CN105113265B - A kind of modified eider down and preparation method thereof - Google Patents

A kind of modified eider down and preparation method thereof Download PDF

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CN105113265B
CN105113265B CN201510615621.5A CN201510615621A CN105113265B CN 105113265 B CN105113265 B CN 105113265B CN 201510615621 A CN201510615621 A CN 201510615621A CN 105113265 B CN105113265 B CN 105113265B
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eider down
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water
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reacted
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CN105113265A (en
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齐鲁
陈琳聿
李慧皓
井丽
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Tianjin Polytechnic University
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Tianjin Polytechnic University
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Abstract

The present invention discloses a kind of modified eider down and preparation method thereof, and the modification eider down is compared with the former suede of eider down, and warmth retention property is improved.The preparation method is to be modified eider down by preparing cyclodextrin inclusion compound, and adsorbing metal zirconium ion obtains metal zirconium ion modification eider down.Preparation method operation is relatively simple, and large-scale production can be achieved.The present invention improves down fiber warmth retention property on the basis of eider down basic structure and down character is not destroyed by adsorbing metal zirconium ion.Insulation rate improves 1~6% compared with former suede.

Description

A kind of modified eider down and preparation method thereof
Technical field
The invention belongs to Eider down processing technical field, specifically a kind of modified eider down and preparation method thereof.
Background technology
Down fiber as a kind of natural protein fibre, with it is soft, light, fluffy, heat insulating ability is excellent the features such as, be preferable Insulation packing material, be often used as the filler of the bedding such as eiderdown quilt, down feather pillow, down-filled sleeping bag, also often by with Make the raw material of the heating clothes such as down jackets, vest, insulated cold wear.Appropriate increase down feather filling amount, warmth retention property can be more preferable, but also can be more It is aobvious too fat to move, use and bring inconvenience to dress.In order to meet the current requirement frivolous, attractive in appearance to down products, businessman releases light Suede amount is filled using reduction more than slim down jackets and reaches frivolous, attractive in appearance, but warmth retention property can be so substantially reduced.
Many patents are related to raising protein fibre and improve warming Journal of Sex Research, and such as Chinese patent CN104358136A is disclosed One kind changes surname eider down and preparation method thereof, and eider down reaches raising eider down insulation using tannic acid as crosslinking agent grafted metal zirconium ion The purpose of rate, but the method for modifying reaction time is longer, and easily down structure is damaged;Chinese patent CN102587034A is public Open one kind and meet heat insulating material natural down flocculus and its manufacture craft, eiderdown flake be by duck's down or goose down and meldable fibre and Composite fibre prepared by polyester staple fiber is mixed with forms by a certain percentage, and the patent does not change eider down warming in itself Property;Chinese patent CN102476828A discloses a kind of method that zirconia heat insulation material is prepared by the use of eider down as template, with day Right eider down is prepares template, using zirconium nitrate solution as impregnating agent, and the eider down after impregnation drying is placed in into sintering furnace high temperature sintering, Obtain that the zirconia heat insulation material of eider down arborizations structure can be kept;Chinese patent CN203144810U discloses a kind of eider down Structure, in the Surface coating nm far infrared releasing layer of down fiber, has eider down in the case of eider down heat insulating ability is not destroyed There is health-care efficacy, but the water-fastness degree of clad is poor, and the easy water elution of far infrared releasing layer falls.
The content of the invention
Not enough to solve prior art, it is an object of the invention to provide a kind of modified eider down and preparation method thereof, this changes Sex feathers suede is compared in the former suede of eider down, and warmth retention property is improved.
The technical scheme that the present invention solves the modified eider down is to design a kind of preparation method of modified eider down, its feature It is that operating procedure is as follows:
1. reaction solution is prepared, cyclodextrin concentration is 10~75g/L, and citric acid concentration is 1~80g/L, sodium hypophosphite and lemon Lemon acid concentration ratio is 1: 5~2: 1, immerses in solution dry eider down according to bath raio 1: 100~1: 200, is put into 50~90 DEG C In water-bath, heating stirring is reacted after 1~6h, is washed 3~5 times;
2. compound concentration is 1~6g/L propylgallate ethanol-water solution, will be through according to bath raio 1: 100~1: 200 Cross in 1. reacted eider down immersion solution, be put into 30~80 DEG C of water-baths, heating stirring, after 1~4h of reaction, washing 3~5 It is secondary;
