CN103924451B - A kind of preparation method of self-cleaning function eider down - Google Patents

A kind of preparation method of self-cleaning function eider down Download PDF

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Publication number
CN103924451B
CN103924451B CN201410168859.3A CN201410168859A CN103924451B CN 103924451 B CN103924451 B CN 103924451B CN 201410168859 A CN201410168859 A CN 201410168859A CN 103924451 B CN103924451 B CN 103924451B
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eider down
ether
ketone
preparation
sulfonated polyether
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CN103924451A (en
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谢玉成
刘建国
王宗乾
刘晨
刘显静
沈世火
吴开明
卢兵
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Ancient Qi Eider Down Joint-Stock Co
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Ancient Qi Eider Down Joint-Stock Co
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Abstract

The invention provides a kind of preparation method of self-cleaning function eider down, the present invention passes through the light degradation system of (1) sulfonated polyether-ether-ketone and polypeptide; (2) submersion dehydration; (3) eider down that water-refusing oil-refusing finishing agent preparation has self-cleaning function is sprayed.Eider down Surface coating one deck sulfonated polyether-ether-ketone/polypeptide powder film and the water and oil repellant composition of preparation.First water and oil repellant composition prevents most of pollutant being infected with eider down, even if there is pollutant to be infected with, sulfonated polyether-ether-ketone/polypeptide powder film can form living radical under UV-irradiation, utilize its photocatalysis performance to degrade to stain to the organic pollution on eider down, pollution abatement thing, reaches self-cleaning function.Self-cleaning function feather sphere prepared by the present invention, render to water surface 72h from the beginning not wetted, render to salad pasta, 48h is not wetted; Be greater than 60% to the degradation rate of simulating pollution thing methyl orange, after 5 washings, its light degradation effect does not reduce.

