CN103147275B - Method for modifying nylon fabric by magnetic nano ferrous oxide with photocatalytic activity - Google Patents
Method for modifying nylon fabric by magnetic nano ferrous oxide with photocatalytic activity Download PDFInfo
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Abstract
The invention discloses a method for modifying nylon fabric by magnetic nano ferrous oxide with photocatalytic activity. The method comprises the following steps of: firstly, preparing diluted hydrochloric acid solution, etching the nylon fabric by the prepared diluted hydrochloric acid solution, and then, swelling the etched nylon fabric; then, preparing a modifying solution of ferric sulfate, sodium hydroxide, sodium dodecyl benzene sulfonate and chitosan, and placing the pre-treated nylon fabric to the modifying solution for hydrothermal reaction to obtain modified nylon fabric; and finally, preparing a coupler solution, placing the modified nylon fabric to the coupler solution for treatment, and then, curing the modified nylon fabric treated by the coupler solution to obtain the nylon fabric coated with a magnetic nano ferrous trioxide particle thin film having photocatalytic activity. The nylon fabric modified by the method disclosed by the invention has good photocatalytic activity, magnetic property and scourability, and the handfeel and ventilation of the nylon fabric are not affected.
Description
Technical field
The invention belongs to function textile material technical field, relate to a kind of method of modifying of nylon fabric, be specifically related to a kind of method of photocatalytic activity and magnetic Nano di-iron trioxide modified nylon fabric.
Background technology
Nanometer di-iron trioxide has good photocatalytic activity and magnetic property, hardness is high, good weatherability, light resistance and chemical stability, be a kind of important inorganic pigment and fine ceramics raw material, can photocatalysis degradation organic contaminant and magnetic pipe recording material be used as.At present, prepare nanometer di-iron trioxide method and can be divided into dry method and wet method generally.Dry method comprises microwave method, flame thermal decomposition, vapour deposition, nonthermal plasma chemistry vapour deposition process and LASER HEAT decomposition method etc.; Wet method comprises hydro-thermal method, forced hydrolysis method, agglutinating nature yeast, microemulsion method, the precipitation method and colloid chemistry methods etc.Wherein to have the particle purity of preparation high for hydro-thermal method, good dispersion, good crystalline and size is controlled, easily realizes the advantages such as suitability for industrialized production high quality of products.Nylon fabric has excellent intensity and anti-wear performance, not only the wearing fabric such as down jackets, anorak can be used as, but also be widely used in decoration and TECHNICAL FABRIC, there is at the coated one deck of nylon fabric fiber surface the nanometer ferric oxide particle film of photocatalytic activity and magnetic, greatly will widen the range of application of nylon fabric, improve added value of product.
The correlation technique of current employing hydro-thermal method to nylon fabric clad nano ferric oxide particle film does not also have.It is the functional fiber of preparation containing nano particle that existing surface of nylon fabric method of modifying mainly contains two kinds: one, namely in spinning process by nanoparticulate dispersed in chemical fibre raw material, to respin a fibroblast, its advantage is consistency of performance, and shortcoming is that nano particle and polymeric material compatibility are poor, and nanoparticulate dispersed is uneven, agglomeration is serious, major part nanoparticles embedded is in fibrous matrix, and the nano particle of fiber surface is little, and therefore performance significantly declines; Two is use adhesive and auxiliary agent that nano particle is mixed with dressing liquid, adopt dipping or the technique such as compregnate, oven dry by adhering nanoparticles to fabric face, equally also be faced with the problem of nanoparticle agglomerates, and arrange after fabric wash resistant fastness bad, feel is deteriorated, and wearability is greatly affected.
Summary of the invention
The object of this invention is to provide a kind of method of photocatalytic activity and magnetic Nano di-iron trioxide modified nylon fabric, modified nylon fabric has good photocatalytic activity, magnetic property and washing durability, and does not affect feel and the gas permeability of nylon fabric.
The technical solution adopted in the present invention is, the method for photocatalytic activity and magnetic Nano di-iron trioxide modified nylon fabric, specifically implements according to following steps:
Step 1, preparation dilute hydrochloric acid solution, utilize hydrochloric acid solution to etch nylon fabric, then uses DMF solution to carry out swelling treatment to the nylon fabric after etching;
The modified solution of step 2, preparation ferric sulfate, NaOH, neopelex and shitosan, puts into modified solution by pretreated nylon fabric and carries out hydro-thermal reaction, obtain modified nylon fabric;
Step 3, preparation coupling agent solution, modified nylon fabric is placed in coupling agent solution process, again the modified nylon fabric through coupling agent solution process is cured process, obtains the nylon fabric of coated photocatalytic activity and magnetic Nano ferric oxide particle film.
Feature of the present invention is also,
Step 1 is specifically implemented according to following steps:
1.1) according to volume ratio 1:4 ~ 6 of hydrochloric acid and water, preparation dilute hydrochloric acid solution, the mass concentration of described hydrochloric acid is 36%;
1.2) nylon fabric is taken, according to bath raio 1:30 ~ 50, the nylon fabric taken is put into step 1.1) dilute hydrochloric acid solution for preparing, under 50 DEG C ~ 70 DEG C conditions, by the nylon fabric dilute hydrochloric acid solution immersion treatment 20min ~ 40min taken, complete the etching processing to nylon fabric;
1.3) by step 1.2) in nylon fabric after etching processing be immersed in DMF, under 70 DEG C ~ 90 DEG C conditions, process 3h ~ 5h, then clean with deionized water rinsing.