3. compound concentration is 0.5~5g/L zirconium salt solution, and ammoniacal liquor regulation solution ph is 9~10, according to bath raio 1: 100 ~1: 200 will be by 2. reacted eider down immersion solution, being put into 40~60 DEG C of water-baths, heating stirring, reacting 4~5h Afterwards, wash 3~5 times, the sample is made in 30~70 DEG C of drying.
The technical scheme that the present invention solves the preparation method is to design a kind of modified eider down, it is characterised in that in use Preparation method preparation is stated, compared with former suede, its insulation rate improves 1~6%, applied to field of thermal insulation.
Compared with prior art, design increase eider down surface metal zirconium ion adsorbance of the present invention, while improving gold Belong to the stability of zirconium ion absorption, higher metal zirconium ionic adsorption amount is still kept after repeatedly washing.The present invention is in not shadow In the case of ringing down fiber self character, the warmth retention property for making down fiber by adsorbing metal zirconium ion is improved, so that Eider down has broader market application foreground.
Embodiment
Explanation is described in detail to the present invention with reference to specific case of having a try.
A kind of preparation method of modified eider down (abbreviation preparation method) of the present invention, it is characterised in that operating procedure is as follows:
1. reaction solution is prepared, cyclodextrin concentration is 10~75g/L, and citric acid concentration is 1~80g/L, sodium hypophosphite and lemon Lemon acid concentration ratio is 1: 5~2: 1, immerses in solution dry eider down according to bath raio 1: 100~1: 200, is put into 50~90 DEG C In water-bath, heating stirring is reacted after 1~6h, is washed 3~5 times;
2. compound concentration is 1~6g/L propylgallate ethanol-water solution, will be through according to bath raio 1: 100~1: 200 Cross in 1. reacted eider down immersion solution, be put into 30~80 DEG C of water-baths, heating stirring, after 1~4h of reaction, washing 3~5 It is secondary;
3. compound concentration is 0.5~5g/L zirconium salt solution, and ammoniacal liquor regulation solution ph is 9~10, according to bath raio 1: 100 ~1: 200 will be by 2. reacted eider down immersion solution, being put into 40~60 DEG C of water-baths, heating stirring, reacting 4~5h Afterwards, wash 3~5 times, the sample is made in 30~70 DEG C of drying.
In the preferred zirconium oxychloride solution of zirconium salt solution, sulfuric acid zirconium solution, potassium fluorozirconate solution or zirconium hydroxide solution One kind.
Heat-insulating property is tested:Eider down is modified with the packed 10g of 30 × 30cm square eider down to survey in flat insulation instrument Insulation rate, and it is used as reference group with the undressed eider down of equivalent.
Eider down described in preparation method of the present invention refers to the down feathers of duck and the down feathers of goose.But it is not precluded from wool, sheep The natural protein fibres such as suede, camel hair, camel's hair.
Through experiment, preparation method of the present invention is even more ideal using the effect of following process parameters range:
1. reaction solution is prepared, cyclodextrin concentration is 10~50g/L, and citric acid concentration is 1~50g/L, sodium hypophosphite and lemon Lemon acid concentration ratio is 1: 5~3: 2, immerses in solution dry eider down according to bath raio 1: 100~1: 200, is put into 60~90 DEG C In water-bath, heating stirring is reacted after 2~5h, is washed 3 times;
2. compound concentration is 2~4g/L propylgallate ethanol-water solution, will be through according to bath raio 1: 100~1: 200 Cross in 1. reacted eider down immersion solution, be put into 40~70 DEG C of water-baths, heating stirring, after 1~4h of reaction, wash 3 times;
3. compound concentration is 0.5~3g/L zirconium salt solution, and ammoniacal liquor regulation solution ph is 9~10, according to bath raio 1: 100 ~1: 200 will be by 2. reacted eider down immersion solution, being put into 45~55 DEG C of water-baths, heating stirring, reacting 4~5h Afterwards, wash 5 times, the sample is made in 50 DEG C of drying.
The modified eider down of the present invention, it is characterised in that change surname eider down using prepared by above-mentioned preparation method, compared with former suede, Its insulation rate improves 1~6%.
Embodiment 1
1. reaction solution is prepared, cyclodextrin concentration is 10g/L, and citric acid concentration is 50g/L, sodium hypophosphite and citric acid concentration Than for 1: 5, immersing in solution, being put into 60 DEG C of water-baths, heating stirring by dry eider down according to bath raio 1: 100,2h is reacted Afterwards, wash 3 times;
2. compound concentration is 2g/L propylgallate ethanol-water solution, will be after 1. reacting according to bath raio 1: 100 Eider down immersion solution in, be put into 40 DEG C of water-baths, heating stirring, reaction 4h after, wash 3 times;
3. compound concentration is 0.5g/L potassium fluorozirconate solution, and ammoniacal liquor regulation solution ph is 9, will according to bath raio 1: 100 By in 2. reacted eider down immersion solution, being put into 45 DEG C of water-baths, heating stirring, after reaction 4h, washing 5 times, 50 DEG C Sample is made in drying.
Heat-insulating property is tested:Dry modification eider down 10g is taken, is fitted into 30 × 30cm eider down bag, with flat insulation Instrument surveys the insulation rate of eider down.Compared with the former suede of the same terms, the insulation rate of modified eider down improves 1.18%.
