阅读说明：本技术 一种抗病毒锦纶6fdy的制备方法 (Preparation method of antiviral chinlon 6FDY ) 是由 郑幼丹 金志学 薛伟仁 高原 于 2020-12-10 设计创作，主要内容包括：本发明的一种抗病毒锦纶6FDY的制备方法,通过添加含有表面负载银纳米颗粒的介孔二氧化钛制成的锦纶6母粒制备得到抗病毒锦纶6FDY,研究了纤维的抗病毒活性以及不同添加量的抗病毒母粒对纤维的性能及生产情况的影响。结果表明：抗病毒母粒的添加赋予了纤维抗病毒活性,但会造成锦纶6的相对分子质量减小、分子量分布变宽、力学性能下降、可纺性与条干不匀率变差,对染色均匀性影响不大,对纤维的沸水收缩率具有改善作用。当添加4%的抗病毒母粒时,抗病毒锦纶6 FDY的抗病毒活性率达到99.97%,其物性指标满足使用要求并且纺况较好。(According to the preparation method of the antiviral chinlon 6FDY, the antiviral chinlon 6FDY is prepared by adding the chinlon 6 master batch prepared from the mesoporous titanium dioxide loaded with the silver nanoparticles on the surface, and the antiviral activity of the fiber and the influence of the antiviral master batches with different addition amounts on the performance and the production condition of the fiber are researched. The results show that: the addition of the antiviral master batch endows the fiber with antiviral activity, but causes the reduction of the relative molecular mass of the chinlon 6, the broadening of the molecular weight distribution, the reduction of the mechanical property, the deterioration of spinnability and evenness, little influence on the dyeing uniformity and improvement on the boiling water shrinkage of the fiber. When 4% of the antiviral master batch is added, the antiviral activity rate of the antiviral chinlon 6FDY reaches 99.97%, the physical property index of the antiviral chinlon meets the use requirement, and the spinning condition is good.)

1. The preparation method of the antiviral chinlon 6FDY is characterized by comprising the following steps: the raw materials adopted by the antiviral nylon-6 FDY comprise nylon-6 slices and antiviral master batches, wherein the antiviral master batches account for 0-6% by weight, and the nylon-6 slices comprise: the viscosity is 2.4-2.48, the water content is less than or equal to 0.06%, the titanium dioxide content is 0.2-0.4%, the antivirus mother particles are mesoporous titanium dioxide with silver nanoparticles loaded on the surface, the powder content is 24-26%, and the water content is less than or equal to 0.08%;

the preparation method comprises the following steps: the online masterbatch adding equipment is used for metering the antiviral masterbatch and the chinlon 6 slices respectively by a metering feeder, conveying the metered antiviral masterbatch and the chinlon 6 slices to a screw extruder, and extruding the metered antiviral masterbatch and the chinlon 6 slices after fully melting and mixing the metered antiviral masterbatch and the chinlon 6 slices by a screw in a machine barrel of the screw extruder; the melt is conveyed to a metering pump through a melt heat-insulation pipeline, is accurately metered by the metering pump and then is distributed to a spinning assembly, and is sprayed out from a spinneret orifice to form melt trickle, wherein the number of the spinneret orifice is 34; the monomer is pumped and cooled by cross air blow to form nascent fiber, the temperature of cooling air is 20-22 ℃, the humidity is 70-80%, and the wind speed is 0.45-0.48 m/s; the nascent fiber is precisely metered, oiled and bundled through an oil nozzle, and the concentration of the used oil agent is 8 percent; after oiling, the tows are continuously stretched by 5 rollers and interlaced, and finally wound into a cylinder on a finished product rotating shaft at the winding speed of 4600m/min to prepare the antiviral chinlon 6 fully drawn yarn.

2. The preparation method of antiviral chinlon 6FDY according to claim 1, characterized in that: the preparation raw materials of the antiviral master batch comprise: tetrabutyl titanate, absolute ethyl alcohol, silver nitrate and glacial acetic acid; the preparation method of the antiviral master batch comprises the following steps: respectively measuring 18-22ml of tetrabutyl titanate solution and 48-52ml of absolute ethyl alcohol by using a measuring cylinder, slowly dripping the tetrabutyl titanate solution into the absolute ethyl alcohol, strongly stirring for 9-12min by using a magnetic stirrer, controlling the temperature to be 28-32 ℃, and forming a light yellow clear solution after uniformly mixing, wherein the solution is marked as solution 1; measuring 5-10ml of glacial acetic acid and 30-50ml of deionized water by using a pipette, simultaneously adding the glacial acetic acid and 30-50ml of deionized water into another part of 48-52ml of absolute ethyl alcohol, adding deionized water to adjust the pH to be less than or equal to 3, then adding 0.1-10ml of silver nitrate into the solution, and violently stirring the mixture for 9-12min at the temperature of 28-32 ℃ to obtain a clear mixed solution, namely a solution 2; slowly dropping the solution 1 into the solution 2 under violent stirring at the dropping speed of 2-4mL/min, obtaining a light yellow solution after the dropping is finished, continuously and quickly stirring for 9-12min at the temperature of 28-32 ℃, then placing the obtained mixed solution into an ultrasonic reactor, controlling the temperature at 38-42 ℃ and the ultrasonic frequency at 45Hz, and fully reacting for a period of time until the inclined beaker gel does not move, thus obtaining the silver-loaded mesoporous titanium dioxide gel;

