CN107142546B - The compound polyester functional fibre of a kind of far infrared, antibacterial mite-removing and its manufacturing method - Google Patents
The compound polyester functional fibre of a kind of far infrared, antibacterial mite-removing and its manufacturing method Download PDFInfo
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- CN107142546B CN107142546B CN201710420970.0A CN201710420970A CN107142546B CN 107142546 B CN107142546 B CN 107142546B CN 201710420970 A CN201710420970 A CN 201710420970A CN 107142546 B CN107142546 B CN 107142546B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/02—Oxides
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/02—Oxides
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- C01G3/00—Compounds of copper
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
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Abstract
This application involves a kind of far infrared, the compound polyester functional fibre of antibacterial mite-removing and its manufacturing methods, added with far infrared additive and antibacterial mite-removing additive in the compound polyester functional fibre, the far infrared additive and antibacterial mite-removing additive quality accounting in compound polyester functional fibre are respectively 5%, 7%；The compound polyester functional fibre of the present invention contains far infrared additive and antibacterial mite-removing additive, can absorb far infrared radiation, while achieving the purpose that fever, can also have stronger antibacterial mite-removing effect, highly practical；By the setting of additive carrier, the far infrared additive and antibacterial mite-removing additive can be dispersed in polyester fiber, effectively prevent the agglomeration of nano-particle.
Description
Technical field
This application involves polyester fiber and its manufacturing technology field more particularly to a kind of far infrared, antibacterial mite-removing are compound
Polyester functional fibre and its manufacturing method.
Background technology
Polyethylene terephthalate (PET) abbreviation polyester since it is with excellent characteristic, receives people's favor,
In recent years, development of the polyester in fiber and non-fiber field is all very fast, and demand is growing；The polyester of industrial mass production is fine
Dimension is made of polyethylene terephthalate, is widely used in textile industry, is manufacture clothes, bedding, interior
The important source material of the fabrics such as decoration, carpet, due in its application process, easily growing bacterium, therefore, to polyester textile fiber into
Row is modified, and makes it have antibacterial mite-removing effect, has larger practical application meaning.
Far-infrared polyester fiber can absorb the electromagnetic wave that environment or human-body emitting go out in very wide wave-length coverage, and radiate
Go out far infrared of the wave-length coverage in 2.5~30m.This is because that is added on polyester fiber has adding for function far infrared radiation function
Adding agent, the energy state of molecule is from low-lying level to high energy order transition, then and never after extraneous electromagnetic radiation energy is absorbed
The high level of stable state is returned to relatively low stable state energy level and gives off far infrared.It is given off by far-infrared polyester fiber
In electromagnetic wave, the far infrared in a wavelength range is identical with the vibration frequency of hydrone in human body cell, when human body table
When face is radiated, the molecular resonance of cell can be caused, generate fuel factor, and human activin superficial cell, promote human body subcutaneous
The microcirculation of tissue blood, the effect of reaching warming, health care, boost metabolism, improve the immunity of the human body.Far-infrared polyester is fine
Dimension has heat accumulation thermal, health care and antibacterial functions.
It is right by adding the substance with far infrared, antibacterial mite-removing effect during polyester fiber functionalization is realized
There is realistic meaning in the functionalized application for realizing polyester fiber；The fabric with functionalization is mainly logical on the market at present
It crosses additive to realize, as patent 201110261719.7 reports a kind of processing side of permanent seal cooling antibacterial and deodouring fabric
Method, this method are to be added to nanometer grade inorganic antibacterial agent in high polymer powder with 3%-30% weight ratios, are uniformly mixed, pass through spiral shell
Bar granulating technique forms antibacterial matrices, antibacterial matrices is mixed with the ratio of 0.3%-10% with high polymer, spinning, by spinning
Fabric is formed after weaving, using antiseptic final finishing, the fabric processed using the method for the invention has antibacterial effect
Well, the advantages of persistence is strong；However, by the way that additive is added directly into melt spinning existing defects in fibre section, for example,
Since the grain size of additive is smaller, surface-active and free energy are higher, and thermodynamic state is unstable, have becoming for spontaneous reunion
Gesture, easily conglomerate, this will largely effect on the performance of functional particle advantage in polyester fiber, and polyester fiber is caused to be modified effect
Fruit unobvious.
The content of the invention
Based on it is set forth above the technical issues of, this application involves the compound polyester function of a kind of far infrared, antibacterial mite-removing is fine
Dimension and its manufacturing method.
