CN1888159A - Multifunctional nano safe and efficient antibacterial fiber - Google Patents

Abstract

The invention relates to a fiber with multiple health care functions. The technical scheme is provided for solving the problems of single function, low bacteriostatic efficiency and short bacteriostatic life of the functional fiber in the prior art. The nanometer inorganic salt with efficient far infrared ray emitting function, efficient negative ion emitting function and efficient bacteriostasis function is fused in the spinning melt for spinning. Solving a large proportion of Ag by using flocculent silicon dioxide as an implant bed⁺The adding problem of (2) to achieve the effect of high-efficiency bacteriostasis. Inorganic salt particles coupled with suitable silane groupsThe agent is a surfactant, promotes the interface reaction with the melt, and reduces the wrap angle of the polymer melt. Meanwhile, the polymer is used as a melt dispersing agent, so that the polymer is more reasonably and uniformly dispersed in the melt. Adding the treated inorganic salt into a small amount of carrier to prepare master batch. Then mixed into the melt for spinning. Not only the dispersibility is increased, the smooth spinning can be realized, but also a plurality of novel products can be developed in a small amount to meet the market demand.

Description

Multifunctional nano safe and efficient antibacterial fiber

Technical Field: The present invention relates to a fiber with multiple health care functions, in particular to a method for preparing a fiber capable of releasing negative ions, emitting far infrared and having antibacterial effects.

Background technology: With the development of modern industrial technology and the improvement of people's living standards, the technology of the textile industry is also improving with each passing day. Following the differential fibers, synthetic fibers with multiple functions have emerged in the market in recent years. There are many single-function fibers such as far-infrared emitting fibers, negative ion emitting fibers, ultraviolet blocking fibers, and antibacterial fibers. With the improvement of people's life, the increasing awareness of health and the emergence of various functional fibers, people no longer just keep warm and cover their bodies in clothing, but expect multifunctionality. Therefore, fiber products with health care functions are more and more popular. Fabrics woven from functional fibers are very popular in the market. With the passage of time, people have realized the corresponding weaknesses of functional fiber fabrics, such as single fiber function, that is, one fiber, one function; antibacterial fiber has low antibacterial efficiency, especially for fungi produced in individual parts of the human body. . In addition, some functions are given to fiber fabrics by dipping and coating. After repeated washing, the functions will disappear and the durability is poor.

Summary of the invention: The purpose of this invention is to solve the above problems of single functional fiber, low fiber antibacterial effect, and lack of long-lasting fiber function. This solution is proposed-multifunctional nano-scale safe and efficient antibacterial fiber.

The multifunctional nano-safe high-efficiency antibacterial fiber proposed by the scheme as above is characterized in that its technological process is as follows:

①Preparation of multi-functional high-efficiency antibacterial masterbatch:

(1) Take high-efficiency antibacterial agent Ag+6.5%, titanium dioxide 93.5%, add silane-based coupling agent again, add silane-based coupling agent to account for 3% of the above material weight, dewater at 140～160 ℃ for 4～ 6 hours, mixing at 140-160°C and 4000rpm;

(2) Take 45% of the high-efficiency far-infrared emitting agent nano-sized zirconia and 55% of titanium dioxide, then add a silane-based coupling agent, add a silane-based coupling agent to account for 3% of the weight of the above substances, and remove water at 140-160°C Treat for 4-6 hours, mix at 140-160°C and 4000rpm;

(3) Get 75% of the nanoscale tourmaline powder of the high-strength negative ion emitter, 25% of titanium dioxide, add a silane-based coupling agent, add a silane-based coupling agent to account for 3% of the above material weight, remove Water treatment for 3-4 hours, mixing at 130-140°C and 4000rpm;

(4) Mix and activate the first three parts of the product at a high speed of 1:1:0.75, and stir at 140°C±5°C and 4000rpm for 20 minutes;

(5) Add B215 in oxygen resistant agent PKB and stir for 5 minutes at 4000rpm;

(6) Add high polymer carrier slices at a low speed of 500rpm, add PP or PET or PA, the addition ratio is high polymer:mixture=72.5:27.5, the temperature is above the softening point of the carrier and below the melting point of 40-50°C, Stirring at high speed 4000rpm for 20 minutes;

(7) Add the organic dispersant polymer polyethylene, the addition amount is 5% of the chip size, stir at high speed for 5 to 7 minutes, and then turn to low speed 200rpm to stir;

(8) Cool to 28°C at room temperature, and minimize the time of contact with air;

(9) Extruded into strips on a twin-screw extruder at a temperature of about 250°C;

(10) cooling in a water bath at 30°C;

(11) Blow dry with an air knife blow dryer;

(12) Pelletize and screen out multifunctional and highly effective antibacterial masterbatches.

