CN1473987A - Method for preparing nano particle modified chemical fibre - Google Patents
Method for preparing nano particle modified chemical fibre Download PDFInfo
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- CN1473987A CN1473987A CNA031418236A CN03141823A CN1473987A CN 1473987 A CN1473987 A CN 1473987A CN A031418236 A CNA031418236 A CN A031418236A CN 03141823 A CN03141823 A CN 03141823A CN 1473987 A CN1473987 A CN 1473987A
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Abstract
The method of preparing nano particle modified chemical fiber features that nano particles after surface treatment in certain proportion is added into and dispersed in solidifying bath, preheating bath or extracting bath for wet spinning or wet-dry spinning via high speed stirring to form bathing liquid with homogeneously dispersed nano particles. After eliminating solvent and drawing, nano particles are diffused into fiber pores, and the nano particle modified chemical fiber possesses raised drawing performance. The said method is simple, low in cost and suitable for industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of chemical fibre, be specifically related to a kind of preparation method who adopts nanometer particle-modified chemical fibre.
Background technology
Nano particle has big specific area, surface atom number, surface energy and surface tension sharply increase with the decline of particle diameter, and small-size effect, skin effect, quantum size effect and macro quanta tunnel effect etc. cause nanoparticle to be different from conventional particle at aspects such as mechanical property, thermal property, magnetic performance, optical property and electric properties.Nano particle is joined in the chemical fibre, these functions can be imparted among the fiber, make nanometer particle-modified chemical fibre.Adopt the different nanoparticle of performance, can develop various functional fibers such as antibiotic, fire-retardant, anti-ultraviolet, far infrared, negative-oxygen ion health, antistatic and electromagnetic shielding, or improve the heat resistance or the mechanical property of fiber.
Prepare nano-material modified chemical fibre, the simplest method is exactly a finishing method.As:
Among the Chinese patent CN93114055 fabric panels such as cotton, fiber crops, silk, synthetic fiber are flooded in the solution of fluoride, organo-silicon compound, surfactant, adhesive, nano ceramics, water and other mixing, slough after the excessive solution 50～200 ℃ of dry down, typings, make have waterproof and dustproof, hate oil, the fabric of ultraviolet resistance; Be mixed with earlier the dressing liquid of nano-tourmaline particulate, far-infrared powder, emulsifying agent and adhesive among the Chinese patent CN00132606 by a certain percentage, then with this dressing liquid to fabric pad, coating or spray treatment, make fabric with health-care far infrared and negative oxygen ion function.
But above-mentioned back finishing technique exists the cohesion and the absorption stability problem of nanometer ultrafine particle, and the fabric of handling can influence its function of use because of washing.Prepare the permanent function nona modified fiber, will be with nano-particles filled in fibrous inside.
In fibrous inside, Chang Yong method is the co-blended spinning method the most with nano-particles filled, comprises melt blending spin processes and solution blending spin processes.
The melt blending spinning is earlier nano particle to be dispersed in the polymer melt, carries out spinning, drawing-off then on traditional spinning equipment, makes nanometer particle-modified fiber, and need not to increase miscellaneous equipment.As among the Chinese patent CN01108688 surface treated nano particle and polyethylene terephthalate being carried out common grinding in the special reaction device, then by a certain percentage with the polyethylene terephthalate melt blending, the preparation polyethylene terephthalate/nano-composite fiber; Among the Chinese patent CN02111209 polyester or modified poly ester and promoter, nano-powder tertiary blending melt-spun are made anti-electrostatic nano compound polyester fibre.
Because nano particle very easily reunites, the polymeric matrix melt viscosity is bigger again, so depends merely on the mechanical blending effect in the said method and be difficult to make nano particle to reach nanoscale in polymeric matrix to disperse, thereby influences spinning, the tensile property of blend.
