CN105780502A - Flame-retardant down fiber and preparation method thereof - Google Patents

Flame-retardant down fiber and preparation method thereof Download PDF

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Publication number
CN105780502A
CN105780502A CN201610343313.6A CN201610343313A CN105780502A CN 105780502 A CN105780502 A CN 105780502A CN 201610343313 A CN201610343313 A CN 201610343313A CN 105780502 A CN105780502 A CN 105780502A
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Prior art keywords
retardant
fire
fiber
down fiber
preparation
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CN201610343313.6A
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CN105780502B (en
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齐鲁
井丽
马超
李慧皓
白立峰
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Tianjin Polytechnic University
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Tianjin Polytechnic University
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M19/00Treatment of feathers
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/30Flame or heat resistance, fire retardancy properties

Abstract

The invention discloses flame-retardant down fiber and a preparation method thereof. Compared with original down, down prepared by the method has the advantage that the flame retardancy is improved. The preparation method comprises the step of with organic acid as a crosslinking agent, grafting an inorganic flame-retardant agent (zirconium salt) to modified down fiber to obtain the flame-retardant down fiber. The flame-retardant down fiber disclosed by the invention has the advantages that the process condition and operation are simple, and large-scale production can be realized; and under the condition of not influencing the basic structure and the characteristics of the original down, the limit oxygen index (LOI) of the modified flame-retardant fiber reaches 28-38 and certain far-infrared action is achieved.

