CN111304776A - Naringin modified polyester filament - Google Patents
Naringin modified polyester filament Download PDFInfo
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- CN111304776A CN111304776A CN202010251695.6A CN202010251695A CN111304776A CN 111304776 A CN111304776 A CN 111304776A CN 202010251695 A CN202010251695 A CN 202010251695A CN 111304776 A CN111304776 A CN 111304776A
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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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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/04—Melting filament-forming substances
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/10—Filtering or de-aerating the spinning solution or melt
- D01D1/103—De-aerating
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
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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
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
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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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Artificial Filaments (AREA)
Abstract
The invention provides a naringin modified polyester filament, wherein the mass content of naringin is 0.1-5%, the monofilament fiber is 0.1-0.4dpf, the breaking strength is 9.0-9.9cN/dtex, and the breaking elongation is 12.4-14.6%, and the invention also provides a preparation method thereof, which comprises the steps of preparing a nano composite suspension dispersion liquid containing naringin, a master batch containing the naringin function, high-speed melting, falling film degassing and melt spinning; the nanometer composite suspended dispersion liquid containing naringin is prepared from saturated water solution of naringin and porous nanometer TiO2‑SiO2Sequentially adding the microspheres and the titanate coupling agent into a high-speed shearing disperser, wherein the shearing force is 5250 and 6000ips, and the shearing and pasting time is 4-9 min; the modified polyester filament yarn has the advantages of antibacterial and antistatic effects, lasting antibacterial and antistatic effects, obviously increased surface wettability and good water absorption performance.
Description
Technical Field
The invention belongs to the technical field of polyester modification, relates to a naringin modified polyester filament, and particularly relates to a naringin modified polyester filament.
Background
Naringin has antiinflammatory, antiviral, anticancer, mutation resisting, antiallergic, antiulcer, analgesic, blood pressure lowering, blood cholesterol reducing, thrombosis reducing, local microcirculation improving and nutrition supply improving effects, and can be used for preventing and treating cardiovascular disease and cerebrovascular disease.
The trade name of the terylene is polyester fiber, wherein the terylene filament is filament with the length of more than kilometer. With the development of science and technology and the demand of people for high-quality life, new requirements are also put forward on the performance of the polyester filament yarns, for example, the polyester filament yarns are required to have certain antibacterial property, antistatic property, durability and strong water absorption function.
Chinese patent publication No. CN 108624968A provides a method for preparing regenerated polyester composite antibacterial polyester filament yarn. The method comprises the following steps: step 1, pre-crystallizing a material, wherein the material is a recovered PET polyester bottle flake material; step 2, feeding the dried PET bottle flake feed back into a screw extruder; step 3, filtering the mixture extruded by the extruder, feeding the filtered mixture into a reaction kettle, and then feeding the filtered mixture into a booster pump; and 4, dividing the melt from the filter into a skin layer and core layer melt, additionally arranging a dynamic mixer on a skin layer melt pipeline, controlling the antibacterial master batch to melt and quantitatively inject by a computer, enabling two paths of melts to enter a spinning assembly, injecting the two groups of melts into the composite spinning assembly through the melt pipeline for spinning, and then winding and forming. The regenerated polyester composite antibacterial polyester filament (POY 275 dtex/36-48 f) fiber prepared by the invention has ultrahigh antibacterial performance, and antibacterial active ingredients can be better and uniformly distributed on the surface of the fiber by adopting a skin-core layer structure, so that the antibacterial effect is improved, but the fiber cannot be made into fine denier fiber with a certain fineness requirement.
Disclosure of Invention
The invention provides a naringin modified polyester filament yarn and a preparation method thereof, aiming at solving the technical problems of the existing naringin modified polyester filament yarn, and realizing the following purposes:
(1) the naringin modified polyester filament yarn has good mechanical property and surface wettability;
(2) the naringin modified polyester filament yarn has good antistatic performance and lasting antistatic performance;
(3) the naringin modified polyester filament yarn has the advantages that the naringin modified polyester filament yarn has an antibacterial effect, the antibacterial effect is lasting, and the reduction range of the antibacterial effect is small through an exposure test;
(4) the preparation method of the naringin modified polyester filament has high spinning efficiency and good spinning quality;
in order to solve the technical problems, the following technical scheme is adopted:
a naringin modified polyester filament contains naringin 0.1-5 wt%.
The following are the preferable technical scheme and the implementation mode of the technical scheme of the invention:
the naringin modified polyester filament has monofilament fiber of 0.1-0.4dpf and breaking elongation of 12.4-14.6%.
The invention also provides a preparation method of the naringin modified polyester filament, which comprises the following steps: preparing nanometer composite suspended dispersion containing naringin, preparing functional mother particle containing naringin, high speed melting, and falling film degassing.
The nanometer composite suspension dispersion liquid containing naringin is prepared by mixing saturated water solution of naringin and porous sodiumTiO rice2-SiO2The microspheres and the titanate coupling agent are sequentially added into a high-speed shearing disperser, the shearing force is 5250-6000ips, and the shearing time is 4-9 min.
Adding 15-20% of polyimide acid solution into the nano composite suspension dispersion liquid containing naringin, carrying out secondary shearing, adding 0.1-5wt% of stabilizer after shearing for 10-12min, wherein the shearing force of the secondary shearing is 2500-3000ips, and the clipping and pasting time is 5-10 min.