Step 2 is specifically implemented according to following steps:
2.1) quality of the nylon fabric after processing according to step 1, measures deionized water with the bath raio of 1:30 ~ 50;
2.2) be 0.01mol/L ~ 0.05mol/L according to total concentration of iron, the mol ratio of ferric ion and hydroxide ion is Fe
3+: OH
-=1:2 ~ 1:4, takes ferric sulfate and NaOH respectively;
2.3) by step 2.2) in the ferric sulfate that takes be dissolved in step 2.1) in the deionized water that measures, obtain ferrum sulfuricum oxydatum solutum, then add NaOH and fully stir, obtaining ferric sulfate and NaOH mixed solution;
2.4) neopelex and shitosan is taken respectively, add the neopelex taken and shitosan to step 2.3) in the ferric sulfate for preparing and NaOH mixed solution, continuous stirring is until neopelex and shitosan are dissolved in ferric sulfate and NaOH mixed solution, form modified solution, wherein add the neopelex of 4g ~ 8g in often liter of ferric sulfate and NaOH mixed solution, the shitosan of 2g ~ 5g;
2.5) pour pretreated for step 1 nylon fabric into step 2.4) in preparation modified solution in flood, dip time is 5min ~ 10min;
2.6) by through step 2.5) nylon fabric after dipping proceeds to sealing after in reaction cylinder together with modified solution, the volume of modified solution is no more than 60% ~ 80% of reaction cylinder volume, reaction cylinder after sealing is risen to 120 DEG C ~ 140 DEG C with 2 ~ 4 DEG C/min speed, then with 5 ~ 10r/min rotating speed isothermal reaction 3h ~ 5h;
2.7) question response complete, cooling after, the nylon fabric of taking-up is soaked 5min ~ 10min in deionized water, and dry 40min ~ 60min under 60 DEG C ~ 90 DEG C vacuum conditions, namely obtains modified nylon fabric.
The shitosan that the shitosan adopted in step 2 is deacetylation is 90%, molecular weight is less than 1000.
Step 3 is specifically implemented according to following steps:
3.1) according to the quality of nylon fabric, ethanolic solution is measured for 1:80 ~ 120 in mass ratio;
3.2) according to 3-glycidylpropyl trimethoxysilane coupling agent and step 3.1) in the volume ratio of ethanolic solution prepared be that 0.02 ~ 0.05:1 measures 3-glycidylpropyl trimethoxysilane coupling agent, the 3-glycidylpropyl trimethoxysilane coupling agent measured slowly is added drop-wise to step 3.1) in the ethanolic solution for preparing, drip while constantly stir, 10min ~ 20min dropwises, by solution left standstill 30min ~ 50min after dropwising, obtain coupling agent solution;
3.3) modified nylon textile impregnation step 2 obtained is in step 3.2) in the coupling agent solution for preparing, and under 30 DEG C ~ 60 DEG C conditions, make modified nylon fabric and coupling agent solution carry out coupling reaction 4h ~ 8h;
3.4) step 3.3) in coupling reaction after, positive and negative for the nylon fabric of taking-up two sides is placed in respectively irradiation 30min ~ 50min under ultraviolet lamp, during irradiation, nylon fabric distance ultraviolet lamp 10cm ~ 20cm, completes the solidification process to nylon fabric;
3.5) by through step 3.4) after nylon fabric after solidification process soaks 5min ~ 10min in acetone, 5min ~ 10min is soaked again in absolute ethyl alcohol, take out with after washed with de-ionized water nylon fabric 5min ~ 10min again, by the nylon fabric that cleans up in 70 DEG C ~ 90 DEG C vacuumizes, till oven dry, namely obtain the nylon fabric of coated photocatalytic activity and magnetic Nano ferric oxide particle film.
In step 3, the power of the ultraviolet lamp that curing reaction adopts is 40W, dominant wavelength is 365nm.
Step 3.1) in ethanolic solution be that 1:5 ~ 10 are formulated by absolute ethyl alcohol and deionized water according to volume ratio.
The invention has the beneficial effects as follows, adopt hydro-thermal method in the process preparing photocatalytic activity and magnetic Nano di-iron trioxide crystal, the nanometer di-iron trioxide crystal grain of generation is directly loaded to nylon fabric fiber surface, at the nanometer ferric oxide particle film of nylon fibre Surface coating one deck densification, give nylon fabric photocatalytic activity and magnetic property; And by regulating source of iron consumption, reaction temperature and time, the selecting and the technique such as coupling post processing of dispersant, the best modification scheme of optimization; The inventive method can save raw material, easy and simple to handle, and nanometer di-iron trioxide attachment fastness is good.Test result shows, the modified nylon fabric of nanometer di-iron trioxide can photo-catalytic degradation of methyl-orange dyestuff, and after 30 standard wash, fabric still has certain magnetic property.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph of common nylon fabric;
Fig. 2 is the stereoscan photograph adopting the inventive method modified to nylon fabric clad nano ferric oxide particle;
Fig. 3 is the coated nanometer ferric oxide particle X-ray diffraction spectrogram of surface of nylon fabric;
Fig. 4 is that the forward and backward UV-visible of nylon fabric nanometer di-iron trioxide modification diffuses spectral curve;
Fig. 5 is the B-H loop adopting the inventive method modified to nylon fabric clad nano di-iron trioxide.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
The method of photocatalytic activity of the present invention and magnetic Nano di-iron trioxide modified nylon fabric, specifically implement according to following steps:
Step 1, preparation dilute hydrochloric acid solution, utilize the dilute hydrochloric acid solution of preparation to etch nylon fabric, then uses DMF solution to carry out swelling treatment to the nylon fabric after etching; Specifically implement according to following steps:
1.1) according to volume ratio 1:4 ~ 6 of hydrochloric acid and water, preparation dilute hydrochloric acid solution, the mass concentration of described hydrochloric acid is 36%;
1.2) nylon fabric is taken, according to bath raio 1:30 ~ 50, the nylon fabric taken is put into step 1.1) dilute hydrochloric acid solution for preparing, under 50 DEG C ~ 70 DEG C conditions, by the nylon fabric dilute hydrochloric acid solution immersion treatment 20min ~ 40min taken, complete the etching processing to nylon fabric;
1.3) by step 1.2) in nylon fabric after etching processing be immersed in DMF, under 70 DEG C ~ 90 DEG C conditions, process 3h ~ 5h, then clean with deionized water rinsing.
