CN112267162A - Preparation method of polyester fiber with zinc oxide deposited on surface of titanium dioxide - Google Patents
Preparation method of polyester fiber with zinc oxide deposited on surface of titanium dioxide Download PDFInfo
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- CN112267162A CN112267162A CN202011112426.8A CN202011112426A CN112267162A CN 112267162 A CN112267162 A CN 112267162A CN 202011112426 A CN202011112426 A CN 202011112426A CN 112267162 A CN112267162 A CN 112267162A
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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
- 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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Abstract
The invention discloses a preparation method of zinc oxide polyester fibers deposited on the surface of titanium dioxide, which comprises the following steps: preparing zinc oxide nano powder deposited on the surface of titanium dioxide; surface modification of the titanium dioxide surface deposited zinc oxide nano powder: carrying out surface modification on the nano antibacterial powder by a high-speed kneading machine, and spraying a surface modifier into the nano antibacterial powder by an atomizing device to mix the surface modifier with the nano antibacterial powder; preparing the antibacterial master batch: uniformly mixing the surface-modified nano antibacterial powder with resin powder, and extruding the mixed raw materials by twin-screw extrusion, blending, granulating and extruding to obtain antibacterial master batches; and drying the antibacterial master batch, uniformly mixing the dried antibacterial master batch with the polyester chips, and feeding the mixture into a feeder of a spinning machine for melt spinning to obtain the antibacterial polyester fiber. The invention prepares the white antibacterial polyester fiber by preparing the nano antibacterial powder and preparing the functional master batch through surface modification and spinning.
Description
Technical Field
The invention belongs to the field of functional textile materials, and particularly relates to a preparation method of a titanium dioxide surface deposited zinc oxide polyester fiber.
Background
The antibacterial problem is a persistent problem faced by chemical fiber fabrics, some solutions are provided at present, for example, the solutions are from the origin of fibers, the antibacterial fibers can be prepared, for example, the antibacterial fibers are prepared by adopting high addition and composite spinning technology, the used antibacterial powder is silver, zinc, copper and the like, the fabrics prepared by adopting the fibers can completely meet the antibacterial requirement of the fabrics, and the antibacterial fiber fabric has wide application in some safety fields.
However, such fibers also have irreparable disadvantages: first, the silver system has high cost, is limited in application because of price and cost control, and has poor stability, and needs to be improved in light resistance; secondly, the zinc system is added in a higher ratio, and zinc oxide is generally used as the antibacterial fiber, and the addition amount of the zinc oxide can reach about 4 percent to achieve a better antibacterial effect; thirdly, the color change effect of the copper system is too strong, the copper system antibacterial fiber in the current market has the advantages of low antibacterial efficiency and black color due to the fact that copper oxide is used as the copper oxide, cuprous oxide or elemental copper is used as an antibacterial medium, the antibacterial effect is good, but the spun fiber is unstable in color and easy to change color, and the application is affected; fourth, in order to solve the above problems, metal salts have been used to prepare antibacterial fibers, but in the later dyeing and finishing, metal ions are precipitated out to lower the antibacterial effect and affect the wash resistance of the antibacterial function of the fabric, so that the application is limited.
At present, more fabrics in the market adopt antibacterial after-treatment to realize the antibacterial function of the fabrics, and compared with the mode of using antibacterial fibers, the mode has the advantages of lower cost and obvious effect, thereby being used by most fabric manufacturers. However, this approach, while inexpensive and effective, has inevitable drawbacks: (1) the additional pollution is generally finished after the antibacterial agent is adopted, so that the pollution degree of the wastewater is increased, and the treatment difficulty of the wastewater is also increased; (2) the durability is not enough, the washing fastness of the adopted antibacterial after-finishing mode is not good, and generally, the washing fastness which can meet the standard requirement is very rare.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made keeping in mind the above and/or other problems occurring in the prior art.