The solution blending spinning is earlier nano particle to be dispersed in the spinning solution, carries out spinning again, desolvates, draft process makes nanometer particle-modified fiber.As earlier nano particle being carried out being dispersed in the spin solvent of ultra high molecular weight polyethylene (UHMWPE) after the surface treatment among the Chinese patent CN02148597, adding the UHMWPE powder then carries out swelling, dissolves and make spinning solution, carry out spinning again, stretch and make nanometer particle-modified UHMWPE fiber, the mechanical moduli of this fiber can improve 20～70% on the original basis.The nano-powder material that will have correlation function among the Chinese patent CN01128377 evenly is blended in the artificial viscose solution carrier, handles through the spray silk and makes the functional artificial viscose that human skin is had regulating action.
Because nano particle is very easily reunited, even after surface treatment and ultrasonic strong dispersion, the aggregate that also has nano particle unavoidably is present in the spinning solution, thereby influences its spinnability and draftability.
In order effectively to solve the even scattering problem of nano particle in the polymer body, people have proposed the compound new method of in-situ polymerization, promptly on the nano particle of polymolecularity, be written into component, and then on this nanoparticle surface, carry out polymerisation and prepare in-situ composite with catalytic activity.As disclosing the nanocomposite of a kind of polyolefin and clay among Chinese patent CN1255510A and the U.S. Pat P6444742, this composite is made up of the polyethylene of 40～99.9 heavy % and the fiber rod stone kind clay of 0.1～60 heavy %, transistion metal compound with the nanoscale clay is a catalyst, with the organo-aluminum compound is co-catalyst, carry out the in-situ polymerization of alkene, prepared composite has excellent mechanical property and hot property.Chinese patent CN01142857 discloses a kind of preparation method of nano composite polyester, be mixed with earlier the mixed liquor of nano zine oxide, nano barium sulfate, ethylene glycol and terephthalic acid (TPA) by a certain percentage, add catalyst and stabilizing agent then and carry out polymerization, discharging, make nano composite polyester.The in-situ polymerization composite algorithm can make nano particle be dispersed in the polymeric matrix uniformly, but this method is comparatively loaded down with trivial details, and the cost of gained composite is higher, and the spinning properties of gained nano composite polymer awaits further to study.
Summary of the invention
The technical issues that need to address of the present invention are the preparation methods that disclose a kind of comparatively easy nanometer particle-modified chemical fibre, to overcome the above-mentioned defective that prior art exists, satisfy the needs in relevant field.
Technical conceive of the present invention is such:
The fiber that reaches of the present invention is limited to wet method or dried wet method spins the fiber that forms, be characterized in surface treated nano particle is joined by a certain percentage the coagulating bath of wet spinning or dry-wet spinning, in pre-heating bath or the extraction bath, carrying out high-speed stirred disperses and ultrasonic dispersion certain hour, the homodisperse body lotion of preparation nano particle, to substitute the coagulating bath of wet spinning or dry-wet spinning, pre-heating bath or extraction bath, make nano particle diffuse into fiber by means of diffusion and desolventize in the micropore that the back forms, postprocessing working procedures such as stretched is then made the homodisperse fiber of nano particle.Can be made into according to the difference that adds nano particle have antibiotic, fire-retardant, anti-ultraviolet, various functional fibers such as far infrared, negative-oxygen ion health, antistatic and electromagnetic shielding, or improve the heat resistance and the mechanical property of fiber.
The inventive method comprises the steps: that wherein described raw material portion rate is the weight fraction ratio except that specified otherwise.
(1) nano particle evenly disperses the preparation of body lotion:
Will be through the nano particle after surface treatment or the modification or its mixture, with media such as coagulating bath, pre-heating bath or extractants, by 0.5～5: carry out high-speed stirred 10～30min in the 100 adding containers, carry out sonicated 20～40min again, nano particle is evenly disperseed in decentralized medium, obtain nano particle and evenly disperse body lotion;
Said nano particle is a zero-dimension nano level inorganic particulate, average grain diameter is 10～100nm, preferred Nano Silver, silica, titanium dioxide, aluminium oxide, zinc oxide, calcium carbonate, barium sulfate, crude tourmaline or very ice a kind of and composition thereof in the stone powder;
Term " surface treatment or modification " refers in solvent surfactant is covered in nanoparticle surface, give particle surface with new character, as in isopropyl alcohol, ethanol or acetone, surfactants such as titanate ester, silane coupling agent, aluminate, hard acid ester salt or laruate being covered in the inorganic nano-particle sub-surface, can adopt the method that provides among the Chinese patent CN02148597 that nano particle is carried out surface treatment or modification, its main purpose is to prevent the nano particle reunion, increases its dispersiveness in decentralized medium.