The modified solution of step 2, preparation ferric sulfate, NaOH, neopelex and shitosan, pretreated nylon fabric is put into modified solution and carries out hydro-thermal reaction, obtain modified nylon fabric, specifically implement according to following steps:
2.1) quality of the nylon fabric after processing according to step 1, measures deionized water with the bath raio of 1:30 ~ 50;
2.2) be 0.01mol/L ~ 0.05mol/L according to total concentration of iron, the mol ratio of ferric ion and hydroxide ion is Fe
3+: OH
-=1:2 ~ 1:4, takes ferric sulfate and NaOH respectively;
2.3) by step 2.2) in the ferric sulfate that takes be dissolved in step 2.1) in the deionized water that measures, obtain ferrum sulfuricum oxydatum solutum, then add NaOH and fully stir, obtaining ferric sulfate and NaOH mixed solution;
2.4) neopelex and shitosan is taken respectively, add the neopelex taken and shitosan to step 2.3) in the ferric sulfate for preparing and NaOH mixed solution, continuous stirring is until neopelex and shitosan are dissolved in ferric sulfate and NaOH mixed solution, form modified solution, wherein add the neopelex of 4g ~ 8g in often liter of ferric sulfate and NaOH mixed solution, the shitosan of 2g ~ 5g;
2.5) pour pretreated for step 1 nylon fabric into step 2.4) in preparation modified solution in flood, dip time is 5min ~ 10min;
2.6) by through step 2.5) nylon fabric after dipping proceeds to sealing after in reaction cylinder together with modified solution, the volume of modified solution is no more than 60% ~ 80% of reaction cylinder volume, reaction cylinder after sealing is risen to 120 DEG C ~ 140 DEG C with 2 ~ 4 DEG C/min speed, then with 5 ~ 10r/min rotating speed isothermal reaction 3h ~ 5h;
2.7) question response complete, cooling after, the nylon fabric of taking-up is soaked 5min ~ 10min in deionized water, and dry 40min ~ 60min under 60 DEG C ~ 90 DEG C vacuum conditions, namely obtains modified nylon fabric.
The shitosan that shitosan is wherein deacetylation is 90%, molecular weight is less than 1000.
Step 3, preparation coupling agent solution, modified nylon fabric is placed in coupling agent solution process, again the modified nylon fabric through coupling agent solution process is cured process, obtain the nylon fabric of coated photocatalytic activity and magnetic Nano ferric oxide particle film, specifically implement according to following steps:
3.1) according to the quality of nylon fabric, measure ethanolic solution in mass ratio for 1:80 ~ 120, ethanolic solution is that 1:5 ~ 10 are formulated by absolute ethyl alcohol and deionized water according to volume ratio.
3.2) according to 3-glycidylpropyl trimethoxysilane coupling agent and step 3.1) in the volume ratio of ethanolic solution prepared be that 0.02 ~ 0.05:1 measures 3-glycidylpropyl trimethoxysilane coupling agent, the 3-glycidylpropyl trimethoxysilane coupling agent measured slowly is added drop-wise to step 3.1) in the ethanolic solution for preparing, drip while constantly stir, 10min ~ 20min dropwises, by solution left standstill 30min ~ 50min after dropwising, obtain coupling agent solution;
3.3) modified nylon textile impregnation step 2 obtained is in step 3.2) in the coupling agent solution for preparing, and under 30 DEG C ~ 60 DEG C conditions, make modified nylon fabric and coupling agent solution carry out coupling reaction 4h ~ 8h;
3.4) step 3.3) in coupling reaction after, positive and negative for the nylon fabric of taking-up two sides is placed in respectively irradiation 30min ~ 50min under ultraviolet lamp, during irradiation, nylon fabric distance ultraviolet lamp 10cm ~ 20cm, completes the solidification process to nylon fabric; The power of the ultraviolet lamp that curing reaction adopts is 40W, dominant wavelength is 365nm.
3.5) by through step 3.4) after nylon fabric after solidification process soaks 5min ~ 10min in acetone, 5min ~ 10min is soaked again in absolute ethyl alcohol, take out with after washed with de-ionized water nylon fabric 5min ~ 10min again, by the nylon fabric that cleans up in 70 DEG C ~ 90 DEG C vacuumizes, till oven dry, namely obtain the nylon fabric of coated photocatalytic activity and magnetic Nano ferric oxide particle film.