and placing the prepared mesoporous titanium dioxide gel containing the silver particles in an oven, drying to constant weight to obtain silver-loaded mesoporous titanium dioxide yellow crystals, cooling to room temperature, grinding the yellow crystals by using a mortar to obtain silver-loaded mesoporous titanium dioxide white powder, placing the ground silver-loaded mesoporous titanium dioxide white powder in a muffle furnace, roasting for a set time, taking out, and naturally cooling to room temperature to obtain silver-loaded mesoporous titanium dioxide nano powder.

3. The preparation method of antiviral chinlon 6FDY according to claim 1, characterized in that: the average particle diameter of the silver-loaded mesoporous titanium dioxide nano powder particles is 480-520 nanometers.

4. The preparation method of antiviral chinlon 6FDY according to claim 1, characterized in that: the preparation method can prepare the antiviral polyamide-6 fully drawn yarn with the addition amounts of 0%, 2%, 4% and 6% of the antiviral master batch respectively.

5. The preparation method of antiviral chinlon 6FDY according to claim 1, characterized in that: the screw is divided into 1-5 zones, and the temperatures of the screw 1-5 zone and the spinning box in the melting process are 253-.

Technical Field

The invention relates to the technical field of preparation of chinlon and fiber, in particular to a preparation method of antiviral chinlon 6 FDY.

Background

The textile is used as one of virus transmission media, and the anti-virus function is endowed to the textile so as to inhibit the transmission of viruses to a certain extent.

Currently, new coronavirus strains are abused worldwide, and human life safety is greatly threatened by viruses. Emerging infectious diseases caused by viruses are the forefront of global health concerns. The textile woven by the fiber material has large surface area and porosity, and the surface of the textile is easily infected with sweat stains and grease discharged by human bodies and becomes a hotbed of viruses under a proper temperature and humidity environment, thereby promoting the spread of the viruses. Therefore, the role played by textiles in the channel of viral transmission is not negligible. Chinlon with excellent wearability is widely applied to textiles such as clothes, home textiles and the like. Compared with other chemical fiber synthetic fibers, the high moisture regain of the chinlon 6 enables the chinlon 6 to provide a comfortable growth environment for viruses more easily, and the development of chinlon 6 textiles capable of restraining the activity of the viruses can effectively interfere the replication and transmission capacity of the viruses, so that the method has great research significance and application value. Research shows that various nano materials have antiviral efficacy, such as silver nanoparticles and metal oxides, which have been widely used in industrial and medical fields.

Disclosure of Invention

In order to overcome the problems, the invention aims to provide a preparation method of antiviral chinlon 6FDY, and the antiviral chinlon 6FDY can effectively intervene in the replication and transmission capacity of viruses.

The invention is realized by adopting the following scheme: the preparation method of the antiviral chinlon 6FDY comprises the following raw materials of chinlon 6 slices and antiviral master batches, wherein the antiviral master batches account for 0-6% of the total weight percentage, and the chinlon 6 slices are as follows: the viscosity is 2.4-2.48, the water content is less than or equal to 0.06%, the titanium dioxide content is 0.2-0.4%, the antivirus mother particles are mesoporous titanium dioxide with silver nanoparticles loaded on the surface, the powder content is 24-26%, and the water content is less than or equal to 0.08%;

the preparation method comprises the following steps: the online masterbatch adding equipment is used for metering the antiviral masterbatch and the chinlon 6 slices respectively by a metering feeder, conveying the metered antiviral masterbatch and the chinlon 6 slices to a screw extruder, and extruding the metered antiviral masterbatch and the chinlon 6 slices after fully melting and mixing the metered antiviral masterbatch and the chinlon 6 slices by a screw in a machine barrel of the screw extruder; wherein the screw is divided into 1-5 zones, and the temperatures of the screw 1-5 zones and the spinning manifold in the melting process are 253-255, 255-257, 256-258, 257-259 and 257-259 respectively; the melt is conveyed to a metering pump through a melt heat-insulation pipeline, is accurately metered by the metering pump and then is distributed to a spinning assembly, and is sprayed out from a spinneret orifice to form melt trickle, wherein the number of the spinneret orifice is 34; the monomer is pumped and cooled by cross air blow to form nascent fiber, the temperature of cooling air is 20-22 ℃, the humidity is 70-80%, and the wind speed is 0.45-0.48 m/s; the nascent fiber is precisely metered, oiled and bundled through an oil nozzle, and the concentration of the used oil agent is 8 percent; after oiling, the tows are continuously stretched by 5 rollers and interlaced, and finally wound into a cylinder on a finished product rotating shaft at the winding speed of 4600m/min to prepare the antiviral chinlon 6 fully drawn yarn.

