CN104711698A - Photochromic water-repellent non-woven fabric and preparation method thereof - Google Patents
Photochromic water-repellent non-woven fabric and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of multifunctional textile fabrics, and particularly relates to a double-function non-woven fabric with the photochromic performance and the water-repellent performance. The photochromic water-repellent non-woven fabric is prepared from the following raw materials: DMF, acetone, polyvinylidene fluoride (PVDF) and spirooxazine, wherein the volume ratio of DMF to acetone is (1:10) to (1:1); the mass ratio of PVDF to the mixed liquid of acetone and DMF is (1:10) to (1:1); the mass ratio of PVDF to spirooxazine is 60-200. The non-woven fabric disclosed by the invention is prepared by an electrospinning technique, and has the characteristics of being high in production efficiency, simple and convenient in process and good in repeatability; furthermore, the spirooxazine/PVDF composite fabric has the characteristics of the photochromic function and the water-repellent function.
Description
Technical field
The invention belongs to and there is multifunctional textile lining field, be specifically related to the weaving face fabric preparing tool photochromic function and WATER REPELLENCY.
Background technology
In recent years, the materials application of photochromic function is had in the every field such as false proof, Computer Storage, textile garment.In textile garment, photochromic material is applied on weaving face fabric can give its light sensitive characteristic, obtains colourful change color.Photochromic textiles is applied to military hidden field, government utility field, building field, photosensitive function dress ornament etc.Therefore, by the method for simple possible, photochromic material is applied on textiles, becomes the focus of weaving face fabric functional study.
Photochemical reaction is there is in Luo oxazine material in photochromism processes, colour can be become from colourless under ultraviolet irradiation condition, wherein N-methyl-3,3-dimethyl-9 '-hydroxyl spiral shell [2H-indoles-2,3 '-[3H] naphtho-[2,1-b] [Isosorbide-5-Nitrae] oxazine] fatigue durability is good, reaction speed is fast, prepares the plurality of advantages such as comparatively simple.But ， Luo oxazine can not be water-soluble, directly upper dye textiles difficulty is comparatively large, but can be dissolved in organic solvent, at present, contaminates textile fabric mainly with organic solvent as on carrier.
Kynoar (PVDF) has higher WATER REPELLENCY, heat endurance, chemical stability, non-oxidizability and hydrolytic stability, is all widely used in filtration, inductor, piezocell, chemoproection and direct contact distillation.And electrostatic spinning has the advantages such as convenient and swift, sanitation and hygiene, obtaining PVDF fiber non-woven fabric by electrostatic spinning is also study hotspot in recent years.
Luo oxazine is Small molecular, be not easy to practical application, traditional approach is by dispersion method and polymerization, but photochromic film or grafting formation copolymer can only be formed, the former is easily formed and is separated, and limits its concentration range, and the molecule of in use photochromic compounds easily moves in polymeric matrix, affect the stability of photochromic properties, the thickness of this outer film often stops the complete variable color of film inside or affects its photochromic response speed.And although the latter improves the stability of photochromic compound, building-up process is complicated, cost is high, is difficult to meet practical application.
Electrostatic spinning technique can comparatively environmental protection, clean, energy-conservation produce photochromic fibre nonwoven fabric, the method uses a small amount of polymer, nano level continuous fibers film can be obtained, overcome most of photochromic material and can not adapt to the dyeing of traditional water as solvent, and the shortcoming such as dyefastness is not high.
Therefore, the spiral shell oxazine of photochromic effect excellence and PVDF are answered merga pass electrostatic spinning, forms the nano fiber non-woven fabric with excellent photochromic properties, it incites somebody to action tool photochromism, WATER REPELLENCY simultaneously.This composite material has wide application prospect in photochromic material, sensing device and photoelectric display etc.At present, not yet have report by PVDF and photochromic material Luo oxazine composite electrostatic spinning, exploitation has the multifunctional textile lining of photochromic properties and water repellency.
Summary of the invention
The object of this invention is to provide and a kind of photochromicly refuse water weaving face fabric, gained textile material has photochromic and refuses the two multiple function of water.
Technical scheme of the present invention:
The invention provides and a kind of photochromicly refuse water weaving face fabric, its raw material comprises N, dinethylformamide (DMF), acetone, PVDF He Luo oxazine, wherein, the volume ratio of DMF and acetone is 1:10 ~ 1:1, the mass ratio of PVDF and acetone and DMF mixed liquor is the mass ratio of 1:10 ~ 1:1, PVDF Yu Luo oxazine is 60 ~ 200.