②Spinning process of multifunctional nanometer high-efficiency antibacterial fiber:

(1) Add masterbatch to polymer dry slices, spin PA-6 filaments and enter the spinning extruder under the protection of nitrogen, and the temperature is 8-10°C lower than the conventional fiber spinning temperature;

(2) Through the melt filter, to the spinning box, the temperature of the box is 5-8 °C lower than that used for conventional fibers;

(3) Adjust the spinning on the spinning assembly, and the melt pressure at the resistance should be lower than that of conventional fiber spinning;

(4) Spinning cooling, the wind speed and wind pressure are lower than conventional fibers, and the wind temperature is slightly higher;

(5) Oil and water are added in the first step of primary fiber, and the oil and water are slightly higher than conventional spinning;

(6) Oil and water are added in the second stage of the primary fibers of the network, and the oil and water are slightly higher than those of conventional spinning;

(7) Spin out multifunctional pre-oriented fiber, multifunctional oriented fiber or multifunctional fully understretched fiber;

(8) Process the POY raw silk into DTY texturized yarn by adopting the method of internal under-stretching, false twist, heating and texturing, and then add oil and water by 3 to 3.5%;

(9) The product DTY is obtained, that is, the multifunctional nanometer safe and highly effective bacteriostatic elastic fiber.

Adopting this scheme can reflect the following advantages: ①The functionality of the fiber is obtained by adding functional inorganic salts. In order to solve the single functional problem of functional fibers, this plan adds three functional inorganic salts to make the fibers have multiple functions. Since these three inorganic salts are added to the fiber at the same time, the fiber has both bactericidal and antibacterial effects, as well as far-infrared rays and negative ion emission functions that are beneficial to the human body; ②General antibacterial fibers are only effective against negative bacteria such as E. coli and positive bacteria For example, Staphylococcus aureus has inhibitory effect, but it lacks antibacterial effect on fungi such as Candida albicans. This program uses a high content of Ag+ bacteriostatic agent with a content of 6.5%, so that the fiber of this program can have an inhibitory effect on Candida albicans of more than 99%; ③ dissolve the above three inorganic salts in the spinning melt Carry out spinning, so that the inorganic salt in the fiber will not lose its function, so that the fiber function will remain unchanged for a long time; ④ This scheme fully reflects the health care function of the fabric, and has multi-functional, safe and efficient antibacterial properties. Its antibacterial rate is as high as more than 95%, the emissivity of far infrared rays is more than 85%, and the emissivity of negative ions is more than 7000/cm3 (see the test report). The combination of three functional inorganic salts is composed of nano-scale powder, and the dispersion of each component in the polymer is solved through the process, which avoids the generation of melt particles in the spinning melt. This not only fully demonstrates the activation characteristics of small size and large specific surface area, but also makes the functions of various functions more fully playable, and can be carried out smoothly through melt spinning.

Description of drawings:

Figure 1 is a flow chart of the production process of the multifunctional nanometer high-efficiency antibacterial masterbatch of this scheme.

Fig. 2 is a flow chart of the spinning process of the multifunctional nanometer high-efficiency antibacterial fiber spinning process.

Detailed ways:

●The combination of three functional inorganic salt formulas added to the fibers of this solution:

①Far-infrared emission agent: 45% of nano-sized zirconia, 55% of titanium dioxide, silane-based coupling agent (accounting for 3% of the weight of the above substances);

② Negative ion emitter: 75% of nano-scale tourmaline powder, 25% of titanium dioxide, silane-based coupling agent (accounting for 3% of the weight of the above substances);

③High-efficiency antibacterial agent: Ag+6.5%, titanium dioxide 93.5%, silane-based coupling agent (accounting for 3% by weight of the above substances);

④Oxygen resistant agent: B215 (Swiss brand) in PKB;

⑤Organic dispersant: Polyethylene polymer.

●The improvements and innovations of this program lie in:

①In order to achieve the multi-functionality of the fiber, this program has been studied to add high-efficiency far-infrared ray emitting agents, high-efficiency anion emitting agents and high-efficiency antibacterial agents, according to their proportions in the fibers, respectively 2%, 2%, and 1.5%, and add them into the spinning Spinning in the melt, the purpose is to make the inorganic salt with a large content fully compatible with the spinning melt; choose a suitable silane-based coupling agent as the particle surface treatment agent of the inorganic salt, and promote the interaction between the inorganic salt and the polymer. Interfacial reaction; the functional inorganic salt will not be precipitated during washing and use, so as to maintain the multifunctionality of the fiber and make the fiber function more durable.

② A small amount of Ag+ in the fiber will be difficult to inhibit fungi, and a large proportion of Ag+ will be difficult to add to the polymer. This solution uses amorphous flocculent titanium dioxide as the implantation bed of Ag+, which solves the problem of adding a large proportion of Ag+ and achieves the inhibitory effect of the fiber on fungi.