Further, the preparation raw materials of the antiviral master batch comprise: tetrabutyl titanate, absolute ethyl alcohol, silver nitrate and glacial acetic acid; the preparation method of the antiviral master batch comprises the following steps: respectively measuring 18-22ml of tetrabutyl titanate solution and 48-52ml of absolute ethyl alcohol by using a measuring cylinder, slowly dripping the tetrabutyl titanate solution into the absolute ethyl alcohol, strongly stirring for 9-12min by using a magnetic stirrer, controlling the temperature to be 28-32 ℃, and forming a light yellow clear solution after uniformly mixing, wherein the solution is marked as solution 1; measuring 5-10ml of glacial acetic acid and 30-50ml of deionized water by using a pipette, simultaneously adding the glacial acetic acid and 30-50ml of deionized water into another part of 48-52ml of absolute ethyl alcohol, adding deionized water to adjust the pH to be less than or equal to 3, then adding 0.1-10ml of silver nitrate into the solution, and violently stirring the mixture for 9-12min at the temperature of 28-32 ℃ to obtain a clear mixed solution, namely a solution 2; slowly dropping the solution 1 into the solution 2 under violent stirring at the dropping speed of 2-4mL/min, obtaining a light yellow solution after the dropping is finished, continuously and quickly stirring for 9-12min at the temperature of 28-32 ℃, then placing the obtained mixed solution into an ultrasonic reactor, controlling the temperature at 38-42 ℃ and the ultrasonic frequency at 45Hz, and fully reacting for a period of time until the inclined beaker gel does not move, thus obtaining the silver-loaded mesoporous titanium dioxide gel;

and placing the prepared mesoporous titanium dioxide gel containing the silver particles in an oven, drying to constant weight to obtain silver-loaded mesoporous titanium dioxide yellow crystals, cooling to room temperature, grinding the yellow crystals by using a mortar to obtain silver-loaded mesoporous titanium dioxide white powder, placing the ground silver-loaded mesoporous titanium dioxide white powder in a muffle furnace, roasting for a period of time, taking out, and naturally cooling to room temperature to obtain silver-loaded mesoporous titanium dioxide nano powder.

Furthermore, the average particle diameter of the silver-loaded mesoporous titanium dioxide nano powder particles is 480-520 nm.

Furthermore, the preparation method can prepare the antiviral polyamide-6 fully drawn yarn with the addition of 0%, 2%, 4% and 6% of the antiviral master batch respectively.

The invention has the beneficial effects that: the nylon-6 functional fiber is prepared by adding the nylon-6 master batch containing mesoporous titanium dioxide loaded with silver nanoparticles on the surface into nylon-6 fiber. By researching the inhibiting effect of the functional fiber on the virus activity and the influence of the addition of the functional master batch on the physical properties and the production condition of a chinlon 6 fiber product, the antiviral chinlon 6FDY is obtained by determining the appropriate addition proportion, and the antiviral chinlon 6FDY can effectively interfere the virus replication and transmission capacity.

Drawings

FIG. 1 is a schematic flow diagram of the process of the present invention.

Detailed Description

The invention is further described below with reference to the accompanying drawings.

Referring to fig. 1, the preparation method of the antiviral nylon-6 FDY comprises the following steps of preparing raw materials of nylon-6 slices and antiviral master batches, wherein the antiviral master batches account for 0-6 wt%, and the raw materials of the nylon-6 slices comprise: the viscosity is 2.4-2.48, the water content is less than or equal to 0.06%, the titanium dioxide content is 0.2-0.4%, the antivirus mother particles are mesoporous titanium dioxide with silver nanoparticles loaded on the surface, the powder content is 24-26%, and the water content is less than or equal to 0.08%;

the preparation method comprises the following steps: the online masterbatch adding equipment is used for metering the antiviral masterbatch and the chinlon 6 slices respectively by a metering feeder, conveying the metered antiviral masterbatch and the chinlon 6 slices to a screw extruder, and extruding the metered antiviral masterbatch and the chinlon 6 slices after fully melting and mixing the metered antiviral masterbatch and the chinlon 6 slices by a screw in a machine barrel of the screw extruder; wherein the screw is divided into 1-5 zones, and the temperatures of the screw 1-5 zones and the spinning manifold in the melting process are 253-255, 255-257, 256-258, 257-259 and 257-259 respectively; the melt is conveyed to a metering pump through a melt heat-insulation pipeline, is accurately metered by the metering pump and then is distributed to a spinning assembly, and is sprayed out from a spinneret orifice to form melt trickle, wherein the number of the spinneret orifice is 34; the monomer is pumped and cooled by cross air blow to form nascent fiber, the temperature of cooling air is 20-22 ℃, the humidity is 70-80%, and the wind speed is 0.45-0.48 m/s; the nascent fiber is precisely metered, oiled and bundled through an oil nozzle, and the concentration of the used oil agent is 8 percent; after oiling, the tows are continuously stretched by 5 rollers and interlaced, and finally wound into a cylinder on a finished product rotating shaft at the winding speed of 4600m/min to prepare the antiviral chinlon 6 fully drawn yarn.

