CN104818623A - Flax short fiber pre-treatment method - Google Patents
Flax short fiber pre-treatment method Download PDFInfo
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Abstract
The invention provides a flax short fiber pre-treatment method. In the method, under the effect of ultrasonic wave, the flax short fiber is subjected to degumming pre-treatment with a composite bio-enzyme with combination of a mediator N-hydroxyl-N-phenylpropanamide. The method includes following steps: preparing the composite bio-enzyme, scouring the flax short fiber under the condition of the composite bio-enzyme/mediator system, blanching the flax short fiber, water-washing the flax short fiber, dewatering the flax short fiber and air-drying the flax short fiber. In the invention, the conditions of scouring the flax short fiber are mild so that the method is less in damage on fibers and is short in treatment time. The treated flax short fiber is better than a flax short fiber, which is pre-treated only with the bio-enzyme, in physical performance indexes (such as weight loss ratio, breaking strength, whiteness and split degree). The pre-treatment method reduces the amount of the bio-enzyme by 1.8-2.5% owf and saves process time by 9-20 min. The method achieves that an acid for carrying out the pre-treatment on the fiber is unnecessary anymore during the degumming process of fiber, reduces treatment of pre-treatment waste water and the use amount of sodium hydroxide, and reduces emission of scouring waste water.
Description
Technical field
The present invention relates to a kind of towy preprocess method, particularly one is under ul-trasonic irradiation, adopts compound biological enzyme to carry out in conjunction with amboceptor N-hydroxy-N-phenyl propionamide rescutched tow pretreated method of coming unstuck, belongs to textile technology field.
Background technology
Well-known linen fibre have the good reputation of " fiber queen ", in the middle of numerous environmental protection ecological fiber, its fabric except having natural antibacterial, shield ultraviolet radiation, moisture absorbing and sweat releasing, be not stained with skin, except adsorb peculiar smell and the performance such as wear-resisting, also there is simple rough, the style such as practicality naturally.
Only have cellulose to be the active ingredient of textile industry in flax composition, except cellulose, in linen fibre, also have hemicellulose, lignin, pectin, adipocere matter and ash to grade accompaniment.In linen fibre, non-fiber content accounts for about 30%, and these impurity directly affect the physical and mechanical properties of linen fibre, and makes its feel coarse, and color and luster turns to be yellow.For improving the wearability of the spinning property of linen fibre, yarn and fabric, yarn forming performance, fabric, need to come unstuck micronization processes to flax, but these non-cellulose accompaniments can not excessively be removed again, otherwise can cause damage to process of fiber, bring difficulty to product development.
Current linen fibre Degumming method is mainly divided into three major types: chemical method, physical-chemical process and microbial method.The degumming technology that current linen fibre is conventional is still chemical degumming law, and chemical method is that chance for utilization dissolves pin matter.Existing more employing alkaline scouring, different from the stability of colloid to alkali according to cellulose, by colloid removal, its chemical Degumming process is divided into the oxidation Decomposition of the infiltration of alkali lye, the swelling of fiber and fiber.Its technological process is long, length consuming time, and energy consumption is large, and wastewater treatment is improper just to pollute the environment.
Physical-chemical process utilizes the colloid in physics and chemistry acting in conjunction removal fiber.There is ultrasonic wave and High Temperature High Pressure kiering method at present.Ultrasonic wave kiering method utilizes hyperacoustic physical action that fibrous refinement is separated, and its cavitation improves the reaction rate of alkali lye, for the rapid emulsification of colloid molecular energy diffused out and dispersion, avoid again being adsorbed on fiber, thus shorten the kiering time, reduce reagent dosage, and improve the quality of products.The alkali number of High Temperature High Pressure kiering method configuration can reduce than under normal pressure, kiering time shorten.Linen fibre after high temperature high pressure process, not only physical property improves.The Impurity removal of fiber is comparatively thorough, and flax fiber separation index, pliability significantly improve, and spinnability is also improved.
Microbial method and enzyme come unstuck, and utilize fermentable, produce pectase, pectase acts on insoluble pectin and makes it to become soluble pectin, then be subject to the hydrolysis of pectinesterase, generate the materials such as pectic acid, pectic acid is generated the materials such as galacturonic acid by the enzyme hydrolysis of galactosan aldehydic acid further.Pectic substance is that fibre bundle is decomposed by the result of decomposed, reaches object of coming unstuck.But the enzyme activity cultivated at present is not high, depend merely on the enzyme residual gum content that comes unstuck higher, and according to the mechanical agitation that continuous print is more violent in ferment treatment process, the hydrolysate after colloid and enzyme effect not easily departs from from fiber, is unfavorable for that beautifying liquid permeates to fibrous inside like this.
Based on chemical method and microorganism pluses and minuses, the present invention, under ul-trasonic irradiation, adopts compound biological enzyme to come unstuck preliminary treatment to rescutched tow in conjunction with amboceptor N-hydroxy-N-phenyl propionamide, achieves good effect.
Summary of the invention
The pretreated method of the rescutched tow that the technical problem to be solved in the present invention is to provide a kind of energy-saving and environment friendly, efficiency of coming unstuck is high.
Technical problem to be solved by this invention is achieved through the following technical solutions:
A kind of towy preprocess method, is characterized in that, under ul-trasonic irradiation, adopts compound biological enzyme to come unstuck preliminary treatment to rescutched tow in conjunction with amboceptor N-hydroxy-N-phenyl propionamide;
Wherein, described compound biological enzyme is made up of laccase, acid pectase and zytase.