Fig. 1 is the stereoscan photograph of common nylon fabric, Fig. 2 is the stereoscan photograph of clad nano di-iron trioxide nylon fabric, can find out: common nylon fabric fiber surface is very clean, other materials are not had to adhere to, and the particulate material that the coated one deck of nylon fabric fiber surface after loaded with nano di-iron trioxide is thicker, also be studded with some tiny particles, high power electromicroscopic photograph shows this particles coat layer and is made up of nano-scale particle simultaneously.Fig. 3 is the coated nanometer ferric oxide particle X-ray diffraction spectrogram of surface of nylon fabric, test result shows: the angle of diffraction 2 θ has occurred stronger diffraction maximum 24 °, 33 °, 36 °, 41 °, 49 °, 54 °, 62 ° and about 64 °, consistent with the No.89-0599 in standard diagram JCPDF, correspond to (012), (104), (110) of bloodstone α-di-iron trioxide, (113), (024), (116), (214) and (300) crystal face respectively.Fig. 4 is that the forward and backward UV-visible of nylon fabric nanometer di-iron trioxide modification diffuses spectral curve.Can find out, after nylon fabric clad nano di-iron trioxide, not only ultraviolet radiation absorption significantly be strengthened, and visible ray is also increased to some extent.Fig. 5 is the B-H loop of clad nano di-iron trioxide nylon fabric, and test result shows: the nylon fabric of clad nano di-iron trioxide shows more weak magnetic property, and remanent magnetization is 0.00043emug
-1, coercivity is 205.0Oe.
Methyl orange dye is selected to carry out photocatalytic activity mensuration.Be that the nylon fabric that 10cm × 10cm quality is about 1.2g is immersed in volume 50mL, mass concentration is in the methyl orange solution of 2mg/l by size, adsorption equilibrium is reached after being placed in darkroom 90min, then irradiation is carried out under being placed on quartz ultraviolet lamp, the power of ultraviolet lamp is 20W, dominant wavelength is 254nm, light source distance methyl orange liquid level is 10cm, by the forward and backward absorbance at maximum absorption wavelength 464nm place of 7220N type spectrophotometric determination methyl orange solution irradiation 5h, calculate the degradation rate D of methyl orange according to formula (1).
In formula, A
0for initial absorbance when methyl orange solution reaches adsorption equilibrium, A
1for the absorbance of the methyl orange solution after ultraviolet irradiation 5h.
According to standard GB/T/T 8629-2001 " Textile Test home washings and drying program ", washing and dry (selecting A type washing machine, 4A washing procedure, A type drying program) are carried out to clad nano di-iron trioxide nylon fabric.And the hysteresis curve of clad nano di-iron trioxide nylon fabric is measured with VSM multifunction vibration sample magnetometer (Quantum Design company of the U.S.), calculate remanent magnetization and coercivity.
From principle aspect, beneficial effect place of the present invention is described:
(1) the present invention is by controlling the concentration of ferric sulfate, the mol ratio of ferric sulfate and NaOH, reaction temperature and time, selecting and consumption of dispersant, the process of nylon fabric acid etch, and coupling modifier post-processing approach, make the nanometer ferric oxide particle being coated on nylon fabric fiber surface firm, fine and close, particle is nanoscale, is combined well with fibre substrate, has certain photocatalytic activity and magnetic property.This is because ferric sulfate concentration, the mol ratio of ferric sulfate and NaOH, reaction temperature and time, dispersant dosage, nylon fabric acid etch, coupling modifier post processing all affects the photocatalytic activity of nanometer di-iron trioxide, magnetic, purity, crystallization degree, pattern, particle size and coated fastness.Show according to a large amount of experiments: when total concentration of iron is 0.01 ~ 0.05mol/L, surface of nylon fabric can coated certain thickness nanometer ferric oxide film, can not deposit too many nano particle in solution simultaneously; When being less than 0.01mol/L, in solution, iron ion content very little, and surface of nylon fabric can not form continuous print clad, affects photocatalytic activity and magnetic property; When being greater than 0.05mol/L, iron concentration is excessive easily causes waste, and because nanometer di-iron trioxide is reunited, the nanometer ferric oxide film fastness making fabric face coated is bad.
(2) when ferric iron and hydroxyl mol ratio are Fe
3+: OH
-during=1:2 ~ 1:4, ferric sulfate can be made all to transform into nanometer di-iron trioxide, and product purity is high; When mol ratio is less than 1:2 or is greater than 1:4, the bloodstone nanometer di-iron trioxide of generation is fewer, and containing other dephasign compositions.
(3) when reaction temperature controls at 120 ~ 140 DEG C, can generate bloodstone nanometer di-iron trioxide crystal grain, crystallization degree is high; When temperature is lower than 120 DEG C, nanometer di-iron trioxide crystal growth is slow, and crystal formation is bad, does not almost have magnetic; When temperature is higher than 150 DEG C, nylon fabric intensity is subject to major injury, can not use.