The preparation method of the antiviral chinlon 6FDY comprises the following steps:

the first embodiment is as follows: the preparation method of the antiviral chinlon 6FDY comprises the following steps of preparing chinlon 6 slices, adding no antiviral master batch, wherein the antiviral master batch accounts for 0 wt%, and preparing the following raw materials: viscosity is 2.4, water content is less than or equal to 0.06 percent, titanium dioxide content is 0.2 percent,

and (3) metering the nylon 6 semi-gloss slices by using a master batch online adding device, conveying the slices to a screw extruder, and fully melting and mixing the slices in the barrel by a screw to extrude the slices. Wherein, the temperatures of the screw 1-5 area and the spinning manifold in the melting process are 254, 256, 257, 258 and 258 ℃ respectively; the melt is conveyed to a metering pump through a melt heat-insulation pipeline, is accurately metered by the metering pump and then is distributed to a spinning assembly, and is sprayed out from a spinneret orifice to form melt trickle, wherein the number of the spinneret orifice is 34; the monomer is pumped and cooled by cross air blow to form nascent fiber, the temperature of cooling air is 21 ℃, the humidity is 75 percent, and the wind speed is 0.47 m/s; the nascent fiber is precisely metered, oiled and bundled through an oil nozzle, and the concentration of the used oil agent is 8 percent; after oiling, the tows are continuously stretched by 5 rollers and interlaced in a network manner, and finally wound into a cylinder on a finished product rotating shaft at the winding speed of 4600m/min to prepare the antiviral polyamide-6 fully drawn yarn (SD FDY 44dtex/34f) with 0 percent of the addition of the antiviral master batch.

Example two: the preparation method of the antiviral chinlon 6FDY comprises the following raw materials of chinlon 6 slices and antiviral master batches, wherein the weight percentage of the antiviral master batches is 2%, and the preparation method of the antiviral chinlon 6FDY comprises the following steps: the viscosity is 2.46, the water content is less than or equal to 0.06 percent, the titanium dioxide content is 0.2 percent, the antivirus master batch is mesoporous titanium dioxide with silver nanoparticles loaded on the surface, the powder content is 24 percent, and the water content is less than or equal to 0.08 percent;

by utilizing the master batch online adding device, the antiviral master batch and the chinlon 6 semi-gloss slices are respectively metered by the metering feeder and then conveyed to the screw extruder, and are fully melted and mixed by the screw in the machine barrel and then extruded. Wherein, the temperatures of a screw 1-5 area and a spinning manifold in the melting process are 255, 257, 258, 259 and 259 respectively; the melt is conveyed to a metering pump through a melt heat-insulation pipeline, is accurately metered by the metering pump and then is distributed to a spinning assembly, and is sprayed out from a spinneret orifice to form melt trickle, wherein the number of the spinneret orifice is 34; the monomer is pumped and cooled by cross air blow to form nascent fiber, the temperature of cooling air is 22 ℃, the humidity is 80 percent, and the wind speed is 0.48 m/s; the nascent fiber is precisely metered, oiled and bundled through an oil nozzle, and the concentration of the used oil agent is 8 percent; after oiling, the tows are continuously stretched by 5 rollers and interlaced in a network manner, and finally wound into a cylinder on a finished product rotating shaft at the winding speed of 4600m/min to prepare the antiviral polyamide-6 fully drawn yarn (SD FDY 44dtex/34f) with the addition of 2 percent of the antiviral master batch.

Example three: the preparation method of the antiviral chinlon 6FDY comprises the following raw materials of chinlon 6 slices and antiviral master batches, wherein the antiviral master batches account for 4% by weight, and the preparation method comprises the following steps: the viscosity is 2.47, the water content is less than or equal to 0.06 percent, the titanium dioxide content is 0.3 percent, the antivirus master batch is mesoporous titanium dioxide with silver nanoparticles loaded on the surface, the powder content is 25 percent, and the water content is less than or equal to 0.08 percent;

by utilizing the master batch online adding device, the antiviral master batch and the chinlon 6 semi-gloss slices are respectively metered by the metering feeder and then conveyed to the screw extruder, and are fully melted and mixed by the screw in the machine barrel and then extruded. Wherein, the temperatures of a screw 1-5 area and a spinning manifold in the melting process are 255, 257, 258, 259 and 259 respectively; the melt is conveyed to a metering pump through a melt heat-insulation pipeline, is accurately metered by the metering pump and then is distributed to a spinning assembly, and is sprayed out from a spinneret orifice to form melt trickle, wherein the number of the spinneret orifice is 34; the monomer is pumped and cooled by cross air blow to form nascent fiber, the temperature of cooling air is 22 ℃, the humidity is 70 percent, and the wind speed is 0.48 m/s; the nascent fiber is precisely metered, oiled and bundled through an oil nozzle, and the concentration of the used oil agent is 8 percent; after oiling, the tows are continuously stretched by 5 rollers and interlaced, and finally wound into a cylinder on a finished product rotating shaft at the winding speed of 4600m/min to prepare the antiviral polyamide 6 fully drawn yarn (SD FDY 44dtex/34f) with 4 percent of the addition amount of the antiviral master batch.

