CN105544226B - A kind of flame-retardant finishing method of wool fabric - Google Patents
A kind of flame-retardant finishing method of wool fabric Download PDFInfo
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- CN105544226B CN105544226B CN201610047595.5A CN201610047595A CN105544226B CN 105544226 B CN105544226 B CN 105544226B CN 201610047595 A CN201610047595 A CN 201610047595A CN 105544226 B CN105544226 B CN 105544226B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
- D06M16/003—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic with enzymes or microorganisms
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
- D06M13/282—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing phosphorus
- D06M13/292—Mono-, di- or triesters of phosphoric or phosphorous acids; Salts thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/10—Animal fibres
- D06M2101/12—Keratin fibres or silk
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/30—Flame or heat resistance, fire retardancy properties
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Abstract
The invention discloses a kind of flame-retardant finishing method of wool fabric, addition potassium dihydrogen phosphate aqueous solution pretreatment wool fabric, globular protein lightly crosslinked between wool fabric fibrocyte is evacuated, utilizes the progress of later stage ferment treatment；Enzymolysis pretreatment is carried out to wool fabric using by the mixing protease that ficin, pronase, bromelain are mixed to get, mixing protease runs through whole fibrous inside after being adsorbed onto wool surface, and spread along fiber and hydrolysis occurs, so that constantly hydrolysis inside wool fiber sebum layer, it is ensured that wool fiber internal layer is not subjected to destroy；Processing is finally modified for wool fabric using alkali protease, reduce the disulfide bond content in wool fiber, increase sulfhydryl content, improve the anti-flammability of wool fabric, the present invention can also improve the water-fastness degree of wool fabric simultaneously, whiteness and feel influence on wool is smaller, has higher economic benefit.
Description
Technical field：
The present invention relates to a kind of flame-retardant finishing method of wool fabric, belong to field of textile biotechnology.
Background technology：
Wool belongs to cyokeratin fibrous protein, containing more cysteine, cystine, Methiothepin etc., is
Cross linking polypeptides with floded molecule structure.Because although wool fabric belongs to combustible fibre, but its nitrogen content is high and pole
Easy moisture absorption, has a higher firing temperature, low burn heat with low flame temperature, thus there is higher anti-flammability.Manufactured sheep
Because functional character is improved during wool fabric, can add auxiliary agent reduces its anti-flammability, causes wool fabric easy firing, limits
The safe and practical property of wool.
The main component of wool is keratin, and it is made up of a variety of a-amino acid residues, and the latter can be coupled to twist
Long-chain molecule, thereon containing carboxyl, amido and hydroxyl etc., in intermolecular formation sat linkage and hydrogen bond etc..By Guang ammonia between long-chain
The cross linkage of the disulfide formation of acid is linked.Above-mentioned chemical constitution determines the characteristic of wool.If wool fibre macromolecular long-chain is by outer
β type extended patterns are transitioned into by α type spiral shapes when power stretches, external force returns to α types again after releasing, then its appearance is wool
Elongation strain and resilience are excellent.The stronger wettability power of wool is relevant with some groups on side chain.Wool it is more acidproof without
It is alkaline-resisting, it is due to that alkali easily decomposes disulfide group in wool cystine, is damaged hair quality.Oxidant can also destroy disulfide group and damage
Evil wool.
Flame-proof treatment is that mainly antiflaming finishing agent is acted on by heat-absorbing action, covering, suppresses even reaction, gas dilution is made
With and condensed phase it is fire-retardant, so as to reach fire-retardant purpose.It can be divided into according to the flame-proof treatment of water-fastness degree wool temporary
Flame-proof treatment, semi-durable flame-proof treatment, durable flame-retardant arrange.At present, mostly using durable flame-retardant finishing, it is arranged
Main two kinds of mode:
The first：Metal complex flame-proof treatment it mainly wool is hindered using the complex compound such as titanium, zirconium and carboxylic acid
Combustion arranges, and is to be most widely used and wool flame-retardant finishing the most ripe.This method can be resistant to the washing of 50 hard water and
Dry-cleaning, can assign fabric good flame retardant effect, and research is found, although the flame-proof treatment effect of titanium complex is complexed better than zirconium
The flame-proof treatment effect of thing, but easily cause the serious yellowing of fabric, the effect of taking of wool fabric is influenceed, therefore in practice
In, generally use zirconium complex carries out flame-proof treatment, but can contain a substantial amounts of poisonous huge sum of money in waste liquid after treatment by using the treatment method
Category, environmental pollution are serious.