It on the one hand, should added with far infrared additive and antibacterial mite-removing additive in the compound polyester functional fibre
Far infrared additive and antibacterial mite-removing additive the quality accounting in compound polyester functional fibre are respectively 5%, 7%；It is above-mentioned
The far infrared additive is constituted by the following substances：Additive carrier, ZrO2Nano-powder；Antibacterial mite-removing described above adds
Add agent constituted by the following substances：Additive carrier, cuprous oxide, titanium dioxide nano-particle, zinc oxide nano-particle, titanium dioxide
Silicon nano, silver iodide nanoparticle；Wherein, additive carrier described above is SnO2Hollow ball, the SnO2Hollow ball is
It is prepared using pollen as template, using hydro-thermal method.
On the other hand, the manufacturing method of the compound polyester functional fibre of a kind of far infrared described above, antibacterial mite-removing：
Step 1, additive carrier is prepared
Prepare the absolute ethyl alcohol of 200ml, then add in the chlorination tin powder (SnCl of 18.5g wherein4·5H2O), constantly
It stirs to clarify, obtains precursor solution；Then the rape petal pollen of 50 μm of diameter is filtered out, by the rape petal pollen of 19.5g
It with alcohol rinsed clean, dries, rape petal pollen is put into above-mentioned precursor solution, strong stirring 20h, by solution centrifugation point
From, alcohol washes three times, the dry 5h in 60 DEG C of drying box；Then above-mentioned processed pollen is placed into precursor solution
Middle immersion 4h, solution is centrifuged, and gained pollen is put into 100ml alcohol by ethanol wash three times：Water (volume ratio 1:1) it is molten
3h is hydrolyzed in liquid, is dispersed in after centrifugation in alcoholic solution, the dry 3h in 60 DEG C of drying box；Finally by pollen in air
580 DEG C of annealing 2h in stove so as to remove pollen template, collect white powder and obtain SnO2Hollow ball is additive carrier；
In the preparation process of additive carrier, pollen, which is put into precursor solution, to be impregnated twice, ensures pollen covering one
The uniform SnO of layer2Layer；
Step 2, ZrO is prepared2Nano-powder
Compound concentration is the ZrOCl of 720g/L, 94g/L respectively2·8H2O and edta solution take suitable two
Kind solution is mixed, and being vigorously stirred 5min is uniformly mixed it, obtains transparent microemulsion, and pH ＞ 10.5 are adjusted with ammonium hydroxide,
Ultrasound 10min obtains transparent gel under 65 DEG C, 30kHz, is then washed with distilled water gel to using AgNO3Solution detects not
Go out Cl-, then washed 3 times with ethyl alcohol, the zirconium oxide precursor solution after washing be put into thermostatic drying chamber, done at 60 DEG C
Dried presoma is calcined 4h by dry 15h at 700 DEG C under nitrogen protection, is finally removed nitrogen protection and is made powder natural
It is cooled to room temperature, obtains ZrO2Nano-powder；
Step 3, far infrared additive is prepared
By additive carrier, ZrO2Nano-powder, titanate coupling agent are added in example water, are stirred,
Far infrared additive slurry is obtained, is then baked to, is pulverized to get far infrared additive；
Step 4, cuprous oxide is prepared
The cupric sulfate pentahydrate of 2.5g is taken to be dissolved in the distilled water of 20ml, 40ml is then added in the case where continuously stirring
Sodium hydroxide (0.8g, 0.5mol/L, 0.75M) formed Kocide SD precipitation, in the case of then continuously stirring at room temperature
The ascorbic acid solution of 0.5g, 40ml are added in, 2h is stirred, 20min is centrifuged under 2000rpm, finally with distilled water and absolute ethyl alcohol
It washs, dry 10h, obtains cuprous oxide at 85 DEG C；
Step 5, antibacterial mite-removing additive is prepared
By additive carrier, cuprous oxide, titanium dioxide nano-particle, zinc oxide nano-particle, silica dioxide nano particle
Son, silver iodide nanoparticle, titanate coupling agent are mixed to join in example water, and ultrasonic agitation is uniform, obtains antibacterial mite-removing
Then additive slurry is baked to, pulverize to get antibacterial mite-removing additive；
Step 6, polyester fiber is prepared
Far infrared additive, antibacterial mite-removing additive and ethylene glycol are mixed, ultrasound 5h at room temperature after stirring is mixed
Liquid is closed, PTA, mixed liquor, catalyst aid are then added in reaction kettle of the esterification, is esterified after stirring evenly, polymerize, is gathered
Ester master batch, wherein, esterification temperature is 280 DEG C, pressure 400KPa, and polycondensation reaction is carried out when esterification yield reaches more than 93.5%, is contracted
Poly- temperature is 300 DEG C, is evacuated to 50Mpa, and when polycondensation to inherent viscosity is 0.65, discharging, blank obtains polyester master particle, then passes through
Spinning obtains polyester fiber, is a kind of far infrared, the compound polyester functional fibre of antibacterial mite-removing of the application.