Described Luo oxazine is N-methyl-3,3-dimethyl-9 '-hydroxyl spiral shell [2H-indoles-2,3 '-[3H] naphtho-[2,1-b] [Isosorbide-5-Nitrae] oxazine].
Present invention also offers the above-mentioned photochromic preparation method refusing water weaving face fabric, first use 1-nitroso-2,7-dihydroxy naphthlene and 1,3,3-trimethyl-2-methylene indoline Reactive Synthesis photochromic spirooxazine N-methyl-3,3-dimethyl-9 '-hydroxyl spiral shell [2H-indoles-2,3 '-[3H] naphtho-[2,1-b] [Isosorbide-5-Nitrae] oxazine], again Jiang Luo oxazine and PVDF in proportion mixed dissolution in the mixed solution of acetone and DMF, obtained by electrostatic spinning.
The above-mentioned photochromic preparation method refusing water weaving face fabric of the present invention, comprises the steps:
1) by 1-nitroso-2,7-dihydroxy naphthlene is dissolved in ethanol, pass into nitrogen and be heated to 80 ~ 100 DEG C of reflux states, dropwise 1 is added after 5 ~ 30 minutes, 3, the mixed solution of 3-trimethyl-2-methylene indoline and ethanol, dropwise in 15 ~ 60 minutes, in nitrogen atmosphere, keep reflux state and constantly stir, reacting complete after 1 ~ 10h, adding 5 ~ 10% active carbon backflow 5 ~ 30 minutes, filter while hot, filtrate decompression is distilled, after removing most of ethanol, allows it naturally cool and hold over night.Filter and separate out product and repeatedly wash with ethanol or be recrystallized, vacuum drying oven drying finally obtains pale solid N-methyl-3,3-dimethyl-9 afterwards '-hydroxyl spiral shell [2H-indoles-2,3 '-[3H] naphtho-[2,1-b] [Isosorbide-5-Nitrae] oxazine], wherein, 1-nitroso-2,7-dihydroxy naphthlene is 0.01mol ~ 0.1mol, and ethanol is 50mL ~ 200mL, 1, the mixed solution of 3,3-trimethyl-2-methylene indoline 0.01mol ~ 0.1mol and ethanol 10mL ~ 30mL;
2) spinning solution preparation: by step 1) synthesize Luo oxazine and mix with PVDF, be dissolved in vol acetone/DMF mixed liquor again, solution temperature 20 ~ 80 DEG C, magnetic agitation 1 ~ 3h, wherein Luo oxazine and PVDF mass ratio are 60 ~ 200, and acetone and DMF mass ratio are 1:10 ~ 1:1, PVDF and mixed solution mass ratio is 1:10 ~ 1:1;
3) step 2) spinning solution prepared carries out electrostatic spinning, and wherein, spinning speed is 0.001mm/s ~ 0.01 mm/s, spinning voltage is 5 ~ 20kV, and receiving range is 10 ~ 20cm, orifice diameter 0.1 ~ 0.7mm, spinning temperature is room temperature, and the spinning time is 0.5 ~ 2h.
Beneficial effect of the present invention:
The present invention adopts electrostatic spinning technique, has that production efficiency is high, simple process, reproducible feature, and obtain photochromic refuse water nonwoven fabric have photochromic, refuse the functional characteristics such as water.The method technique is simple, can give nonwoven fabric photochromic and refuse the functions such as water.
Accompanying drawing explanation
Fig. 1 is photochromic nonwoven fabric and the common PVDF nonwoven fabric scanning electron microscope (SEM) photograph (amplifying 50000 times) of the embodiment of the present invention 1 preparation.As seen from Figure 1, weaving face fabric presents threadiness, and fiber surface is uneven, and the average diameter of fiber is 0.6 μm.
Fig. 2 is the photochromic contact angle refusing water nonwoven fabric prepared by the embodiment of the present invention 2, the photochromic contact angle refusing water surface material first increases rear reduction along with the increase adding Luo oxazine concentration, fabric average contact angle is 130 °, and the spiral shell oxazine of variable concentrations has impact to contact angle.
Detailed description of the invention
The invention provides and a kind of photochromicly refuse water weaving face fabric, its raw material comprises N, dinethylformamide (DMF), acetone, PVDF He Luo oxazine, wherein, the volume ratio of DMF and acetone is 1:10 ~ 1:1, the mass ratio of PVDF and acetone and DMF mixed liquor is the mass ratio of 1:10 ~ 1:1, PVDF Yu Luo oxazine is 60 ~ 200.