Therefore, the invention aims to overcome the defects in the prior art and provide a preparation method of the polyester fiber with zinc oxide deposited on the surface of titanium dioxide.
In order to solve the technical problems, the invention provides the following technical scheme: a preparation method of a polyester fiber with zinc oxide deposited on the surface of titanium dioxide comprises the steps of selecting titanium dioxide with the particle size of 20-50 nanometers as a base material, mixing the titanium dioxide with distilled water to prepare a nano titanium dioxide aqueous solution, wherein the concentration of the nano titanium dioxide is 1-10%, and adding zinc chloride to prepare a mixed solution, wherein the concentration of the zinc chloride is 0.5-5%; dropwise adding 0.1% sodium hydroxide solution, adjusting the pH value to 5-9, reacting for 1-6 h at 140-200 ℃ by a hydrothermal kettle, and performing rotary evaporation to obtain nano powder; carrying out surface modification on the nano antibacterial powder by a high-speed kneading machine, wherein the temperature is 30-90 ℃, the stirring speed is 1000-3000 r/min, a surface modifier is sprayed in by an atomizing device and mixed with the nano antibacterial powder, the addition amount of the surface modifier is 0.1-3 wt% of the mass of the nano antibacterial powder, and the nano antibacterial powder is mixed for 30-90 min at a high speed; uniformly mixing the surface-modified nano antibacterial powder and polyester powder, wherein the nano antibacterial powder accounts for 10-50 wt% of the whole mass, and extruding the mixed raw materials through twin-screw extrusion, blending, granulating and extruding to obtain antibacterial master batches; drying the antibacterial master batch at the temperature of 100-180 ℃ for 2-8 hours; and uniformly mixing the dried antibacterial master batch with the PET polyester chips, or feeding the dried antibacterial master batch and the PET polyester chips into a feeder of a spinning machine through a separate metering device for melt spinning, wherein the spinning speed is 600-3000 m/min, and the initial pressure of a spinning assembly is 8-16 MPa, so as to obtain the antibacterial polyester fiber.
As a preferred scheme of the preparation method of the titanium dioxide surface deposited zinc oxide polyester fiber, the preparation method comprises the following steps: the concentration of the nano titanium dioxide is 10%.
As a preferred scheme of the preparation method of the titanium dioxide surface deposited zinc oxide polyester fiber, the preparation method comprises the following steps: the concentration of the zinc chloride is 2 percent.
As a preferred scheme of the preparation method of the titanium dioxide surface deposited zinc oxide polyester fiber, the preparation method comprises the following steps: the surface modifier is one of active organosilicon series surface modifiers or titanate series surface modifiers.
As a preferred scheme of the preparation method of the titanium dioxide surface deposited zinc oxide polyester fiber, the preparation method comprises the following steps: the polyester powder is one of PET or PBT powder.
As a preferred scheme of the preparation method of the titanium dioxide surface deposited zinc oxide polyester fiber, the preparation method comprises the following steps: the basic resin slice is a spinning-grade PET polyester slice.
As a preferred scheme of the preparation method of the titanium dioxide surface deposited zinc oxide polyester fiber, the preparation method comprises the following steps: in the spinning process, the spinning temperature is 270-300 ℃.
As a preferred scheme of the preparation method of the titanium dioxide surface deposited zinc oxide polyester fiber, the preparation method comprises the following steps: the monofilament titer of the antibacterial fiber is 0.5-5D.
The invention has the beneficial effects that:
(1) the invention adopts a brand new antibacterial mechanism to prepare the new antibacterial fiber, the surface zinc oxide can realize the antibacterial function of zinc ions by compounding titanium dioxide and zinc oxide, the nano titanium dioxide has the characteristic of sensitivity to light and electricity, the antibacterial effect of the surface zinc oxide can be increased to a certain extent, and the titanium dioxide has the illumination oxidation function, can realize illumination antibacterial under outdoor and illumination conditions, is compounded with the antibacterial performance of the zinc oxide, and has better antibacterial effect.