The technical solution that the embodiment of the present invention provides can include the following benefits：
The compound polyester functional fibre of the present invention contains far infrared additive and antibacterial mite-removing additive, can absorb remote
Infra-red radiation while achieving the purpose that fever, can also have stronger antibacterial mite-removing effect, highly practical；Pass through additive
The setting of carrier, the far infrared additive and antibacterial mite-removing additive can be dispersed in polyester fiber, effectively prevent
The agglomeration of nano-particle.
The additional aspect of the application and advantage will be set forth in part in the description, and will partly become from the following description
It obtains substantially or is recognized by the practice of the application.It should be appreciated that above general description and following detailed description are only
It is exemplary and explanatory, the application can not be limited.
Specific embodiment
With reference to specific embodiment, the present invention is further explained.It should be appreciated that these embodiments are merely to illustrate this hair
It is bright rather than limit the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, art technology
Personnel can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Fixed scope.
This application involves a kind of far infrared, the compound polyester functional fibre of antibacterial mite-removing and its manufacturing methods.
It on the one hand, should added with far infrared additive and antibacterial mite-removing additive in the compound polyester functional fibre
Far infrared additive and antibacterial mite-removing additive the quality accounting in compound polyester functional fibre are respectively 5%, 7%.
Far infrared additive described above is constituted by the following substances：Additive carrier, ZrO2Nano-powder；Wherein, far
The mass fraction of each substance is in infrared additive：5 parts of additive carrier, ZrO22 parts of nano-powder；The grain size of each substance is：
50 μm of additive carrier, ZrO2Nano-powder 15nm.
Antibacterial mite-removing additive described above is constituted by the following substances：Additive carrier, cuprous oxide, titanium dioxide are received
Rice corpuscles, zinc oxide nano-particle, Nano particles of silicon dioxide, silver iodide nanoparticle；Wherein, it is each in antibacterial mite-removing additive
The mass fraction of substance is：15 parts of additive carrier, 5 parts of cuprous oxide, 4 parts of titanium dioxide nano-particle, the zinc oxide nano grain of rice
3 parts of son, 1 part of Nano particles of silicon dioxide, 2 parts of silver iodide nanoparticle；The grain size of each substance is：50 μm of additive carrier, oxygen
Change cuprous 5 μm, titanium dioxide nano-particle 100nm, zinc oxide nano-particle 50nm, Nano particles of silicon dioxide 100nm, iodate
Nano silver grain 50nm.
In far infrared additive and antibacterial mite-removing additive described above, contain additive carrier, the additive
Carrier is a kind of SnO2Hollow ball, the SnO2Hollow ball is to be prepared using pollen as template, using hydro-thermal method, then by annealing
Process removes pollen template, so as to obtain SnO2Hollow ball.Pollen is used to be advantageous in that for template：Since pollen surface has
There is the structure of porous layering, the SnO prepared using hydro-thermal method2The structure can be replicated so that the SnO2The surface of hollow ball is favourable
In the absorption of nano-particle, the agglomeration of nano-particle is effectively prevented.
In far infrared additive described above, additive carrier SnO2Hollow ball, far infrared particle are ZrO2Nanometer
Powder.ZrO2Belong to fluorite structure, ZrO2Powder is to make zirconium oxide special cermacis, high grade refractory, optical communication device, new
The basic material of energy and material, ZrO2With low-temperature sintering, ZrO2Nano-powder has as a kind of non-toxic and non-radioactive
The material of Low Temperature Far Infrared emitting performance is a kind of important far infrared additive, still, is directly appended to polyester fiber
In, the control reunited to it is bad, in the application, by SnO2Hollow ball and ZrO2Mixing, due to SnO2Hollow ball surface has excellent
Good porous structure, for ZrO2Absorption and it is homodisperse play a key effect, be conducive to ZrO2Far infrared performance it is equal
Even performance.