Description

A kind of fire-retardant down fiber and preparation method thereof
Technical field
The present invention relates to natural fiber treatment technology, a kind of fire-retardant down fiber and preparation method thereof.
Background technology
Down fiber, as a kind of natural protein fibre, has the features such as softness, light weight, thermal property are good, Down fiber, due to the advantage on its chemical composition and structure, has good warmth retention property, therefore down fiber quilt It is widely used in the packing material of winter warming textile product.Along with the development of science and technology, countries in the world are to weaving The flame-retardancy requirements of product is more and more higher.But more reduce plumage as its preferable combustibility of natural protein fibre The security performance of chenille article.
Many patents relate to the research of protein fire resistance fibre, and such as Chinese patent CN102720053A discloses one The flame-proof treatment method of kind of wool fiber, uses the carbon ball of Nitric Acid Modified to do fire retardant, with deionized water, γ- Mercaptopropyltriethoxysilane makes the fire-retardant suspension of carbon ball, Pilus Caprae seu Ovis be impregnated in suspension and process, this Method uses suspension rather than solution can cause reaction to be difficult to carry out, and wastes raw material;Chinese patent CN104947234A discloses a kind of fire-retardant ecological bacteriostatic down fiber, by eider down, chicken feather, cotton fiber, Pu Gong English Down Fiber, chitin, bentonite, nano magnesia, peach gum powder, zinc acetate, chlorination-1-butyl-3-first Base imidazoles, water grind according to a certain percentage and make spinning solution, prepared spinning solution is carried out spinning and obtains, Although this fiber has certain anti-flammability but also destroy the structure of down fiber itself, prepared fiber is warming Property just cannot compare favourably with eider down;Chinese patent CN102433762A discloses the preparation of a kind of flame retardant down feathers Method, down feathers is grafted fire retardant with tartaric acid for cross-linking agent, reaches to prepare the purpose of flame retardant down feathers;China Patent CN101509193A discloses a kind of method of improving wool fire-retardancy with biological enzyme, utilizes and turns glutamy One class is contained the grafting compounds of primary amino radical and a large amount of P elements to Pilus Caprae seu Ovis by the catalytic action of amine transaminase MTG On, this method needs to carry out pretreatment and removes the scale of wool surfaces, but the internal structure of eider down and Pilus Caprae seu Ovis with And the structure of fiber surface has and there is the biggest difference.
Summary of the invention
For solving the deficiencies in the prior art, it is an object of the invention to provide a kind of fire-retardant down fiber and preparation thereof Method.The fire-retardant down fiber fire resistance that this preparation method obtains is high, it is permanent to have, and can keep eider down Original structure and the characteristic of itself.These preparation method process conditions, operational approach are the simplest, it is easy to accomplish Produce in enormous quantities.
The present invention solves the technical scheme of described technical problem, designs a kind of fire-retardant down fiber and preparation side thereof Method, it is characterised in that operating procedure is as follows: (1) weighs a certain amount of down fiber, at room temperature, adds one Quantitative distilled water infiltration;(2) reaction reagent is weighed: the concentration of zirconium salt solution is 0.4-5g/L;Organic acid Concentration is 0.1-10g/L;(3) then reaction reagent is added in the eider down of infiltration, regulate bath raio 1: 100-200; (4) being placed in there-necked flask by above-mentioned reactant, Stirring 1-7h in thermostat water bath, temperature is set as 30-100℃;(5) modification eider down is taken out, distilled water wash 3-5 time;(6) modification eider down is done in an oven Dry, temperature 40-100 DEG C, until drying is to described fire-retardant down fiber.
The present invention solves the technical scheme of described preparation method, designs a kind of fire-retardant down fiber, and its feature exists In using above-mentioned preparation method to prepare, its limited oxygen index (LOI) is 28-38, and has certain far infrared merit Energy.
Compared with prior art, the present invention has the beneficial effects that: the present invention designs the preparation side of the right fiber of fire-retardant plumage Method process conditions and simple to operate, and structure and the characteristic of itself of eider down can be kept, cost is relatively low, is made Reagent environmental protection, nontoxic, pollution-free;It is grafted on eider down reach by fire retardant as cross-linking agent by organic acid To the purpose of permanent fire retardant, expand the range of down fiber.
Detailed description of the invention
Below in conjunction with being embodied as case, the present invention is described in detail explanation.
Fire-retardant down fiber of one of present invention design and preparation method thereof, it is characterised in that operating procedure is as follows: (1) weigh a certain amount of down fiber, at room temperature, add the infiltration of a certain amount of distilled water;(2) weigh instead Answer reagent: the concentration of zirconium salt solution is 0.4-5g/L;The concentration of organic acid is 0.1-10g/L;(3) then instead Answer reagent to add in the eider down of infiltration, regulate bath raio 1: 100-200;(4) above-mentioned reactant is placed in three mouthfuls of burnings In Ping, Stirring 1-7h in thermostat water bath, temperature is set as 30-100 DEG C;(5) modification eider down is taken Go out, distilled water wash 3-5 time;(6) modification eider down is dried in an oven, temperature 40-100 DEG C, until drying Do and i.e. obtain described fire-retardant down fiber.
Described zirconium salt solution is preferably ammonium fluozirconate solution, zirconium oxychloride solution, zirconium carbonate solution, Disulfatozirconic acid. Solution, zirconium oxysulfate solution at least one.
Described organic acid is preferably at least one in oxalic acid, malic acid, adipic acid, tartaric acid.
Down fiber 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 The fine hair such as cashmere, camel's hair.