(4) reaction time and stirring major effect crystal morphology and the particle size of nanometer di-iron trioxide: control when 3 ~ 5h when reacted, the nanometer ferric oxide particle generated is little and be evenly distributed, and the nanometer ferric oxide film coated at surface of nylon fabric is complete, fine and close; When being less than 3h, nanometer di-iron trioxide grain development is incomplete, poor with nylon fibre binding strength; When being greater than 5h, the nano ferriferrous oxide granule of generation is reunited obviously, and particle size becomes large, and covered effect is bad, easily comes off, and nylon fabric intensity declines larger.
(5) neopelex and shitosan is added, the size of nanometer ferric oxide particle can be controlled preferably: when neopelex consumption is at 4 ~ 8g/L, chitosan dosage is when 2 ~ 5g/L, and the nanometer ferric oxide particle of generation is nanoscale; When neopelex consumption is less than 4g/L, when chitosan dosage is less than 2g/L, do not have the effect controlling nanometer di-iron trioxide crystal size; When neopelex consumption is greater than 8g/L, when chitosan dosage is greater than 5g/L, affect nanometer ferric oxide coated nylon fabric.
(6) watery hydrochloric acid process nylon fabric is used, some micropores and pitting can be formed on nylon fibre surface, improve the coated fastness of nanometer ferric oxide particle: when the volume ratio of hydrochloric acid and water is 1:4 ~ 6, temperature 50 ~ 70 DEG C, during time 20 ~ 40min, more little micropore and pit can be gone out in nylon fibre surface etch; When the volume ratio of hydrochloric acid and water is greater than 1:4, temperature is lower than 50 DEG C, and when the time is less than 20min, etching effect is not obvious; When the volume ratio of hydrochloric acid and water is less than 1:4, temperature is higher than 70 DEG C, and when the time is longer than 40min, nylon fibre etching is serious, and strength damage is larger.
(7) 3-glycidylpropyl trimethoxysilane coupling agent modification, greatly can improve the binding strength of nanometer di-iron trioxide and nylon fabric: when the volume ratio of 3-glycidylpropyl trimethoxy silane and absolute ethyl alcohol is 0.02 ~ 0.05:1, when absolute ethyl alcohol and deionized water volume ratio are 1:5 ~ 10, can the hydrolysis rate of control 3-glycidylpropyl trimethoxy silane well, improve the binding strength of nanometer di-iron trioxide and nylon fibre; When the volume ratio of 3-glycidylpropyl trimethoxy silane and absolute ethyl alcohol is greater than 0.05:1, when absolute ethyl alcohol and deionized water volume ratio are less than 1:5, slowly, coupling effect extends the hydrolysis of 3-glycidylpropyl trimethoxy silane; When the volume ratio of 3-glycidylpropyl trimethoxy silane and absolute ethyl alcohol is less than 0.02:1, when absolute ethyl alcohol and deionized water volume ratio are greater than 1:10, the hydrolysis of 3-glycidylpropyl trimethoxy silane is accelerated, and loses coupling activity.When reaction temperature is at 40 ~ 60 DEG C, the reaction time, when 4 ~ 8h, can improve the attachment fastness of nanometer di-iron trioxide; When reaction temperature is lower than 40 DEG C, the hydrolysis of 3-glycidylpropyl trimethoxy silane slowly; When reaction temperature is higher than 60 DEG C, the hydrolysis of 3-glycidylpropyl trimethoxy silane is accelerated.When being less than 4h when reacted, coupling effect is bad; When being greater than 8h when reacted, lose time.Use ultraviolet is cured, can to improve between nanometer ferric oxide particle and and nylon fibre between bond strength.
Embodiment 1
According to hydrochloric acid and water volume ratio 1:6, preparation hydrochloric acid weak solution, take the nylon fabric of 5g, according to bath raio 1:50, nylon fabric is put into the dilute hydrochloric acid solution of 250mL, under 50 DEG C of conditions, process 20min, then the nylon fabric etched is immersed in N, in dinethylformamide, under 70 DEG C of conditions, process 3h, clean with deionized water, according to nylon fabric quality, measuring the deionized water of 150mL with bath raio 1:30, is 0.01mol/L according to total concentration of iron, and ferric iron and hydroxyl mol ratio are Fe
3+: OH
-=1:2, take ferric sulfate and NaOH respectively, ferric sulfate is dissolved in deionized water, obtain ferrum sulfuricum oxydatum solutum, then add NaOH and fully stir, obtain ferric sulfate and NaOH mixed solution, the neopelex of 0.6g and the shitosan of 0.3g are added in ferric sulfate and NaOH mixed solution, wherein deacetylating degree of chitosan is 90%, molecular weight is less than 1000, and constantly stir, be mixed with modified solution, pretreated nylon fabric is poured in the modified solution prepared and floods 5min, then nylon fabric is proceeded in reaction cylinder together with modified solution and seal, modified solution volume is no more than 60% of reaction cylinder volume, 120 DEG C are risen to 2 DEG C/min speed, with 5r/min rotating speed isothermal reaction 5h, the complete taking-up nylon fabric of question response, soak 5min in deionized water, dry 60min under 60 DEG C of vacuum conditions, namely modified nylon fabric is obtained, according to nylon fabric quality, measure ethanolic solution with bath raio 1:80, this ethanolic solution is that 1:5 is formulated by absolute ethyl alcohol and deionized water according to volume ratio.Be that 0.02:1 measures 3-glycidylpropyl trimethoxysilane coupling agent according to the volume ratio of 3-glycidylpropyl trimethoxysilane coupling agent and ethanolic solution, and it is slowly added drop-wise in ethanolic solution, drip while constantly stir, 10min dropwises, then 30min is left standstill, obtain coupling agent solution, by modified nylon textile impregnation in coupling agent solution, coupling reaction 4h is carried out under 60 DEG C of conditions, after completion of the reaction by nylon fabric just, anti-two sides is placed in hardening with radiation 30min under ultraviolet lamp respectively, fabric is apart from ultraviolet lamp 10cm, wherein the power of ultraviolet lamp is 40W, dominant wavelength is 365nm, nylon fabric after solidification process is immersed in acetone, each 5min in absolute ethyl alcohol, use washed with de-ionized water 5min again, vacuumize under 70 DEG C of conditions, namely the nylon fabric of coated photocatalytic activity and magnetic Nano ferric oxide particle film is obtained.