(2) The fiber diameter of the invention can be made into superfine fiber, the fiber can be made into white, the fiber has permanent antibacterial function, the mechanical property can reach the standard of common fiber, the fiber completely meets various weaving requirements, the cost is equivalent to the cost of antibacterial after finishing, compared with the currently used antibacterial fiber, the cost is reduced by 50-80%, the pollution is reduced, the invention can expand the export of textiles, and the added value of the textiles is improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein:
fig. 1 is an SEM image of the antibacterial fiber obtained in the example of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, specific embodiments thereof are described in detail below with reference to examples of the specification.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1
A preparation method of a titanium dioxide surface deposited zinc oxide polyester fiber comprises the following steps:
(1) the preparation method of the nano antibacterial powder with the grain diameter less than 100nm comprises the following steps: selecting titanium dioxide with the particle size of 25 nanometers as a base material, depositing nano zinc oxide on the surface of the titanium dioxide by a chemical precipitation method, specifically, selecting a nano titanium dioxide aqueous solution with the concentration of 10 percent, adding zinc chloride with the concentration of 0.5 percent, adjusting the pH value to 7 by dropwise adding a low-concentration (0.1 percent) sodium hydroxide solution, reacting for 3 hours at 180 ℃ by a hydrothermal kettle, and obtaining nano powder by rotary evaporation;
(2) surface modification of nano-antibacterial powder: carrying out surface modification on the nano antibacterial powder by a high-speed kneading machine, wherein the temperature is 20 ℃, the stirring speed is 2000 r/min, a surface modifier is sprayed by an atomizing device to be mixed with the nano antibacterial powder, the addition amount of the surface modifier is 1 wt% of the mass of the nano antibacterial powder, and the nano antibacterial powder is mixed for 90min at a high speed; the surface modifier is tetrabutyl titanate;
(3) preparing the antibacterial master batch: uniformly mixing the nano antibacterial powder subjected to surface modification in the step (2) with resin powder, wherein the resin powder is PBT resin powder, the nano antibacterial powder accounts for 10 wt% of the whole mass, and the mixed raw materials are extruded by a double screw, blended, granulated and extruded at a processing temperature of 270 ℃ to obtain antibacterial master batches;
(4) drying the antibacterial master batch at the temperature of 150 ℃ for 8 hours; uniformly mixing the antibacterial master batch and the basic resin slices in a mass ratio of 1:19, feeding the mixture into a feeder of a spinning machine for melt spinning, wherein the basic resin slices are PET slices, the spinning temperature is 285 ℃, the spinning speed is 2000m/min, and the initial pressure of a spinning assembly is 8MPa, so that the antibacterial fiber is obtained, and the color of the antibacterial fiber is white. The particle size of the obtained nano antibacterial material is 170nm through a laser particle sizer test, the antibacterial effect of the prepared fiber is tested according to the test standard of GB/T20944.3-2008, and the antibacterial effect on escherichia coli, staphylococcus aureus and trametes versicolor is 62/63/65.