Second：Microcapsules technology is a kind of new flame-retarded technology, and its preparation method is that fire retardant is passed through into physics side
After method is dispersed into power, wrapped up using method physically or chemically, form microcapsule flame retardant of the diameter at 1-150 μm,
Either using the very big inorganic matter of specific surface area as carrier, fire retardant is adsorbed in the space of inorganic carrier, and exquisiteness forms honeybee
Socket microcapsule flame retardant.The technology substantially improves the stability of fire retardant and its compatibility with resin, and expanding it should
Wool fabric is set to obtain the flame retardant effect of permanence with scope, and by control release technic, but feel is harder after arranging, such as
What makes wool fabric both obtain flame retardant effect, has the feel of softness again, still needs further to be studied.
Chinese invention patent CN200910025310.8 discloses a kind of method of improving wool fire-retardancy with biological enzyme, profit
Compound of the one kind containing primary amino radical and a large amount of P elements is grafted on wool with transglutaminase MTG catalytic action,
Wool fire-retardancy is improved, technological process includes：Pretreatment, the processing of phosphorous finishing agent, washing and drying containing MTG, are the present invention
Closest to prior art, by the wool yarn and fabric handled by the invented technology, fire resistance is improved, limit oxygen
Index is improved, but its complex treatment process, and technique is cumbersome, and fabric washability is poor, is unfavorable for industrialization promotion.
Chinese invention patent CN201210318957.1 discloses a kind of biological enzyme real silk fabric flame-retardant finishing method, category
In field of textile biotechnology, it is intended to during washability is high when solving conventional chemical methods real silk fabric flame-proof treatment, high temperature bakes
The defects of silk easy damaged, fibre whiteness easily decline.The invention is using tyrosinase to tyrosine residue in cocoon fiber
Characteristic with catalysed oxidn, tyrosine residue in fibroin albumen is oxidized to the stronger DOPA quinone structure of reactivity, promoted
Make the organophosphorous fire retardant containing primary amine groups that graft reaction occur with it, and the resistance of real silk fabric is improved by nitrogen-phosphorus cooperative effect
Effect is fired, realizes that biological enzyme silk flame-retardancy arranges.Compared with traditional chemical routes, entered using tyrosinase catalysis real silk fabric
Row flame retardant treatment, process energy consumption is low, efficiency high, pollution are few, is advantageous to environmental protection, silk refers generally to silk, including mulberry
Silk, tussah silk, ricinus silk, cassava silkwormsilk etc., silk category protein fibre, it is a kind of nitrogenous high-molecular compound, its
Single base of macromolecular is alpha amino acid.The general structure of alpha amino acid is RCH (NH) 2COOH, because its amino is located close to hydroxy acid
Alpha-carbon atom on, therefore referred to as alpha amino acid, itself has higher hygroscopicity, and this is more similar to wool fabric, but silkworm
Silk is made up of silk gum and fibroin, and outside, including fibroin, both are closely coupled for silk gum, and dead angle short texture, feel is coarse, typically
The soft fibroin structure of close structure gloss is obtained after needing degumming.
The content of the invention：
It is an object of the invention to provide a kind of flame-retardant finishing method of wool fabric, the pole of wool fabric can be significantly improved
Limited oxygen index, while both possessed efficient, gentle, green non-pollution the beneficial effect of general cellulase treatment, but also with operation
Simply, raw material is easy to get, small for wool fabric loss, the water-fastness degree of wool fabric is enough improved, to the whiteness and feel of wool
Less advantage is influenceed, there is higher economic benefit.
The present invention provides following technical scheme：
A kind of flame-retardant finishing method of wool fabric, including the pretreatment of biphosphate sodium water solution, protease pretreatment, egg
White enzyme modification processing step, wherein：
The first step：Sodium dihydrogen phosphate pre-processes：
Wool fabric is put into 50-70 points of immersion treatment in the biphosphate sodium water solution that concentration is 0.1-0.15mol/L
Clock, bath raio 1:20, soaking temperature is 20-25 DEG C；Drying is washed after sodium dihydrogen phosphate pretreatment processing；
Second step：Protease pre-processes：
Ficin, pronase, bromelain are mixed to get mixing protease, wool fabric is put into
Concentration is 1-1.5% mixed protein enzyme water-soluble middle immersion treatment 10-15 minutes, and soaking temperature is 50-60 DEG C, bath raio 1:
20-30；Drying is washed after protease pretreatment；
3rd step：Modification by Protease processing：
Wool fabric is put into basic protein enzyme aqueous solution, alkali protease addition is 0.5-0.7%, digests pH value
For 8.5-9, hydrolysis temperature is 60 DEG C, bath raio 1：20-30, alkali protease modified enzymolysis time are 25-30 minutes, protease
Drying is washed after modification.