Example four: the preparation method of the antiviral chinlon 6FDY comprises the following raw materials of chinlon 6 slices and antiviral master batches, wherein the antiviral master batches account for 6% by weight, and the preparation method comprises the following steps: the viscosity is 2.48, the water content is less than or equal to 0.06 percent, the titanium dioxide content is 0.4 percent, the antivirus master batch is mesoporous titanium dioxide with silver nanoparticles loaded on the surface, the powder content is 26 percent, and the water content is less than or equal to 0.08 percent;

by utilizing the master batch online adding device, the antiviral master batch and the chinlon 6 semi-gloss slices are respectively metered by the metering feeder and then conveyed to the screw extruder, and are fully melted and mixed by the screw in the machine barrel and then extruded. Wherein, the temperatures of a screw 1-5 area and a spinning manifold in the melting process are 255, 257, 258, 259 and 259 respectively; the melt is conveyed to a metering pump through a melt heat-insulation pipeline, is accurately metered by the metering pump and then is distributed to a spinning assembly, and is sprayed out from a spinneret orifice to form melt trickle, wherein the number of the spinneret orifice is 34; the monomer is pumped and cooled by cross air blow to form nascent fiber, the temperature of cooling air is 22 ℃, the humidity is 80 percent, and the wind speed is 0.48 m/s; the nascent fiber is precisely metered, oiled and bundled through an oil nozzle, and the concentration of the used oil agent is 8 percent; after oiling, the tows are continuously stretched by 5 rollers and interlaced, and finally wound into a cylinder on a finished product rotating shaft at the winding speed of 4600m/min to prepare the antiviral polyamide 6 fully drawn yarn (SD FDY 44dtex/34f) with 6 percent of the addition amount of the antiviral master batch.

In the invention, the raw materials for preparing the antiviral master batch comprise: tetrabutyl titanate, absolute ethyl alcohol, silver nitrate and glacial acetic acid; the preparation method of the antiviral master batch comprises the following steps: respectively measuring 18-22ml of tetrabutyl titanate solution and 48-52ml of absolute ethyl alcohol by using a measuring cylinder, slowly dripping the tetrabutyl titanate solution into the absolute ethyl alcohol, strongly stirring for 9-12min by using a magnetic stirrer, controlling the temperature to be 28-32 ℃, and forming a light yellow clear solution after uniformly mixing, wherein the solution is marked as solution 1; measuring 5-10ml of glacial acetic acid and 30-50ml of deionized water by using a pipette, simultaneously adding the glacial acetic acid and 30-50ml of deionized water into another part of 48-52ml of absolute ethyl alcohol, adding deionized water to adjust the pH to be less than or equal to 3, then adding 0.1-10ml of silver nitrate into the solution, and violently stirring the mixture for 9-12min at the temperature of 28-32 ℃ to obtain a clear mixed solution, namely a solution 2; slowly dropping the solution 1 into the solution 2 under violent stirring at the dropping speed of 2-4mL/min, obtaining a light yellow solution after the dropping is finished, continuously and quickly stirring for 9-12min at the temperature of 28-32 ℃, then placing the obtained mixed solution into an ultrasonic reactor, controlling the temperature at 38-42 ℃ and the ultrasonic frequency at 45Hz, and fully reacting for a period of time until the inclined beaker gel does not move, thus obtaining the silver-loaded mesoporous titanium dioxide gel;

and placing the prepared mesoporous titanium dioxide gel containing the silver particles in an oven, drying to constant weight to obtain silver-loaded mesoporous titanium dioxide yellow crystals, cooling to room temperature, grinding the yellow crystals by using a mortar to obtain silver-loaded mesoporous titanium dioxide white powder, placing the ground silver-loaded mesoporous titanium dioxide white powder in a muffle furnace, roasting for a period of time, taking out, and naturally cooling to room temperature to obtain silver-loaded mesoporous titanium dioxide nano powder.

The preparation method of the antiviral master batch comprises the following steps:

the first embodiment is as follows: the preparation method of the antiviral master batch comprises the following steps: respectively measuring 18mL of tetrabutyl titanate solution (absolute drying of the measuring must be kept before the tetrabutyl titanate is measured) and 48mL of absolute ethyl alcohol by using a measuring cylinder, slowly dropping the tetrabutyl titanate solution into the 48mL of absolute ethyl alcohol, strongly stirring for 9min by using a magnetic stirrer, controlling the temperature at 28 ℃, and forming a light yellow clear solution after uniform mixing, which is marked as solution 1. 5mL of glacial acetic acid and 30mL of deionized water are measured by a pipette, added into another 48mL of absolute ethyl alcohol, added with a certain amount of deionized water, adjusted to pH less than or equal to 3, added with 0.1mL of silver nitrate, and stirred vigorously at 28 ℃ for 9min to obtain a clear mixed solution, which is marked as solution 2. Slowly dropping the solution 1 into the solution 2 under violent stirring at the dropping speed of about 2mL/min to obtain a light yellow solution after the dropping is finished, continuously and quickly stirring for 9min at the temperature of 28 ℃, then placing the obtained mixed solution into an ultrasonic reactor, controlling the temperature to be about 38 ℃ and the ultrasonic frequency to be 45Hz, and fully reacting for a period of time until the beaker is inclined and the gel cannot move, thus obtaining the silver-loaded mesoporous titanium dioxide gel.

