CN104928799A - Preparation method for sustainable antibacterial nano-zinc oxide alginate fibers - Google Patents

Abstract

The invention discloses a preparation method for sustainable antibacterial nano-zinc oxide alginate fibers. The preparation method comprises the following steps: at first, uniformly mixing sodium alginate powder and nano-zinc oxide powder; adding distilled water, and carrying out uniform ultrasonic dispersion to prepare sodium alginate-based nano-zinc oxide colloid; adding plenty of fiber-grade sodium alginate powder to prepare a spinning solution; preparing the finished product, namely the nano-zinc oxide alginate fiber by a wet spinning step. The preparation method has the advantages that a series of technological means, such as stepped introducing of sodium alginate, are adopted skillfully, nano-zinc oxide can be uniformly dispersed and exist stably in a system, the final product, namely the nano-zinc oxide alginate fiber, is uniform and stable in quality, the prepared nano-zinc oxide alginate fiber is remarkable in antibacterial effect, bacteria growth can be inhibited effectively, and the nano-zinc oxide alginate fiber is safe and nontoxic, and can be widely applied to fields of medical treatment, military, health textile and the like.

Description

A preparation method of sustainable antibacterial nano zinc oxide seaweed fiber

technical field

The invention relates to a preparation method of seaweed fiber, in particular to a preparation method of sustainable antibacterial nano zinc oxide seaweed fiber.

Background technique

In the process of wound treatment, traditional dressings play the role of hemostasis, analgesia, anti-inflammation, and promotion of wound healing.

Studies have shown that medical dressings made of calcium alginate fibers can exchange with wound exudate and sodium ions in blood to release calcium ions. Because calcium ions can accelerate the formation of blood clots at the end of capillaries, it has good hemostatic effect.

As the amount of absorbed sodium ions increases, calcium alginate gradually turns into water-soluble sodium alginate, forming a thin gel layer on the surface of the wound, thereby preventing the adhesion of the dressing and the wound, reducing the pain of the patient, and at the same time keeping the wound surface A certain humidity and temperature create a good microcirculation environment for wound healing and promote early wound healing.

The formed gel thin layer will also contain bacteria. If it is not removed in time, after the gel surface is saturated with adsorbed bacteria, the bacteria will fall off and cause wound infection.

Therefore, in the process of use, it is necessary to replace it in time, which not only increases the cost of dressing, but also limits the promotion of calcium alginate fiber dressing to a certain extent.

Due to their small size and other characteristics, nanomaterials can enter cells in many ways.

Zinc oxide is an active oxide antibacterial material with good biocompatibility, safety and long-term effect.

Contents of the invention

The object of the present invention is to provide a method for preparing sustainable antibacterial nano-zinc oxide seaweed fiber. The method consumes less public works, has a short technological process, is less difficult to control, and has low manufacturing cost. The occurrence of broken ends caused by the plugging of the silk board; the prepared seaweed fiber, in which the nano-zinc oxide particles are evenly dispersed, has good antibacterial persistence and stability.

The technical solution adopted by the present invention to achieve the above object is a preparation method of sustainable antibacterial nano-zinc oxide seaweed fiber, which is characterized in that it comprises the following steps:

In the first step, according to the mass ratio of 0.1:100-20:100, the sodium alginate powder and the nano zinc oxide powder are evenly mixed;

Adding distilled water and ultrasonically dispersing to make sodium alginate-based nano-zinc oxide colloid; wherein, the mass of sodium alginate accounts for 0.1-5% of the total mass of sodium alginate-based nano-zinc oxide colloid;

In the second step, add a sufficient amount of fiber-grade sodium alginate powder to the above-mentioned sodium alginate-based nano-zinc oxide colloid, stir for 1-3 hours, and prepare a seaweed The mass percentage of sodium nitrate is 1-10% spinning solution;

The third step is to use a calcium chloride solution with a mass percentage concentration of 1-15% as a coagulation bath, put the above spinning solution through standing, filtering, defoaming, and then perform wet spinning, and then draw, shape, Dehydration, drying, that is, the finished product;

Wherein, the bath temperature of the coagulation bath is 30-60° C., and the draw ratio is 120-300%.