Preferably, wool fabric is put into concentration in the first step sodium dihydrogen phosphate pre-treatment step is
Immersion treatment 50-70 minutes, bath raio 1 in 0.1mol/L biphosphate sodium water solution:20, soaking temperature is 20-25 DEG C.
Preferably, washed 2-3 times in the first step sodium dihydrogen phosphate pre-treatment step, drying temperature 50-60
℃。
Preferably, mixing protease is by ficin, pronase, spinach during the second step protease pre-processes
Trailing plants protease is according to weight than 1:2-3:1-2 mixing is formed.
Preferably, wool fabric is put into the egg mix that concentration is 1.2-1.5% in the second step protease pretreatment
The water-soluble middle immersion treatment of white matter enzyme 15 minutes, soaking temperature are 55-60 DEG C, bath raio 1:20-30.
Preferably, washed 1-2 times in the second step protease pretreatment, drying temperature is 70-75 DEG C.
Preferably, wool fabric is put into basic protein enzyme aqueous solution in the 3rd step Modification by Protease processing step
In, alkali protease addition is 0.6%, and enzymolysis pH value is 8.5, and hydrolysis temperature is 60 DEG C, bath raio 1：25, alkali protease
The modified enzymolysis time is 25 minutes.
Preferably, washed 3-4 times in the 3rd step Modification by Protease processing step, drying temperature is 80-90 DEG C.
Potassium dihydrogen phosphate aqueous solution is in acidity, and the pH value of 1% potassium dihydrogen phosphate is 4.6, and potassium dihydrogen phosphate is mainly used
In preparing buffer solution, measure arsenic, antimony, phosphorus, aluminium and iron, phosphorus titer is prepared, prepare the various culture mediums of haploid breeding, measure
Phos, alkaline acid enzyme vigor in serum, culture medium of bacterium serum test Leptospira etc. is prepared, it is industrial to be used as buffering
Agent, nutrient chemical；Also serve as the flavor enhancement that spills clearly of casate synthesis, the raw material of potassium metaphosphate processed, the nutrient chemical of brewer's yeast,
Hardening agent, leavening agent, fermentation assistant.Agriculturally it is used as efficient phosphorus potassium complex fertilizer.Present invention addition potassium dihydrogen phosphate aqueous solution
Wool fabric is pre-processed, globular protein lightly crosslinked between wool fabric fibrocyte is evacuated, utilizes later stage ferment treatment
Carry out, while the efficiency of enzyme and the washability of wool can be improved, and the scale structure of wool is limbered up, reduce intensity damage
Lose.
Ficin is coloured glaze base protease, and for its action site without specificity, pronase is mixed type protease,
Its action site is also without specificity, and bromelain is thiol protease, and action site is without specificity, and the present invention is using by without flower
The mixing protease that fruit protease, pronase, bromelain are mixed to get carries out enzymolysis pretreatment to wool fabric, mixes
Hop protein enzyme runs through whole fibrous inside after being adsorbed onto wool surface, and is spread along fiber and hydrolysis occurs and made
With constantly hydrolysis inside so that wool fiber sebum layer, wool fineness is obviously reduced after handling wool, and enzymolysis is from outward appearance to inner essence simultaneously
And even action, it is ensured that wool fiber internal layer is not subjected to destroy, and is ideal enzyme, while it is sulfydryl to divide disulphide,
The disulfide bond in wool is opened, it is easily attacked by alkali protease enzyme.
Processing is finally modified for wool fabric using alkali protease, the disulfide bond reduced in wool fiber contains
Amount, increase sulfhydryl content, improve the anti-flammability of wool fabric.
Beneficial effects of the present invention：
1. present invention addition potassium dihydrogen phosphate aqueous solution pretreatment wool fabric, will slightly be handed between wool fabric fibrocyte
The globular protein evacuation of connection, using the progress of later stage ferment treatment, while can improve the efficiency of enzyme and the washability of wool, and
So that the scale structure of wool limbers up, loss of strength is reduced.