③Use of nanomaterials:

This solution uses inorganic salt nanomaterials. The small size and large specific surface area of nanomaterials reflect their greater activity, and fully exert the functionality of multifunctional inorganic salts. Adding a smaller proportion can get a big effect. However, the use of nano-sized particles added to the spinning melt has the problem of difficult dispersion. In this plan, various particles are treated separately, that is, they are treated with a surface treatment agent, and then a powder is used as a dispersant. For example, the negative ion emitter uses tourmaline as the main dispersion and uses titanium dioxide as the dispersion for preliminary dispersion. Then add high molecular polyethylene as a melt dispersant before mixing into the melt to make a spinning melt. After separate treatment of nano-scale powder and two dispersions as above, a melt with no gel particles and excellent dispersibility can be obtained, which is beneficial to the normal spinning.

④ Production of multifunctional fibers by masterbatch method:

As a masterbatch method, the multifunctional inorganic salt is first dispersed in a small amount of carrier (PP, PET or PA) to make a masterbatch, and then mixed into the spinning melt at a certain ratio for spinning. This not only increases the melt dispersion again but also can arrange production of multiple varieties and small batches according to market needs.

●Determination of process parameters for the production of multi-functional nano-safety and high-efficiency antibacterial masterbatch:

① High-efficiency antibacterial formula combination (J) and high-strength negative ions and far-infrared emitters (F) dehydration and activation at high temperature:

Temperature: 140°C-160°C;

Time: 3～6h;

J:F=1:2.

If the temperature is high and the time is too long, the components will agglomerate; if the temperature is low and the time is too short, the powder will not lose enough water to achieve the purpose of activation.

② Surface treatment of formula components (high stirring treatment):

Temperature: 140℃±5℃;

Treatment agent: silane-based surface treatment agent;

High stirring speed: 4000rpm;

Time: 20 minutes.

The temperature is the same as the temperature in ① above; too much treatment agent will cause the powder to stick, and the number of high stirring rotations is insufficient, and the time is too short to cause the powder to agglomerate and disperse unevenly.

③ Addition of polymer carrier (adding at low speed and stirring at high speed):

Temperature: 40°C-50°C above the softening point of the polymer and below the melting point of the polymer;

Low speed: 200rpm;

High speed: 4000rpm;

Time: 20 minutes.

If the temperature is too low, the activation of the powder will be reduced, and if the temperature is too high, the polymer will approach the melting point, which will affect the dispersion of the powder. Stirring at low speed for short periods of time will result in uneven dispersion of the powder.

④ Stir at high speed and add organic dispersant and temperature-resistant and oxygen-resistant auxiliary agent dispersant:

Choose high molecular weight polyethylene,

Temperature: 10°C higher than the melting point of the dispersant flux;

Time: 5-7 minutes;

Amount of additive added: polymer weight* (3-5%).

Polymer dispersant polyethylene has a melting point of about 114°C, and the melting point temperature adopts the melting point of dispersant + 10°C.

If the temperature is too high and the time is too long, the viscosity of the dispersant is too low, and the coating will be uneven; otherwise, the viscosity is too high, and the polymer slices cannot be wrapped. If the amount of additives is too small, the viscosity loss of the polymer will be too large; otherwise, the color of the polymer will change easily.

⑤ Twin-screw temperature:

The twin-screw temperature generally takes the melting point of the polymer + (10-15°C);

If the temperature is too low, it is not conducive to forming strips (granulation), and the dispersion of powder and additives is uneven.

●Determination of process parameters for the production of multifunctional nanometer safe and efficient antibacterial fibers:

①Spinning temperature:

The spinning temperature is 8-15°C lower than the conventional spinning temperature;

Generally, the melting point of polymers added with powder and additives is 8-10°C lower than the temperature of conventional spinning polymers

Too high or too low spinning temperature will affect the fluidity of the spinning melt and cause spinning difficulties.

②Spinning cooling conditions:

Wind speed and wind pressure are slightly lower than conventional spinning;

Rheumatism and wind temperature are higher than conventional spinning;

Since the melting point of powder-containing polymers is slightly lower than that of conventional polymers and the enthalpy is lower, accelerated cooling will affect spinning understretch.

③ Spinning first and second oil agent:

The first and second spinning oils should be slightly higher than about 5% of conventional spinning;

High polymers containing powder have strong water absorption, and low oil and water will affect the underdrawing of spinning and the molding of POY.

●The working principle of this scheme is to add three functional inorganic salts to one fiber at the same time to make it multi-functional and promote the health care of the human body more comprehensively.