Using ultraviolet lamp irradiation methyl orange dye solution to evaluate the photocatalytic activity of nanometer di-iron trioxide modified nylon fabric, through the ultraviolet irradiation of 5h, is 81% to the degradation rate of methyl orange dye.According to standard GB/T/T 8629-2001 " Textile Test home washings and drying program ", washing is carried out to clad nano di-iron trioxide nylon fabric and (selects A type washing machine with dry, 4A washing procedure, A type drying program), and the hysteresis curve of clad nano di-iron trioxide nylon fabric is measured with VSM multifunction vibration sample magnetometer (Quantum Design company of the U.S.), after 30 standard wash, the remanent magnetization of clad nano di-iron trioxide nylon fabric is 0.00031emug
-1, coercivity is 187Oe.
Embodiment 2
According to hydrochloric acid and water volume ratio 1:4, preparation hydrochloric acid weak solution, take the nylon fabric of 5g, according to bath raio 1:30, nylon fabric is put into the dilute hydrochloric acid solution of 150mL, under 70 DEG C of conditions, process 40min, then the nylon fabric etched is immersed in N, in dinethylformamide solution, under 90 DEG C of conditions, process 5h, clean with deionized water, according to nylon fabric quality, measuring the deionized water of 250mL with bath raio 1:50, is 0.05mol/L according to total concentration of iron, and ferric iron and hydroxyl mol ratio are Fe
3+: OH
-=1:4, take ferric sulfate and NaOH respectively, ferric sulfate is dissolved in deionized water, obtain ferrum sulfuricum oxydatum solutum, then add NaOH and fully stir, obtain ferric sulfate and NaOH rufous mixed solution, the neopelex of 2g and the shitosan of 1.25g are added in ferric sulfate and NaOH mixed solution, wherein deacetylating degree of chitosan is 90%, molecular weight is less than 1000, and constantly stir, be mixed with modified solution, pretreated nylon fabric is poured in the modified solution prepared and floods 10min, then nylon fabric is proceeded in reaction cylinder together with modified solution and seal, modified solution volume is no more than 80% of reaction cylinder volume, 140 DEG C are risen to 4 DEG C/min speed, with 10r/min rotating speed isothermal reaction 3h, the complete taking-up nylon fabric of question response, soak 10min in deionized water, dry 40min under 90 DEG C of vacuum conditions, namely modified nylon fabric is obtained, according to nylon fabric quality, measure ethanolic solution with bath raio 1:120, this ethanolic solution is that 1:10 is formulated by absolute ethyl alcohol and deionized water according to volume ratio.Be that 0.05:1 measures 3-glycidylpropyl trimethoxysilane coupling agent according to the volume ratio of 3-glycidylpropyl trimethoxysilane coupling agent and ethanolic solution, and it is slowly added drop-wise in absolute ethyl alcohol, drip while constantly stir, 20min dropwises, then 50min is left standstill, obtain coupling agent solution, by modified nylon textile impregnation in coupling agent solution, coupling reaction 8h is carried out under 30 DEG C of conditions, after completion of the reaction by nylon fabric just, anti-two sides is placed in hardening with radiation 50min under ultraviolet lamp respectively, fabric is apart from ultraviolet lamp 20cm, wherein the power of ultraviolet lamp is 40W, dominant wavelength is 365nm, nylon fabric after solidification process is immersed in acetone successively, each 10min in absolute ethyl alcohol, use washed with de-ionized water 10min again, vacuumize under 90 DEG C of conditions, namely the nylon fabric of coated photocatalytic activity and magnetic Nano ferric oxide particle film is obtained.
Using ultraviolet lamp irradiation methyl orange dye solution to evaluate the photocatalytic activity of nanometer di-iron trioxide modified nylon fabric, through the ultraviolet irradiation of 5h, is 92% to the degradation rate of methyl orange dye.According to standard GB/T/T 8629-2001 " Textile Test home washings and drying program ", washing is carried out to clad nano di-iron trioxide nylon fabric and (selects A type washing machine with dry, 4A washing procedure, A type drying program), and the hysteresis curve of clad nano di-iron trioxide nylon fabric is measured with VSM multifunction vibration sample magnetometer (Quantum Design company of the U.S.), after 30 standard wash, the remanent magnetization of clad nano di-iron trioxide nylon fabric is 0.00074emug
-1, coercivity is 325Oe.