In the present invention, preferably, specifically comprise the following steps:
(1) preparation of compound biological enzyme
Take laccase 10-20 part, acid pectase 10-20 part, zytase 30-50 part, is uniformly mixed, obtains final product;
(2) the rescutched tow kiering under compound biological enzyme-mediator system condition
Under ul-trasonic irradiation, rescutched tow is carried out kiering in kiering liquid, the mass ratio of rescutched tow and kiering liquid is 1:30, and control kiering temperature at 45-75 DEG C, the kiering processing time is 40-90 minute; Described kiering liquid is made up of following component: compound biological enzyme, amboceptor N-hydroxy-N-phenyl propionamide, fast penetrant T aerosol-OT salt and water;
(3) bleach
Rescutched tow after kiering is added containing sodium metasilicate 3.0g/L, in the bleaching liquid of natrium carbonicum calcinatum 2.0g/L and hydrogen peroxide 4.0g/L, under 80 DEG C of conditions, bleaching 60min;
(4) wash, dewater and dry
By the cold wash twice of the hot water wash twice of flax tow Wesy 80-90 DEG C after bleaching, 20-30 DEG C, dry to constant weight at 100-105 DEG C after dehydration.
In the present invention, preferably, the relatively described towy mass fraction of step (2) described compound biological enzyme is 4-8%, the relatively described towy mass fraction of described amboceptor N-hydroxy-N-phenyl propionamide is 0.9-2.5%, the relatively described towy mass fraction of fast penetrant T aerosol-OT salt is 0.5-1.5%, and the pH value of described kiering liquid is 3-5.
In the present invention, preferably, step (3) described hydrogen peroxide is the hydrogen peroxide of concentration 30%.
In the present invention, preferably, described hyperacoustic generator working power is AC220V, and operating frequency is 40KHz, and power output is 40W, and the applying groove of ultrasonic oscillator is of a size of 300mm × 150mm × 100mm.
In the present invention, preferably, the following method of described N-hydroxy-N-phenyl propionamide prepares:
(1) synthesis of intermediate phenylhydroxylamine
By nitrobenzene, ammonium chloride and water are placed in flask according to mass ratio 1.5-3:0.5-1.5:30-34, mechanical agitator is installed, thermometer, be heated to 57-60 DEG C while stirring, then several times zinc powder is added in reactant liquor, continue after zinc powder adds to stir 30min, until react completely, without dense bitter almond odor, with circulating water type vavuum pump suction filtration system fast filtering removing reaction waste residue, the residue washed with water again in flask is poured funnel into and is filtered, then add in filtrate and slowly add sodium chloride, form sodium chloride saturated solution, stir while adding, yellow needles is produced gradually in filtrate, suction filtration obtains phenylhydroxylamine crude product again, then make it to dissolve with a small amount of carrene, the impurity such as removing inorganic salts wherein, add benzinum again, after stirring, suction filtration obtains phenylhydroxylamine white crystal, then be recrystallized with carrene and benzinum,
(2) synthesis of N-hydroxy-N-phenyl propionamide
The phenylhydroxylamine oxolane of step (1) is dissolved in flask, then adds the pasty liquid of sodium bicarbonate and water, load onto mechanical agitator, thermometer and dropping funel, adjusting rotary speed, reactant liquor is stirred.Reaction is placed in cryosel bath, makes reacting liquid temperature maintain 0 DEG C to-10 DEG C, then from dropping funel, slowly instills acylating reagent several times, and the mol ratio controlling phenylhydroxylamine and acylating reagent is 1:0.8-1.2, after acylating reagent adds, continues to stir 60min.Then in reactant liquor, add sodium hydroxide solution and benzinum, after stratification, separate organic phase and inorganic phase with separatory funnel; Divide with sodium hydroxide solution again and wash organic phase three times, separate inorganic phase, above inorganic phase solution is merged, with dichloromethane extraction twice, use salt acid for adjusting pH value to about 6.0 again, then with Rotary Evaporators, dichloromethane solution is steamed to original about 1/5th, then add benzinum, obtain crystallized product N-hydroxy-N-phenyl propionamide through cooling.
In the present invention, preferably, step (1) zinc powder adds reactant liquor according to the mass ratio 1-1.5:1 of zinc powder and nitrobenzene at every turn, and controls zinc powder and add the temperature of rear reactant liquor at 57-68 DEG C.
In the present invention, preferably, the mass ratio of step (2) described phenylhydroxylamine, sodium bicarbonate and water is 8-10:14-16:9-11, and the mass fraction of described sodium hydroxide solution is 20%; Described acylating reagent is propionyl chloride.
Comparatively traditional handicraft is low for the wastewater treatment load of bast fiber fabrics cellulase treatment, but processing cost is high and reaction rate is low, hinders its application in textile industry.Ultrasonic technology is introduced biology enzyme processing, can greatly improve enzyme usefulness, and then improve reaction rate.Be mainly reflected in: accelerate enzyme to matrix/fiber surface motion; The strong stirring of liquid-solid interface contributes to the location of enzyme at fiber surface; Prevent biology enzyme from assembling; Contribute to the removal of conversion zone enzymolysis product.Amboceptor N-hydroxy-N-phenyl propionamide is introduced on the other hand in cellulase treatment fiber process, laccase can be oxidized the lignin model compounds of non-phenolic under the existence of some molecular compound (being called amboceptor mediator), because amboceptor can be formed active high and have the intermediate of certain stability under the effect of enzyme, and intermediate can obtain electron transmission and makes lignin degradation to lignin molecule from oxygen molecule, and then remove lignin.And the aromatic containing the heterocyclic compound of N-OH group or this group alternatively base can play electronics transfer vector, promote the residual lignin that polyphenol oxidase-laccase is oxidized non-phenolic lignin model compounds or removes in cellulose.