2. the present invention is using the mixing protease being mixed to get by ficin, pronase, bromelain
Enzymolysis pretreatment is carried out to wool fabric, mixing protease runs through whole fibrous inside after being adsorbed onto wool surface, and
And spread along fiber and hydrolysis occurs so that constantly hydrolysis inside wool fiber sebum layer, handle wool after wool
Fineness is obviously reduced, and enzymolysis is from outward appearance to inner essence and even action, it is ensured that wool fiber internal layer is not subjected to destroy, and is ideal
Enzyme, while it is sulfydryl to divide disulphide, opens the disulfide bond in wool, it is easily attacked by alkali protease enzyme.
3. the present invention is modified processing using alkali protease for wool fabric, the disulfide bond in wool fiber is reduced
Content, increase sulfhydryl content, improve the anti-flammability of wool fabric.
4. the inventive method had both possessed efficient, gentle, green non-pollution the beneficial effect of general cellulase treatment, have again
Standby operation is simple, and raw material is easy to get, small for wool fabric loss, the water-fastness degree of wool fabric is enough improved, to the whiteness of wool
And feel influences less advantage, has higher economic benefit.
Brief description of the drawings：
Fig. 1：Influence of the sodium dihydrogen phosphate concentration of aqueous solution for wool fabric flame retardant effect；
Fig. 2：Influence of the sodium dihydrogen phosphate aqueous solution soaking processing time for wool fabric flame retardant effect；
Fig. 3：Influence of the sodium dihydrogen phosphate aqueous solution soaking treatment temperature for wool fabric flame retardant effect；
Fig. 4：Influence of the mixing protease mass concentration for wool fabric flame retardant effect；
Fig. 5：Influence of the mixing protease soaking temperature for wool fabric flame retardant effect；
Fig. 6：Influence of the alkali protease addition for wool fabric flame retardant effect；
Fig. 7：Influence of the alkali protease enzymolysis time for wool fabric flame retardant effect.
Embodiment：
Embodiments of the invention are described in detail below, the present embodiment is carried out lower premised on inventive technique scheme
Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following realities
Apply example.The experimental program of unreceipted actual conditions in embodiment, the condition proposed by generally according to normal condition or manufacturer
Implement.
Wool fabric is all-wool gabardine fabric used by the embodiment of the present invention, 220g/m2
Embodiment one：
A kind of flame-retardant finishing method of wool fabric, including following operating procedure：
The first step：Sodium dihydrogen phosphate pre-processes：
Wool fabric is put into immersion treatment 50 minutes, bath raio in the biphosphate sodium water solution that concentration is 0.1mol/L is
1:20, soaking temperature is 20 DEG C；Drying is washed after sodium dihydrogen phosphate pretreatment processing；
Wherein wash 2 times, drying temperature is 50 DEG C；
Second step：Protease pre-processes：
Wool fabric is put into the water-soluble middle immersion treatment of mixed protein enzyme 10 minutes that concentration is 1%, soaking temperature is
50 DEG C, bath raio 1:20；Drying is washed after protease pretreatment；
Wherein, mixing protease by ficin, pronase, bromelain according to weight than 1:2:1 is mixed
Close and form；
Washing 1 time, drying temperature are 70 DEG C；
3rd step：Modification by Protease processing：
Wool fabric is put into basic protein enzyme aqueous solution, alkali protease addition is 0.5%, and enzymolysis pH value is
8.5, hydrolysis temperature is 60 DEG C, bath raio 1：20, the alkali protease modified enzymolysis time is 25 minutes, after Modification by Protease processing
Washing drying；
Wherein wash 3 times, drying temperature is 80 DEG C.
Embodiment two
A kind of flame-retardant finishing method of wool fabric, including following operating procedure：
The first step：Sodium dihydrogen phosphate pre-processes：
Wool fabric is put into immersion treatment 70 minutes, bath raio in the biphosphate sodium water solution that concentration is 0.15mol/L
For 1:20, soaking temperature is 25 DEG C；Drying is washed after sodium dihydrogen phosphate pretreatment processing；
Wherein wash 3 times, drying temperature is 60 DEG C；
Second step：Protease pre-processes：
Wool fabric is put into the water-soluble middle immersion treatment of mixed protein enzyme 15 minutes that concentration is 1.5%, soaking temperature
For 60 DEG C, bath raio 1:30；Drying is washed after protease pretreatment；
Wherein, mixing protease by ficin, pronase, bromelain according to weight than 1:3:2 is mixed
Close and form；
Washing 2 times, drying temperature are 75 DEG C；
3rd step：Modification by Protease processing：
Wool fabric is put into basic protein enzyme aqueous solution, alkali protease addition is 0.7%, and enzymolysis pH value is 9,
Hydrolysis temperature is 60 DEG C, bath raio 1：30, the alkali protease modified enzymolysis time is 30 minutes, is washed after Modification by Protease processing
Drying；
Wherein wash 4 times, drying temperature is 90 DEG C.