In antibacterial mite-removing additive described above, additive carrier SnO2Hollow ball, antibacterial mite-removing particle are oxygen
Change cuprous, titanium dioxide nano-particle, zinc oxide nano-particle, Nano particles of silicon dioxide, silver iodide nanoparticle.Oxidation is sub-
Copper is a kind of p-type semiconductor of cuprite structure, and energy gap is 2.0~2.2eV, in photocatalysis, lithium cell cathode material, too
Sun can be converted, gas sensor, magnetic storage apparatus etc. are widely used, and in terms of fungicide, cuprous oxide is important
Inorganic antiseptic, however, being uniformly dispersed for cuprous oxide in polyester fiber and the compatibility of two-phase interface is to influence
The key factor that its antibacterial action plays, in the technical solution of the application, by SnO2Hollow ball is mixed with antibacterial mite-removing particle, first
First, due to SnO2Hollow ball surface has excellent porous structure, and above-mentioned each antibacterial mite-removing particle can be adsorbed in SnO2It is hollow
Ball surface, secondly as SnO2Hollow ball grain size is larger, and a nanometer agglomeration will not occur in polyester fiber, reduce
Due to influence of the nanometer reunion for antibacterial mite-removing effect.
In addition, in this application, antibacterial mite-removing particle is cuprous oxide, titanium dioxide nano-particle, the zinc oxide nano grain of rice
Son, Nano particles of silicon dioxide, silver iodide nanoparticle, wherein cuprous oxide and silver iodide nanoparticle play main function,
Other particles are dopant, and each particle diameter is Nano grade, can uniformly be adsorbed in SnO2Hollow ball surface,
Collaboration plays antibacterial mite-removing effect.
On the other hand, the manufacturing method of the compound polyester functional fibre of a kind of far infrared described above, antibacterial mite-removing：
Step 1, additive carrier is prepared
Prepare the absolute ethyl alcohol of 200ml, then add in the chlorination tin powder (SnCl of 18.5g wherein4·5H2O), constantly
It stirs to clarify, obtains precursor solution；Then the rape petal pollen of 50 μm of diameter is filtered out, by the rape petal pollen of 19.5g
It with alcohol rinsed clean, dries, rape petal pollen is put into above-mentioned precursor solution, strong stirring 20h, by solution centrifugation point
From, alcohol washes three times, the dry 5h in 60 DEG C of drying box；Then above-mentioned processed pollen is placed into precursor solution
Middle immersion 4h, solution is centrifuged, and gained pollen is put into 100ml alcohol by ethanol wash three times：Water (volume ratio 1:1) it is molten
3h is hydrolyzed in liquid, is dispersed in after centrifugation in alcoholic solution, the dry 3h in 60 DEG C of drying box；Finally by pollen in air
580 DEG C of annealing 2h in stove so as to remove pollen template, collect white powder and obtain SnO2Hollow ball is additive carrier；
In the preparation process of additive carrier, pollen, which is put into precursor solution, to be impregnated twice, ensures pollen covering one
The uniform SnO of layer2Layer；
Step 2, ZrO is prepared2Nano-powder
Compound concentration is the ZrOCl of 720g/L, 94g/L respectively2·8H2O and edta solution take suitable two
Kind solution is mixed, and being vigorously stirred 5min is uniformly mixed it, obtains transparent microemulsion, and pH ＞ 10.5 are adjusted with ammonium hydroxide,
Ultrasound 10min obtains transparent gel under 65 DEG C, 30kHz, is then washed with distilled water gel to using AgNO3Solution detects not
Go out Cl-, then washed 3 times with ethyl alcohol, the zirconium oxide precursor solution after washing be put into thermostatic drying chamber, done at 60 DEG C
Dried presoma is calcined 4h by dry 15h at 700 DEG C under nitrogen protection, is finally removed nitrogen protection and is made powder natural
It is cooled to room temperature, obtains ZrO2Nano-powder；
Step 3, far infrared additive is prepared
By additive carrier, ZrO2Nano-powder, titanate coupling agent are added in example water, are stirred,
Far infrared additive slurry is obtained, is then baked to, is pulverized to get far infrared additive；
