperature, add silicone based waterproof currying agent, paddling 60min; Add organic fluorine class water-resisting agent, paddling 60min; Add formic acid, paddling 30 ~ 60min, regulate pH to 4.0;
(33) nine washings: liquor ratio is 25, and interior temperature is room temperature, paddling 15min, discharge opeing;
(34) technique is carried out water dumping, drying, moisture regain, stretching, extension, toggling, placement, brush alcohol, is scalded hair, cropping, dry boiling hot hair and cropping routinely;
(35) dermatotome WATER REPELLENT: organic fluorine class water-resisting agent 500g/kg, ethyl acetate or butylacetate 500g/kg, evenly be sprayed with machine fluoro water proofing agent and ethyl acetate or butylacetate mixed solution on dermatotome, blending ratio is mass ratio 1:4, on average often opens spray 150g;
(36) naturally dry;
(37) plate: at temperature is 100 DEG C, pave one by one, plate with through type natural lustre finishing machine; A full skin plates, without extremely rolling over;
(38) fleece WATER REPELLENT: organic fluorine class water-resisting agent 500g/kg, ethyl acetate or butylacetate 500g/kg, evenly be sprayed with machine fluoro water proofing agent and ethyl acetate or butylacetate mixed solution on fleece, blending ratio is mass ratio 1:4, on average often opens spray 150g;
(39) naturally dry;
(40) dry boiling hot hair: at 150 DEG C, scald hair with through type ironing machine;
(41) cropping: carry out cropping with reshear;
(42) boiling hot hair is again done: at 150 DEG C, carry out boiling hot hair with through type ironing machine;
(43) two waterproof type is namely obtained after dedusting without chrome tanning sheep skin.
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| CN112376297B (en) * | 2020-08-26 | 2023-08-01 | 焦作隆丰皮草企业有限公司 | Waterproof agent, dyeing agent and environment-friendly dyeing process for chrome-free tanned sheep-cut napped leather |
| CN116287487B (en) * | 2023-02-06 | 2024-02-06 | 珍寿实业(商丘)有限公司 | Preparation method of waterproof sheep vamp leather based on high-performance polymer material |
| CN116855645A (en) * | 2023-06-12 | 2023-10-10 | 宁夏羊博士皮草科技有限公司 | Method for manufacturing non-chemically crosslinked ecological beach sheep fur |
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