The present invention adopts complex enzyme-mediator system technique to carry out rescutched tow pre-treatment, utilizes the synergy of respective biology enzyme, adopts zytase, acid pectase, laccase three kinds of composite uses of biology enzyme, produces synergistic function; Further, add amboceptor N-hydroxy-N-phenyl propionamide has reacted electronics transfer vector effect to this enzymeization, promotion polyphenol oxidase-laccase is oxidized the residual lignin that non-phenolic lignin model compounds helps to remove in linen fibre.Adding of surfactant fast penetrant T aerosol-OT salt, more further synergistic effect is played to enzyme.
Specifically in the present invention:
Laccase (analyzing pure): Beijing Hua Maike biotechnology Co., Ltd.CAS numbers: 80498-15-3 laccase is copper-containing metal enzyme, has four copper atoms in molecule.The typical reaction of laccase is oxidation phenolic compound, along with reducing molecular oxygen Cheng Shui in course of reaction.
Acid pectase (analyzing pure): Zhaodong Sun Shine Enzyme Co., Ltd..Can be used for come unstuck preliminary treatment and the boiling-off additive of textile fabric.Acidproof, can use under sour environment, have good place to go to act on to inoglia, and less to native cellulose fibre damage, fiber can be kept to have good physical property.
Zytase (analyzing pure): Jin Sui bio tech ltd, Shanghai.Can single-minded degradation of hemicellulose xylan be the general name of one group of enzyme of xylo-oligosaccharide and wood sugar, be mainly used in destarch and the kiering of the bast fiber fabrics such as ramie, flax, jute at field of textiles, can effective degradation of hemicellulose class impurity, make it dissolving.
N-hydroxy-N-phenyl propionamide, Propiohydroxamic acid, N-phenyl-(8CI), CAS RegistryNumber:27687-56-5 (oneself synthesis).
Fast penetrant T aerosol-OT salt, Sodium diethylhexyl sulfosuccinate, CASRegistry Number:577-11-7: Linyi City Lanshan District Lv Sen Chemical Co., Ltd..
Relative to prior art, beneficial effect of the present invention is mainly reflected in:
The towy kiering treatment conditions of the present invention are gentle, little to fibre damage, processing time is short, towy physical performance index (reduction rate, fracture strength, whiteness and fiber thinness) after process is better than the rescutched tow being used alone biology enzyme pre-treatment, biological enzyme amount 1.8 ~ 2.5%owf can be reduced, save process time 9 ~ 20min.Present invention achieves and no longer with acid, preliminary treatment be carried out to fiber in fiber degumming process, decrease the process of pretreated waste water, decrease the use of NaOH, reduce the discharge of kiering waste water.
Accompanying drawing explanation
Fig. 1 is the infrared spectrogram of phenylhydroxylamine;
Fig. 2 is the nmr spectrum chart of phenylhydroxylamine;
Fig. 3 is the infrared spectrogram of N-hydroxy-N-phenyl propionamide;
Fig. 4 is the nmr spectrum chart of N-hydroxy-N-phenyl propionamide.
Detailed description of the invention
Further describe the present invention below in conjunction with specific embodiment, advantage and disadvantage of the present invention will be more clear along with description.But embodiment is only exemplary, does not form any restriction to scope of the present invention.It will be understood by those skilled in the art that and can modify to the details of technical solution of the present invention and form or replace down without departing from the spirit and scope of the present invention, but these amendments and replacement all fall within the scope of protection of the present invention.
The linen fibre processed in the embodiment of the present invention is without any chemically treated rescutched tow, and by Qiqihar, flax factory provides.
In the embodiment of the present invention, fast penetrant T aerosol-OT salt used is purchased from Linyi City Lanshan District Lv Sen Chemical Co., Ltd., bleeding agent fatty alcohol-polyoxyethylene ether (JFC) is purchased from Liaoyang Losec Chemical Company, and I-hydroxybenzotriazole (HBT) is purchased from Hubei Yuancheng Saichuang Technology Co., Ltd..
In the embodiment of the present invention, N-hydroxy-N-phenyl propionamide used adopts following method to prepare:
(1) synthesis of intermediate phenylhydroxylamine
12.5g nitrobenzene, 6.25g ammonium chloride and 200ml water are placed in flask, mechanical agitator is installed, thermometer, be heated to 57-60 DEG C while stirring, then several times 15.5g zinc powder is added in reactant liquor, because this reaction is exothermic reaction, so will control each input amount when putting zinc powder well, control reacting liquid temperature not higher than 68 degrees Celsius.Continue after zinc powder adds to stir 30min, until react completely, without dense bitter almond odor.With circulating water type vavuum pump suction filtration system fast filtering removing reaction waste residue, pour funnel into the residue in 25ml water washing flask again to filter, then add in filtrate and slowly add about 70g sodium chloride, form sodium chloride saturated solution, stir while adding, produce yellow needles gradually in filtrate, suction filtration obtains phenylhydroxylamine crude product again.Then make it to dissolve with a small amount of carrene, the impurity such as removing inorganic salts wherein, then add benzinum, after stirring, suction filtration obtains phenylhydroxylamine white crystal.Then be recrystallized with carrene and benzinum.