Embodiment three
A kind of flame-retardant finishing method of wool fabric, including following operating procedure：
The first step：Sodium dihydrogen phosphate pre-processes：
Wool fabric is put into immersion treatment 70 minutes, bath raio in the biphosphate sodium water solution that concentration is 0.1mol/L is
1:20, soaking temperature is 20 DEG C；Drying is washed after sodium dihydrogen phosphate pretreatment processing；
Wherein wash 3 times, drying temperature is 50 DEG C；
Second step：Protease pre-processes：
Wool fabric is put into the water-soluble middle immersion treatment of mixed protein enzyme 15 minutes that concentration is 1%, soaking temperature is
50 DEG C, bath raio 1:30；Drying is washed after protease pretreatment；
Wherein, mixing protease by ficin, pronase, bromelain according to weight than 1:2:2 is mixed
Close and form；
Washing 1 time, drying temperature are 75 DEG C；
3rd step：Modification by Protease processing：
Wool fabric is put into basic protein enzyme aqueous solution, alkali protease addition is 0.5%, and enzymolysis pH value is 9,
Hydrolysis temperature is 60 DEG C, bath raio 1：20, the alkali protease modified enzymolysis time is 30 minutes, is washed after Modification by Protease processing
Drying；
Wherein wash 3 times, drying temperature is 90 DEG C.
Example IV
A kind of flame-retardant finishing method of wool fabric, including following operating procedure：
The first step：Sodium dihydrogen phosphate pre-processes：
Wool fabric is put into immersion treatment 50 minutes, bath raio in the biphosphate sodium water solution that concentration is 0.15mol/L
For 1:20, soaking temperature is 25 DEG C；Drying is washed after sodium dihydrogen phosphate pretreatment processing；
Wherein wash 2 times, drying temperature is 60 DEG C；
Second step：Protease pre-processes：
Wool fabric is put into the water-soluble middle immersion treatment of mixed protein enzyme 15 minutes that concentration is 1%, soaking temperature is
50 DEG C, bath raio 1:30；Drying is washed after protease pretreatment；
Wherein, mixing protease by ficin, pronase, bromelain according to weight than 1:2:1 is mixed
Close and form；
Washing 2 times, drying temperature are 70 DEG C.
3rd step：Modification by Protease processing：
Wool fabric is put into basic protein enzyme aqueous solution, alkali protease addition is 0.7%, and enzymolysis pH value is
8.5, hydrolysis temperature is 60 DEG C, bath raio 1：30, the alkali protease modified enzymolysis time is 25 minutes, after Modification by Protease processing
Washing drying；
Wherein wash 4 times, drying temperature is 80 DEG C.
Embodiment five
A kind of flame-retardant finishing method of wool fabric, including following operating procedure：
The first step：Sodium dihydrogen phosphate pre-processes：
Wool fabric is put into immersion treatment 50 minutes, bath raio in the biphosphate sodium water solution that concentration is 0.1mol/L is
1:20, soaking temperature is 20 DEG C, and drying is washed after sodium dihydrogen phosphate pretreatment processing；
Wherein wash 3 times, drying temperature is 50 DEG C；
Second step：Protease pre-processes：
Wool fabric is put into the water-soluble middle immersion treatment of mixed protein enzyme 15 minutes that concentration is 1.2%, soaking temperature
For 55 DEG C, bath raio 1:20；Drying is washed after protease pretreatment；
Wherein, mixing protease by ficin, pronase, bromelain according to weight than 1:2:1 is mixed
Close and form；
Washing 1 time, drying temperature are 75 DEG C.
3rd step：Modification by Protease processing：
Wool fabric is put into basic protein enzyme aqueous solution, alkali protease addition is 0.6%, and enzymolysis pH value is
8.5, hydrolysis temperature is 60 DEG C, bath raio 1：25, the alkali protease modified enzymolysis time is 25 minutes, after Modification by Protease processing
Washing drying；
Wherein wash 4 times, drying temperature is 80 DEG C.