Described Luo oxazine is N-methyl-3,3-dimethyl-9 '-hydroxyl spiral shell [2H-indoles-2,3 '-[3H] naphtho-[2,1-b] [Isosorbide-5-Nitrae] oxazine].
Present invention also offers the above-mentioned photochromic preparation method refusing water weaving face fabric, first use 1-nitroso-2,7-dihydroxy naphthlene and 1,3,3-trimethyl-2-methylene indoline Reactive Synthesis photochromic spirooxazine N-methyl-3,3-dimethyl-9 '-hydroxyl spiral shell [2H-indoles-2,3 '-[3H] naphtho-[2,1-b] [Isosorbide-5-Nitrae] oxazine], again Jiang Luo oxazine and PVDF in proportion mixed dissolution in the mixed solution of acetone and DMF, obtained by electrostatic spinning.
The above-mentioned photochromic preparation method refusing water weaving face fabric of the present invention, comprises the steps:
1) by 1-nitroso-2, 7-dihydroxy naphthlene is dissolved in ethanol, pass into nitrogen and be heated to 80 ~ 100 DEG C of reflux states, dropwise 1 is added after 5 ~ 30 minutes, 3, the mixed solution of 3-trimethyl-2-methylene indoline and ethanol, dropwise in 15 ~ 60 minutes, in nitrogen atmosphere, keep reflux state and constantly stir, react complete after 1 ~ 10h, add 5 ~ 10% active carbon backflow 5 ~ 30 minutes, filter while hot, filtrate decompression is distilled, after removing most of ethanol, it is allowed naturally to cool and hold over night, filter and separate out product and repeatedly wash with ethanol or be recrystallized, vacuum drying oven drying finally obtains pale solid N-methyl-3 afterwards, 3-dimethyl-9 '-hydroxyl spiral shell [2H-indoles-2, 3 '-[3H] naphtho-[2, 1-b] [1, 4] oxazines], wherein, 1-nitroso-2, 7-dihydroxy naphthlene is 0.01mol ~ 0.1mol, ethanol is 50mL ~ 200mL, 1, 3, the mixed solution of 3-trimethyl-2-methylene indoline 0.01mol ~ 0.1mol and ethanol 10mL ~ 30mL,
2) spinning solution preparation: by step 1) synthesize Luo oxazine and mix with PVDF, be dissolved in vol acetone/DMF mixed liquor again, solution temperature 20 ~ 80 DEG C, magnetic agitation 1 ~ 3h, wherein Luo oxazine and PVDF mass ratio are 60 ~ 200, and acetone and DMF mass ratio are 1:10 ~ 1:1, PVDF and mixed solution mass ratio is 1:10 ~ 1:1;
3) spinning solution is carried out electrostatic spinning, cylinder receives, and spinning time 0.5 ~ 2h, wherein, voltage 5 ~ 20kV, receiving range 10 ~ 20cm, spinning speed 0.001mm/s ~ 0.01 mm/s, spinning temperature is room temperature, and orifice diameter is 0.1 ~ 0.7mm.
The present invention's design has the PVDF fiber non-woven fabric of photochromic properties, and its scanning electron microscope (SEM) photograph is shown in Fig. 1, and fabric is irregular threadiness, surface irregularity.
Below by embodiment, the present invention is specifically described; it is important to point out that embodiment is only for further illustrating of the present invention; can not be interpreted as limiting the scope of the invention, these those skilled in the art can make some nonessential improvement and adjustment according to the present invention.
embodiment 1
By 5.67g(0.03mol) 1-nitroso-2,7-dihydroxy naphthlene is dissolved in 140mL ethanol, pass into nitrogen and be heated to 90 DEG C of reflux states, dropwise 5.2g(0.03mol is added after 15 minutes) 1,3, the mixed solution of 3-trimethyl-2-methylene indoline and 25mL ethanol, dropwised in 30 minutes.In nitrogen atmosphere, keep reflux state and constantly stir.React complete after 5h, add 5% active carbon and reflux 15 minutes, filter while hot, filtrate decompression is distilled, after removing most of ethanol, allow it naturally cool and hold over night.Filter and separate out product and repeatedly wash with ethanol or be recrystallized, vacuum drying oven drying finally obtains pale solid N-methyl-3,3-dimethyl-9 afterwards '-hydroxyl spiral shell [2H-indoles-2,3 '-[3H] naphtho-[2,1-b] [Isosorbide-5-Nitrae] oxazine].1.23gPVDF and 0.012g Luo oxazine is mixed, is dissolved in the mixed solution of 3mL acetone and 7 mLDMF, solution temperature 40 DEG C, time 2h.Get 5mL mixing material electrostatic spinning, cylinder receives, and spinning time 1.5h, voltage 10kV, receiving range 15cm, spinning speed 0.001mm/s, spinning temperature is room temperature, and orifice diameter is 0.5mm.