Description

A kind of preparation method of self-cleaning function eider down
Technical field
The invention belongs to a kind of processing method of eider down, be specifically related to a kind of preparation method of self-cleaning function eider down.
Background technology
Down products has shown unique fluffy insulation performance because of its impayable natural fabric advantage, the favor of the person that is subject to market and consumption.
In use, sweat and other dirts contact with eider down down products, and cause eider down to go mouldy, give off a peculiar smell, microorganism exceeds standard; To down products rinsing process, by the fluffy performance of damage eider down and warmth retention property; And a small amount of pathogen that eider down itself carries is in rinse cycle, is difficult to eradicate, affects the comfort of down products.The particularly public down products in hotel, bacteria breed phenomenon is more obvious.
How provide sustained anti-microbial, antiviral to society, environmental protection, ecological down products is that pendulum is at eider down manufacturing enterprise serious and urgent task at the moment.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of preparation method of self-cleaning function eider down, the self-cleaning function eider down of production has water and oil repellant function, has from degradation function the organic pollution be infected with on eider down.
The preparation method of a kind of self-cleaning function eider down provided by the invention, comprises the following steps:
(1) light degradation system is prepared: sulfonated polyether-ether-ketone solution and fibroin polypeptide powder solution are heated and mix, add hydrochloric acid, regulator solution pH to 5.5, the light degradation system of obtained sulfonated polyether-ether-ketone and polypeptide;
(2) submersion dehydration: be impregnated in by eider down in the light degradation system aqueous solution of sulfonated polyether-ether-ketone and polypeptide, adopts two leaching two dewatering process;
(3) finishing agent is sprayed: dried by the eider down after submersion dehydration, water-refusing oil-refusing finishing agent emulsion evenly sprayed on eider down in drying course, obtained self-cleaning function eider down.
Sulfonated polyether-ether-ketone solution concentration 50-150g/L, fibroin polypeptide powder solution concentration 15-50g/L in step (1).
In light degradation system obtained in step (1), the mass ratio 1:1-2.5 of fibroin polypeptide powder and sulfonated polyether-ether-ketone.
Sulfonated polyether-ether-ketone preparation method in step (1), comprise the following steps: dried polyether-ether-ketone is dissolved in 98% concentrated sulfuric acid, solution is poured in 6-10 times of volume frozen water, stir, leave standstill, sediment is centrifugal, washing, filter, repeats 3 times, with alkali lye adjustment pH to 7, vacuumize obtains sulfonated polyether-ether-ketone, wherein the mass ratio 1:80-100 of polyether-ether-ketone and 98% concentrated sulfuric acid.
The mixing of heating described in step (1), heating-up temperature is 60-80 DEG C.
In step (2), two leaching two dewatering process are: flood 8-10min, it is 180-200% that dehydration controls liquid carrying rate at every turn.
Spraying in step (3) and arranging dosage and eider down mass ratio is 2-5:1000.
In step (3), the emulsion concentration 3-4.5g/L of finishing agent, sprays speed 30-60ml/min.
In step (3), eider down bake out temperature is 115-125 DEG C, time 30-60min.
The present invention adopts and sprays water-refusing oil-refusing finishing agent in dipping sulfonated polyether-ether-ketone and the light degradation system of polypeptide, dehydration, drying course and successfully prepare the eider down with self-cleaning function, and the art of this patent prepares eider down Surface coating one deck sulfonated polyether-ether-ketone/polypeptide powder film and water and oil repellant composition.First water and oil repellant composition prevents most of pollutant being infected with eider down, even if there is pollutant to be infected with, sulfonated polyether-ether-ketone/polypeptide powder film can form living radical under UV-irradiation, utilize its photocatalysis performance to degrade to stain to the organic pollution on eider down, therefore impart eider down pollution abatement thing and reach self-cleaning function.Prepare eider down bulking intensity>=17.0cm, oxygen demand≤10.0mg/100ml, cleannes>=450mm, Oil and Fat Content≤0.6%; Addicted to warm nature aerobic bacteria < 10 6cfu/g, bacillus < 10 2cfu/g, staple surface contact angle is greater than 150 °.Self-cleaning function feather sphere prepared by the present invention, render to water surface 72h from the beginning not wetted, render to salad pasta, 48h is not wetted; Prepare the degradation rate of self-cleaning function eider down to simulating pollution thing methyl orange and be greater than 60%, after 5 washings, its light degradation effect does not reduce.
Accompanying drawing explanation
Fig. 1 is the structure of sulfonated polyether-ether-ketone;
Fig. 2 is sulfonated polyether-ether-ketone active oxygen mechanism degraded course.
Detailed description of the invention
Embodiment 1
A preparation method for self-cleaning function eider down, comprises the following steps:
(1) light degradation system is prepared: take 50g sulfonated polyether-ether-ketone and be dissolved in 500ml water, under ultrasonic environment, be heated to 50 DEG C of accelerate dissolution; The fibroin polypeptide powder (granularity 50 μm, purity is greater than 95%) taking 30g to be dissolved in 500ml cold water after abundant swelling 3h, is heated to 70 DEG C of dissolvings.Under 70 DEG C of conditions, two kinds of solution are fully uniformly mixed, add HCl, control pH5.5, preparation light degradation system;
Wherein sulfonated polyether-ether-ketone preparation method is: by polyether-ether-ketone (Victrex, 450G) pellet is at 100 DEG C, dry 6h under vacuum, then take 4g is dissolved in the 200mL concentrated sulfuric acid (98%) at 50 DEG C, rotating speed is 400r/min, vigorous stirring 15min, reaction solution is poured in the frozen water of 8 times of volumes, rotating speed is 100r/min, Keep agitation 1h, leaves standstill 24h, sediment is through centrifugal, distilled water washing, filtration, repeat 3 times, soda bath adjust ph to 7, in 50 DEG C of vacuumizes, obtained sulfonated polyether-ether-ketone product, stores for future use;
(2) submersion dehydration: get fine purifiation white duck down 20kg, impregnated in the light degradation system aqueous solution of 0.1kg sulfonated polyether-ether-ketone and polypeptide, floods 8min at every turn, dehydration, and adopt two leaching two dewatering process, controlling liquid carrying rate is 180%.