Embodiment six
A kind of flame-retardant finishing method of wool fabric, including following operating procedure：
The first step：Sodium dihydrogen phosphate pre-processes：
Wool fabric is put into immersion treatment 60 minutes, bath raio in the biphosphate sodium water solution that concentration is 0.1mol/L is
1:20, soaking temperature is 25 DEG C, and drying is washed after sodium dihydrogen phosphate pretreatment processing；
Wherein wash 3 times, drying temperature is 50 DEG C；
Second step：Protease pre-processes：
Wool fabric is put into the water-soluble middle immersion treatment of mixed protein enzyme 15 minutes that concentration is 1.2%, soaking temperature
For 60 DEG C, bath raio 1:25；Drying is washed after protease pretreatment；
Wherein, mixing protease by ficin, pronase, bromelain according to weight than 1:3:1 is mixed
Close and form；
Washing 2 times, drying temperature are 70 DEG C.
3rd step：Modification by Protease processing：
Wool fabric is put into basic protein enzyme aqueous solution, alkali protease addition is 0.6%, and enzymolysis pH value is
8.5, hydrolysis temperature is 60 DEG C, bath raio 1：25, the alkali protease modified enzymolysis time is 25 minutes, after Modification by Protease processing
Washing drying；
Wherein wash 3 times, drying temperature is 80 DEG C.
Embodiment seven
A kind of flame-retardant finishing method of wool fabric, including following operating procedure：
The first step：Sodium dihydrogen phosphate pre-processes：
Wool fabric is put into immersion treatment 60 minutes, bath raio in the biphosphate sodium water solution that concentration is 0.1mol/L is
1:20, soaking temperature is 20 DEG C, and drying is washed after sodium dihydrogen phosphate pretreatment processing；
Wherein wash 2 times, drying temperature is 60 DEG C；
Second step：Protease pre-processes：
Wool fabric is put into the water-soluble middle immersion treatment of mixed protein enzyme 15 minutes that concentration is 1.3%, soaking temperature
For 55 DEG C, bath raio 1:20；Drying is washed after protease pretreatment；
Wherein, mixing protease by ficin, pronase, bromelain according to weight than 1:2:2 is mixed
Close and form；
Washing 2 times, drying temperature are 70 DEG C.
3rd step：Modification by Protease processing：
Wool fabric is put into basic protein enzyme aqueous solution, alkali protease addition is 0.6%, and enzymolysis pH value is
8.5 hydrolysis temperature is 60 DEG C, bath raio 1：25, the alkali protease modified enzymolysis time is 25 minutes, after Modification by Protease processing
Washing drying；
Wherein wash 4 times, drying temperature is 90 DEG C.
Limited oxygen index determines：Tested using HC-2 type oxygen index measurers according to GB5454-1997；
Testing vertical flammability：Ability meter is immersed using YG815 type normal beam techniques to test according to GB5456-1985.
Wool fabric fracture strength determines：Using 026D-250 types imported electronic fabric strength tester according to GB/T 39231-1997
Measure.
Wool fabric measuring brightness：Determined using WSD-111 type whiteness instrument.
Table one：Influence after the processing of embodiment method to fabrics flame resistance and strength and whiteness
As shown in Table 1, after the inventive method is handled, the flame retardant effect of wool fabric is greatly increased,
Limited oxygen index significantly improves, and the carbon length of fabric also has lifting, while fabric whiteness improves a lot, and this is due to that working solution uses
During cause wool fabric above impurity come off, improve and enter for.The warp-wise strength of fabric does not arrange after flame-proof treatment
It has been declined that, but the fabric after strength reduces does not influence wearability, and its strength is reduced and made moderate progress compared with prior art.
Biphosphate sodium water solution pre-processes the influence experiment in wool fabric flame retardant effect
Experiment one：Influence of the sodium dihydrogen phosphate concentration of aqueous solution for wool fabric flame retardant effect
With the methods described of embodiment seven, sodium dihydrogen phosphate concentration of aqueous solution is for sheep during inquiring into the processing first step
The influence of woolen flame retardant effect.
According to Fig. 1 it will be seen that with the increase of sodium dihydrogen phosphate concentration of aqueous solution, its limited oxygen index is on
Rise, but after sodium dihydrogen phosphate concentration of aqueous solution is more than 0.15mol/L, its limited oxygen index drops with the rising of concentration
Low, this is probably because sodium dihydrogen phosphate concentration of aqueous solution is excessive, and the pH of its solution is served brokenly with rising to wool fiber
Bad effect, reduces its limited oxygen index, and the present invention uses sodium dihydrogen phosphate concentration of aqueous solution as 0.1-0.15mol/L.