(2) synthesis of N-hydroxy-N-phenyl propionamide
9g phenylhydroxylamine 50ml oxolane is dissolved in flask, and the pasty liquid of 15g sodium bicarbonate and 10ml water, load onto mechanical agitator, thermometer and dropping funel, adjusting rotary speed, reactant liquor is stirred.Reaction is placed in cryosel bath, makes reacting liquid temperature maintain 0 DEG C to-10 DEG C, then from dropping funel, slowly instills acylating reagent several times; the mol ratio controlling phenylhydroxylamine and acylating reagent is 1:1.05; after acylating agent adds, continue to stir 60min, acylating reagent is propionyl chloride.Then in reactant liquor, add 50ml sodium hydroxide solution (wNaOH=20%) and 40ml benzinum, after stratification, separate organic phase and inorganic phase with separatory funnel.Use 25ml sodium hydroxide solution (wNaOH=20%) point three washing organic phases again, separate inorganic phase, above inorganic phase solution is merged, with dichloromethane extraction twice, use salt acid for adjusting pH value to about 6.0 again, then with Rotary Evaporators, dichloromethane solution is steamed to original about 1/5th, then add benzinum, obtain crystallized product N-hydroxy-N-phenyl propionamide through cooling.
The infrared spectrum of phenylhydroxylamine and nuclear magnetic resonance spectroscopy:
By the phenylhydroxylamine after recrystallization, infrared spectrum is measured to it, sees Fig. 1.
Wave number (cm
-1) be 3384 (hydroxyl, N-OH), 3243 (N-H), 3053 stretching vibration of C-H (on the phenyl ring), 1602,1492 (stretching vibrations of phenyl ring skeleton), 1469,1087 (N-O stretching vibrations).
The proton nmr spectra of phenylhydroxylamine is shown in Fig. 2.
Spectroscopic data δ (10
-6) be 7.28 (2H, C
3-H and C
5-H), 7.01 (2H, C
2-H and C
6-H), 6.99 (1H, C
4-H), 5.0-6.0 (2H, H-N and H-O), further demonstrate that the structure of phenylhydroxylamine.
The infrared spectrum of N-hydroxy-N-phenyl propionamide and nuclear magnetic resonance spectroscopy:
Phenylhydroxylamine propionating product N-hydroxy-N-phenyl propionamide, colorless plate crystal.Infrared spectrum wave number (cm
-1) be 3171 (hydroxyl, N-OH), 2942 (-CH
2with-CH
3c-H stretching vibration), 1682 (acyl carbonyls), 1591,1494 (stretching vibrations of phenyl ring skeleton), 1290 (stretching vibrations of C-N).As shown in Figure 3.
The proton nmr spectra of N-hydroxy-N-phenyl propionamide as shown in Figure 4.
Spectroscopic data δ (10
-6) be 8.928 (N-OH), 7.47,7.46,7.45 (3H, C
2-H and C
4-H and C
6-H), 7.42,7.41 (2H, C
3-H and C
5-H) further demonstrate that the structure of N-hydroxy-N-phenyl propionamide, structure is as follows.
Embodiment 1
(1) preparation of compound biological enzyme
Take laccase 10-20 part, acid pectase 10-20 part, zytase 30-50 part, is uniformly mixed, i.e. this compound biological enzyme obtained.
(2) the rescutched tow kiering under compound biological enzyme-mediator system condition
Under room temperature, compound biological enzyme, amboceptor N-hydroxy-N-phenyl propionamide, fast penetrant T aerosol-OT salt are added to the water, by citric acid-sodium citrate buffer solution adjust ph to 3-5, are uniformly mixed, obtained kiering liquid; Described kiering liquid is made up of the component of following weight percentage: compound biological enzyme 6.0%, amboceptor N-hydroxy-N-phenyl propionamide 1.5%, and fast penetrant T aerosol-OT salt 1.0%, surplus is water.Under ul-trasonic irradiation, rescutched tow is carried out kiering in kiering liquid, the mass ratio of rescutched tow and kiering liquid is 1:30, and control kiering temperature at 50 DEG C, the kiering processing time is 50 minutes.Supersonic generator working power is AC220V, and operating frequency is 40KHz, and power output is 40W, and the applying groove of ultrasonic oscillator is of a size of 300mm × 150mm × 100mm.
(3) bleach
Added by rescutched tow after kiering containing sodium metasilicate 3.0g/L, natrium carbonicum calcinatum 2.0g/L, in the bleaching liquid of hydrogen peroxide 4.0g/L, wherein hydrogen peroxide is the hydrogen peroxide of concentration 30%, under 80 DEG C of conditions, and bleaching 60min.
(4) wash, dewater and dry
By the cold wash twice of the hot water wash twice of flax tow Wesy 80-90 DEG C after bleaching, 20-30 DEG C, dry to constant weight at 100-105 DEG C after dehydration.
Embodiment 2
(1) the rescutched tow kiering under compound biological enzyme-mediator system condition
Under room temperature, compound biological enzyme embodiment 1 prepared, amboceptor N-hydroxy-N-phenyl propionamide, bleeding agent fatty alcohol-polyoxyethylene ether (JFC) are added to the water, by citric acid-sodium citrate buffer solution adjust ph to 3-5, be uniformly mixed, obtained kiering liquid; Described kiering liquid is made up of the component of following weight percentage: compound biological enzyme 6.5%, amboceptor N-hydroxy-N-phenyl propionamide 2%, and bleeding agent fatty alcohol-polyoxyethylene ether (JFC) 1.5%, surplus is water.Under ul-trasonic irradiation, rescutched tow is carried out kiering in kiering liquid, the mass ratio of rescutched tow and kiering liquid is 1:30, and control kiering temperature at 50 DEG C, the kiering processing time is 60 minutes.Supersonic generator working power is AC220V, and operating frequency is 40KHz, and power output is 40W, and the applying groove of ultrasonic oscillator is of a size of 300mm × 150mm × 100mm.