The fire retardant that preparation method of the present invention is designed with is zirconates.It is high that this fire retardant has flame retarding efficiency, and And increase the feature such as surplus carbon rate of down fiber.Compared with prior art, the fire retardant that the present invention uses can have Effect reduces the combustibility of down fiber, suppresses spreading of flame, after flame once leaves, fire-retardant down fiber Can fire extinguishing quickly, flame retarding efficiency is high, and has washability and reach the effect of permanent fire retardant.Through system of the present invention The down fiber that Preparation Method processes, owing to containing metal zirconium ion in fire retardant, the most this down fiber is not only There is anti-flammability, and the most certain far-infrared transmitting function, and down fiber can be kept soft, fluffy and Warming inherent characteristics such as grade.
Through test, the effect of the preparation method of the present invention following process parameters range of employing is even more ideal: (1) weighs A certain amount of down fiber, at room temperature, adds the infiltration of a certain amount of distilled water;(2) reaction reagent is weighed: The concentration of zirconium salt solution is 0.4-3g/L;The concentration of organic acid is 0.1-9g/L;(3) then reaction reagent is added Enter in the eider down of infiltration, regulate bath raio 1: 100-200;(4) above-mentioned reactant is placed in there-necked flask, Stirring 2-6h in thermostat water bath, temperature is set as 40-90 DEG C;(5) modification eider down is taken out, distillation Water washs 3 times;(6) modification eider down is dried in an oven, temperature 50 C, until drying is to described resistance Combustion down fiber.
The fire-retardant down fiber of the present invention, it is characterised in that use fire-retardant down fiber prepared by above-mentioned preparation method Limited oxygen index (LOI) be 28-38.
Case study on implementation 1
Step one: configuration concentration is 0.4g/L Disulfatozirconic acid. and concentration is 0.1g/L oxalic acid treatment liquid 150ml, according to Bath raio 1: 100 takes 1.5g Drying Down and immerses in treatment fluid.
Step 2: above-mentioned reactant is placed in there-necked flask, Stirring 1h in thermostat water bath, temperature Degree is set as 30 DEG C, is taken out by reacted eider down, distilled water wash 5 times, finally after reaching the setting time Being dried in an oven by reacted eider down, temperature is 50 DEG C, and time 3.5h i.e. obtains fire-retardant down fiber.
The limited oxygen index of the fire-retardant down fiber sample prepared after testing is 28, and sample is soft, bulkiness is good.
Case study on implementation 2
Step one: configuration concentration is 5g/L zirconium carbonate and concentration is 10g/L adipic acid treatment fluid 400ml, according to Bath raio 1: 200 takes 2g Drying Down and immerses in treatment fluid.
Step 2: above-mentioned reactant is placed in there-necked flask, Stirring 7h in thermostat water bath, temperature Degree is set as 100 DEG C, is taken out by reacted eider down, distilled water wash 5 times, finally after reaching the setting time Being dried in an oven by reacted eider down, temperature is 50 DEG C, and time 3.5h i.e. obtains fire-retardant down fiber.
The limited oxygen index of the fire-retardant down fiber sample prepared after testing is 38, and sample is soft, bulkiness is good.
Case study on implementation 3
Step one: configuration concentration is 1g/L ammonium fluozirconate and concentration is 2g/L malic acid treatment fluid 240ml, presses Take 2g Drying Down according to bath raio 1: 120 to immerse in treatment fluid.
Step 2: above-mentioned reactant is placed in there-necked flask, Stirring 2.5h in thermostat water bath, temperature Degree is set as 50 DEG C, is taken out by reacted eider down, distilled water wash 5 times, finally after reaching the setting time Being dried in an oven by reacted eider down, temperature is 50 DEG C, and time 3.5h i.e. obtains fire-retardant down fiber.
The limited oxygen index of the fire-retardant down fiber sample prepared after testing is 34, and sample is soft, bulkiness is good.
Case study on implementation 4
Step one: configuration concentration is 2.5g/L Disulfatozirconic acid. and concentration is 4g/L oxalic acid treatment liquid 450ml, according to Bath raio 1: 150 takes 3g Drying Down and immerses in treatment fluid.
Step 2: above-mentioned reactant is placed in there-necked flask, Stirring 4h in thermostat water bath, temperature Degree is set as 70 DEG C, is taken out by reacted eider down, distilled water wash 5 times, finally after reaching the setting time Being dried in an oven by reacted eider down, temperature is 50 DEG C, and time 3.5h i.e. obtains fire-retardant down fiber.
The limited oxygen index of the fire-retardant down fiber sample prepared after testing is 36.5, and sample is soft, bulkiness Good.
Case study on implementation 5
Step one: configuration concentration is 3g/L basic zirconium chloride and concentration is 8g/L tartaric acid treatment fluid 540ml, presses Take 3g Drying Down according to bath raio 1: 180 to immerse in treatment fluid.
Step 2: above-mentioned reactant is placed in there-necked flask, Stirring 6h in thermostat water bath, temperature Degree is set as 90 DEG C, is taken out by reacted eider down, distilled water wash 5 times, finally after reaching the setting time Being dried in an oven by reacted eider down, temperature is 50 DEG C, and time 3.5h i.e. obtains fire-retardant down fiber.
The limited oxygen index of the fire-retardant down fiber sample prepared after testing is 37, and sample is soft, bulkiness is good.
Case study on implementation 6
Step one: configuration concentration is 4g/L zirconium carbonate and concentration is 9g/L adipic acid treatment fluid 450ml, according to Bath raio 1: 150 takes 3g Drying Down and immerses in treatment fluid.
Step 2: above-mentioned reactant is placed in there-necked flask, Stirring 6h in thermostat water bath, temperature Degree is set as 90 DEG C, is taken out by reacted eider down, distilled water wash 5 times, finally after reaching the setting time Being dried in an oven by reacted eider down, temperature is 50 DEG C, and time 3.5h i.e. obtains fire-retardant down fiber.
The limited oxygen index of the fire-retardant down fiber sample prepared after testing is 37.5, and sample is soft, bulkiness Good.
Finally should be noted that: above case is only the detailed description to the technical program, but can not be detailed The scope of this patent.Portion of techniques feature for the present invention carries out equivalent without deviating from the technology of the present invention side The principle of case, it all should be contained in the middle of the technical scheme scope that the present invention is claimed.
The present invention does not addresses part and is applicable to prior art.