The addition amount of the titanate coupling agent is 0.1-5% of the mass of the nano composite suspension dispersion liquid containing the naringin;
the stabilizer is N, N' -dimethylacetamide solution;
the mass of the naringin in the naringin saturated aqueous solution accounts for the porous nano TiO2-SiO2The mass fraction of the microspheres is 5-11%.
The mass ratio of the nano composite suspension dispersion liquid containing the naringin to the PET slices is 1: 8-11.
The density of the PET slices is 1.35-1.42g/cm3The intrinsic viscosity is 0.78-0.85dL/g, and the breaking elongation is 19.2-24.5%.
The high-speed melting is carried out, the high-speed mixing rotating speed is 2.5-2.8Kr/min, and the melting temperature is 254-292 ℃.
The falling film degassing has degassing time of 5-24min and melt viscosity of 0.45-0.60 dL/g.
In the melt spinning, the temperature difference between a hot plate and a hot plate is 20-30 ℃, and the speed difference between the hot plate and the hot plate is 100-150 m/min.
The invention also aims to provide a preparation method of the naringin modified polyester filament, which comprises the following steps: naringin-dissolved porous nano TiO2-SiO2Preparing microspheres, preparing a nano composite suspension dispersion liquid containing naringin, preparing a functional master batch containing the naringin, melting at a high speed, degassing in a falling film manner and melt spinning.
Step 1: dissolving naringin
Selecting commercially available naringin powder, grinding to particle size of more than 99%, sieving with 10000 mesh sieve to obtain naringin, transferring naringin to beaker, adding water, heating in water bath to 50-80 deg.C, dissolving completely, and making into saturated water solution of naringin.
The naringin powder contains effective component 98.0%, volatile oil 0.3-0.5%, and molecular formula C27H32O14Relative molecular weight 580.53, CAS number 10236-47-2.
Step 2: porous nano TiO2-SiO2Preparation of microspheres
Downward active TiO at 20 DEG C2Sequentially adding sorbitan, softened water and sodium methylsilicate into hydrosol, stirring uniformly, adding dilute hydrochloric acid for acidification to obtain light yellow transparent colloid, adding n-hexane solvent, heating to 50-55 deg.C at a speed of 2 deg.C/min, maintaining the temperature, stirring until emulsion appears, adding sodium hydroxide, heating to the solution at a speed of 5 deg.C/min, keeping the temperature for 10-15min, filtering to obtain white precipitate, washing, and drying to obtain porous nano TiO2-SiO2And (3) microspheres.
The active TiO2The mass ratio of hydrosol, sorbitan, softened water, sodium methyl silicate, n-hexane solvent, hydrochloric acid and sodium hydroxide is 20-50: 0.05-0.2: 5-15: 1: 20-50: 0.1-2: 1-3.
The porous nano TiO2-SiO2The particle size of the microspheres is 200-300nm, the pore diameter is 10-100nm, and the sphericity rate is 98.9-99.4%; the grain diameter is 2-8um and is more than 90 percent.
And step 3: naringin-containing nano composite suspension dispersion liquid
Mixing naringin saturated water solution and porous nanometer TiO2-SiO2Sequentially adding the microspheres and the titanate coupling agent into a high-speed shearing disperser, wherein the shearing force is 5250-6000ips, the clipping and pasting time is 4-9min, heating to 50 ℃ at the speed of 3 ℃/min, preserving heat, then adding a polyimide acid solution with the total mass of the substances accounting for 15-20%, carrying out secondary shearing, adding a stabilizer with the total mass of the substances accounting for 0.1-5wt% after shearing for 10-12min, the shearing force of the secondary shearing is 2500-3000ips, the clipping and pasting time is 5-10min, carrying out shearing dispersion, and allowing naringin molecules to enter the porous nano TiO molecules through the porous nano pore canal2-SiO2Inside the microsphere, "encapsulationIn porous nano TiO2-SiO2And (4) obtaining a stable nano composite suspension dispersion liquid containing the naringin in the microspheres.
The addition amount of the titanate coupling agent is 0.1-5% of the mass of the nano composite suspension dispersion liquid containing the naringin;
the stabilizer is N, N' -dimethylacetamide solution;
the mass of the naringin in the naringin saturated aqueous solution accounts for the porous nano TiO2-SiO2The mass fraction of the microspheres is 5-11%.
And 4, step 4: preparation of functional mother particle containing naringin
Volatilizing solvent to obtain dried naringin composite nanometer material, adding the dried naringin composite nanometer material into a grinder, adding 12wt% triglyceride, grinding to obtain agglomerated porous nanometer TiO2-SiO2Dispersing the microspheres to obtain the modified naringin composite modifier.
Adding naringin composite modifier into PET slice, melting at high temperature, maintaining the melting for 10-15min to sufficiently remove stabilizer N, N' dimethyl acetamide to obtain functional mother granule containing naringin, wherein the viscosity of the functional mother granule containing naringin is 0.36-0.72 dl/g.
The density of the PET slices in the step is 1.35-1.42g/cm3Intrinsic viscosity of 0.78-0.85dL/g and breaking elongation of 19.2-24.5%;
the mass ratio of the nano composite suspension dispersion liquid containing the naringin to the PET slices in the step is 1: 8-11.