(2) bleach
Added by rescutched tow after kiering containing sodium metasilicate 3.0g/L, natrium carbonicum calcinatum 2.0g/L, in the bleaching liquid of hydrogen peroxide 4.0g/L, wherein hydrogen peroxide is the hydrogen peroxide of concentration 30%, under 80 DEG C of conditions, and bleaching 60min.
(3) wash, dewater and dry
Method and step are with embodiment 1.
Embodiment 3
(1) the rescutched tow kiering under compound biological enzyme-mediator system condition
Under room temperature, compound biological enzyme embodiment 1 prepared, amboceptor N-hydroxy-N-phenyl propionamide, fast penetrant T aerosol-OT salt are added to the water, by citric acid-sodium citrate buffer solution adjust ph to 3-5, be uniformly mixed, obtained kiering liquid; Described kiering liquid is made up of the component of following weight percentage: compound biological enzyme 6%, amboceptor N-hydroxy-N-phenyl propionamide 1.5%, and fast penetrant T aerosol-OT salt 1.5%, surplus is water.Rescutched tow is carried out kiering in kiering liquid, and the mass ratio of rescutched tow and kiering liquid is 1:30, and control kiering temperature at 60 DEG C, the kiering processing time is 80 minutes.
(2) bleach
Added by rescutched tow after kiering containing sodium metasilicate 3.0g/L, natrium carbonicum calcinatum 2.0g/L, in the bleaching liquid of hydrogen peroxide 4.0g/L, wherein hydrogen peroxide is the hydrogen peroxide of concentration 30%, under 80 DEG C of conditions, and bleaching 60min.
(3) wash, dewater and dry
Method and step are with embodiment 1.
Embodiment 4
(1) the rescutched tow kiering under compound biological enzyme-mediator system condition
Under room temperature, compound biological enzyme embodiment 1 prepared, amboceptor I-hydroxybenzotriazole (HBT), fast penetrant T aerosol-OT salt are added to the water, by citric acid-sodium citrate buffer solution adjust ph to 3-5, be uniformly mixed, obtained kiering liquid; Described kiering liquid is made up of the component of following weight percentage: compound biological enzyme 6%, amboceptor I-hydroxybenzotriazole (HBT) 1.5%, fast penetrant T aerosol-OT salt 2.0%, and surplus is water.Under ul-trasonic irradiation, rescutched tow is carried out kiering in kiering liquid, the mass ratio of linen fibre and kiering liquid is 1:30, and control kiering temperature at 55 DEG C, the kiering processing time is 90 minutes.Supersonic generator working power is AC220V, and operating frequency is 40KHz, and power output is 40W, and the applying groove of ultrasonic oscillator is of a size of 300mm × 150mm × 100mm.
(2) bleach
Added by rescutched tow after kiering containing sodium metasilicate 3.0g/L, natrium carbonicum calcinatum 2.0g/L, in the bleaching liquid of hydrogen peroxide 4.0g/L, wherein hydrogen peroxide is the hydrogen peroxide of concentration 30%, under 80 DEG C of conditions, and bleaching 60min.
(3) wash, dewater and dry
Method and step are with embodiment 1.
Embodiment 5
(1) the rescutched tow kiering under compound biological enzyme condition
Under room temperature, compound biological enzyme embodiment 1 prepared, fast penetrant T aerosol-OT salt are added to the water, and by citric acid-sodium citrate buffer solution adjust ph to 3-5, are uniformly mixed, obtained kiering liquid; Described kiering liquid is made up of the component of following weight percentage: compound biological enzyme 6%, fast penetrant T aerosol-OT salt 1.5%, and surplus is water.Under ul-trasonic irradiation, rescutched tow is carried out kiering in kiering liquid, the mass ratio of rescutched tow and kiering liquid is 1:30, and control kiering temperature at 60 DEG C, the kiering processing time is 80 minutes.Supersonic generator working power is AC220V, and operating frequency is 40KHz, and power output is 40W, and the applying groove of ultrasonic oscillator is of a size of 300mm × 150mm × 100mm.
(2) bleach
Added by rescutched tow after kiering containing sodium metasilicate 3.0g/L, natrium carbonicum calcinatum 2.0g/L, in the bleaching liquid of hydrogen peroxide 4.0g/L, wherein hydrogen peroxide is the hydrogen peroxide of concentration 30%, under 80 DEG C of conditions, and bleaching 60min.
(3) wash, dewater and dry
Method and step are with embodiment 1.
Embodiment 6
(1) the rescutched tow kiering under compound biological enzyme condition
Under room temperature, compound biological enzyme embodiment 1 prepared, bleeding agent fatty alcohol-polyoxyethylene ether (JFC) are added to the water, and by citric acid-sodium citrate buffer solution adjust ph to 3-5, are uniformly mixed, obtained kiering liquid; Described kiering liquid is made up of the component of following weight percentage: compound biological enzyme 5%, bleeding agent fatty alcohol-polyoxyethylene ether (JFC) 1.0%, and surplus is water.Under ul-trasonic irradiation, rescutched tow is carried out kiering in kiering liquid, the mass ratio of rescutched tow and kiering liquid is 1:30, and control kiering temperature at 50 DEG C, the kiering processing time is 80 minutes.Supersonic generator working power is AC220V, and operating frequency is 40KHz, and power output is 40W, and the applying groove of ultrasonic oscillator is of a size of 300mm × 150mm × 100mm.
(2) bleach
Added by rescutched tow after kiering containing sodium metasilicate 3.0g/L, natrium carbonicum calcinatum 2.0g/L, in the bleaching liquid of hydrogen peroxide 4.0g/L, wherein hydrogen peroxide is the hydrogen peroxide of concentration 30%, under 80 DEG C of conditions, and bleaching 60min.