Embodiment 3
According to hydrochloric acid and water volume ratio 1:5, preparation hydrochloric acid weak solution, take the nylon fabric of 5g, according to bath raio 1:40, nylon fabric is put into the dilute hydrochloric acid solution of 200mL, under 60 DEG C of conditions, process 30min, then the nylon fabric etched is immersed in N, in dinethylformamide, under 80 DEG C of conditions, process 4h, clean with deionized water, according to nylon fabric quality, measuring the deionized water of 200mL with bath raio 1:40, is 0.03mol/L according to total concentration of iron, and ferric iron and hydroxyl mol ratio are Fe
3+: OH
-=1:3, take ferric sulfate and NaOH respectively, ferric sulfate is dissolved in deionized water, obtain ferrum sulfuricum oxydatum solutum, then add NaOH and fully stir, obtain ferric sulfate and NaOH mixed solution, the neopelex of 1.2g and the shitosan of 0.6g are added in ferric sulfate and NaOH mixed solution, wherein deacetylating degree of chitosan is 90%, molecular weight is less than 1000, and constantly stir, be mixed with modified solution, pretreated nylon fabric is poured in the modified solution prepared and floods 8min, then nylon fabric is proceeded in reaction cylinder together with modified solution and seal, modified solution volume is no more than 70% of reaction cylinder volume, 130 DEG C are risen to 3 DEG C/min speed, with 8r/min rotating speed isothermal reaction 4h, the complete taking-up nylon fabric of question response, soak 7min in deionized water, dry 50min under 80 DEG C of vacuum conditions, namely modified nylon fabric is obtained, according to nylon fabric quality, measure ethanolic solution with bath raio 1:100, this ethanolic solution is that 1:8 is formulated by absolute ethyl alcohol and deionized water according to volume ratio.Be that 0.03:1 measures 3-glycidylpropyl trimethoxysilane coupling agent according to the volume ratio of 3-glycidylpropyl trimethoxysilane coupling agent and ethanolic solution, and it is slowly added drop-wise in absolute ethyl alcohol, drip while constantly stir, 15min dropwises, then 40min is left standstill, obtain coupling agent solution, by modified nylon textile impregnation in coupling agent solution, coupling reaction 6h is carried out under 40 DEG C of conditions, after completion of the reaction by nylon fabric just, anti-two sides is placed in hardening with radiation 40min under ultraviolet lamp respectively, fabric is apart from ultraviolet lamp 15cm, wherein the power of ultraviolet lamp is 40W, dominant wavelength is 365nm, nylon fabric after solidification process is immersed in acetone respectively, each 7min in absolute ethyl alcohol, use washed with de-ionized water 7min again, vacuumize under 80 DEG C of conditions, namely the nylon fabric of coated photocatalytic activity and magnetic Nano ferric oxide particle film is obtained.
Using ultraviolet lamp irradiation methyl orange dye solution to evaluate the photocatalytic activity of nanometer di-iron trioxide modified nylon fabric, through the ultraviolet irradiation of 5h, is 86% to the degradation rate of methyl orange dye.According to standard GB/T/T 8629-2001 " Textile Test home washings and drying program ", washing is carried out to clad nano di-iron trioxide nylon fabric and (selects A type washing machine with dry, 4A washing procedure, A type drying program), and the hysteresis curve of clad nano di-iron trioxide nylon fabric is measured with VSM multifunction vibration sample magnetometer (Quantum Design company of the U.S.), after 30 standard wash, the remanent magnetization of clad nano di-iron trioxide nylon fabric is 0.00042emug
-1, coercivity is 214Oe.
Claims (6)
1. the method for photocatalytic activity and magnetic Nano di-iron trioxide modified nylon fabric, is characterized in that, specifically implement according to following steps:
Step 1, preparation dilute hydrochloric acid solution, utilize the dilute hydrochloric acid solution of preparation to etch nylon fabric, then uses DMF solution to carry out swelling treatment to the nylon fabric after etching;
The modified solution of step 2, preparation ferric sulfate, NaOH, neopelex and shitosan, puts into modified solution by pretreated nylon fabric and carries out hydro-thermal reaction, obtain modified nylon fabric; Specifically implement according to following steps:
2.1) quality of the nylon fabric after processing according to step 1, measures deionized water with the bath raio of 1:30 ~ 50;
2.2) be 0.01mol/L ~ 0.05mol/L according to total concentration of iron, the mol ratio of ferric ion and hydroxide ion is Fe
3+: OH
-=1:2 ~ 1:4, takes ferric sulfate and NaOH respectively;
2.3) by step 2.2) in the ferric sulfate that takes be dissolved in step 2.1) in the deionized water that measures, obtain ferrum sulfuricum oxydatum solutum, then add NaOH and fully stir, obtaining ferric sulfate and NaOH mixed solution;
2.4) neopelex and shitosan is taken respectively, add the neopelex taken and shitosan to step 2.3) in the ferric sulfate for preparing and NaOH mixed solution, continuous stirring is until neopelex and shitosan are dissolved in ferric sulfate and NaOH mixed solution, form modified solution, wherein add the neopelex of 4g ~ 8g in often liter of ferric sulfate and NaOH mixed solution, the shitosan of 2g ~ 5g;
2.5) pour pretreated for step 1 nylon fabric into step 2.4) in preparation modified solution in flood, dip time is 5min ~ 10min;
2.6) by through step 2.5) nylon fabric after dipping proceeds to sealing after in reaction cylinder together with modified solution, the volume of modified solution is no more than 60% ~ 80% of reaction cylinder volume, reaction cylinder after sealing is risen to 120 DEG C ~ 140 DEG C with 2 ~ 4 DEG C/min speed, then with 5r/min ~ 10r/min rotating speed isothermal reaction 3h ~ 5h;
2.7) question response complete, cooling after, the nylon fabric of taking-up is soaked 5min ~ 10min in deionized water, and dry 40min ~ 60min under 60 DEG C ~ 90 DEG C vacuum conditions, namely obtains modified nylon fabric;
Step 3, preparation coupling agent solution, be placed in coupling agent solution by modified nylon fabric and process; Again the modified nylon fabric through coupling agent solution process is cured process, obtains the nylon fabric of coated photocatalytic activity and magnetic Nano ferric oxide particle film.