Coagulating bath, pre-heating bath or the medium that extractant adopted are conventional medium, in this general technical literature report are arranged all.
(2) the nanometer particle-modified chemical fibre of preparation:
Wet spinning or fiber that dry-wet spinning obtains are placed the dispersion body lotion of step (1), make nano particle diffuse into fiber under ultrasonic or static condition and desolventize in the micropore that the back forms, postprocessing working procedures such as stretched is then made the homodisperse fiber of nano particle;
The polyacrylonitrile fibre that described chemical fibre comprises, viscose, ultra high molecular weight polyethylene fiber, vinal and aramid fiber etc.;
Fiber time of staying in coagulating bath, pre-heating bath or extraction bath is 0.2～5min under the ultrasonic state, and under the static condition fiber time of staying in coagulating bath, pre-heating bath or extraction bath be 3～30min.
Key technology of the present invention is to make nano particle diffuse into fiber by diffusion to desolventize in the back micropore that forms, because wet spinning or the formed pore size of dry-jet wet-spinning fiber removal solvent are generally nanoscale, even have the nano particle aggregate to exist in then coagulating bath, pre-heating bath or the extraction bath, the nano particle aggregate also is difficult for diffusing into fibrous inside.Therefore adopt the prepared nanometer particle-modified chemical fibre of method of the present invention, nano particle in fiber, to reach the nanoscale dispersion, thereby improved the tensile property of fiber.The preparation method is comparatively simple, and cost of manufacture is lower, is convenient to industrializing implementation.
Description of drawings
Fig. 1 is the cross section stereoscan photograph that contains the nano particle polyethylene fiber.
The specific embodiment
Embodiment 1
Surface treated nano silicon and dimethylbenzene joined in 1: 100 ratio carry out high-speed stirred 20min in the container that has supersonic generator, make the homodisperse extract of nano particle, the polyethylene gel fiber is placed in one under static condition, carries out altogether 20min of twice extraction, carry out drying at room temperature then.The dry freeze glue fiber is carried out 12 times one-level stretching under 100 ℃, carry out 2 times of secondary drawing under 110 ℃, carry out 1.4 times of three grades of stretchings under 120 ℃, the intensity of gained fiber is 30.5cN/dtex, and modulus is 1720cN/dtex, and extension at break is 3.31%.And with the polyethylene gel fiber in the extraction bath that does not contain nano particle, under similarity condition, carry out drying then in extraction under the similarity condition, the fibre strength make that stretches is 29.6cN/dtex, modulus is 1170cN/dtex, extension at break is 3.83%.The cross section stereoscan photograph of fiber as shown in Figure 1 after one-level stretched.
Embodiment 2
Each 2 parts of surface treated nano-tourmaline particulates, nano titanium dioxide particles are joined in 98 parts of aqueous solution that contain 3% sodium sulfocyanate, and high-speed stirred 20min under ultrasonic state makes the homodisperse pre-heating bath of nano particle.
The polyacrylonitrile as-spun fibre that goes out coagulating bath enters in the above-mentioned pre-heating bath, bathing temperature is 55 ℃, stretches 1.5 times under ultrasonic state, and fiber time of staying in pre-heating bath is 1min, carry out two roads afterwards and stretch, wash and other postprocessing working procedures, make the acrylic fiber that contains nano particle.The average negative oxygen ion number of final products release is 150/cm after testing
3, far infrared transmissivity is 83%, it is 81% to colibacillary bacteriostasis rate, is 77% to the bacteriostasis rate of staphylococcus aureus.