And 5: high speed melting
The functional master batch containing naringin, PET slices, amino trimethylene phosphonic acid, an antioxidant and a dispersing agent are mixed and melted at a high speed, the melting temperature of the mixed melt is 254-292 ℃, and the high-speed mixing rotating speed is 2.5-2.8 Kr/min.
In the step, the weight parts of the PET slices, the amino trimethylene phosphonic acid, the antioxidant and the dispersant are respectively 100 parts, 0.1-20 parts, 0.01-10 parts and 0.01-20 parts.
The addition amount of the functional master batch containing the naringin is 1 to 15 percent of the mass of the mixed melt.
The content of active substances of the amino trimethylene phosphonic acid is 95.5 percent, the content of chloride ions is 0.01 to 0.1 percent, and the CAS number is 6419 to 19 to 8;
the antioxidant is antioxidant T-9228, the pH value is 5-7, the content of active substances is 99.5%, and the CAS number is 154862-43-8;
the dispersing agent consists of 5-10 parts by weight of hydroxymethyl cellulose, 1-5 parts by weight of sodium abietate, 5-10 parts by weight of BYK-358, 5-10 parts by weight of BYK-410 and 10-50 parts by weight of polyethylene oxide.
Step 6: falling film degassing
The melt after melting reaches a falling film evaporator through a melt pump for degassing, the melt feeding speed is 500-800Kg/h, the temperature value of the falling film evaporator is controlled within the range of 85-115 ℃, the pressure value of a vacuum pump is controlled within the range of 20-95Pa, the degassing time is 5-24min, and the viscosity of the final melt is 0.45-0.60 dL/g.
And 7: melt spinning
And the melt reaches a spinning box through a melt pump, is subjected to melt spinning, drafting and winding through a spinneret plate, and is cut into filaments to obtain the naringin modified polyester filaments.
In the spinning, the pressure of a spinning assembly is 38-41MPa, and circular blowing is adopted for drying;
the spinning has the oil-free silk production rate lower than 0.1 percent, and the floating silk production rate and the staggered silk production rate lower than 0.2 percent and 0.001 percent respectively.
The specification of the adopted spinneret plate is 100 holes, and the aperture is 0.3 mm;
the drafting is carried out, the temperature of a hot plate is 78-82 ℃, the temperature difference between a hot plate and the hot plate is 20-30 ℃, and the speed difference between the hot plate and the hot plate is 100-150 m/min;
the winding speed is 5800 and 6500 m/min.
By adopting the technical scheme, compared with the prior art, the invention has the following beneficial effects:
(1) the naringin modified polyester filament has the antibacterial rate of 98.0-99.6% for staphylococcus aureus, escherichia coli, candida albicans and other bacteria and the antibacterial rate of 80.2-89.7% for tetanus bacillus;
(2) the naringin modified polyester filament yarn has lasting antibacterial effect, and the antibacterial effect reduction range is small when an exposure test is carried out according to the method of GB/T16422.3 part 3: the antibacterial rate to staphylococcus aureus, colibacillus, candida albicans and other bacteria is 97.3-99.0%, and the antibacterial rate to tetanus bacillus is 77.0-88.7%;
(3) the naringin modified polyester filament yarn provided by the invention has good mechanical properties, wherein the monofilament fiber is 0.1-0.4dpf, the breaking strength is 9.0-9.9cN/dtex, and the breaking elongation is 12.4-14.6%;
(4) the polyester fabric made of the naringin modified polyester filament yarn has good water absorption performance, the contact angle is 122-125 degrees, the contact angle is reduced compared with that of the common polyester fabric, and the surface wettability is obviously increased;
(5) the polyester fabric made of the naringin modified polyester filament yarn has good antistatic performance, and the charge surface density is less than 3.3 mu C/m2，(ii) a After 50 times of washing, the antistatic property is durable, and the charge surface density is less than 3.5 mu C/m2；
(6) The preparation method of the naringin modified polyester filament yarn has the advantages of improving the spinning speed, improving the spinning quality, realizing the spinning speed, reducing the oil-free yarn generation rate to be lower than 0.1%, and reducing the generation rates of floating yarns and fault-separating yarns to be lower than 0.2% and 0.001% respectively;
(7) compared with the simple direct mixing and adding, the preparation method of the naringin modified polyester filament yarn has the advantages that the dispersibility of the powder is poor, the powder needs to be prepared into dry powder after being dissolved and volatilized, the powder is easy to agglomerate when being added into a PET slice, and the dispersibility is poor. According to the invention, after the dry powder is prepared, the fat-soluble solvent is added again for grinding, and the fluid is added into the double-screw extruder to be mixed with the PET chips, so that the dispersibility is better, and the agglomeration is not easy to occur.
Detailed Description
Embodiment 1 naringin modified polyester filament yarn and preparation method thereof
A method for preparing naringin modified polyester filament comprises: naringin-dissolved porous nano TiO2-SiO2Preparing microspheres, preparing a nano composite suspension dispersion liquid containing naringin, preparing a functional master batch containing the naringin, melting at a high speed, degassing in a falling film manner and melt spinning.