Putting the prepared mesoporous titanium dioxide gel containing silver particles in an oven, and drying to constant weight to obtain the silver-loaded mesoporous titanium dioxide yellow crystal. Cooling to room temperature, and grinding the yellow crystal by using a mortar to obtain silver-loaded mesoporous titanium dioxide white powder. And placing the white powder of the silver-loaded mesoporous titanium dioxide obtained by grinding into a muffle furnace, roasting for a period of time, taking out, and naturally cooling to room temperature to obtain the silver-loaded mesoporous titanium dioxide nano powder.

Example two: the preparation method of the antiviral master batch comprises the following steps: the measuring cylinder is used for respectively measuring 20mL of tetrabutyl titanate solution (absolute drying of the measuring cylinder is required to be kept before the tetrabutyl titanate is measured) and 50mL of absolute ethyl alcohol, slowly dripping the tetrabutyl titanate solution into the 50mL of absolute ethyl alcohol, strongly stirring for 10min by using a magnetic stirrer, controlling the temperature at 30 ℃, and forming a light yellow clear solution after uniform mixing, which is marked as solution 1. A pipette measures 7mL of glacial acetic acid and 40mL of deionized water, simultaneously adds the glacial acetic acid and the deionized water into another 50mL of absolute ethyl alcohol, then adds a certain amount of deionized water, adjusts the pH to be less than or equal to 3, then adds 5mL of silver nitrate into the solution, and vigorously stirs the mixture for 10min at the temperature of 30 ℃ to obtain a clear mixed solution, which is marked as solution 2. Slowly dropping the solution 1 into the solution 2 under violent stirring at the dropping speed of about 3mL/min to obtain a light yellow solution after the dropping is finished, continuously and quickly stirring for 10min at the temperature of 30 ℃, then placing the obtained mixed solution into an ultrasonic reactor, controlling the temperature to be about 40 ℃ and the ultrasonic frequency to be 45Hz, and fully reacting for a period of time until the beaker is inclined and the gel cannot move, thus obtaining the silver-loaded mesoporous titanium dioxide gel.

Putting the prepared mesoporous titanium dioxide gel containing silver particles in an oven, and drying to constant weight to obtain the silver-loaded mesoporous titanium dioxide yellow crystal. Cooling to room temperature, and grinding the yellow crystal by using a mortar to obtain silver-loaded mesoporous titanium dioxide white powder. And placing the white powder of the silver-loaded mesoporous titanium dioxide obtained by grinding into a muffle furnace, roasting for a period of time, taking out, and naturally cooling to room temperature to obtain the silver-loaded mesoporous titanium dioxide nano powder.

Example three: the preparation method of the antiviral master batch comprises the following steps: measuring 22mL of tetrabutyl titanate solution (absolute drying of the measuring must be kept before the tetrabutyl titanate is measured) and 52mL of absolute ethyl alcohol by using a measuring cylinder respectively, slowly dropping the tetrabutyl titanate solution into the 52mL of absolute ethyl alcohol, and strongly stirring for 12min by using a magnetic stirrer, wherein the temperature is controlled at 32 ℃, and a light yellow clear solution is formed after uniform mixing and is marked as solution 1. 10mL of glacial acetic acid and 50mL of deionized water are measured by a pipette, added into another 52mL of absolute ethyl alcohol, added with a certain amount of deionized water, adjusted to pH less than or equal to 3, added with 10mL of silver nitrate, and stirred vigorously at 32 ℃ for 12min to obtain a clear mixed solution, which is marked as solution 2. Slowly dropping the solution 1 into the solution 2 under violent stirring at the dropping speed of about 4mL/min to obtain a light yellow solution after the dropping is finished, continuously and quickly stirring for 12min at the temperature of 32 ℃, then placing the obtained mixed solution into an ultrasonic reactor, controlling the temperature to be about 42 ℃ and the ultrasonic frequency to be 45Hz, and fully reacting for a period of time until the beaker is inclined and the gel cannot move, thus obtaining the silver-loaded mesoporous titanium dioxide gel.

Putting the prepared mesoporous titanium dioxide gel containing silver particles in an oven, and drying to constant weight to obtain the silver-loaded mesoporous titanium dioxide yellow crystal. Cooling to room temperature, and grinding the yellow crystal by using a mortar to obtain silver-loaded mesoporous titanium dioxide white powder. And placing the white powder of the silver-loaded mesoporous titanium dioxide obtained by grinding into a muffle furnace, roasting for a period of time, taking out, and naturally cooling to room temperature to obtain the silver-loaded mesoporous titanium dioxide nano powder.