Gained is photochromic refuse the microstructure of water surface material and macro property as follows:
1, the microscopic appearance of photochromic fibre:
Fig. 1 is photochromic ESEM (SEM) photo refusing water non-woven fibre.As seen from Figure 1, photochromic water nonwoven fabric of refusing is in threadiness, and fiber surface is uneven, and average fibre diameter is 0.6 μm;
2, the photochromic color changeable effect refusing water surface material:
Table 1 is not for adding color space values (L*, a*, b*) and the two value of chromatism (△ E) of the nonwoven fabric of Luo oxazine nonwoven fabric and interpolation 1.2g/l Luo oxazine.Value of chromatism is larger, show that color changeable effect is better, it is blue that b* value is less than null representation color deflection, do not add a* and the b* value of Luo oxazine all close to 0, illustrate that nonwoven fabric is in white, and the nonwoven fabric b* value after illumination that with the addition of Luo oxazine is clearly less than zero, and absolute value is comparatively large, and the color changeable effect of the aberration △ E value also photochromic nonwoven fabric of larger explanation is better;
The photochromic nonwoven fabric colour space of table 1 Luo oxazine and aberration
| Luo oxazine concentration (g/l) | L* | a* | b* | △E |
| 0 | 93.5 | -0.18 | -0.24 | |
| 1.2 | 80.28 | -4.05 | -9.19 | 16.4325 |
3, the photochromic fading time refusing water surface material:
The photochromic fading time refusing water surface material is 15 minutes, i.e. 15 minutes metachroic nonwoven fabrics but also can return back to reset condition.
To sum up the photochromic water nonwoven fabric of refusing of ， Luo oxazine has fibre structure, and average fibre diameter is 0.6 μm.And photochromic effect is better, fading time is 15 minutes.
embodiment 2
By 5.67g(0.03mol) 1-nitroso-2,7-dihydroxy naphthlene is dissolved in 140mL ethanol, pass into nitrogen and be heated to 90 DEG C of reflux states, dropwise 5.2g(0.03mol is added after 15 minutes) 1,3, the mixed solution of 3-trimethyl-2-methylene indoline and 25mL ethanol, dropwised in 30 minutes.In nitrogen atmosphere, keep reflux state and constantly stir.React complete after 5h, add 5% active carbon and reflux 15 minutes, filter while hot, filtrate decompression is distilled, after removing most of ethanol, allow it naturally cool and hold over night.Filter and separate out product and repeatedly wash with ethanol or be recrystallized, vacuum drying oven drying finally obtains pale solid N-methyl-3,3-dimethyl-9 afterwards '-hydroxyl spiral shell [2H-indoles-2,3 '-[3H] naphtho-[2,1-b] [Isosorbide-5-Nitrae] oxazine].1.23gPVDF is mixed with 0.008g, 0.01g, 0.012g, 0.014g, 0.016g Luo oxazine respectively, and is dissolved in the mixed solution of 3mL acetone and 7mLDMF respectively, solution temperature 40 DEG C, time 2h.Respectively get 5mL mixing material electrostatic spinning, cylinder receives, and spinning time 1.5h, voltage 10kV, receiving range 15cm, spinning speed 0.001mm/s, spinning temperature is room temperature, and orifice diameter is 0.5mm.Adding different Luo oxazine affects as shown in table 2 on the photochromic photochromic effect refusing water nonwoven fabric.
Table 2 adds the photochromic effect of different Luo oxazine
As shown in Table 2, along with the concentration of Luo oxazine increases, aberration first raises and reduces, and namely color changeable effect first increases and reduces, and variable concentrations Luo oxazine has impact to photochromic effect.