Example 2:
a preparation method of a titanium dioxide surface deposited zinc oxide polyester fiber comprises the following steps:
(1) preparing nano antibacterial powder with the grain diameter of less than 100nm, specifically selecting titanium dioxide with the grain diameter of 25 nm as a base material, and depositing nano zinc oxide on the surface of the titanium dioxide by a chemical precipitation method. Selecting a nano titanium dioxide aqueous solution with the concentration of 10%, adding zinc chloride with the concentration of 1%, dropwise adding a low-concentration (0.1%) sodium hydroxide solution to adjust the pH value to 7, reacting for 3 hours at 180 ℃ through a hydrothermal kettle, and performing rotary evaporation to obtain nano powder; (ii) a
(2) Surface modification of nano-antibacterial powder: carrying out surface modification on the nano antibacterial powder by a high-speed kneading machine, wherein the temperature is 20 ℃, the stirring speed is 2000 r/min, a surface modifier is sprayed by an atomizing device to be mixed with the nano antibacterial powder, the addition amount of the surface modifier is 1 wt% of the mass of the nano antibacterial powder, and the nano antibacterial powder is mixed for 90min at a high speed; the surface modifier is tetrabutyl titanate;
(3) preparing the antibacterial master batch: uniformly mixing the nano antibacterial powder subjected to surface modification in the step (2) with resin powder, wherein the resin powder is PBT resin powder, the nano antibacterial powder accounts for 10 wt% of the whole mass, and the mixed raw materials are extruded by a double screw, blended, granulated and extruded at a processing temperature of 270 ℃ to obtain antibacterial master batches;
(4) drying the antibacterial master batch at the temperature of 150 ℃ for 8 hours; uniformly mixing the antibacterial master batch and the basic resin slices in a mass ratio of 1:19, feeding the mixture into a feeder of a spinning machine for melt spinning, wherein the basic resin slices are PET slices, the spinning temperature is 285 ℃, the spinning speed is 2000m/min, and the initial pressure of a spinning assembly is 8MPa, so that the antibacterial fiber is obtained, and the color of the antibacterial fiber is white. The particle size of the obtained nano antibacterial material is 170nm through a laser particle sizer test, the antibacterial effect of the prepared fiber is tested according to the test standard of GB/T20944.3-2008, and the antibacterial effect on escherichia coli, staphylococcus aureus and trametes versicolor is 68/68/69.
Example 3:
a preparation method of a titanium dioxide surface deposited zinc oxide polyester fiber comprises the following steps:
(1) preparing nano antibacterial powder with the grain diameter of less than 100nm, specifically selecting titanium dioxide with the grain diameter of 25 nm as a base material, and depositing nano zinc oxide on the surface of the titanium dioxide by a chemical precipitation method. Selecting a nano titanium dioxide aqueous solution with the concentration of 10%, adding zinc chloride with the concentration of 2%, dropwise adding a low-concentration (0.1%) sodium hydroxide solution to adjust the pH value to 7, reacting for 3 hours at 180 ℃ through a hydrothermal kettle, and performing rotary evaporation to obtain nano powder;
(2) surface modification of nano-antibacterial powder: carrying out surface modification on the nano antibacterial powder by a high-speed kneading machine, wherein the temperature is 20 ℃, the stirring speed is 2000 r/min, a surface modifier is sprayed by an atomizing device to be mixed with the nano antibacterial powder, the addition amount of the surface modifier is 1 wt% of the mass of the nano antibacterial powder, and the nano antibacterial powder is mixed for 90min at a high speed; the surface modifier is tetrabutyl titanate;
(3) preparing the antibacterial master batch: uniformly mixing the nano antibacterial powder subjected to surface modification in the step (2) with resin powder, wherein the resin powder is PBT resin powder, the nano antibacterial powder accounts for 10 wt% of the whole mass, and the mixed raw materials are extruded by a double screw, blended, granulated and extruded at a processing temperature of 270 ℃ to obtain antibacterial master batches;
(4) drying the antibacterial master batch at the temperature of 150 ℃ for 8 hours; uniformly mixing the antibacterial master batch and the basic resin slices in a mass ratio of 1:19, feeding the mixture into a feeder of a spinning machine for melt spinning, wherein the basic resin slices are PET slices, the spinning temperature is 285 ℃, the spinning speed is 2000m/min, and the initial pressure of a spinning assembly is 8MPa, so that the antibacterial fiber is obtained, and the color of the antibacterial fiber is white. The particle size of the obtained nano antibacterial material is 170nm through a laser particle sizer test, the antibacterial effect of the prepared fiber is tested according to the test standard of GB/T20944.3-2008, and the antibacterial effect on escherichia coli, staphylococcus aureus and trametes versicolor is 75/76/75.