①The principle of high-efficiency antibacterial is mostly based on the highly active Ag+ being free. When it reaches the negatively charged microbial cells, the two are firmly adsorbed due to Coulomb gravity, and Ag+ enters the cell through the cell wall and reacts with "SH", destroying the cell Synthetase activity, cells lose their ability to divide and proliferate and die. (see test report).

②Nano-scale negative ion inorganic salt, which has the function of emitting high-strength negative ions (above 7000/cm3). After the human body accepts it, it can activate blood, relieve fatigue, and balance autonomic nerves. The inhalation of negative ions causes biological effects on the human body and regulates the central nervous system and autonomic nervous system. Regulating the function of the cerebral cortex has a good effect on improving the circulatory system. Due to the presence of negative ions, it can absorb odors and improve environmental conditions.

③The formula combination of far infrared and inorganic salt can emit 2-14um far infrared rays that can be absorbed by the human body.

The combination of the above three nano-scale inorganic salt functional formulas is dispersed in a high polymer carrier through a specific process to make a masterbatch. The masterbatch is quantitatively dispersed in the polymer to make a functional polymer melt. Then through a special spinning process, high-speed spinning into functional fibers FDY is multi-functional fully oriented fiber, POY is multi-functional pre-oriented fiber, HOY is multi-functional oriented fiber, DTY is multi-functional nano-safe and efficient antibacterial elastic fiber. Provide good textile raw materials for spinning fabric enterprises to develop new functional fabrics.

Claims (1)

1. A multifunctional nanometer safe and efficient bacteriostatic fiber is characterized in that its technological process is as follows: ①Preparation of multi-functional high-efficiency antibacterial masterbatch: (1) Take high-efficiency antibacterial agent Ag+6.5%, titanium dioxide 93.5%, add silane-based coupling agent again, add silane-based coupling agent to account for 3% of the above material weight, dewater at 140～160 ℃ for 4～ 6 hours, mixing at 140-160°C and 4000rpm; (2) Take 45% of the high-efficiency far-infrared emitting agent nano-sized zirconia and 55% of titanium dioxide, then add a silane-based coupling agent, add a silane-based coupling agent to account for 3% of the weight of the above substances, and remove water at 140-160°C Treat for 4-6 hours, mix at 140-160°C and 4000rpm; (3) Get 75% of the nanoscale tourmaline powder of the high-strength negative ion emitter, 25% of titanium dioxide, add a silane-based coupling agent, add a silane-based coupling agent to account for 3% of the above material weight, remove Water treatment for 3-4 hours, mixing at 130-140°C and 4000rpm; (4) Mix and activate the first three parts of the product at a high speed of 1:1:0.75, and stir at 140°C±5°C and 4000rpm for 20 minutes; (5) Add B215 in oxygen resistant agent PKB and stir for 5 minutes at 4000rpm; (6) Add high polymer carrier slices at a low speed of 500rpm, add PP or PET or PA, the addition ratio is high polymer:mixture=72.5:27.5, the temperature is above the softening point of the carrier and below the melting point of 40-50°C, Stirring at high speed 4000rpm for 20 minutes; (7) Add the organic dispersant polymer polyethylene, the addition amount is 5% of the chip size, stir at high speed for 5 to 7 minutes, and then turn to low speed 200rpm to stir; (8) Cool to 28°C at room temperature, and minimize the time of contact with air; (9) Extruded into strips on a twin-screw extruder at a temperature of about 250°C; (10) cooling in a water bath at 30°C; (11) Blow dry with an air knife blow dryer; (12) Pelletize and screen out multifunctional and highly effective antibacterial masterbatches. ②Spinning process of multifunctional nanometer high-efficiency antibacterial fiber: (1) Add masterbatch to polymer dry slices, spin PA-6 filaments and enter the spinning extruder under the protection of nitrogen, and the temperature is 8-10°C lower than the conventional fiber spinning temperature; (2) Through the melt filter, to the spinning box, the temperature of the box is 5-8 °C lower than that used for conventional fibers; (3) Adjust the spinning on the spinning assembly, and the melt pressure at the resistance should be lower than that of conventional fiber spinning; (4) Spinning cooling, the wind speed and wind pressure are lower than conventional fibers, and the wind temperature is slightly higher; (5) Oil and water are added in the first step of primary fiber, and the oil and water are slightly higher than conventional spinning; (6) Oil and water are added in the second stage of the primary fibers of the network, and the oil and water are slightly higher than those of conventional spinning; (7) Spin out multi-functional giving orientation fiber, multi-functional elastic fiber or multi-functional fully understretched fiber; (8) Process the POY raw silk into DTY texturized yarn by adopting the method of internal under-stretching, false twist, heating and texturing, and then add oil and water by 3 to 3.5%; (9) The product DTY is obtained, that is, the multifunctional nanometer safe and highly effective bacteriostatic elastic fiber.

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