(3) finishing agent is sprayed: dried by the eider down after submersion dehydration, bake out temperature 115 DEG C, time 30min, in eider down drying course, water-refusing oil-refusing finishing agent TG435 (UNIDYNE) is diluted, preparation concentration is the finish solution 0.04kg of 3g/L, sprays on eider down with the rate uniform of 30ml/min, obtained self-cleaning function eider down.
Embodiment 2
A preparation method for self-cleaning function eider down, comprises the following steps:
(1) light degradation system is prepared: take 50g sulfonated polyether-ether-ketone and be dissolved in 500ml water, under ultrasonic environment, be heated to 50 DEG C of accelerate dissolution; The fibroin polypeptide powder (granularity 50 μm, purity is greater than 95%) taking 20g to be dissolved in 500ml cold water after abundant swelling 3h, is heated to 80 DEG C of dissolvings.Under 80 DEG C of conditions, two kinds of solution are fully uniformly mixed, add HCl, control pH5.5, preparation light degradation system;
Wherein sulfonated polyether-ether-ketone preparation method is: by polyether-ether-ketone (Victrex, 450G) pellet is at 100 DEG C, dry 6h under vacuum, then take 4.5g is dissolved in the 200mL concentrated sulfuric acid (98%) at 50 DEG C, rotating speed is 400r/min, vigorous stirring 15min, reaction solution is poured in the frozen water of 7 times of volumes, rotating speed is 100r/min, Keep agitation 1h, leaves standstill 24h, sediment is through centrifugal, distilled water washing, filtration, repeat 3 times, soda bath adjust ph to 7, in 50 DEG C of vacuumizes, obtained sulfonated polyether-ether-ketone product, stores for future use;
(2) submersion dehydration: get fine purifiation white duck down 20kg, impregnated in the light degradation system aqueous solution of 0.1kg sulfonated polyether-ether-ketone and polypeptide, floods 9min at every turn, dehydration, and adopt two leaching two dewatering process, controlling liquid carrying rate is 200%.
(3) finishing agent is sprayed: dried by the eider down after submersion dehydration, bake out temperature 120 DEG C, time 50min, in eider down drying course, water-refusing oil-refusing finishing agent TG435 (UNIDYNE) is diluted, preparation concentration is the finish solution 0.08kg of 4g/L, sprays on eider down with the rate uniform of 30ml/min, obtained self-cleaning function eider down.
Embodiment 3
A preparation method for self-cleaning function eider down, comprises the following steps:
(1) light degradation system is prepared: take 70g sulfonated polyether-ether-ketone and be dissolved in 500ml water, under ultrasonic environment, be heated to 50 DEG C of accelerate dissolution; The fibroin polypeptide powder (granularity 50 μm, purity is greater than 95%) taking 56g to be dissolved in 500ml cold water after abundant swelling 3h, is heated to 70 DEG C of dissolvings.Under 70 DEG C of conditions, two kinds of solution are fully uniformly mixed, add HCl, control pH5.5, preparation light degradation system;
Wherein sulfonated polyether-ether-ketone preparation method is: by polyether-ether-ketone (Victrex, 450G) pellet is at 100 DEG C, dry 6h under vacuum, then take 4g is dissolved in the 200mL concentrated sulfuric acid (98%) at 50 DEG C, rotating speed is 400r/min, vigorous stirring 15min, reaction solution is poured in the frozen water of 8 times of volumes, rotating speed is 100r/min, Keep agitation 1h, leaves standstill 24h, sediment is through centrifugal, distilled water washing, filtration, repeat 3 times, soda bath adjust ph to 7, in 50 DEG C of vacuumizes, obtained sulfonated polyether-ether-ketone product, stores for future use;
(2) submersion dehydration: get fine purifiation white duck down 20kg, impregnated in the light degradation system aqueous solution of 0.1kg sulfonated polyether-ether-ketone and polypeptide, floods 10min at every turn, dehydration, and adopt two leaching two dewatering process, controlling liquid carrying rate is 180%.
(3) finishing agent is sprayed: dried by the eider down after submersion dehydration, bake out temperature 125 DEG C, time 50min, in eider down drying course, water-refusing oil-refusing finishing agent TG435 (UNIDYNE) is diluted, preparation concentration is the finish solution 0.1kg of 4.5g/L, sprays on eider down with the rate uniform of 60ml/min, obtained self-cleaning function eider down.
Embodiment 4
Water repellency test and judgement
Prepare feather sphere: eider down suede piece rubbed by machinery, make it mutually be wound around, be made into the feather sphere that diameter is 1cm, and with gauze parcel, load sealing bag and preserve, for subsequent use.
Get the beaker of 500mL, add the distilled water of 400mL, take from cleaning function feather sphere and common feather sphere gently put into beaker, record feather sphere is respectively t1 from putting into beaker to the time at the bottom of sinking to glass, judges the water repellency of feather down according to t1.The WATER REPELLENCY of eider down judges by table 1:
Table 1 water repellency grade judges
Self-cleaning function eider down prepared by embodiment of the present invention 1-3, refuses water effect 3 grades, and water effect 1 grade refused by common eider down.
Embodiment 5
Oil repellent can be tested and judge
Get the beaker of a 500mL, add the salad oil of 400mL, take from cleaning function feather sphere and common feather sphere gently put into beaker, record feather sphere is respectively t2 from putting into beaker to the time at the bottom of sinking to glass, judges the oil repellent energy of feather down according to t2.The oil repellent of eider down judges by table 2.
Table 2 oil repellent energy grade judges
Self-cleaning function eider down prepared by embodiment of the present invention 1-3, refuses oily effect 3 grades, and oily effect 1 grade refused by common eider down.
Embodiment 6
Organic matter degradation performance test and judgement
Adopt methyl orange as simulation organic pollution, research automatically cleaning eider down and common eider down 100w ultraviolet mercury lamp (centre wavelength 365nm) irradiate under, to its light degradation property.Following table 3 gives simulating pollution thing methyl orange degradation effect.
Table 3 simulating pollution thing methyl orange degradation effect
After self-cleaning function eider down washing prepared by the present invention, light degradation effect does not reduce.
Prepare self-cleaning function eider down after methyl orange is painted, through 5 washings, light degradation effect does not reduce, and result is as following table 4.
The impact on methyl orange degradation effect washed by table 4