Example 4:
a preparation method of a titanium dioxide surface deposited zinc oxide polyester fiber comprises the following steps:
(1) preparing nano antibacterial powder with the grain diameter of less than 100nm, specifically selecting titanium dioxide with the grain diameter of 25 nm as a base material, and depositing nano zinc oxide on the surface of the titanium dioxide by a chemical precipitation method. Selecting a nano titanium dioxide aqueous solution with the concentration of 10%, adding zinc chloride with the concentration of 3%, dropwise adding a low-concentration (0.1%) sodium hydroxide solution to adjust the pH value to 7, reacting for 3 hours at 180 ℃ through a hydrothermal kettle, and performing rotary evaporation to obtain nano powder; (ii) a
(2) Surface modification of nano-antibacterial powder: carrying out surface modification on the nano antibacterial powder by a high-speed kneading machine, wherein the temperature is 20 ℃, the stirring speed is 2000 r/min, a surface modifier is sprayed by an atomizing device to be mixed with the nano antibacterial powder, the addition amount of the surface modifier is 1 wt% of the mass of the nano antibacterial powder, and the nano antibacterial powder is mixed for 90min at a high speed; the surface modifier is tetrabutyl titanate;
(3) preparing the antibacterial master batch: uniformly mixing the nano antibacterial powder subjected to surface modification in the step (2) with resin powder, wherein the resin powder is PBT resin powder, the nano antibacterial powder accounts for 10 wt% of the whole mass, and the mixed raw materials are extruded by a double screw, blended, granulated and extruded at a processing temperature of 270 ℃ to obtain antibacterial master batches;
(4) drying the antibacterial master batch at the temperature of 150 ℃ for 8 hours; uniformly mixing the antibacterial master batch and the basic resin slices in a mass ratio of 1:19, feeding the mixture into a feeder of a spinning machine for melt spinning, wherein the basic resin slices are PET slices, the spinning temperature is 285 ℃, the spinning speed is 2000m/min, and the initial pressure of a spinning assembly is 8MPa, so that the antibacterial fiber is obtained, and the color of the antibacterial fiber is white. The particle size of the obtained nano antibacterial material is 170nm through a laser particle sizer test, the antibacterial effect of the prepared fiber is tested according to the test standard of GB/T20944.3-2008, and the antibacterial effect on escherichia coli, staphylococcus aureus and trametes versicolor is 76/76/75.
Example 5:
a preparation method of a titanium dioxide surface deposited zinc oxide polyester fiber comprises the following steps:
(1) preparing nano antibacterial powder with the grain diameter of less than 100nm, specifically selecting titanium dioxide with the grain diameter of 25 nm as a base material, and depositing nano zinc oxide on the surface of the titanium dioxide by a chemical precipitation method. Selecting a nano titanium dioxide aqueous solution with the concentration of 10%, adding zinc chloride with the concentration of 4%, dropwise adding a low-concentration (0.1%) sodium hydroxide solution to adjust the pH value to 7, reacting for 3 hours at 180 ℃ through a hydrothermal kettle, and performing rotary evaporation to obtain nano powder;
(2) surface modification of nano-antibacterial powder: carrying out surface modification on the nano antibacterial powder by a high-speed kneading machine, wherein the temperature is 20 ℃, the stirring speed is 2000 r/min, a surface modifier is sprayed by an atomizing device to be mixed with the nano antibacterial powder, the addition amount of the surface modifier is 1 wt% of the mass of the nano antibacterial powder, and the nano antibacterial powder is mixed for 90min at a high speed; the surface modifier is tetrabutyl titanate;
(3) preparing the antibacterial master batch: uniformly mixing the nano antibacterial powder subjected to surface modification in the step (2) with resin powder, wherein the resin powder is PBT resin powder, the nano antibacterial powder accounts for 10 wt% of the whole mass, and the mixed raw materials are extruded by a double screw, blended, granulated and extruded at a processing temperature of 270 ℃ to obtain antibacterial master batches;
(4) drying the antibacterial master batch at the temperature of 150 ℃ for 8 hours; uniformly mixing the antibacterial master batch and the basic resin slices in a mass ratio of 1:19, feeding the mixture into a feeder of a spinning machine for melt spinning, wherein the basic resin slices are PET slices, the spinning temperature is 285 ℃, the spinning speed is 2000m/min, and the initial pressure of a spinning assembly is 8MPa, so that the antibacterial fiber is obtained, and the color of the antibacterial fiber is white. The particle size of the obtained nano antibacterial material is 170nm through a laser particle sizer test, the antibacterial effect of the prepared fiber is tested according to the test standard of GB/T20944.3-2008, and the antibacterial effect on escherichia coli, staphylococcus aureus and trametes versicolor is 72/70/70.