2. the method for photocatalytic activity according to claim 1 and magnetic Nano di-iron trioxide modified nylon fabric, it is characterized in that, described step 1 is specifically implemented according to following steps:
1.1) according to volume ratio 1:4 ~ 6 of hydrochloric acid and water, preparation dilute hydrochloric acid solution, the mass concentration of described hydrochloric acid is 36%;
1.2) nylon fabric is taken, according to bath raio 1:30 ~ 50, the nylon fabric taken is put into step 1.1) dilute hydrochloric acid solution for preparing, under 50 DEG C ~ 70 DEG C conditions, by the nylon fabric dilute hydrochloric acid solution immersion treatment 20min ~ 40min taken, complete the etching processing to nylon fabric;
1.3) by step 1.2) in nylon fabric after etching processing be immersed in DMF, under 70 DEG C ~ 90 DEG C conditions, process 3h ~ 5h, then clean with deionized water rinsing.
3. the method for photocatalytic activity according to claim 1 and magnetic Nano di-iron trioxide modified nylon fabric, is characterized in that, the shitosan that described shitosan is deacetylation is 90%, molecular weight is less than 1000.
4. the method for photocatalytic activity according to claim 1 and magnetic Nano di-iron trioxide modified nylon fabric, it is characterized in that, described step 3 is specifically implemented according to following steps:
3.1) according to the quality of nylon fabric, ethanolic solution is measured for 1:80 ~ 120 in mass ratio;
3.2) according to 3-glycidylpropyl trimethoxysilane coupling agent and step 3.1) in the volume ratio of ethanolic solution prepared be that 0.02 ~ 0.05:1 measures 3-glycidylpropyl trimethoxysilane coupling agent, the 3-glycidylpropyl trimethoxysilane coupling agent measured is added drop-wise to step 3.1) in the ethanolic solution for preparing, drip while constantly stir, 10min ~ 20min dropwises, by solution left standstill 30min ~ 50min after dropwising, obtain coupling agent solution;
3.3) modified nylon textile impregnation step 2 obtained is in step 3.2) in the coupling agent solution for preparing, and under 30 DEG C ~ 60 DEG C conditions, make modified nylon fabric and coupling agent solution carry out coupling reaction 4h ~ 8h;
3.4) step 3.3) in coupling reaction after, positive and negative for the nylon fabric of taking-up two sides is placed in respectively irradiation 30min ~ 50min under ultraviolet lamp, during irradiation, nylon fabric distance ultraviolet lamp 10cm ~ 20cm, completes the solidification process to nylon fabric;
3.5) by through step 3.4) after nylon fabric after solidification process soaks 5min ~ 10min in acetone, 5min ~ 10min is soaked again in absolute ethyl alcohol, take out with after washed with de-ionized water nylon fabric 5min ~ 10min again, by the nylon fabric that cleans up in 70 DEG C ~ 90 DEG C vacuumizes, till oven dry, namely obtain the nylon fabric of coated photocatalytic activity and magnetic Nano ferric oxide particle film.
5. the method for a kind of photocatalytic activity according to claim 4 and magnetic Nano di-iron trioxide modified nylon fabric, it is characterized in that, described step 3.1) described in ethanolic solution be that 1:5 ~ 10 are formulated by absolute ethyl alcohol and deionized water according to volume ratio.
6. the method for a kind of photocatalytic activity according to claim 1 or 4 and magnetic Nano di-iron trioxide modified nylon fabric, is characterized in that, the power solidifying the ultraviolet lamp that process adopts in described step 3 is 40W, dominant wavelength is 365nm.
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| CN102277727A (en) * | 2011-06-22 | 2011-12-14 | 西安工程大学 | Method for nanometer ferroferric oxide modification of chinlon fabric via hydrothermal process |
| CN102926187A (en) * | 2012-10-18 | 2013-02-13 | 西安工程大学 | Method for modifying polyester fabric by using magnetic nano iron trioxide |
| CN102943374A (en) * | 2012-11-21 | 2013-02-27 | 武汉爱帝高级服饰有限公司 | Anti-radiation warm-keeping antistatic fabric fiber, preparation method thereof and device |
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| CN102277727A (en) * | 2011-06-22 | 2011-12-14 | 西安工程大学 | Method for nanometer ferroferric oxide modification of chinlon fabric via hydrothermal process |
| CN102926187A (en) * | 2012-10-18 | 2013-02-13 | 西安工程大学 | Method for modifying polyester fabric by using magnetic nano iron trioxide |
| CN102943374A (en) * | 2012-11-21 | 2013-02-27 | 武汉爱帝高级服饰有限公司 | Anti-radiation warm-keeping antistatic fabric fiber, preparation method thereof and device |
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