The data of four examples of the preparation method of the antiviral chinlon 6FDY are analyzed as follows: namely, the first embodiment: adopting 0 percent of antiviral master batch by weight to prepare antiviral nylon-6 with 0 percent of antiviral master batch addition; example two: namely, the antiviral polyamide-6 with 2 percent of the addition amount of the antiviral master batch is prepared by adopting 2 percent of the weight percentage of the antiviral master batch; example three: namely, the antiviral nylon-6 with 4 percent of the addition amount of the antiviral master batch is prepared by adopting 4 percent of the weight percentage of the antiviral master batch; example four: namely, the antiviral polyamide-6 with 6 percent of the addition amount of the antiviral master batch is prepared by adopting 6 percent of the weight percentage of the antiviral master batch;

1. performance test of antiviral chinlon 6FDY

Antiviral activity test: the test is carried out according to ISO 18184:2014(E) antiviral textile test standard, the virus used in the test is influenza A virus H3N2MDCK cells, the common logarithmic mean value of 3 infection titer values immediately after the virus is inoculated in a control group is obtained through the test, the common logarithmic mean value of 3 infection titer values after the virus is contacted with an antiviral fabric specimen for 2 hours is obtained through the test, and the antiviral activity value is obtained through calculation. The standard specifies: if the antiviral activity value of the textile is less than 3.0, that is, the antiviral activity rate is less than 99.9%, the antiviral effect of the sample is small. The calculation of the antiviral activity value is shown in formula (1).

Mv＝1g(Va/Vc)＝1g(Va)-1g(Vc) (1)

In the formula:

mv is the antiviral activity value; lg (va) is the common log mean of the 3 infection titer values immediately after inoculation of the control group; lg (Vc) is the common log mean of the 3 infection titer values after 2 hours exposure to the antiviral fabric swatches.

The calculation of the antiviral activity ratio Mr is shown in the formula (2).

Mr＝(1-10-Mv)*100％ (2)

2. Results and analysis

2.1 Master batch

The antiviral powder contained in the antiviral master batch is mesoporous titanium dioxide loaded with silver nanoparticles on the surface. Inorganic nano particles are easy to agglomerate in a melt, and the particle size of the particles after agglomeration is greatly increased, so that the pressure rise speed of a spinning assembly is too high, a filter screen is blocked, the period of the assembly is short, the stable spinning process is hindered, and the number of broken ends of spinning is large. These problems can be solved by selecting nanoparticles of a suitable size and controlling the content thereof in the polymer matrix within a suitable range. The average particle size of the silver-loaded mesoporous titanium dioxide nanoparticles selected by the method is about 500 nanometers, and the spinning requirement is met.

2.2 antiviral Activity

Antiviral activity is the property of any substance that alters an element of the virion structure, rendering the virion incapable of replication. The test results of the antiviral activity performance of the antiviral chinlon 6FDY with the addition amounts of the antiviral master batches of 2%, 4% and 6% are shown in Table 1, and the data listed in the analysis table show that the antiviral activity rate of the antiviral chinlon 6FDY is increased along with the increase of the addition amount of the antiviral master batches. When 2% of the antiviral master batch is added, the antiviral activity rate of the fiber is only 98.93%, and the antiviral effect is small; when 4% of the antiviral master batch is added, the antiviral activity value is greatly improved, the antiviral activity rate reaches 99.97%, and the fiber has full-effect antiviral effect; when the addition amount of the antiviral master batch is further increased to 6%, the antiviral activity rate reaches 99.99%, and the improvement effect is not obvious.

TABLE 1 test results of antiviral Activity test of antiviral Chinlon 6FDY

2.3 relative molecular masses and distributions thereof

The relative molecular mass and the distribution of the high molecules have great influence on the stability of the spinning fluid mass, so the patent researches the relative molecular mass and the distribution of the antiviral polyamide-6 FDY with different addition amounts of the antiviral master batches, and as can be seen from the table 2, the larger the addition amount of the antiviral master batches is, the smaller the weight average molecular weight and the number average molecular weight of the polyamide-6 FDY is, and the wider the molecular weight distribution is. The reason is that in the spinning process, the chinlon 6 slices are heated and melted into a melt, and a repolymerization reaction occurs in the melting process, so that the relative molecular mass of the polymer can be continuously increased, but because mesoporous titanium dioxide loaded with silver nanoparticles on the surface is introduced into the antiviral chinlon 6FDY as an antiviral modifier, the inorganic nanoparticles are embedded among polymer chains, so that the distance among the polyamide molecular chains is increased, the thermal motion of the polyamide molecular chains is limited, the probability of mutual collision among the polyamide molecular chains is hindered, and the continuous increase of the molecular weight of the polyamide is hindered.