Step 1: dissolving naringin
Selecting commercially available naringin powder, grinding to particle size of more than 99%, sieving with 10000 mesh sieve to obtain naringin, transferring naringin to beaker, adding water, heating in water bath to 52 deg.C for completely dissolving, and preparing into saturated water solution of naringin (note: naringin has solubility of 10% at 75 deg.C).
The naringin powder contains effective component 98.0%, volatile oil 0.3-0.5%, and molecular formula C27H32O14Relative molecular weight 580.53, CAS number 10236-47-2.
Step 2: porous nano TiO2-SiO2Preparation of microspheres
Downward active TiO at 20 DEG C2Sequentially adding sorbitan, softened water and sodium methylsilicate into hydrosol, stirring uniformly, adding dilute hydrochloric acid for acidification to obtain light yellow transparent colloid, adding n-hexane solvent, heating to 50 ℃ at the speed of 2 ℃/min, keeping the temperature, stirring until emulsion appears, adding sodium hydroxide, heating to the solution at the speed of 5 ℃/min, layering, keeping the temperature for 15min, filtering to obtain white precipitate, washing, and drying to obtain porous nano TiO2-SiO2And (3) microspheres.
The active TiO2The mass ratio of the hydrosol to the sorbitol anhydride to the softened water to the sodium methyl silicate to the n-hexane solvent to the hydrochloric acid to the sodium hydroxide is 20: 0.2: 5: 1: 50: 0.1: 1.
the porous nano TiO2-SiO2The particle size of the microspheres is 200-300nm, the pore diameter is 10-100nm, and the sphericity rate is 98.9-99.4%; the grain diameter is 2-8um and is more than 90 percent.
And step 3: naringin-containing nano composite suspension dispersion liquid
Mixing naringin saturated water solution and porous nanometer TiO2-SiO2Sequentially adding the microspheres and the titanate coupling agent into the high-speed shearing machineIn a disperser, the shearing force is 5250ips, the cutting and pasting time is 9min, the temperature is increased to 50 ℃ at the speed of 3 ℃/min, the temperature is kept, then polyimide acid solution with the total mass of the substances accounting for 15 percent is added, secondary shearing is carried out, stabilizer with the total mass of the substances accounting for 5 percent by weight is added after the materials are sheared for 10-12min, the shearing force is 2500ips, the cutting and pasting time is 10min, shearing and dispersing are carried out, naringin molecules enter the porous nano TiO through a porous nano pore channel2-SiO2Inside the microsphere, "packaging" in the porous nano TiO2-SiO2And (4) obtaining a stable nano composite suspension dispersion liquid containing the naringin in the microspheres.
The addition amount of the titanate coupling agent is 0.1 percent of the mass of the nano composite suspension dispersion liquid containing the naringin;
the stabilizer is N, N' -dimethylacetamide solution;
the mass of the naringin in the naringin saturated aqueous solution accounts for the porous nano TiO2-SiO2The mass fraction of the microspheres was 11%.
And 4, step 4: preparation of functional mother particle containing naringin
Volatilizing solvent to obtain dried naringin composite nanometer material, adding the dried naringin composite nanometer material into a grinder, adding 12wt% triglyceride, grinding to obtain agglomerated porous nanometer TiO2-SiO2Dispersing the microspheres to obtain the modified naringin composite modifier.
Adding naringin composite modifier into PET slice, melting at high temperature, maintaining the melting for 10min to remove stabilizer N, N' dimethyl acetamide sufficiently to obtain functional mother granule containing naringin, wherein the viscosity of the functional mother granule containing naringin is 0.36-0.65 dl/g.
The density of the PET slices in the step is 1.35-1.42g/cm3Intrinsic viscosity of 0.78-0.85dL/g and breaking elongation of 19.2-24.5%;
the mass ratio of the nano composite suspension dispersion liquid containing the naringin to the PET slices in the step is 1: 8.
And 5: high speed melting
The functional master batch containing naringin, PET slices, amino trimethylene phosphonic acid, an antioxidant and a dispersing agent are mixed and melted at a high speed, the melting temperature of the mixed melt is 254-292 ℃, and the high-speed mixing rotating speed is 2.6 Kr/min.
In the step, the weight parts of the PET slices, the amino trimethylene phosphonic acid, the antioxidant and the dispersant are respectively 100 parts, 2 parts, 0.5 part and 0.5 part.
The addition amount of the functional master batch containing the naringin is 8 percent of the mass of the mixed melt.
The content of active substances of the amino trimethylene phosphonic acid is 95.5 percent, the content of chloride ions is 0.01 to 0.1 percent, and the CAS number is 6419 to 19 to 8;
the antioxidant is antioxidant T-9228, the pH value is 5-7, the content of active substances is 99.5%, and the CAS number is 154862-43-8;
the dispersing agent consists of 5 parts by weight of hydroxymethyl cellulose, 1 part by weight of sodium abietate, 5 parts by weight of BYK-358, 5 parts by weight of BYK-410 and 10 parts by weight of polyethylene oxide.
Step 6: falling film degassing
The melt after melting reaches a falling film evaporator through a melt pump for degassing, the feeding speed of the melt is 500Kg/h, the temperature value of the falling film evaporator is controlled within the range of 85-90 ℃, the pressure value of a vacuum pump is controlled within the range of 25-50Pa, the degassing time is 12min, and the viscosity of the final melt is 0.45-0.56 dL/g.