The technical effect directly brought by the above-mentioned technical solution is that the preparation method of the above-mentioned technical solution has a wide source of raw materials, low cost, and does not need to use expensive chemical raw materials; low cost.

In the above technical solution, the sodium alginate solution can be used as a stabilizer, which can effectively prevent the nano zinc oxide particles from agglomerating during the preparation of the spinning solution. Thus, it is beneficial to make a uniform and stable spinning solution dispersion system, ensure the spinning forming effect, and eliminate the clogging of the spinneret spinneret holes caused by "agglomeration", which in turn causes the phenomenon of broken ends.

The nano-zinc oxide seaweed fiber prepared by the above technical scheme can be seen through testing that the nano-particles are evenly distributed in the fiber.

This effectively solves the problem that in the prior art, antibacterial materials are often only adsorbed on the surface of the substrate; in particular, during the spinning and forming process of calcium alginate fibers, after the exchange of sodium ions and calcium ions, the surface of the fibers becomes coagulated. Glue, and then affect the antibacterial effect of antibacterial agents and other shortcomings or deficiencies.

The above technical solution can ensure that the nano zinc oxide particles are uniformly dispersed in the fiber.

In this way, the prepared fiber has long-lasting and stable antibacterial properties, and is especially suitable for use as a medical dressing.

Preferably, the particle diameter of the above-mentioned nano zinc oxide powder is 1-100 nm.

The technical effect directly brought by this preferred technical solution is that the filtration pressure of the spinning solution can be effectively reduced, and the spinning and forming can be facilitated.

Further preferably, the fiber-grade sodium alginate has a molecular weight of 300,000-600,000 and an M/G value of 0.5-1.5.

The technical effect directly brought by this preferred technical solution is that the viscosity of the spinning solution can be controlled more easily and better, so as to ensure the smooth progress of spinning and then ensure the quality of the final product.

To sum up, compared with the prior art, the present invention has the following advantages: less consumption of public works, short technological process, less difficult control, low manufacturing cost, and no broken ends due to plugging of the spinneret during the spinning process occurrence; the prepared seaweed fiber has beneficial effects such as uniform dispersion of nano-zinc oxide particles, good antibacterial persistence and stability.

Detailed ways

The present invention will be described in detail below in conjunction with the embodiments.

illustrate:

In each of the following examples:

The molecular weight of sodium alginate is 300,000-600,000, and the M/G value is 0.5-1.5;

The particle size of nano zinc oxide powder is 1-100nm;

The antibacterial results are obtained according to the antibacterial test method in the international standard ISO846.

Example 1

Mix 0.2g of sodium alginate powder and 0.002g of nano-zinc oxide split particles evenly, pour them into a beaker containing 200ml of distilled water, and disperse evenly under ultrasonic conditions to prepare a sodium alginate base with a mass percentage of sodium alginate of 0.1%. Nano zinc oxide colloidal system.

Add 1.8 g of sodium alginate powder to the colloidal solution, and stir at 30° C. for 1 hour to prepare a nano-zinc oxide spinning solution with a mass percentage of sodium alginate of 1% and a viscosity of 2000 mpa·s.

The spinning solution is left to stand, filtered, defoamed, wet-spun, and the nano-zinc oxide seaweed primary fiber is produced in coagulation.

The spinning temperature is 10°C, the coagulation bath is 1% by mass calcium chloride solution, and the coagulation bath temperature is 30°C. The primary nano zinc oxide seaweed fiber is stretched, shaped, dehydrated and dried to obtain the nano zinc oxide seaweed fiber.

The draft ratio was 120%.

test:

The prepared nano-zinc oxide seaweed fiber can be observed by transmission electron microscope: the nano-zinc oxide particles are evenly dispersed;

The results of antibacterial experiments show that it has a good inhibitory effect on Staphylococcus aureus and Escherichia coli, and the bacteriostatic rate is ≥ 90%, and the lasting effect is 2 days.