Step 4, cuprous oxide is prepared
The cupric sulfate pentahydrate of 2.5g is taken to be dissolved in the distilled water of 20ml, 40ml is then added in the case where continuously stirring
Sodium hydroxide (0.8g, 0.5mol/L, 0.75M) formed Kocide SD precipitation, in the case of then continuously stirring at room temperature
The ascorbic acid solution of 0.5g, 40ml are added in, 2h is stirred, 20min is centrifuged under 2000rpm, finally with distilled water and absolute ethyl alcohol
It washs, dry 10h, obtains cuprous oxide at 85 DEG C；
Step 5, antibacterial mite-removing additive is prepared
By additive carrier, cuprous oxide, titanium dioxide nano-particle, zinc oxide nano-particle, silica dioxide nano particle
Son, silver iodide nanoparticle, titanate coupling agent are mixed to join in example water, and ultrasonic agitation is uniform, obtains antibacterial mite-removing
Then additive slurry is baked to, pulverize to get antibacterial mite-removing additive；
Step 6, polyester fiber is prepared
Far infrared additive, antibacterial mite-removing additive and ethylene glycol are mixed, ultrasound 5h at room temperature after stirring is mixed
Liquid is closed, PTA, mixed liquor, catalyst aid are then added in reaction kettle of the esterification, is esterified after stirring evenly, polymerize, is gathered
Ester master batch, wherein, esterification temperature is 280 DEG C, pressure 400KPa, and polycondensation reaction is carried out when esterification yield reaches more than 93.5%, is contracted
Poly- temperature is 300 DEG C, is evacuated to 50Mpa, and when polycondensation to inherent viscosity is 0.65, discharging, blank obtains polyester master particle, then passes through
Spinning obtains polyester fiber, is a kind of far infrared, the compound polyester functional fibre of antibacterial mite-removing of the application.
The foregoing is merely the preferred modes of the present invention, are not intended to limit the invention, all in the spiritual and former of the present invention
Within then, any modifications, equivalent replacements and improvements are made should all be included in the protection scope of the present invention.
Claims (4)
1. the compound polyester functional fibre of a kind of far infrared, antibacterial mite-removing, which is characterized in that in the compound polyester functional fibre
Added with far infrared additive and antibacterial mite-removing additive, the far infrared additive and antibacterial mite-removing additive are in compound polyester
Quality accounting is respectively 5%, 7% in functional fibre；
The far infrared additive is constituted by the following substances：Additive carrier, ZrO2Nano-powder；
The antibacterial mite-removing additive is constituted by the following substances：Additive carrier, cuprous oxide, titanium dioxide nano-particle, oxidation
Zinc nano-particle, Nano particles of silicon dioxide, silver iodide nanoparticle；
Also, the additive carrier is SnO2Hollow ball, the SnO2Hollow ball is to be prepared using pollen as template, using hydro-thermal method.
2. the compound polyester functional fibre of a kind of far infrared according to claim 1, antibacterial mite-removing, which is characterized in that should
In far infrared additive, the mass fraction of each substance is：5 parts of additive carrier, ZrO22 parts of nano-powder；The grain size of each substance
For：50 μm of additive carrier, ZrO2Nano-powder 15nm.
3. the compound polyester functional fibre of a kind of far infrared according to claim 1, antibacterial mite-removing, which is characterized in that should
In antibacterial mite-removing additive, the mass fraction of each substance is：15 parts of additive carrier, 5 parts of cuprous oxide, titanium dioxide nano granule
4 parts of son, 3 parts of zinc oxide nano-particle, 1 part of Nano particles of silicon dioxide, 2 parts of silver iodide nanoparticle；The grain size of each substance is：
50 μm of additive carrier, 5 μm of cuprous oxide, titanium dioxide nano-particle 100nm, zinc oxide nano-particle 50nm, silica
Nano-particle 100nm, silver iodide nanoparticle 50nm.