Embodiment 2
1. reaction solution is prepared, cyclodextrin concentration is 50g/L, and citric acid concentration is 50g/L, sodium hypophosphite and citric acid concentration Than for 3: 5, immersing in solution, being put into 70 DEG C of water-baths, heating stirring by dry eider down according to bath raio 1: 150,5h is reacted Afterwards, wash 3 times;
2. compound concentration is 3g/L propylgallate ethanol-water solution, will be after 1. reacting according to bath raio 1: 150 Eider down immersion solution in, be put into 60 DEG C of water-baths, heating stirring, reaction 1h after, wash 3 times;
3. compound concentration is 1g/L sulfuric acid zirconium solution, and ammoniacal liquor regulation solution ph is 10, will be passed through according to bath raio 1: 150 2. in reacted eider down immersion solution, it is put into 55 DEG C of water-baths, heating stirring, after reaction 4h, washs 5 times, 50 DEG C of drying Sample is made.
Heat-insulating property is tested:Dry modification eider down 10g is taken, is fitted into 30 × 30cm eider down bag, with flat insulation Instrument surveys the insulation rate of eider down.Compared with the former suede of the same terms, the insulation rate of modified eider down improves 2.45%.
Embodiment 3
1. reaction solution is prepared, cyclodextrin concentration is 30g/L, and citric acid concentration is 30g/L, sodium hypophosphite and citric acid concentration Than for 1: 1, immersing in solution, being put into 80 DEG C of water-baths, heating stirring by dry eider down according to bath raio 1: 200,3h is reacted Afterwards, wash 3 times;
2. compound concentration is 3g/L propylgallate ethanol-water solution, will be after 1. reacting according to bath raio 1: 200 Eider down immersion solution in, be put into 70 DEG C of water-baths, heating stirring, reaction 2h after, wash 3 times;
3. compound concentration is 2g/L zirconium hydroxide solution, and ammoniacal liquor regulation solution ph is 9, will be through according to bath raio 1: 200 Cross in 2. reacted eider down immersion solution, be put into 55 DEG C of water-baths, heating stirring, after reaction 5h, wash 5 times, 50 DEG C of bakings It is drying to obtain sample.
Heat-insulating property is tested:Dry modification eider down 10g is taken, is fitted into 30 × 30cm eider down bag, with flat insulation Instrument surveys the insulation rate of eider down.Compared with the former suede of the same terms, the insulation rate of modified eider down improves 3.29%.
Embodiment 4
1. reaction solution is prepared, cyclodextrin concentration is 10g/L, and citric acid concentration is 1g/L, sodium hypophosphite and citric acid concentration Than for 3: 2, immersing in solution, being put into 90 DEG C of water-baths, heating stirring by dry eider down according to bath raio 1: 100,3h is reacted Afterwards, wash 3 times;
2. compound concentration is 4g/L propylgallate ethanol-water solution, will be after 1. reacting according to bath raio 1: 100 Eider down immersion solution in, be put into 50 DEG C of water-baths, heating stirring, reaction 3h after, wash 3 times;
3. compound concentration is 3g/L zirconium oxychloride solution, and ammoniacal liquor regulation solution ph is 9, will be through according to bath raio 1: 100 Cross in 2. reacted eider down immersion solution, be put into 50 DEG C of water-baths, heating stirring, after reaction 4h, wash 5 times, 50 DEG C of bakings It is drying to obtain sample.
Heat-insulating property is tested:Dry modification eider down 10g is taken, is fitted into 30 × 30cm eider down bag, with flat insulation Instrument surveys the insulation rate of eider down.Compared with the former suede of the same terms, the insulation rate of modified eider down improves 4.81%.
Embodiment 5
1. reaction solution is prepared, cyclodextrin concentration is 10g/L, and citric acid concentration is 4g/L, sodium hypophosphite and citric acid concentration Than for 4: 5, immersing in solution, being put into 80 DEG C of water-baths, heating stirring by dry eider down according to bath raio 1: 100,4h is reacted Afterwards, wash 3 times;
2. compound concentration is 4g/L propylgallate ethanol-water solution, will be after 1. reacting according to bath raio 1: 100 Eider down immersion solution in, be put into 50 DEG C of water-baths, heating stirring, reaction 1h after, wash 3 times;
3. compound concentration is 3g/L zirconium oxychloride solution, and ammoniacal liquor regulation solution ph is 10, will be through according to bath raio 1: 100 Cross in 2. reacted eider down immersion solution, be put into 50 DEG C of water-baths, heating stirring, after reaction 4h, wash 5 times, 50 DEG C of bakings It is drying to obtain sample.
Heat-insulating property is tested:Dry modification eider down 10g is taken, is fitted into 30 × 30cm eider down bag, with flat insulation Instrument surveys the insulation rate of eider down.Compared with the former suede of the same terms, the insulation rate of modified eider down improves 6.01%.
Above case is only the detailed description to the technical program, but can not detailed this patent scope.For this hair Bright some technical characteristics carry out principle of the equivalent substitution without departing from technical solution of the present invention, and it all should cover please in the present invention Ask among the technical scheme scope of protection.
The present invention does not address part and is applied to prior art.