It can be seen that the antibacterial effect decreases as the zinc chloride content continues to increase, presumably because the increase in zinc oxide content results in an excessively rapid increase in particle size and a decrease in antibacterial efficiency, and therefore the zinc chloride concentration of 2% is selected to continue optimization.
Example 6:
a preparation method of a titanium dioxide surface deposited zinc oxide polyester fiber comprises the following steps:
(1) preparing nano antibacterial powder with the grain diameter of less than 100nm, specifically selecting titanium dioxide with the grain diameter of 25 nm as a base material, and depositing nano zinc oxide on the surface of the titanium dioxide by a chemical precipitation method. Selecting a nano titanium dioxide aqueous solution with the concentration of 10%, adding zinc chloride with the concentration of 2%, dropwise adding a low-concentration (0.1%) sodium hydroxide solution to adjust the pH value to 7, reacting for 3 hours at 180 ℃ through a hydrothermal kettle, and performing rotary evaporation to obtain nano powder;
(2) surface modification of nano-antibacterial powder: carrying out surface modification on the nano antibacterial powder by a high-speed kneading machine, wherein the temperature is 20 ℃, the stirring speed is 2000 r/min, a surface modifier is sprayed by an atomizing device to be mixed with the nano antibacterial powder, the addition amount of the surface modifier is 1 wt% of the mass of the nano antibacterial powder, and the nano antibacterial powder is mixed for 90min at a high speed; the surface modifier is tetrabutyl titanate;
(3) preparing the antibacterial master batch: uniformly mixing the nano antibacterial powder subjected to surface modification in the step (2) with resin powder, wherein the resin powder is PBT resin powder, the nano antibacterial powder accounts for 20 wt% of the whole mass, and the mixed raw materials are extruded by a double screw, blended, granulated and extruded at a processing temperature of 270 ℃ to obtain antibacterial master batches;
(4) drying the antibacterial master batch at the temperature of 150 ℃ for 8 hours; uniformly mixing the antibacterial master batch and the basic resin slices in a mass ratio of 1:19, feeding the mixture into a feeder of a spinning machine for melt spinning, wherein the basic resin slices are PET slices, the spinning temperature is 285 ℃, the spinning speed is 2000m/min, and the initial pressure of a spinning assembly is 8MPa, so that the antibacterial fiber is obtained, and the color of the antibacterial fiber is white. The particle size of the obtained nano antibacterial material is 170nm through a laser particle sizer test, the antibacterial effect of the prepared fiber is tested according to the test standard of GB/T20944.3-2008, and the antibacterial effect on escherichia coli, staphylococcus aureus and trametes versicolor is 98/98/97.