4. the manufacturing method of the compound polyester functional fibre of a kind of far infrared, antibacterial mite-removing, which is characterized in that described compound poly-
Ester function fiber is made by following steps：
Step 1, additive carrier is prepared
Prepare the absolute ethyl alcohol of 200mL, then add in the stannic chloride pentahydrate powder of 18.5g wherein, be stirred continuously to clarification, obtain
To precursor solution；Then the rape petal pollen of 50 μm of diameter is filtered out, the rape petal pollen of 19.5g with alcohol is rinsed and is done
Only, dry, rape petal pollen is put into above-mentioned precursor solution, strong stirring 20h centrifuges solution, alcohol washes
Three times, the dry 5h in 60 DEG C of drying box；Then above-mentioned processed pollen is placed into and 4h is impregnated in precursor solution, it will
Solution centrifuges, ethanol wash three times, and it is 1 that gained pollen is put into 100mL alcohol and water volume ratio:It is hydrolyzed in 1 solution
3h is dispersed in after centrifugation in alcoholic solution, the dry 3h in 60 DEG C of drying box；Finally by pollen 580 in air furnace
DEG C annealing 2h, so as to remove pollen template, collects white powder and obtains SnO2Hollow ball is additive carrier；
In the preparation process of additive carrier, pollen, which is put into precursor solution, to be impregnated twice, ensures that pollen covers one layer
Even SnO2Layer；
Step 2, ZrO is prepared2Nano-powder
Compound concentration is the ZrOCl of 720g/L, 94g/L respectively2·8H2O and edta solution, take suitable two kinds it is molten
Liquid is mixed, and being vigorously stirred 5min is uniformly mixed it, obtains transparent microemulsion, and pH is adjusted with ammonium hydroxide>10.5,65
DEG C, ultrasound 10min obtains transparent gel under 30kHz, be then washed with distilled water gel to using AgNO3Solution inspection does not measure
Cl-, it is then washed 3 times with ethyl alcohol, the zirconium oxide precursor solution after washing is put into thermostatic drying chamber, it is dry at 60 DEG C
Dried presoma is calcined 4h by 15h at 700 DEG C under nitrogen protection, is finally removed nitrogen protection and is made powder naturally cold
But to room temperature, ZrO is obtained2Nano-powder；
Step 3, far infrared additive is prepared
By additive carrier, ZrO2Nano-powder, titanate coupling agent are added in deionized water, are stirred, and are obtained remote
Infrared additive slurry, is then baked to, and pulverizes to get far infrared additive；
Step 4, cuprous oxide is prepared
The cupric sulfate pentahydrate of 2.5g is taken to be dissolved in the distilled water of 20mL, the hydrogen of 40mL is then added in the case where continuously stirring
Sodium oxide molybdena forms Kocide SD precipitation, and the ascorbic acid that 0.5g, 40mL are added in the case of then continuously stirring at room temperature is molten
Liquid stirs 2h, centrifuges 20min under 2000rpm, finally washed with distilled water and absolute ethyl alcohol, and dry 10h, obtains oxygen at 85 DEG C
Change cuprous；
Step 5, antibacterial mite-removing additive is prepared
By additive carrier, cuprous oxide, titanium dioxide nano-particle, zinc oxide nano-particle, Nano particles of silicon dioxide, iodine
Change Nano silver grain, titanate coupling agent are mixed to join in deionized water, and ultrasonic agitation is uniform, obtains antibacterial mite-removing additive
Then slurry is baked to, pulverize to get antibacterial mite-removing additive；
Step 6, polyester fiber is prepared
Far infrared additive, antibacterial mite-removing additive and ethylene glycol are mixed, ultrasound 5h at room temperature after stirring is mixed
Then liquid adds in PTA, mixed liquor, catalyst aid in reaction kettle of the esterification, is esterified after stirring evenly, polymerize, obtain polyester
Master batch, wherein, esterification temperature is 280 DEG C, and pressure 400kPa carries out polycondensation reaction, polycondensation when esterification yield reaches more than 93.5%
Temperature is 300 DEG C, is evacuated to 50MPa, and when polycondensation to inherent viscosity is 0.65, discharging, blank obtains polyester master particle, then through spinning
Silk obtains polyester fiber, is a kind of far infrared, the compound polyester functional fibre of antibacterial mite-removing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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| CN1259357C (en) * | 2002-04-15 | 2006-06-14 | 上海金樱环保科技有限公司 | Chemical fibre grade polyester resin with health function and making method thereof |
| CN101238817B (en) * | 2008-03-06 | 2011-09-14 | 刘燕平 | Bacteriostat, far-infrared ray emitting agent, mother particle, fiber and manufacturing method thereof |
| CN102330189A (en) * | 2011-06-21 | 2012-01-25 | 江苏鹰翔化纤股份有限公司 | Preparation method of nano-tin dioxide modified polyester fiber |
| CN104928781B (en) * | 2015-06-03 | 2017-06-30 | 东华大学 | A kind of preparation method of the energy-saving and temperature-regulating fiber with far-infrared functional |
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