Claims (8)
1. the preparation method of a nanometer particle-modified chemical fibre is characterized in that, comprises the steps:
(1) will be through the nano particle after surface treatment or the modification or its mixture, with coagulating bath, pre-heating bath or extractant medium, add in the container and carry out high-speed stirred, carry out sonicated again, nano particle is evenly disperseed in decentralized medium, obtain nano particle and evenly disperse body lotion;
(2) wet spinning or as-spun fibre that dry-wet spinning obtains are placed the dispersion body lotion of step (1), under ultrasonic or static condition, make nano particle diffuse into fiber and desolventize in the back micropore that forms, adopt conventional postprocessing working procedures to make the homodisperse fiber of nano particle then.
2. the preparation method of nanometer particle-modified chemical fibre according to claim 1, it is characterized in that, will be through the nano particle after surface treatment or the modification or its mixture, with coagulating bath, pre-heating bath or extractant medium, by 0.5～5: carry out high-speed stirred 10～30min in the 100 adding containers, carry out sonicated 20～40min again, described raw material umber is the weight fraction ratio.
3. the preparation method of nanometer particle-modified chemical fibre according to claim 1 is characterized in that, said nano particle is a zero-dimension nano level inorganic particulate.
4. the preparation method of nanometer particle-modified chemical fibre according to claim 3 is characterized in that, the nano particle average grain diameter is 10～100nm.
5. the preparation method of nanometer particle-modified chemical fibre according to claim 3, it is characterized in that nano particle is Nano Silver, silica, titanium dioxide, aluminium oxide, zinc oxide, calcium carbonate, barium sulfate, crude tourmaline or very ices a kind of and composition thereof in the stone powder;
6. the preparation method of nanometer particle-modified chemical fibre according to claim 1, it is characterized in that described chemical fibre comprises a kind of in polyacrylonitrile fibre, viscose, ultra high molecular weight polyethylene fiber, vinal or the aramid fiber of wet spinning or dry-wet spinning.
7. according to the preparation method of each described nanometer particle-modified chemical fibre of claim 1～6, it is characterized in that fiber time of staying in coagulating bath, pre-heating bath or extraction bath is 0.2～5min under the ultrasonic state.
8. according to the preparation method of each described nanometer particle-modified chemical fibre of claim 1～6, it is characterized in that fiber time of staying in coagulating bath, pre-heating bath or extraction bath is 3～30min under the static condition.
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| CN1293257C (en) * | 2005-06-16 | 2007-01-03 | 浙江新阳服饰股份有限公司 | Technique for fabricating antibacterial Nano knitted dress of preventing acarus |
| CN100395395C (en) * | 2005-08-04 | 2008-06-18 | 东华大学 | Nano functional textile finishing method |
| CN102677206A (en) * | 2012-05-14 | 2012-09-19 | 毛盈军 | Fiber warming and heating naturally under moist condition, preparation method and textile |
| CN102677205A (en) * | 2012-05-14 | 2012-09-19 | 毛盈军 | Fiber warming and heating naturally under moist condition, preparation method and textile |
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| CN102912466A (en) * | 2012-05-14 | 2013-02-06 | 毛盈军 | Fiber for warming and heat accumulation and preparation method of fiber and textile |
| CN101910257B (en) * | 2007-12-14 | 2013-04-03 | 罗狄亚聚酰胺特殊品有限公司 | Polymeric composition, method for the manufacture of the polymeric composition, articles based on this polymeric composition and use of these articles |
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| CN103556309A (en) * | 2013-10-30 | 2014-02-05 | 吴江市科时达纺织有限公司 | Method for preparing chemical fibers of nano-silver coagulating bath |
| CN103741249A (en) * | 2013-12-31 | 2014-04-23 | 马海燕 | Large-diameter polyvinyl alcohol monofilament and production method thereof |
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| CN110241470A (en) * | 2019-06-27 | 2019-09-17 | 浙江天祥新材料有限公司 | A kind of cool feeling process for colored profiled PET filament |
| CN110616467A (en) * | 2019-06-27 | 2019-12-27 | 浙江天祥新材料有限公司 | Antibacterial colored special-shaped polyester filament yarn |
| CN110616482A (en) * | 2019-06-27 | 2019-12-27 | 浙江天祥新材料有限公司 | Flame-retardant flashing colored textured yarn |
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