Example 7:
a preparation method of a titanium dioxide surface deposited zinc oxide polyester fiber comprises the following steps:
(1) preparing nano antibacterial powder with the grain diameter of less than 100nm, specifically selecting titanium dioxide with the grain diameter of 25 nm as a base material, and depositing nano zinc oxide on the surface of the titanium dioxide by a chemical precipitation method. Selecting a nano titanium dioxide aqueous solution with the concentration of 10%, adding zinc chloride with the concentration of 2%, dropwise adding a low-concentration (0.1%) sodium hydroxide solution to adjust the pH value to 7, reacting for 3 hours at 180 ℃ through a hydrothermal kettle, and performing rotary evaporation to obtain nano powder;
(2) surface modification of nano-antibacterial powder: carrying out surface modification on the nano antibacterial powder by a high-speed kneading machine, wherein the temperature is 20 ℃, the stirring speed is 2000 r/min, a surface modifier is sprayed by an atomizing device to be mixed with the nano antibacterial powder, the addition amount of the surface modifier is 1 wt% of the mass of the nano antibacterial powder, and the nano antibacterial powder is mixed for 90min at a high speed; the surface modifier is tetrabutyl titanate;
(3) preparing the antibacterial master batch: uniformly mixing the nano antibacterial powder subjected to surface modification in the step (2) with resin powder, wherein the resin powder is PBT resin powder, the nano antibacterial powder accounts for 30 wt% of the whole mass, and the mixed raw materials are extruded by a double screw, blended, granulated and extruded at a processing temperature of 270 ℃ to obtain antibacterial master batches;
(4) drying the antibacterial master batch at the temperature of 150 ℃ for 8 hours; uniformly mixing the antibacterial master batch and the basic resin slices in a mass ratio of 1:19, feeding the mixture into a feeder of a spinning machine for melt spinning, wherein the basic resin slices are PET slices, the spinning temperature is 285 ℃, the spinning speed is 2000m/min, and the initial pressure of a spinning assembly is 8MPa, so that the antibacterial fiber is obtained, and the color of the antibacterial fiber is white. The particle size of the obtained nano antibacterial material is 170nm through a laser particle sizer test, the antibacterial effect of the prepared fiber is tested according to the test standard of GB/T20944.3-2008, and the antibacterial effect on escherichia coli, staphylococcus aureus and trametes versicolor is 100/100/100. Fig. 1 is an SEM image of the antibacterial fiber obtained in this example, and it can be seen that the fiber diameter of the present invention can be made into an ultrafine fiber, the fiber can be made into a white color, and has a permanent antibacterial function, and the mechanical properties can reach the standard of a common fiber, and completely meet various weaving requirements.
Example 8:
the concentration of the titanium dioxide aqueous solution, the concentration of zinc chloride and the amount of the surface modifier added were controlled to be different from those of example 7, and the conditions and results were shown in tables 1 and 2, except that the procedure was the same as in example 7.
TABLE 1
TABLE 2
It can be seen that when the concentration of the titanium dioxide aqueous solution is too high, the particle size is too large during the preparation of the composite system, so that the antibacterial performance is affected, and when the concentration of the titanium dioxide is fixed, the addition amount of the surface modifier is adjusted, so that a certain synergistic effect is generated, and the antibacterial effect is increased. According to the invention, the titanate is adopted, so that the binding force with the powder is strong, and the surface modification effect is realized, the inventor finds that the antibacterial effect is not very different when the addition amount of the surface modifier is 0.5-0.8 wt%, but when the addition amount of the surface modifier reaches 1 wt%, the antibacterial effect is further enhanced, the titanate is decomposed to generate titanium oxides possibly due to the participation of water, the charge accumulation effect of a system is increased, and the charges can destroy the ionization balance point of bacteria, so that the surface of the fiber is not beneficial to the growth of the bacteria, and the antibacterial function can be enhanced. But the dosage is not too high or too low, the too low dosage can not play a role in surface modification, the too high dosage can lead the powder to be agglomerated, the agglomeration is caused, the small-size effect is lost, the fiber spinning is difficult, and the spinneret plate can be blocked due to the too large agglomerated particle size.
The invention adopts a brand new antibacterial mechanism to prepare the new antibacterial fiber, the surface zinc oxide can realize the antibacterial function of zinc ions by compounding titanium dioxide and zinc oxide, the nano titanium dioxide has the characteristic of sensitivity to light and electricity, the antibacterial effect of the surface zinc oxide can be increased to a certain extent, and the titanium dioxide has the illumination oxidation function, can realize illumination antibacterial under outdoor and illumination conditions, is compounded with the antibacterial performance of the zinc oxide, and has better antibacterial effect.