(3) wash, dewater and dry
Method and step are with embodiment 1.
Comparative example 1
(1) towy alkaline scouring
NaOH, natrium carbonicum calcinatum, sodium metasilicate, sodium sulfite, bleeding agent fatty alcohol-polyoxyethylene ether (JFC) are added to the water, are uniformly mixed, obtained kiering liquid; Described kiering liquid is made up of the component of following weight percentage: NaOH 3.5g/L, natrium carbonicum calcinatum 1.5g/L, sodium metasilicate 2.0g/L, sodium sulfite 3.0g/L, bleeding agent fatty alcohol-polyoxyethylene ether (JFC) 0.5g/L.The mass ratio of rescutched tow and kiering liquid is 1:30, and control kiering temperature at 90 DEG C, the kiering processing time is 80 minutes.
(2) bleach
Added by rescutched tow after kiering containing sodium metasilicate 3.0g/L, natrium carbonicum calcinatum 2.0g/L, in the bleaching liquid of hydrogen peroxide 4.0g/L, wherein hydrogen peroxide is the hydrogen peroxide of concentration 30%, under 80 DEG C of conditions, and bleaching 60min.
(3) wash, dewater and dry
Method and step are with embodiment 1.
Comparative example 2
(1) towy alkaline scouring
NaOH, natrium carbonicum calcinatum, sodium metasilicate, sodium sulfite, fast penetrant T aerosol-OT salt are added to the water, are uniformly mixed, obtained kiering liquid; Described in described kiering liquid, kiering liquid is made up of the component of following weight percentage: NaOH 3.0g/L, natrium carbonicum calcinatum 2.0g/L, sodium metasilicate 2.0g/L, sodium sulfite 3.0g/L, fast penetrant T aerosol-OT salt 0.5g/L.The mass ratio of rescutched tow and kiering liquid is 1:30, and control kiering temperature at 85 DEG C, the kiering processing time is 70 minutes.
(2) bleach
Rescutched tow after kiering is added containing sodium nitrate 2.0g/L, sodium chlorite 3.0g/L, in the bleaching liquid of sulfuric acid 2.2g/L, under 50 DEG C of conditions, bleaching 50min.
(3) wash, dewater and dry
Method and step are with embodiment 1.
Test example
The mensuration of reduction rate: take out the rescutched tow before and after according to embodiment 1-6, comparative example 1-2 process from Constant Temperature and Humidity Chambers, point its quality of another name is m
0and m
1, then towy weight-loss ratio=(1-m
1/ m
0) × 100%.
The mensuration of whiteness: whiteness is generally by apparatus measures, and the present invention passes through YQ-Z-48A whiteness and colure meter to the mensuration of the flax tow peacekeeping untreated rescutched tow polarity whiteness after embodiment 1-6, comparative example 1-2 process.According to GBT8424.2-2001, " textile color stability tests the objective ranking method of relative whiteness " method of testing is as follows: get rescutched tow to be measured, the pallet being arranged closely in measuring brightness instrument measures, each sample rotates to three different directions to be measured, write down corresponding R457 whiteness value, whiteness gets three mean values measured.
The mensuration of fracture strength: according to GB/T3916-1997 " single yarn ultimate strength and elongation at break standard " method, fibrous fracture intensity all adopts LLY-06 electronic fiber tensometer to test.Test condition is: line density 12dex, range 200cN, and number of times 5 times, space 25mm, speed 100mm/min.
The mensuration of fiber thinness: randomly draw rescutched tow sample, carry out combing, cut 10mm in middle part, analytical balance accurately takes the sample of 5 about 1mg, by root counting (do not divide or slight crack counts 1 less than the fiber of 5mm, split the counting respectively of more than root 5mm).Formula (1) and (2) is adopted to calculate flax fiber separation index:
a
i＝n
i×10(mm)/m
i(1)
A
on average=1/5 ∑ a
i(2)
In formula: a
ithe fiber thinness of-the i-th part of fiber;
N
ithe number of fiber of-the i-th part;
M
ithe fiber quality (mg) of-the i-th part, i=1,2,3,4,5;
A
on average-survey the fiber thinness of fiber.
Measurement result is in table 1.
Table 1 subfiber fiber crops the performance test results
Rational kiering process is carried out to rescutched tow, can obviously remove pectin and lignin, improve fiber thinness and the fineness of fiber, ensure certain fracture strength and percentage elongation, thus improve towy spinnability.As can be seen from the numerical value in table 1, rescutched tow is after preliminary treatment, and its fiber thinness and whiteness have significant improvement, and the fracture strength of fiber has reduction in various degree.This is because fiber is after kiering bleaching, the impurity contents such as the pectin lignin contained by itself reduce greatly, due to the reduction of pectin content, the degree of bonding mutually between fiber is reduced, causes the raising of flax fiber separation index.Grade along with lignin in fiber, ash the removal of fiber accompaniment, and the whiteness of fiber naturally can increase.In the process that fiber accompaniment is removed, the structure of fiber itself also obtains destruction to a certain extent in pretreatment process, causes fibrous fracture intensity to reduce.
The present invention is under ul-trasonic irradiation, adopt compound biological enzyme to come unstuck preliminary treatment to rescutched tow in conjunction with amboceptor N-hydroxy-N-phenyl propionamide, the towy physical performance index (reduction rate, fracture strength, whiteness and fiber thinness) after process is better than the rescutched tow being used alone biology enzyme pre-treatment.Present invention achieves and no longer with acid, preliminary treatment be carried out to fiber in fiber degumming process, decrease the process of pretreated waste water, decrease the use of NaOH, reduce the discharge of kiering waste water.