Experiment two：Influence of the sodium dihydrogen phosphate aqueous solution soaking processing time for wool fabric flame retardant effect
With the methods described of embodiment seven, when sodium dihydrogen phosphate aqueous solution soaking is handled during the discussion processing first step
Between influence for wool fabric flame retardant effect.
According to Fig. 2 it will be seen that with the postponement of sodium dihydrogen phosphate aqueous solution soaking processing time, its wool fabric
Limited oxygen index with increase, after the immersion treatment time reaches 50-70 minutes, the increased frequency of its limited oxygen index is notable
Reduce, consider from industrial cost and time cost angle, the present invention uses sodium dihydrogen aqueous solution soaking processing time
For 50-70 minutes.
Experiment three：Influence of the sodium dihydrogen phosphate aqueous solution soaking treatment temperature for wool fabric flame retardant effect
With the methods described of embodiment seven, sodium dihydrogen phosphate aqueous solution soaking processing temperature during the processing first step is inquired into
Spend the influence for wool fabric flame retardant effect.
According to Fig. 3, it will be seen that when soaking temperature is less than 25 DEG C, with the rising of soaking temperature, wool is knitted
The limited oxygen index of thing is with rising, and after temperature is more than 25 DEG C, its limited oxygen index reduces with the rising of temperature, and this can
Can be due to early stage as temperature rises, wool fabric and the comprehensive engagement of biphosphate sodium water solution and its activity is higher, but
It is after temperature reach a certain height, the biphosphate sodium water solution under high temperature has destruction to wool fabric, reduces on the contrary
The limited oxygen index of wool fabric, the flame-retardant nature of wool fiber is reduced, so process of the present invention uses sodium dihydrogen phosphate
The aqueous solution is 20-25 DEG C to the temperature of wool fabric immersion treatment.
Protease Pretreatment Test
Experiment four：Influence of the mixing protease mass concentration for wool fabric flame retardant effect
With the methods described of embodiment seven, mixing protease mass concentration is for wool during inquiring into the processing second step
The influence of fabrics flame resistance effect.
According to Fig. 4 it will be seen that with the rising of mixed protein mass concentration, the limited oxygen index of wool fabric
Also with rising, enzyme fully acts on wool fabric, passes through progressively fully carrying out for enzymolysis, mixing protease mass concentration
Limited oxygen index increase almost increase in direct ratio with wool fabric, but after mixing protease mass concentration is more than 1,
The limited oxygen index increase of its wool fabric is slow, tends towards stability, it may be possible to because the usage amount of mixing protease tends to saturation,
Its effect tends to complete；After mixing protease mass concentration is more than 2%, the limited oxygen index of its wool fabric is with egg mix
The rising of white enzyme mass concentration and reduce, this is probably due to mixing protease excessive addition, is caused mutual between protease
Enzymolysis, its effect to wool fabric is reduced, so as to reduce the raising of wool fabric flame-retardant nature, so of the invention
Process uses mixing protease mass concentration as 1-1.5%.
Experiment five：Influence of the mixing protease soaking temperature for wool fabric flame retardant effect
With the methods described of embodiment seven, mixing protease soaking temperature is for wool during inquiring into the processing second step
The influence of fabrics flame resistance effect.
According to Fig. 5, we can draw, mixing protease soaking temperature for wool fabric flame-retardant nature early stage with
The rising of soaking temperature and improve, after soaking temperature reaches 60 DEG C, its anti-flammability reduces with the rising of temperature, this may
Be due to that the activity of enzyme changes itself with the influence of temperature, during lower temperature, as temperature rises, enzyme activity enhancing, when up to
To after certain temperature range, with the raising of temperature, its enzyme inactivation, reactivity is reduced, so the present invention uses egg mix
White enzyme soaking temperature is 50-60 DEG C.
Modification by Protease processing experiment
Experiment six：Influence of the alkali protease addition for wool fabric flame retardant effect
With the methods described of embodiment seven, inquire into the processing three step process neutral and alkali protease addition and knitted for wool
The influence of thing flame retardant effect.
According to Fig. 6 it will be seen that pass between the addition of alkali protease and the limited oxygen index of wool fabric
Similar influence of the mixing protease mass concentration of figure four for wool fabric flame retardant effect of system, its principle is similar, so of the invention
Alkali protease addition is used as 0.5-0.7%.