The fiber diameter of the invention can be made into superfine fiber, the fiber can be made into white, the fiber has permanent antibacterial function, the mechanical property can reach the standard of common fiber, the fiber completely meets various weaving requirements, the cost is equivalent to the cost of antibacterial after finishing, compared with the currently used antibacterial fiber, the cost is reduced by 50-80%, the pollution is reduced, the invention can expand the export of textiles, and the added value of the textiles is improved.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (8)
1. A preparation method of a polyester fiber with zinc oxide deposited on the surface of titanium dioxide is characterized by comprising the following steps: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
selecting titanium dioxide with the particle size of 20-50 nanometers as a base material, mixing the titanium dioxide with distilled water to prepare a nano titanium dioxide aqueous solution, wherein the concentration of the nano titanium dioxide is 1-10%, and adding zinc chloride to prepare a mixed solution, wherein the concentration of the zinc chloride is 0.5-5%;
dropwise adding 0.1% sodium hydroxide solution, adjusting the pH value to 5-9, reacting for 1-6 h at 140-200 ℃ by a hydrothermal kettle, and performing rotary evaporation to obtain nano powder;
carrying out surface modification on the nano antibacterial powder by a high-speed kneading machine, wherein the temperature is 30-90 ℃, the stirring speed is 1000-3000 r/min, a surface modifier is sprayed in by an atomizing device and mixed with the nano antibacterial powder, the addition amount of the surface modifier is 0.1-3 wt% of the mass of the nano antibacterial powder, and the nano antibacterial powder is mixed for 30-90 min at a high speed;
uniformly mixing the surface-modified nano antibacterial powder and polyester powder, wherein the nano antibacterial powder accounts for 10-50 wt% of the whole mass, and extruding the mixed raw materials through twin-screw extrusion, blending, granulating and extruding to obtain antibacterial master batches;
drying the antibacterial master batch at the temperature of 100-180 ℃ for 2-8 hours;
and uniformly mixing the dried antibacterial master batch with the PET polyester chips, or feeding the dried antibacterial master batch and the PET polyester chips into a feeder of a spinning machine through a separate metering device for melt spinning, wherein the spinning speed is 600-3000 m/min, and the initial pressure of a spinning assembly is 8-16 MPa, so as to obtain the antibacterial polyester fiber.
2. The method for preparing the polyester fiber with zinc oxide deposited on the surface of the titanium dioxide as claimed in claim 1, wherein the method comprises the following steps: the concentration of the nano titanium dioxide is 10%.
3. The method for preparing the polyester fiber with zinc oxide deposited on the surface of the titanium dioxide as claimed in claim 1, wherein the method comprises the following steps: the concentration of the zinc chloride is 2 percent.
4. The method for preparing the polyester fiber with zinc oxide deposited on the surface of the titanium dioxide as claimed in claim 1, wherein the method comprises the following steps: the surface modifier is one of active organosilicon series surface modifiers or titanate series surface modifiers.
5. The method for preparing the polyester fiber with zinc oxide deposited on the surface of the titanium dioxide as claimed in claim 1, wherein the method comprises the following steps: the polyester powder is one of PET or PBT powder.
6. The method for preparing the polyester fiber with zinc oxide deposited on the surface of the titanium dioxide as claimed in claim 1, wherein the method comprises the following steps: the basic resin slice is a spinning-grade PET polyester slice.
7. The method for preparing the polyester fiber with zinc oxide deposited on the surface of the titanium dioxide as claimed in claim 1, wherein the method comprises the following steps: in the spinning process, the spinning temperature is 270-300 ℃.
8. The method for preparing the polyester fiber with zinc oxide deposited on the surface of the titanium dioxide as claimed in claim 1, wherein the method comprises the following steps: the monofilament titer of the antibacterial fiber is 0.5-5D.
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