And 7: melt spinning
And the melt reaches a spinning box through a melt pump, is subjected to melt spinning, drafting and winding through a spinneret plate, and is cut into filaments to obtain the naringin modified polyester filaments.
In the spinning, the pressure of a spinning assembly is 38-41MPa, and circular blowing is adopted for drying;
the spinning has the oil-free silk production rate of 0.01 percent, and the floating silk production rate and the staggered silk production rate of 0.02 percent and 0.000 percent respectively.
The specification of the adopted spinneret plate is 100 holes, and the aperture is 0.3 mm;
the temperature of a hot plate is 78 ℃, the temperature difference between a hot plate and the hot plate is 20-22 ℃, and the speed difference between the hot plate and the hot plate is 100 m/min;
and the winding speed is 5800 m/min.
The naringin modified polyester filament prepared by the method has obvious plant antibacterial action, the antibacterial rates to staphylococcus aureus, escherichia coli and candida albicans are respectively 98.0%, 98.4% and 98.2%, and the antibacterial rate to tetanus bacillus is 80.2%; and the antibacterial time is long, after the naringin modified polyester filament is subjected to an exposure test according to the method of GB/T16422.3 part 3, the antibacterial rates of the naringin modified polyester filament on staphylococcus aureus, escherichia coli, candida albicans and other bacteria are 97.3%, 98.1% and 97.0%, respectively, the antibacterial rate on tetanus bacillus is 77.1%, and the antibacterial action is reduced.
Embodiment 2 naringin modified polyester filament yarn and preparation method thereof
A preparation method of naringin modified polyester filament yarn comprises the following steps: naringin-dissolved porous nano TiO2-SiO2Preparing microspheres, preparing a nano composite suspension dispersion liquid containing naringin, preparing a functional master batch containing the naringin, melting at a high speed, degassing in a falling film manner and melt spinning.
Step 1: dissolving naringin
Selecting commercially available naringin powder, grinding to particle size of more than 99%, sieving with 10000 mesh sieve to obtain naringin, transferring naringin to beaker, adding water, heating in water bath to 65 deg.C, dissolving completely to obtain saturated water solution of naringin (note: naringin has solubility of 10% at 75 deg.C).
The naringin powder contains effective component 98.0%, volatile oil 0.4%, and molecular formula C27H32O14Relative molecular weight 580.53, CAS number 10236-47-2.
Step 2: porous nano TiO2-SiO2Preparation of microspheres
Downward active TiO at 20 DEG C2Sequentially adding sorbitan, softened water and sodium methylsilicate into hydrosol, stirring, adding diluted hydrochloric acid for acidification to obtain light yellow transparent colloid, adding n-hexane solvent, heating to 52 deg.C at a speed of 2 deg.C/min, stirring to obtain emulsion, adding sodium hydroxide, heating to 5 deg.C/min until the solution begins to layer, and keeping the temperatureFiltering for 13min to obtain white precipitate, washing, and drying to obtain porous nanometer TiO2-SiO2And (3) microspheres.
The active TiO2The mass ratio of hydrosol, sorbitan, softened water, sodium methyl silicate, n-hexane solvent, hydrochloric acid and sodium hydroxide is 35: 0.1: 11: 1: 36: 1: 2.
the porous nano TiO2-SiO2The particle size of the microspheres is 200-300nm, the pore diameter is 10-100nm, and the sphericity rate is 98.9-99.4%; the grain diameter is 2-8um and is more than 90 percent.
And step 3: naringin-containing nano composite suspension dispersion liquid
Mixing naringin saturated water solution and porous nanometer TiO2-SiO2Sequentially adding microspheres and titanate coupling agent into a high-speed shearing disperser, wherein the shearing force is 5750ips, the cutting and pasting time is 6min, heating to 50 ℃ at the speed of 3 ℃/min, preserving heat, then adding a polyimide acid solution with the total mass of the substances accounting for 17%, carrying out secondary shearing, adding a stabilizer with the total mass of the substances accounting for 2.7wt% after shearing for 10-12min, the shearing force is 2750ips, the cutting and pasting time is 8min, carrying out shearing and dispersing, and allowing naringin molecules to enter the porous nano TiO through the porous nano pore channel2-SiO2Inside the microsphere, "packaging" in the porous nano TiO2-SiO2And (4) obtaining a stable nano composite suspension dispersion liquid containing the naringin in the microspheres.
The addition amount of the titanate coupling agent is 3.0 percent of the mass of the nano composite suspension dispersion liquid containing the naringin;
the stabilizer is N, N' -dimethylacetamide solution;
the mass of the naringin in the naringin saturated aqueous solution accounts for the porous nano TiO2-SiO2The mass fraction of the microspheres is 10%.
And 4, step 4: preparation of functional mother particle containing naringin
Volatilizing solvent to obtain dried naringin composite nanometer material, adding dried naringin composite nanometer material into grinding machine, adding 13wt% triglyceride, grinding to obtain agglomerated porous nanometer TiO2-SiO2Dispersing the microspheres to obtain the modified naringin composite modifier.
Adding naringin composite modifier into PET slice, melting at high temperature, maintaining the melting for 13min to fully remove stabilizer N, N' dimethyl acetamide to obtain functional mother granule containing naringin, wherein the viscosity of the functional mother granule containing naringin is 0.36-0.72 dl/g.