Experiment seven：Influence of the alkali protease enzymolysis time for wool fabric flame retardant effect
With the methods described of embodiment seven, the processing three step process neutral and alkali protease hydrolyzed time is inquired into for wool
The influence of fabrics flame resistance effect.
According to Fig. 7 it will be seen that with the increase of alkaline protein enzymolysis time, the limit oxygen of its wool fabric refers to
Number is gradually increasing, and its flame-retardant nature is also gradually increasing.After the time certain limit is reached, the increase of its limited oxygen index tends to be flat
Delay to keeping constant, in order to which economic benefit considers, the present invention uses alkali protease enzymolysis time as 25-30 minutes.
Above content is only the better embodiment of the present invention, for one of ordinary skill in the art, according to the present invention
Thought, there will be changes, this specification content should not be construed as to this hair in specific embodiments and applications
Bright limitation.
Claims (8)
- A kind of 1. flame-retardant finishing method of wool fabric, it is characterised in that：Including the pretreatment of biphosphate sodium water solution, protease Pretreatment, Modification by Protease processing step, wherein：The first step：Sodium dihydrogen phosphate pre-processes：Wool fabric is put into immersion treatment 50-70 minutes, bath in the biphosphate sodium water solution that concentration is 0.1-0.15mol/L Than for 1:20, soaking temperature is 20-25 DEG C；Drying is washed after sodium dihydrogen phosphate pretreatment processing；Second step：Protease pre-processes：Ficin, pronase, bromelain are mixed to get mixing protease, wool fabric is put into concentration For immersion treatment 10-15 minutes in 1-1.5% mixed protein enzyme aqueous solution, soaking temperature is 50-60 DEG C, bath raio 1:20- 30；Drying is washed after protease pretreatment；3rd step：Modification by Protease processing：Wool fabric is put into basic protein enzyme aqueous solution, alkali protease addition is 0.5-0.7%, and enzymolysis pH value is 8.5-9, hydrolysis temperature are 60 DEG C, bath raio 1：20-30, alkali protease modified enzymolysis time are 25-30 minutes；Drying is washed after Modification by Protease processing.
- A kind of 2. flame-retardant finishing method of wool fabric according to claim 1, it is characterised in that：The first step phosphoric acid Wool fabric is put into the biphosphate sodium water solution that concentration is 0.1mol/L at immersion in dihydro sodium solution pre-treatment step Manage 50-70 minutes, bath raio 1:20, soaking temperature is 20-25 DEG C.
- A kind of 3. flame-retardant finishing method of wool fabric according to claim 1, it is characterised in that：The first step phosphoric acid Washed 2-3 times in dihydro sodium solution pre-treatment step, drying temperature is 50-60 DEG C.
- A kind of 4. flame-retardant finishing method of wool fabric according to claim 1, it is characterised in that：The second step albumen Enzyme pretreatment in mixing protease by ficin, pronase, bromelain according to weight than 1:2-3:1-2 is mixed Close and form.
- A kind of 5. flame-retardant finishing method of wool fabric according to claim 1, it is characterised in that：The second step albumen Wool fabric is put into immersion treatment 15 minutes, leaching in the mixed protein enzyme aqueous solution that concentration is 1.2-1.5% in enzyme pretreatment It is 55-60 DEG C to steep temperature, bath raio 1:20-30.
- A kind of 6. flame-retardant finishing method of wool fabric according to claim 1, it is characterised in that：The second step albumen Washed 1-2 times in enzyme pretreatment, drying temperature is 70-75 DEG C.
- A kind of 7. flame-retardant finishing method of wool fabric according to claim 1, it is characterised in that：The 3rd step albumen Wool fabric is put into basic protein enzyme aqueous solution in enzyme modification processing step, alkali protease addition is 0.6%, enzymolysis PH value is 8.5, and hydrolysis temperature is 60 DEG C, bath raio 1：25, the alkali protease modified enzymolysis time is 25 minutes.
- A kind of 8. flame-retardant finishing method of wool fabric according to claim 1, it is characterised in that：The 3rd step albumen Washed 3-4 times in enzyme modification processing step, drying temperature is 80-90 DEG C.
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| CN110965325A (en) * | 2019-12-10 | 2020-04-07 | 山东芦氏阻燃纤维科技有限公司 | Continuous processing method of flame-retardant protein short fiber and flame-retardant protein short fiber obtained by same |
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| CN102965958A (en) * | 2012-10-31 | 2013-03-13 | 江南大学 | Wool product two-bath process anti-felting treatment technology based on composite bio-enzyme |
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