Claims (8)
1. photochromicly refuse water nonwoven fabric for one kind, it is characterized in that, its raw material comprises N, dinethylformamide (DMF), acetone, (PVDF) is with Luo oxazine for poly-inclined tetrafluoroethylene, wherein, the mass ratio of the volume ratio of DMF and acetone to be the mass ratio of 1:10 ~ 1:1, PVDF and acetone and DMF mixed liquor be 1:10 ~ 1:1, PVDF Yu Luo oxazine is 60 ~ 200.
2. photochromic material Luo oxazine according to claim 1, is characterized in that, described photochromic spirooxazine is N-methyl-3,3-dimethyl-9 '-hydroxyl spiral shell [2H-indoles-2,3 '-[3H] naphtho-[2,1-b] [Isosorbide-5-Nitrae] oxazine].
3. the photochromic preparation method refusing water nonwoven fabric described in any one of claim 1-2, it is characterized in that, first by 1-nitroso-2,7-dihydroxy naphthlene and 1,3,3-trimethyl-2-methylene indoline the hold over night after 1 ~ 10h that refluxes in nitrogen atmosphere obtains photochromic material Luo oxazine, then PVDF Yu Luo oxazine is mixed in 20 ~ 80 DEG C according to aforementioned proportion and is dissolved in acetone/DMF mixed liquor, get 1 ~ 10mL electrostatic spinning 0.5 ~ 2h under 5 ~ 20kV voltage.
4. the photochromic preparation method refusing water nonwoven fabric according to claim 3, is characterized in that, described in refuse water nonwoven fabric be PVDF; Described photochromic material is N-methyl-3,3-dimethyl-9 '-hydroxyl spiral shell [2H-indoles-2,3 '-[3H] naphtho-[2,1-b] [Isosorbide-5-Nitrae] oxazine].
5. the photochromic preparation method refusing water nonwoven fabric according to claim 3, is characterized in that, the preparation method of described uniform spinning solution is that: is Jiang Luo oxazine, PVDF, acetone and DMF in 20 ~ 80 DEG C of magnetic agitation 1 ~ 3h.
6. the preparation method of photochromic nonwoven fabric according to claim 3, is characterized in that, comprise the steps:
1) by 1-nitroso-2, 7-dihydroxy naphthlene is dissolved in ethanol, pass into nitrogen and be heated to 80 ~ 100 DEG C of reflux states, dropwise 1 is added after 5 ~ 30 minutes, 3, the mixed solution of 3-trimethyl-2-methylene indoline and ethanol, dropwise in 15 ~ 60 minutes, in nitrogen atmosphere, keep reflux state and constantly stir, react complete after 1 ~ 10h, add 5 ~ 10% active carbon backflow 5 ~ 30 minutes, filter while hot, filtrate decompression is distilled, after removing most of ethanol, it is allowed naturally to cool and hold over night, filter and separate out product and repeatedly wash with ethanol or be recrystallized, vacuum drying oven drying finally obtains pale solid N-methyl-3 afterwards, 3-dimethyl-9 '-hydroxyl spiral shell [2H-indoles-2, 3 '-[3H] naphtho-[2, 1-b] [1, 4] oxazines], wherein, 1-nitroso-2, 7-dihydroxy naphthlene is 0.01mol ~ 0.1mol, ethanol is 50mL ~ 200mL, 1, 3, the mixed solution of 3-trimethyl-2-methylene indoline 0.01mol ~ 0.1mol and ethanol 10mL ~ 30mL,
2) by step 1) synthesize Luo oxazine and mix with PVDF, be dissolved in vol acetone/DMF mixed liquor again, solution temperature 20 ~ 80 DEG C, magnetic agitation 1 ~ 3h, wherein Luo oxazine and PVDF mass ratio are 60 ~ 200, and acetone and DMF mass ratio are 1:10 ~ 1:1, PVDF and mixed solution mass ratio is 1:10 ~ 1:1.
7. the preparation method of photochromic nonwoven fabric according to claim 6, is characterized in that, step 1) described in 1-nitroso-2,7-dihydroxy naphthlene and 1,3,3-trimethyl-2-methylene indoline, its mol ratio is 1:1 ~ 2:1.
8. the preparation method of photochromic nonwoven fabric according to claim 6, it is characterized in that, step 2) in spinning speed be 0.001mm/s ~ 0.01 mm/s, spinning voltage is 5 ~ 20kV, receiving range is 10 ~ 20cm, orifice diameter 0.1 ~ 0.7mm, spinning temperature is room temperature, and the spinning time is 0.5 ~ 2h.
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