The density of the PET slices in the step is 1.35-1.42g/cm3Intrinsic viscosity of 0.78-0.85dL/g and breaking elongation of 19.2-24.5%;
the mass ratio of the nano composite suspension dispersion liquid containing the naringin to the PET slices in the step is 1: 10.
Compared with the simple direct mixing and adding, the preparation method of the naringin modified polyester filament yarn has the advantages that the dispersibility of the powder is poor, the powder needs to be prepared into dry powder after being dissolved and volatilized, the powder is easy to agglomerate when being added into a PET slice, and the dispersibility is poor. According to the invention, after the dry powder is prepared, the fat-soluble solvent is added again for grinding, and the fluid is added into the double-screw extruder to be mixed with the PET chips, so that the dispersibility is better, and the agglomeration is not easy to occur.
And 5: high speed melting
The functional master batch containing naringin, PET slices, amino trimethylene phosphonic acid, an antioxidant and a dispersing agent are mixed and melted at a high speed, the melting temperature of the mixed melt is 254-292 ℃, and the high-speed mixing rotating speed is 2.7 Kr/min.
In the step, the weight parts of the PET slices, the amino trimethylene phosphonic acid, the antioxidant and the dispersant are respectively 100 parts, 10 parts, 8 parts and 11 parts.
The addition amount of the functional master batch containing the naringin is 9 percent of the mass of the mixed melt.
The content of active substances of the amino trimethylene phosphonic acid is 95.5 percent, the content of chloride ions is 0.01 to 0.1 percent, and the CAS number is 6419 to 19 to 8;
the antioxidant is antioxidant T-9228, the pH value is 5-7, the content of active substances is 99.5%, and the CAS number is 154862-43-8;
the dispersing agent consists of 9 parts by weight of hydroxymethyl cellulose, 4 parts by weight of sodium abietate, 9 parts by weight of BYK-358, 8 parts by weight of BYK-410 and 45 parts by weight of polyethylene oxide.
Step 6: falling film degassing
The melt after melting reaches a falling film evaporator through a melt pump for degassing, the melt feeding speed is 750Kg/h, the temperature value of the falling film evaporator is controlled within the range of 96-110 ℃, the pressure value of a vacuum pump is controlled within the range of 70-84Pa, the degassing time is 13-22min, and the viscosity of the final melt is 0.45-0.60 dL/g.
And 7: melt spinning
And the melt reaches a spinning box through a melt pump, is subjected to melt spinning, drafting and winding through a spinneret plate, and is cut into filaments to obtain the naringin modified polyester filaments.
In the spinning, the pressure of a spinning assembly is 38-41MPa, and circular blowing is adopted for drying;
the spinning has the oil-free silk production rate of 0.003 percent, and the floating silk production rate and the staggered silk production rate of 0.001 percent and 0.000 percent respectively.
The specification of the adopted spinneret plate is 100 holes, and the aperture is 0.3 mm;
the temperature of a hot plate is 80 ℃, the temperature difference between a hot plate and the hot plate is 25-27 ℃, and the speed difference between the hot plate and the hot plate is 120 m/min;
the winding speed is 6000-.
The naringin modified polyester filament prepared by the method has a remarkable plant antibacterial effect, and has the antibacterial rates of 98.7%, 99.0% and 99.6% for staphylococcus aureus, escherichia coli and candida albicans, and the antibacterial rate of 89.7% for tetanus bacillus; and the antibacterial time is long, after the naringin modified polyester filament is subjected to an exposure test according to the method of GB/T16422.3 part 3, the antibacterial rate to staphylococcus aureus, escherichia coli, candida albicans and other bacteria is 98.6%, 98.6% and 99.0%, the antibacterial rate to tetanus bacillus is 88.7%, and the antibacterial action is reduced.
Embodiment 3 naringin modified polyester filament yarn and preparation method thereof
A preparation method of naringin modified polyester filament yarn comprises the following steps: naringin-dissolved porous nano TiO2-SiO2Preparing microspheres, preparing a nano composite suspension dispersion liquid containing naringin, preparing a functional master batch containing the naringin, melting at a high speed, degassing in a falling film manner and melt spinning.
Step 1: dissolving naringin
Selecting commercially available naringin powder, grinding to particle size of more than 99%, sieving with 10000 mesh sieve to obtain naringin, transferring naringin to beaker, adding water, heating in water bath to 50 deg.C for completely dissolving, and preparing into saturated water solution of naringin (note: naringin has solubility of 10% at 75 deg.C).
The naringin powder contains effective component 98.0%, volatile oil 0.5%, and molecular formula C27H32O14Relative molecular weight 580.53, CAS number 10236-47-2.
Step 2: porous nano TiO2-SiO2Preparation of microspheres
Downward active TiO at 20 DEG C2Sequentially adding sorbitan, softened water and sodium methylsilicate into hydrosol, stirring uniformly, adding dilute hydrochloric acid for acidification to obtain light yellow transparent colloid, adding n-hexane solvent, heating to 55 ℃ at the speed of 2 ℃/min, keeping the temperature, stirring until emulsion appears, adding sodium hydroxide, heating to the solution at the speed of 5 ℃/min, layering, keeping the temperature for 10min, filtering to obtain white precipitate, washing, and drying to obtain porous nano TiO2-SiO2And (3) microspheres.