TABLE 2 relative molecular masses of antiviral Chinlon 6FDY

2.4 mechanical Properties and spinnability

Because fibers in the textile need to have necessary mechanical properties in the using process, the patent researches the influence of the antiviral master batches with different addition amounts on the breaking strength and the breaking elongation of the fibers. From the data of the mechanical property, the spinnability and the like of the antiviral chinlon 6FDY in the table 3, under the condition of consistent other conditions, compared with the common chinlon 6FDY with the same specification, the mechanical property of the antiviral chinlon 6FDY is reduced to different degrees, the reduction degree is increased along with the increase of the addition amount of the master batch, and the spinnability is also reduced along with the increase of the addition amount of the master batch. The main reasons are that the relative molecular mass of the antiviral chinlon 6FDY is reduced along with the introduction of the nano particles, and the mechanical property of the high polymer material is in positive correlation with the relative molecular mass; secondly, the silver-loaded mesoporous titanium dioxide nanoparticles have poor interface compatibility with a polymer matrix, when the content is increased, the probability of agglomeration of the nanoparticles is increased, the agglomerated particles become defect points in the polymer matrix due to damage of the regularity of the polymer, the stress around the defect points is increased rapidly under a stress state, so that stress concentration is generated, the defect points become weak points of material damage in a mechanical test process, and the breaking strength is reduced along with the increase of the addition amount. The main reasons for the reduction of the elongation at break are the presence of defect sites in the fibres and the nanoparticles limiting the ability of the polymeric chains to undergo relative displacement during stretching.

TABLE 3 mechanical Properties and spinnability of antiviral Chinlon 6FDY

2.5 evenness of yarn

Table 4 lists the evenness data of the antiviral chinlon 6FDY with different addition amounts of the master batches, and as can be seen from Table 4, the linear density variation coefficient and the evenness of the fiber are increased while the linear density variation coefficient of the fiber is not greatly influenced by the addition of the antiviral master batches, and the influence degree is increased along with the increase of the addition amounts. The reason is mainly two ways, firstly, because the antiviral nano particles are not only dispersed in the fiber, but also distributed on the surface of the fiber, the friction coefficients of the surface of the fiber are inconsistent, and the tension fluctuation of the strand silk is caused, so that the strand silk is not uniformly stretched; secondly, due to the introduction of the antiviral nano-particles, the defects in the fiber are increased, and the stress concentration caused by the defects also can cause uneven stretching of the strand.

TABLE 4 evenness of antiviral Chinlon 6FDY

2.6 dyeing uniformity

Table 5 lists the dyeing uniformity of the antiviral nylon-6 FDY at different master batch addition amounts, and it can be seen from the data in table 6 that the dyeing uniformity of the antiviral nylon-6 FDY at different master batch addition amounts is 4.5 grade, which indicates that the addition of the antiviral master batch has little influence on the dyeing uniformity of the antiviral nylon-6 FDY, so that there is no need to worry about the influence of the antiviral nanoparticles on the dyeing uniformity in the production process.

TABLE 5 dyeing uniformity of antiviral Chinlon 6FDY

2.7 shrinkage in boiling Water

The boiling water shrinkage rates of the antiviral nylon-6 FDY with different addition amounts of the master batch are listed in Table 6, and it can be seen from the data in Table 5 that the addition amount of the antiviral master batch reduces the boiling water shrinkage rate of the antiviral nylon-6 FDY, the larger the addition amount is, the smaller the boiling water shrinkage rate is, mainly because the antiviral nanoparticles play a role in limiting the movement of a high molecular chain in the fiber, so that the shape stability of the antiviral nylon-6 FDY is improved.

TABLE 6 boiling Water shrinkage of antiviral Chinlon 6FDY

3 conclusion

(1) The nylon-6 FDY with the antiviral effect is prepared by adding the nylon-6 master batch containing the silver-loaded mesoporous titanium dioxide nanoparticles, the antiviral activity of the fiber is detected by an antiviral activity test, the antiviral activity rate of the fiber is increased along with the increase of the addition amount of the antiviral master batch, but when the addition amount of the antiviral master batch is increased from 2% to 4%, the antiviral activity rate of the fiber is increased from 98.93% to 99.72%, and the antiviral effect is greatly improved.

(2) Compared with the chinlon 6FDY without the antiviral material, the higher the addition amount of the antiviral master batch is, the larger the relative molecular mass of the chinlon 6 is reduced, the molecular weight distribution is widened, the mechanical property is reduced, and the spinnability and the evenness are worsened; but has little influence on dyeing uniformity and has the function of improving the boiling water shrinkage of the fiber.

(3) When 4% of the antiviral master batch is added, the antiviral chinlon 6FDY has good antiviral effect, the physical index of the antiviral chinlon meets the use requirement, the spinning condition is good, the production cost can be saved, and meanwhile, the fiber with high antiviral activity is obtained.

In a word, the antiviral nylon-6 FDY is prepared by adding the nylon-6 master batch prepared from the mesoporous titanium dioxide loaded with the silver nanoparticles on the surface, and the antiviral activity of the fiber and the influence of the antiviral master batches with different addition amounts on the performance and the production condition of the fiber are researched. The results show that: the addition of the antiviral master batch endows the fiber with antiviral activity, but causes the reduction of the relative molecular mass of the chinlon 6, the broadening of the molecular weight distribution, the reduction of the mechanical property, the deterioration of spinnability and evenness, little influence on the dyeing uniformity and improvement on the boiling water shrinkage of the fiber. When 4% of the antiviral master batch is added, the antiviral activity rate of the antiviral chinlon 6FDY reaches 99.97%, the physical property index of the antiviral chinlon meets the use requirement, and the spinning condition is good.

The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.