Claims (8)

1. a preparation method for self-cleaning function eider down, is characterized in that, comprises the following steps:
(1) light degradation system is prepared: sulfonated polyether-ether-ketone solution and fibroin polypeptide powder solution are heated and mix, add hydrochloric acid, regulator solution pH to 5.5, the light degradation system of obtained sulfonated polyether-ether-ketone and polypeptide;
(2) submersion dehydration: be impregnated in by eider down in the light degradation system aqueous solution of sulfonated polyether-ether-ketone and polypeptide, adopts two leaching two dewatering process;
(3) finishing agent is sprayed: dried by the eider down after submersion dehydration, water-refusing oil-refusing finishing agent emulsion evenly sprayed on eider down in drying course, obtained self-cleaning function eider down;
Sulfonated polyether-ether-ketone solution concentration 50-150g/L, fibroin polypeptide powder solution concentration 15-50g/L in step (1).
2. preparation method according to claim 1, is characterized in that, in light degradation system obtained in step (1), and the mass ratio 1:1-2.5 of fibroin polypeptide powder and sulfonated polyether-ether-ketone.
3. preparation method according to claim 1, it is characterized in that, sulfonated polyether-ether-ketone preparation method, comprises the following steps: be dissolved in by dried polyether-ether-ketone in 98% concentrated sulfuric acid, is poured into by solution in 6-10 times of volume frozen water, stir, leave standstill, sediment is centrifugal, washing, filter, repeats 3 times, with alkali lye adjustment pH to 7, vacuumize obtains sulfonated polyether-ether-ketone, wherein the mass ratio 1:80-100 of polyether-ether-ketone and 98% concentrated sulfuric acid.
4. preparation method according to claim 1, is characterized in that, the mixing of heating described in step (1), heating-up temperature is 60-80 DEG C.
5. preparation method according to claim 1, is characterized in that, in step (2), two leaching two dewatering process are: flood 8-10min, it is 180-200% that dehydration controls liquid carrying rate at every turn.
6. preparation method according to claim 1, is characterized in that, spraying in step (3) and arranging dosage and eider down mass ratio is 2-5:1000.
7. preparation method according to claim 1, is characterized in that, in step (3), the emulsion concentration 3-4.5g/L of finishing agent, sprays speed 30-60ml/min.
8. preparation method according to claim 1, is characterized in that, in step (3), eider down bake out temperature is 115-125 DEG C, time 30-60min.
CN201410168859.3A 2014-04-24 2014-04-24 A kind of preparation method of self-cleaning function eider down Expired - Fee Related CN103924451B (en)

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Publication number Priority date Publication date Assignee Title
CN107700223B (en) * 2017-11-08 2020-03-27 安徽工程大学 Processing method of anti-contamination wash-free feather down
CN108477693B (en) * 2018-03-29 2020-06-05 江苏工程职业技术学院 Down jacket preparation process
CN110791967A (en) * 2019-11-02 2020-02-14 六安市皖西羽绒有限公司 Method for preparing down feather with high water repellency grade

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1854384A (en) * 2005-04-20 2006-11-01 中科波司登纳米服饰(苏州)有限公司 Production of feather dress fabric with self-cleaning function
CN103478943A (en) * 2012-06-15 2014-01-01 高邮市润和制衣有限公司 Thermal-insulation heating down coat

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1854384A (en) * 2005-04-20 2006-11-01 中科波司登纳米服饰(苏州)有限公司 Production of feather dress fabric with self-cleaning function
CN103478943A (en) * 2012-06-15 2014-01-01 高邮市润和制衣有限公司 Thermal-insulation heating down coat

Non-Patent Citations (1)

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Title
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