The active TiO2The mass ratio of hydrosol, sorbitan, softened water, sodium methyl silicate, n-hexane solvent, hydrochloric acid and sodium hydroxide is 50: 0.05: 15: 1: 20: 2: 1.
the porous nano TiO2-SiO2The particle size of the microspheres is 200-300nm, the pore diameter is 10-100nm, and the sphericity rate is 98.9-99.4%; the grain diameter is 2-8um and is more than 90 percent.
And step 3: naringin-containing nano composite suspension dispersion liquid
Mixing naringin saturated water solution and porous nanometer TiO2-SiO2The microspheres and the titanate coupling agent are sequentially added into a high-speed shearing disperser, the shearing force is 6000ips, and the cutting and pasting time isHeating to 50 deg.C at a speed of 3 deg.C/min for 4min, maintaining the temperature, adding polyimide acid solution 20% of the total mass of the above substances, shearing for 10-12min, adding stabilizer 0.1wt% of the total mass of the above substances, shearing at 3000ips for 5min, shearing, dispersing, allowing naringin molecules to enter into porous nanometer TiO molecules via porous nanometer pore canal2-SiO2Inside the microsphere, "packaging" in the porous nano TiO2-SiO2And (4) obtaining a stable nano composite suspension dispersion liquid containing the naringin in the microspheres.
The addition amount of the titanate coupling agent is 3.5 percent of the mass of the nano composite suspension dispersion liquid containing the naringin;
the stabilizer is N, N' -dimethylacetamide solution;
the mass of the naringin in the naringin saturated aqueous solution accounts for the porous nano TiO2-SiO2The mass fraction of the microspheres was 9%.
And 4, step 4: preparation of functional mother particle containing naringin
Volatilizing solvent to obtain dried naringin composite nanometer material, adding the dried naringin composite nanometer material into a grinder, adding 12wt% triglyceride, grinding to obtain agglomerated porous nanometer TiO2-SiO2Dispersing the microspheres to obtain the modified naringin composite modifier.
Adding naringin composite modifier into PET slice, melting at high temperature, maintaining the melting for 15min to remove stabilizer N, N' dimethyl acetamide sufficiently to obtain functional mother granule containing naringin, wherein the viscosity of the functional mother granule containing naringin is 0.36-0.72 dl/g.
The density of the PET slices in the step is 1.35-1.42g/cm3Intrinsic viscosity of 0.78-0.85dL/g and breaking elongation of 19.2-24.5%;
the mass ratio of the nano composite suspension dispersion liquid containing the naringin to the PET slices in the step is 1: 12.
And 5: high speed melting
The functional master batch containing naringin, PET slices, amino trimethylene phosphonic acid, an antioxidant and a dispersing agent are mixed and melted at a high speed, the melting temperature of the mixed melt is 254-292 ℃, and the high-speed mixing rotating speed is 2.8 Kr/min.
In the step, the weight parts of the PET slices, the amino trimethylene phosphonic acid, the antioxidant and the dispersant are respectively 100 parts, 10 parts, 8 parts and 20 parts.
The addition amount of the functional master batch containing the naringin is 12 percent of the mass of the mixed melt.
The content of active substances of the amino trimethylene phosphonic acid is 95.5 percent, the content of chloride ions is 0.01 to 0.1 percent, and the CAS number is 6419 to 19 to 8;
the antioxidant is antioxidant T-9228, the pH value is 5-7, the content of active substances is 99.5%, and the CAS number is 154862-43-8;
the dispersing agent consists of 5-10 parts by weight of hydroxymethyl cellulose, 1-5 parts by weight of sodium abietate, 5-10 parts by weight of BYK-358, 5-10 parts by weight of BYK-410 and 10-50 parts by weight of polyethylene oxide.
Step 6: falling film degassing
The melt after melting reaches a falling film evaporator through a melt pump for degassing, the melt feeding speed is 800Kg/h, the temperature value of the falling film evaporator is controlled within the range of 98-105 ℃, the pressure value of a vacuum pump is controlled within the range of 87-92Pa, the degassing time is 14min, and the viscosity of the final melt is 0.45-0.60 dL/g.
And 7: melt spinning
And the melt reaches a spinning box through a melt pump, is subjected to melt spinning, drafting and winding through a spinneret plate, and is cut into filaments to obtain the naringin modified polyester filaments.
In the spinning, the pressure of a spinning assembly is 38-41MPa, and circular blowing is adopted for drying;
the spinning has the oil-free silk production rate of 0.004 percent, and the floating silk production rate and the staggered silk production rate of 0.000 percent and 0.0001 percent respectively.
The specification of the adopted spinneret plate is 100 holes, and the aperture is 0.3 mm;
the temperature of a hot plate is 79 ℃, the temperature difference between a hot plate and the hot plate is 25-27 ℃, and the speed difference between the hot plate and the hot plate is 145 m/min;
the winding speed is 6000-.