Claims (8)
1. a towy preprocess method, is characterized in that, under ul-trasonic irradiation, adopts compound biological enzyme to come unstuck preliminary treatment to rescutched tow in conjunction with amboceptor N-hydroxy-N-phenyl propionamide;
Wherein, described compound biological enzyme is made up of laccase, acid pectase and zytase.
2. preprocess method according to claim 1, is characterized in that, specifically comprises the following steps:
(1) preparation of compound biological enzyme
Take laccase 10-20 part, acid pectase 10-20 part, zytase 30-50 part, is uniformly mixed, obtains final product;
(2) the rescutched tow kiering under compound biological enzyme-mediator system condition
Under ul-trasonic irradiation, rescutched tow is carried out kiering in kiering liquid, the mass ratio of rescutched tow and kiering liquid is 1:30, and control kiering temperature at 45-75 DEG C, the kiering processing time is 40-90 minute; Described kiering liquid is made up of following component: compound biological enzyme, amboceptor N-hydroxy-N-phenyl propionamide, fast penetrant T aerosol-OT salt and water;
(3) bleach
Rescutched tow after kiering is added containing sodium metasilicate 3.0g/L, in the bleaching liquid of natrium carbonicum calcinatum 2.0g/L and hydrogen peroxide 4.0g/L, under 80 DEG C of conditions, bleaching 60min;
(4) wash, dewater and dry
By the cold wash twice of the hot water wash twice of flax tow Wesy 80-90 DEG C after bleaching, 20-30 DEG C, dry to constant weight at 100-105 DEG C after dehydration.
3. preprocess method according to claim 2, it is characterized in that, the relatively described towy mass fraction of step (2) described compound biological enzyme is 4-8%, the relatively described towy mass fraction of described amboceptor N-hydroxy-N-phenyl propionamide is 0.9-2.5%, the relatively described towy mass fraction of fast penetrant T aerosol-OT salt is 0.5-1.5%, and the pH value of described kiering liquid is 3-5.
4. preprocess method according to claim 2, is characterized in that, step (3) described hydrogen peroxide is the hydrogen peroxide of concentration 30%.
5. the preprocess method according to any one of claim 1-4, it is characterized in that, described hyperacoustic generator working power is AC220V, and operating frequency is 40KHz, power output is 40W, and the applying groove of ultrasonic oscillator is of a size of 300mm × 150mm × 100mm.
6. the preprocess method according to any one of claim 1-4, is characterized in that, the following method of described N-hydroxy-N-phenyl propionamide prepares:
(1) synthesis of intermediate phenylhydroxylamine
By nitrobenzene, ammonium chloride and water are placed in flask according to mass ratio 1.5-3:0.5-1.5:30-34, mechanical agitator is installed, thermometer, be heated to 57-60 DEG C while stirring, then several times zinc powder is added in reactant liquor, continue after zinc powder adds to stir 30min, until react completely, without dense bitter almond odor, with circulating water type vavuum pump suction filtration system fast filtering removing reaction waste residue, the residue washed with water again in flask is poured funnel into and is filtered, then add in filtrate and slowly add sodium chloride, form sodium chloride saturated solution, stir while adding, yellow needles is produced gradually in filtrate, suction filtration obtains phenylhydroxylamine crude product again, then make it to dissolve with a small amount of carrene, the impurity such as removing inorganic salts wherein, add benzinum again, after stirring, suction filtration obtains phenylhydroxylamine white crystal, then be recrystallized with carrene and benzinum,
(2) synthesis of N-hydroxy-N-phenyl propionamide
The phenylhydroxylamine oxolane of step (1) is dissolved in flask, then adds the pasty liquid of sodium bicarbonate and water, load onto mechanical agitator, thermometer and dropping funel, adjusting rotary speed, reactant liquor is stirred.Reaction is placed in cryosel bath, makes reacting liquid temperature maintain 0 DEG C to-10 DEG C, then from dropping funel, slowly instills acylating reagent several times, and the mol ratio controlling phenylhydroxylamine and acylating reagent is 1:0.8-1.2, after acylating reagent adds, continues to stir 60min.Then in reactant liquor, add sodium hydroxide solution and benzinum, after stratification, separate organic phase and inorganic phase with separatory funnel; Divide with sodium hydroxide solution again and wash organic phase three times, separate inorganic phase, above inorganic phase solution is merged, with dichloromethane extraction twice, use salt acid for adjusting pH value to about 6.0 again, then with Rotary Evaporators, dichloromethane solution is steamed to original about 1/5th, then add benzinum, obtain crystallized product N-hydroxy-N-phenyl propionamide through cooling.
7. preprocess method according to claim 6, is characterized in that, step (1) zinc powder adds reactant liquor according to the mass ratio 1-1.5:1 of zinc powder and nitrobenzene at every turn, and controls zinc powder and add the temperature of rear reactant liquor at 57-68 DEG C.