Claims (3)

1. a kind of modified eider down preparation method, it is characterised in that operating procedure is as follows:
1. reaction solution is prepared, cyclodextrin concentration is 10~75g/L, and citric acid concentration is 1~80g/L, sodium hypophosphite and citric acid Concentration ratio is 1: 5~2: 1, immerses in solution dry eider down according to bath raio 1: 100~1: 200, is put into 50~90 DEG C of water-baths In pot, heating stirring is reacted after 1~6h, is washed 3~5 times;
2. compound concentration is 1~6g/L propylgallate ethanol-water solution, will be by 1. according to bath raio 1: 100~1: 200 In reacted eider down immersion solution, it is put into 30~80 DEG C of water-baths, heating stirring, after 1~4h of reaction, washs 3~5 times;
3. compound concentration is 0.5~5g/L zirconium salt solution, and ammoniacal liquor regulation solution ph is 9~10, according to bath raio 1: 100~1: 200 will immerse in solution by 2. reacted eider down, be put into 40~60 DEG C of water-baths, heating stirring, after 4~5h of reaction, The sample is made in washing 3~5 times, 30~70 DEG C of drying.
2. modified eider down preparation method according to claim 1, it is characterised in that:The preferred fluorine zirconic acid of described zirconium salt solution Potassium solution.
3. modified eider down preparation method according to claim 1, it is characterised in that the step is:
1. reaction solution is prepared, cyclodextrin concentration is 10~50g/L, and citric acid concentration is 1~50g/L, sodium hypophosphite and citric acid Concentration ratio is 1: 5~3: 2, immerses in solution dry eider down according to bath raio 1: 100~1: 200, is put into 60~90 DEG C of water-baths In pot, heating stirring is reacted after 2~5h, is washed 3 times;
2. compound concentration is 2~4g/L propylgallate ethanol-water solution, will be by 1. according to bath raio 1: 100~1: 200 In reacted eider down immersion solution, it is put into 40~70 DEG C of water-baths, heating stirring, after 1~4h of reaction, washs 3 times;
3. compound concentration is 0.5~3g/L zirconium salt solution, and ammoniacal liquor regulation solution ph is 9~10, according to bath raio 1: 100~1: 200 will immerse in solution by 2. reacted eider down, be put into 45~55 DEG C of water-baths, heating stirring, after 4~5h of reaction, The sample is made in washing 5 times, 50 DEG C of drying.
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CN105862431A (en) * 2016-04-21 2016-08-17 安徽皖翎羽绒制品有限公司 Water-born polyurethane coating agent containing ultrafine down fibre-beta-cyclodextrin microspheres
CN108342906B (en) * 2017-04-19 2020-05-26 安徽工程大学 Down-based composite material, preparation method and application thereof
CN107476075A (en) * 2017-06-23 2017-12-15 宁波市海曙区伊万卡农业科技有限公司 A kind of down jackets anti-static ventilation eider down and preparation method thereof
CN110067133B (en) * 2018-01-23 2021-10-29 天津工业大学 Negative ion down feather and preparation method thereof
CN114790600B (en) * 2022-04-26 2023-05-09 嘉兴市云龙服饰科技股份有限公司 Three-layer sweat-releasing thermal fabric and preparation method thereof
CN114657801A (en) * 2022-05-07 2022-06-24 江苏鼎新印染有限公司 Dyeing process for improving dyeing reproducibility

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CN1435516A (en) * 2002-12-12 2003-08-13 内蒙古鄂尔多斯羊绒集团有限责任公司 Technique for processing regenerated keratin functional fibre
CN104138734A (en) * 2014-07-22 2014-11-12 浙江工业职业技术学院 Preparing and applying method for negative oxygen ion microcapsules for fabric
CN104358136B (en) * 2014-11-06 2016-06-15 天津工业大学 A kind of modified eider down and preparation method thereof

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