Claims (5)

1. the preparation method of a fire-retardant down fiber, it is characterised in that operating procedure and formula are as follows: weigh Quantitative down fiber, at room temperature infiltrates;Being subsequently adding reaction reagent, wherein zirconium salt solution concentration is 0.4-5g/L, organic acid concentration are 0.1-10g/L;Adding a certain amount of water, regulation eider down with solution ratio is 1∶100-200;At a temperature of 30-100 DEG C, reaction treatment 1-7h, use distilled water wash 3-5 time afterwards, Dry at a temperature of 40-100 DEG C, obtain fire-retardant down fiber.
The preparation method of fire-retardant down fiber the most according to claim 1, it is characterised in that: described zirconium Saline solution is that ammonium fluozirconate solution, zirconium oxychloride solution, zirconium carbonate solution, Disulfatozirconic acid. solution, zirconium oxysulfate are molten At least one of liquid.
The preparation method of fire-retardant down fiber the most according to claim 1, it is characterised in that: described has Machine acid is at least one in oxalic acid, malic acid, adipic acid, tartaric acid.
The preparation method of fire-retardant down fiber the most according to claim 1, it is characterised in that described step For: (1) weighs a certain amount of down fiber, at room temperature, adds the infiltration of a certain amount of distilled water;(2) weigh Reaction reagent: the concentration of zirconium salt solution is 0.4-3g/L;The concentration of organic acid is 0.1-9g/L;(3) then Reaction reagent adds in the eider down of infiltration, regulates bath raio 1: 100-200;(4) above-mentioned reactant is placed in three mouthfuls In flask, Stirring 2-6h in thermostat water bath, temperature is set as 40-90 DEG C;(5) by modification eider down Take out, distilled water wash 3 times;(6) modification eider down is dried in an oven, temperature 50 C, until drying i.e. Obtain described fire-retardant down fiber.
The most according to claim 4, the fire-retardant down fiber prepared, its limited oxygen index (LOI) reaches 28-38。
CN201610343313.6A 2016-05-20 2016-05-20 A kind of fire-retardant down fiber and preparation method thereof Active CN105780502B (en)

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Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN106567255A (en) * 2016-11-09 2017-04-19 南通纺织丝绸产业技术研究院 Colored flame-retardant and water-repellent natural silk fabric and preparation method thereof
CN107916573A (en) * 2017-11-30 2018-04-17 英泰时尚服饰(苏州)有限公司 A kind of preparation method of flame-retardant and anti-static finishing agent
CN114657801A (en) * 2022-05-07 2022-06-24 江苏鼎新印染有限公司 Dyeing process for improving dyeing reproducibility
CN115404700A (en) * 2022-10-17 2022-11-29 六安市皖兴羽绒有限公司 Preparation method of flame-retardant down fiber

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CN104358136A (en) * 2014-11-06 2015-02-18 天津工业大学 Modified down feather and preparation method thereof

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106567255A (en) * 2016-11-09 2017-04-19 南通纺织丝绸产业技术研究院 Colored flame-retardant and water-repellent natural silk fabric and preparation method thereof
CN106567255B (en) * 2016-11-09 2019-07-05 南通纺织丝绸产业技术研究院 A kind of coloured flame-retardant water repellent real silk fabric and preparation method thereof
CN107916573A (en) * 2017-11-30 2018-04-17 英泰时尚服饰(苏州)有限公司 A kind of preparation method of flame-retardant and anti-static finishing agent
CN114657801A (en) * 2022-05-07 2022-06-24 江苏鼎新印染有限公司 Dyeing process for improving dyeing reproducibility
CN115404700A (en) * 2022-10-17 2022-11-29 六安市皖兴羽绒有限公司 Preparation method of flame-retardant down fiber
CN115404700B (en) * 2022-10-17 2024-01-16 六安市皖兴羽绒有限公司 Preparation method of flame-retardant down fiber

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