Example 2

Mix 1.0g of sodium alginate powder and 0.06g of nano-zinc oxide powder particles evenly, pour them into a beaker containing 200ml of distilled water, and disperse evenly under ultrasonic conditions to prepare a sodium alginate base with a mass percentage of sodium alginate of 0.5%. Nano zinc oxide colloidal system.

Add 4.0 g of sodium alginate powder to the colloidal solution, and stir for 2 hours at 30° C. to prepare a nano-zinc oxide spinning solution with a mass percentage of sodium alginate of 3% and a viscosity of 15,000 mpa·s.

The spinning solution is left to stand, filtered, defoamed, wet-spun, and the nano-zinc oxide seaweed primary fiber is produced in coagulation.

The spinning temperature is 20°C, the coagulation bath is a calcium chloride solution with a mass percentage of 5%, and the temperature of the coagulation bath is 30°C.

The primary nano zinc oxide seaweed fiber is stretched, shaped, dehydrated and dried to obtain the nano zinc oxide seaweed fiber. The draft ratio was 150%.

test:

The prepared nano-zinc oxide seaweed fiber can be observed by transmission electron microscope: the nano-zinc oxide particles are evenly dispersed;

The results of antibacterial experiments show that it has a good inhibitory effect on Staphylococcus aureus and Escherichia coli, with a bacteriostatic rate ≥ 92%, and the lasting effect is 3 days.

Example 3

Mix 2.0g of sodium alginate powder and 0.3g of nano-zinc oxide powder particles evenly, pour them into a beaker containing 200ml of distilled water, and disperse evenly under ultrasonic conditions to prepare a sodium alginate base with a mass percentage of sodium alginate of 1%. Nano zinc oxide colloidal system.

Add 8.0 g of sodium alginate powder to the colloid solution, and stir for 2 hours at 40° C. to prepare a nano-zinc oxide spinning solution with a mass percentage of sodium alginate of 5% and a viscosity of 30,000 mpa·s.

The spinning solution is left to stand, filtered, defoamed, wet-spun, and the nano-zinc oxide seaweed primary fiber is produced in coagulation. The spinning temperature is 30°C, the coagulation bath is 10% by mass calcium chloride solution, and the coagulation bath temperature is 40°C.

The primary nano zinc oxide seaweed fiber is stretched, shaped, dehydrated and dried to obtain the nano zinc oxide seaweed fiber.

The draft ratio was 200%.

test:

The prepared nano-zinc oxide seaweed fiber can be observed by transmission electron microscope: the nano-zinc oxide particles are evenly dispersed;

Antibacterial test results show that: it has a good inhibitory effect on Staphylococcus aureus and Escherichia coli, with a bacteriostatic rate ≥ 95%, and the lasting effect is 5 days.

Example 4

Mix 6.0g of sodium alginate powder and 0.5g of nano-zinc oxide powder particles evenly, pour them into a beaker containing 200ml of distilled water, and disperse evenly under ultrasonic conditions to obtain a sodium alginate base with a mass percentage of sodium alginate of 3%. Nano zinc oxide colloidal system.

Add 4.0 g of sodium alginate powder to the colloidal solution, and stir for 3 hours at 50° C. to prepare a nano-zinc oxide spinning solution with a concentration of 5% and a viscosity of 30,000 mpa·s.

The spinning solution is left to stand, filtered, defoamed, wet-spun, and the nano-zinc oxide seaweed primary fiber is produced in coagulation.

The spinning temperature is 40°C, the coagulation bath is a calcium chloride solution with a mass percentage of 15%, and the coagulation bath temperature is 50°C.

The primary nano zinc oxide seaweed fiber is stretched, shaped, dehydrated and dried to obtain the nano zinc oxide seaweed fiber.

The draft ratio was 300%.

test:

The prepared nano-zinc oxide seaweed fiber can be observed by transmission electron microscope: the nano-zinc oxide particles are evenly dispersed;

Antibacterial test results show that: it has a good inhibitory effect on Staphylococcus aureus and Escherichia coli, with a bacteriostatic rate ≥ 95%, and the lasting effect is 7 days.