The naringin modified polyester filament prepared by the method has a remarkable plant antibacterial effect, and has the antibacterial rate of 97.8, 97.9 and 98.8 percent on staphylococcus aureus, escherichia coli and candida albicans and the antibacterial rate of 87.7 percent on tetanus bacillus; and the antibacterial time is long, after the naringin modified polyester filament is subjected to an exposure test according to the method of GB/T16422.3 part 3, the antibacterial rate to staphylococcus aureus, escherichia coli, candida albicans and other bacteria is 97.4, 98.0 and 98.8 percent, the antibacterial rate to tetanus bacillus is 79.8 percent, and the antibacterial action reduction is small. The obtained naringin modified polyester filament has the naringin mass content of 4.5%.
Detection of the naringin modified polyester filament yarn
1. According to the national standard GB/T12703.2-2009 part 2 of evaluation of textile Electrostatic Properties: the method of charge surface density "measures the antistatic performance of the polyester fabric made of the naringin modified polyester filament yarn of the present invention and the polyester fabric made of the naringin modified polyester filament yarn of the present invention after washing for 50 times, and the results are as follows:
therefore, the polyester fabric prepared from the naringin modified polyester filament yarn has good antistatic performance, and the charge surface density is less than 3.3 mu C/m2The charge surface density meets the index requirement of the durable antistatic textile; after 50 times of washing, the antistatic performance is durable, and the charge surface density is less than 3.5 mu C/m2The charge surface density meets the index requirements of the durable antistatic textile.
1. The contact angle of the polyester fabrics made of the naringin modified polyester filaments prepared by the methods of examples 1 to 3 was measured, and the angle between the tangent and the phase boundary was measured by using a JC2000A sessile drop contact angle/interfacial tension measuring instrument (morning digital equipment in the Shanghai), and the contact angle was directly measured, and the results are as follows:
therefore, the contact angle of the polyester fabric made of the naringin modified polyester filament prepared by the method in the embodiment 1-3 is 125 degrees, which is smaller than that of the common polyester fabric, the surface wettability is obviously increased, a plurality of free radicals and unsaturated centers are generated on the surface of the polyester filament, after the free radicals and the unsaturated centers are respectively contacted with air, a plurality of carbonyl groups and hydroxyl groups are generated on the surface of the fiber, the surface of the polyester filament is activated, and the water absorption performance is improved.
3. Index detection is carried out on the naringin modified polyester filament prepared by the method of the embodiment 1-3, and the detection result is as follows (X drawing):
it can be seen that the naringin modified polyester filament prepared by the method of examples 1-3 has 0.1-0.4dpf of monofilament fiber, the breaking strength of 9.0-9.9cN/dtex, the elongation at break of 12.4-14.5%, the numerical range of elongation at break is narrow, the uniformity of elongation at break is high, and the pilling rate of the fabric prepared by the naringin modified polyester filament is obviously lower than that of the common polyester fabric, which is unexpected by the research and development team of the invention.
All percentages used herein are weight percentages and all ratios described herein are mass ratios, unless otherwise indicated.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. The naringin modified polyester filament is characterized in that the naringin modified polyester filament has the naringin mass content of 0.1-5%; the preparation method of the naringin modified polyester filament yarn comprises the following steps: preparing nanometer composite suspended dispersion containing naringin, preparing functional mother particle containing naringin, high speed melting, and falling film degassing.
2. The naringin modified polyester filament according to claim 1, wherein the naringin modified polyester filament has a monofilament fiber of 0.1-0.4dpf and a breaking elongation of 12.4-14.6%.
3. The naringin modified polyester filament according to claim 1,
the nanometer composite suspended dispersion liquid containing naringin is prepared from saturated water solution of naringin and porous nanometer TiO2-SiO2The microspheres and the titanate coupling agent are sequentially added into a high-speed shearing disperser, the shearing force is 5250-6000ips, and the shearing time is 4-9 min.
4. The naringin modified polyester filament according to claim 1,
adding 15-20% of polyimide acid solution into the nano composite suspension dispersion liquid containing naringin, carrying out secondary shearing, adding 0.1-5wt% of stabilizer after shearing for 10-12min, wherein the shearing force of the secondary shearing is 2500-3000ips, and the clipping and pasting time is 5-10 min.
5. The naringin modified polyester filament according to claim 1,
the addition amount of the titanate coupling agent is 0.1-5% of the mass of the nano composite suspension dispersion liquid containing the naringin;
the stabilizer is N, N' -dimethylacetamide solution;
the mass of the naringin in the naringin saturated aqueous solution accounts for the porous nano TiO2-SiO2The mass fraction of the microspheres is 5-11%.
6. The naringin modified polyester filament according to claim 1,
the preparation method of the functional master batch containing the naringin comprises the following steps of preparing a nano composite suspension dispersion containing the naringin and a PET (polyethylene terephthalate) slice in a mass ratio of 1: 8-11;
the density of the PET slices is 1.35-1.42g/cm3The intrinsic viscosity is 0.78-0.85dL/g, and the breaking elongation is 19.2-24.5%.
7. The naringin modified polyester filament according to claim 1,
the high-speed melting is carried out, the high-speed mixing rotating speed is 2.5-2.8Kr/min, and the melting temperature is 254-292 ℃.
8. The naringin modified polyester filament according to claim 1,
the falling film degassing has degassing time of 5-24min and melt viscosity of 0.45-0.60 dL/g.
9. The naringin modified polyester filament according to claim 1,
in the melt spinning, the temperature difference between a hot plate and a hot plate is 20-30 ℃, and the speed difference between the hot plate and the hot plate is 100-150 m/min.
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