8. preprocess method according to claim 6, is characterized in that, the mass ratio of step (2) described phenylhydroxylamine, sodium bicarbonate and water is 8-10:14-16:9-11, and the mass fraction of described sodium hydroxide solution is 20%; Described acylating reagent is propionyl chloride.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106498506A (en) * | 2016-12-02 | 2017-03-15 | 长兴锦桥纺织有限公司 | A kind of ramie degumming method suitable for close-fitting fabric |
| CN107675270A (en) * | 2017-09-29 | 2018-02-09 | 中国农业科学院麻类研究所 | A kind of method that echelon utilizes crudefiber crop bast raw material |
| CN108044758A (en) * | 2017-11-17 | 2018-05-18 | 中国农业科学院麻类研究所 | A kind of resource utilization method of waste agronomic crop bast raw material |
| CN108325581A (en) * | 2018-02-07 | 2018-07-27 | 中国农业机械化科学研究院 | A kind of comprehensive utilization process of linseed |
| CN108505125A (en) * | 2017-02-27 | 2018-09-07 | 赵松竹 | A kind for the treatment of process dissociating natural plant fibre using mechanical oscillation wave energy |
| CN113046881A (en) * | 2021-03-26 | 2021-06-29 | 穆棱市龙穆雅品亚麻纺织有限公司 | Hemp cotton spinning and degumming process thereof |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0967777A (en) * | 1995-08-31 | 1997-03-11 | Japan Synthetic Rubber Co Ltd | Fiber treating agent and treatment of fiber |
| CN1986953A (en) * | 2006-12-20 | 2007-06-27 | 宁夏华实亚麻纺织有限公司 | Composite biological emzyme/amboceptor system and use for textile scouring process |
| KR100785827B1 (en) * | 2006-10-18 | 2007-12-13 | 이경세 | Bio-towel using enzyme scouring and manufacturing method thereof |
| CN101126177A (en) * | 2007-09-27 | 2008-02-20 | 江苏紫荆花纺织科技股份有限公司 | Enzymatic degumming method for jute or ambari hemp |
| CN101649555A (en) * | 2009-08-13 | 2010-02-17 | 齐齐哈尔大学 | Method for preprocessing rough linen yarn bio-enzyme under action of ultrasonic wave |
| CN101649554A (en) * | 2009-08-13 | 2010-02-17 | 齐齐哈尔大学 | Process for producing high-count linen yarn |
| CN102125261A (en) * | 2010-12-09 | 2011-07-20 | 齐齐哈尔大学 | Extraction of lignans from flaxseeds through ultrasonic enzymolysis |
| CN102168381A (en) * | 2011-02-25 | 2011-08-31 | 东华大学 | Method for pretreating cotton fabric by using biological enzyme/mediator system and bleaching cotton fabric by using hydrogen peroxide |
| JP2012026053A (en) * | 2010-07-23 | 2012-02-09 | Kb Tsuzuki Kk | Fiber processing method |
| CN104099670A (en) * | 2014-06-25 | 2014-10-15 | 齐齐哈尔大学 | Method for degelatinizing hemp fiber with biological enzyme degelatinizing method combined with chemical degelatinizing method |
-
2015
- 2015-05-05 CN CN201510223927.6A patent/CN104818623A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0967777A (en) * | 1995-08-31 | 1997-03-11 | Japan Synthetic Rubber Co Ltd | Fiber treating agent and treatment of fiber |
| KR100785827B1 (en) * | 2006-10-18 | 2007-12-13 | 이경세 | Bio-towel using enzyme scouring and manufacturing method thereof |
| CN1986953A (en) * | 2006-12-20 | 2007-06-27 | 宁夏华实亚麻纺织有限公司 | Composite biological emzyme/amboceptor system and use for textile scouring process |
| CN101126177A (en) * | 2007-09-27 | 2008-02-20 | 江苏紫荆花纺织科技股份有限公司 | Enzymatic degumming method for jute or ambari hemp |
| CN101649555A (en) * | 2009-08-13 | 2010-02-17 | 齐齐哈尔大学 | Method for preprocessing rough linen yarn bio-enzyme under action of ultrasonic wave |
| CN101649554A (en) * | 2009-08-13 | 2010-02-17 | 齐齐哈尔大学 | Process for producing high-count linen yarn |
| JP2012026053A (en) * | 2010-07-23 | 2012-02-09 | Kb Tsuzuki Kk | Fiber processing method |
| CN102125261A (en) * | 2010-12-09 | 2011-07-20 | 齐齐哈尔大学 | Extraction of lignans from flaxseeds through ultrasonic enzymolysis |
| CN102168381A (en) * | 2011-02-25 | 2011-08-31 | 东华大学 | Method for pretreating cotton fabric by using biological enzyme/mediator system and bleaching cotton fabric by using hydrogen peroxide |
| CN104099670A (en) * | 2014-06-25 | 2014-10-15 | 齐齐哈尔大学 | Method for degelatinizing hemp fiber with biological enzyme degelatinizing method combined with chemical degelatinizing method |
Non-Patent Citations (1)
| Title |
|---|
| 付时雨 等: ""苯基羟胺及N-酰基衍生物的合成与表征"", 《华南理工大学学报（自然科学版）》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106498506A (en) * | 2016-12-02 | 2017-03-15 | 长兴锦桥纺织有限公司 | A kind of ramie degumming method suitable for close-fitting fabric |
| CN108505125A (en) * | 2017-02-27 | 2018-09-07 | 赵松竹 | A kind for the treatment of process dissociating natural plant fibre using mechanical oscillation wave energy |
| CN107675270A (en) * | 2017-09-29 | 2018-02-09 | 中国农业科学院麻类研究所 | A kind of method that echelon utilizes crudefiber crop bast raw material |
| CN107675270B (en) * | 2017-09-29 | 2018-10-02 | 中国农业科学院麻类研究所 | A kind of method that echelon utilizes crudefiber crop bast raw material |
| CN108044758A (en) * | 2017-11-17 | 2018-05-18 | 中国农业科学院麻类研究所 | A kind of resource utilization method of waste agronomic crop bast raw material |
| CN108325581A (en) * | 2018-02-07 | 2018-07-27 | 中国农业机械化科学研究院 | A kind of comprehensive utilization process of linseed |
| CN113046881A (en) * | 2021-03-26 | 2021-06-29 | 穆棱市龙穆雅品亚麻纺织有限公司 | Hemp cotton spinning and degumming process thereof |
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