Example 5

Mix 6.0g of sodium alginate powder and 1.0g of nano-zinc oxide powder particles evenly, pour them into a beaker containing 200ml of distilled water, and disperse evenly under ultrasonic conditions to obtain a sodium alginate base with a mass percentage of sodium alginate of 3%. Nano zinc oxide colloidal system.

Add 10.0 g of sodium alginate powder to the colloid solution, and stir for 2 hours at 50° C. to prepare a nano-zinc oxide spinning solution with a mass percentage of sodium alginate of 8% and a viscosity of 75,000 mpa·s.

The spinning solution is left to stand, filtered, defoamed, wet-spun, and the nano-zinc oxide seaweed primary fiber is produced in coagulation. The spinning temperature is 50°C, the coagulation bath is 10% by mass calcium chloride solution, and the coagulation bath temperature is 50°C.

The primary nano zinc oxide seaweed fiber is stretched, shaped, dehydrated and dried to obtain the nano zinc oxide seaweed fiber.

The draft ratio was 300%.

test:

The prepared nano-zinc oxide seaweed fiber can be observed by transmission electron microscope: the nano-zinc oxide particles are evenly dispersed;

The results of antibacterial experiments show that it has a good inhibitory effect on Staphylococcus aureus and Escherichia coli, with a bacteriostatic rate ≥ 97%, and the lasting effect is 10 days.

Example 6

Mix 10.0g of sodium alginate powder and 2.0g of nano-zinc oxide powder particles evenly, pour them into a beaker containing 200ml of distilled water, and disperse evenly under ultrasonic conditions to prepare a sodium alginate base with a mass percentage of sodium alginate of 5%. Nano zinc oxide colloidal system.

Add 10.0 g of sodium alginate powder to the colloid solution, and stir for 3 hours at 50° C. to prepare a nano-zinc oxide spinning solution with a mass percentage of sodium alginate of 10% and a viscosity of 100,000 mpa·s.

The spinning solution is left to stand, filtered, defoamed, wet-spun, and the nano-zinc oxide seaweed primary fiber is produced in coagulation. The spinning temperature is 50°C, the coagulation bath is a calcium chloride solution with a mass percentage of 15%, and the coagulation bath temperature is 60°C.

The primary nano zinc oxide seaweed fiber is stretched, shaped, dehydrated and dried to obtain the nano zinc oxide seaweed fiber.

The draft ratio was 300%.

test:

The prepared nano-zinc oxide seaweed fiber can be observed by transmission electron microscope: the nano-zinc oxide particles are evenly dispersed;

The antibacterial test results show that it has a good inhibitory effect on Staphylococcus aureus and Escherichia coli, with a bacteriostatic rate ≥ 99%, and the lasting effect is 12 days.

Claims (3)

1. a preparation method of sustainable antibacterial nano zinc oxide seaweed fiber, is characterized in that, comprises the following steps: In the first step, according to the mass ratio of 0.1:100-20:100, the sodium alginate powder and the nano zinc oxide powder are evenly mixed; Adding distilled water and ultrasonically dispersing to make sodium alginate-based nano-zinc oxide colloid; wherein, the mass of sodium alginate accounts for 0.1-5% of the total mass of sodium alginate-based nano-zinc oxide colloid; In the second step, add a sufficient amount of fiber-grade sodium alginate powder to the above-mentioned sodium alginate-based nano-zinc oxide colloid, stir for 1-3 hours, and prepare a seaweed The mass percentage of sodium nitrate is 1-10% spinning solution; The third step is to use a calcium chloride solution with a mass percentage concentration of 1-15% as a coagulation bath, put the above spinning solution through standing, filtering, defoaming, and then perform wet spinning, and then draw, shape, Dehydration, drying, that is, the finished product; Wherein, the bath temperature of the coagulation bath is 30-60° C., and the draw ratio is 120-300%. 2. The preparation method of sustainable antibacterial nano-zinc oxide fiber according to claim 1, characterized in that, the particle diameter of the nano-zinc oxide powder is 1-100nm. 3. The preparation method of sustainable antibacterial nano-zinc oxide fiber according to claim 1, characterized in that, the molecular weight of the fiber-grade sodium alginate is 300,000-600,000, and the M/G value is 0.5-1.5.