阅读说明：本技术 抗菌天丝用氧化锌粉体及其制备方法 (Zinc oxide powder for antibacterial tencel and preparation method thereof ) 是由 廖宇涛 常彬彬 郭英鹏 许鸿胜 邢宇 何宝坤 于 2019-09-10 设计创作，主要内容包括：本发明公开了一种抗菌天丝用氧化锌粉体及其制备方法,其首先将纤维素纤维溶解在特定浓度的NMMO水溶液并调整溶液呈碱性形成第一混合溶液,再将活性氧化锌粉体置于另一特定浓度的NMMO水溶液中调整至碱性后再进行研磨形成第二混合溶液,将上述第一、二混合溶液按一定比例混合后继续研磨形成氧化锌粉体分散液后通过喷雾干燥形成氧化锌粉体。该氧化锌粉体可直接添加到天丝用纺丝溶液中,由于氧化锌在强碱环境中不与NMMO反应,也不产生游离的银离子,不变色,所以容易回收且不会带来杂质,不会使得天丝变色,能够为天丝提供持久高效的抗菌性能。(The invention discloses zinc oxide powder for antibacterial tencel and a preparation method thereof. The zinc oxide powder can be directly added into a spinning solution for tencel, and because zinc oxide does not react with NMMO in a strong alkali environment, free silver ions are not generated, and discoloration is avoided, the zinc oxide powder is easy to recover and does not bring impurities, the tencel is not discolored, and the high-efficiency lasting antibacterial performance can be provided for the tencel.)

1. The preparation method of the zinc oxide powder for the antibacterial tencel is characterized by comprising the following preparation steps:

(1) dissolving N-methylmorpholine-N-oxide in purified water to form aqueous solutions of N-methylmorpholine-N-oxide with the mass percentage concentration of 80-90 wt.% and 10-80 wt.%, respectively;

(2) taking an aqueous solution of N-methylmorpholine-N-oxide with the concentration of 80-90 wt.%, adding cellulose fiber into the aqueous solution of N-methylmorpholine-N-oxide, adjusting the pH value to 10-12 by using a pH regulator, and heating and dissolving at the temperature of 100 ℃ and 110 ℃ to form a uniform transparent liquid to form a first mixed solution for later use; wherein the amount of cellulose fibers is 10-25 wt.% of the total mass of the first mixed solution;

(3) taking an N-methylmorpholine-N-oxide aqueous solution with the concentration of 10-80 wt.%, adding active zinc oxide powder into the N-methylmorpholine-N-oxide aqueous solution for mixing, adjusting the pH value to 10-12 by using a pH regulator, adding into a sand mill, and grinding until the particle size of the active zinc oxide powder is less than 1 mu m to form a second mixed solution for later use; wherein the dosage of the active zinc oxide powder accounts for 10-50 wt% of the total mass of the second mixed solution;

(4) pouring the first mixed solution into the second mixed solution in a continuous grinding state in a sand mill, continuously grinding for 5-10min, and discharging to form a zinc oxide powder dispersion liquid; wherein the mass ratio of the first mixed solution to the second mixed solution is 1 (9-99);

(5) and (3) spray-drying the zinc oxide powder dispersion liquid to form the zinc oxide powder for the antibacterial tencel, wherein the temperature of a spray-drying outlet is lower than 120 ℃.

2. The method for preparing zinc oxide powder for antibacterial tencel according to claim 1, wherein the cellulose fiber is one of natural wood pulp and raw wood pulp.

3. The method for preparing the zinc oxide powder for antibacterial silk according to claim 1, wherein the zinc oxide powder is a zinc oxide powder aggregate having a micro-nano structure, the particle size of the zinc oxide powder aggregate is less than 5 μm, and any one-dimensional size of the powder surface in the zinc oxide powder aggregate is less than 100 nm.

4. The method for preparing zinc oxide powder for antibacterial silk according to claim 3, wherein the crystal shape of the zinc oxide powder in the zinc oxide powder agglomerates is at least one of rod-like, spherical and petal-like.

5. The method for preparing zinc oxide powder for antibacterial silk according to claim 1, wherein the pH regulator is sodium hydroxide, potassium hydroxide or ammonia water.

6. The zinc oxide powder for antibacterial tencel prepared by the preparation method of any one of claims 1 to 5.

Technical Field

The invention relates to a zinc oxide powder and a preparation method thereof, in particular to a zinc oxide powder for antibacterial tencel and a preparation method thereof, belonging to the technical field of inorganic powder modification.

Background

The tencel fiber is produced by pulp and the like formed by pounding natural plant fibers such as reproducible bamboo, wood and the like as raw materials, is published in the middle of the 90 s in the 20 th century, has advanced production process, high solvent recovery rate up to 99.7 percent, does not release harmful gases such as sulfur dioxide, hydrogen sulfide and the like in the production process like the traditional viscose fiber and the like, has rich raw material sources, and is energy-saving and environment-friendly in production. And the tencel fiber has a plurality of excellent performances of natural fiber and synthetic fiber, such as the advantages of natural fiber cotton such as comfort, good hand feeling and easy dyeing, and the advantages of synthetic fiber such as high strength and no shrinkage, and the clothes prepared from the tencel fiber not only have natural luster, smooth hand feeling, high strength, no shrinkage and the like, but also have excellent moisture permeability and air permeability, and particularly have good fabric effect when being blended with wool, so the tencel fiber is known as a product with most value in artificial fiber history for nearly half century.

With the social development and the improvement of living standard, the demands of people on textiles are not limited to durability, and the textiles which can meet the daily demands of people and have functionality for making life healthier, more comfortable and more environment-friendly have gradually become the development trend of textiles, wherein especially antibacterial textiles are developed more quickly, especially tencel with antibacterial property.

The antibacterial tencel is a tencel fiber added with an antibacterial substance, the antibacterial substance used in the prior art is mostly a silver ion type antibacterial agent, however, as the spinning solution of the tencel uses alkaline N-methylmorpholine-N-oxide as a solvent, most of the silver ion type antibacterial agent used in the prior art is easy to dissolve out in the solvent and is oxidized into brown silver oxide, so that the tencel is discolored, too many impurities in the solution are difficult to recover, the antibacterial performance of the antibacterial substance is ineffective, and the like.

Disclosure of Invention

In order to solve the technical problems, the invention provides the zinc oxide powder for the antibacterial tencel and the preparation method thereof, the prepared zinc oxide powder can be directly added into a spinning solution for the tencel, and the zinc oxide does not react with NMMO in a strong alkaline environment, does not generate free silver ions, does not change color, is easy to recover, does not bring impurities, does not change the color of the tencel, and can provide lasting and efficient antibacterial performance for the tencel.

The technical scheme of the invention is as follows:

the invention discloses a preparation method of zinc oxide powder for antibacterial tencel, which comprises the following preparation steps:

(1) dissolving N-methylmorpholine-N-oxide in purified water to form aqueous solutions of N-methylmorpholine-N-oxide with the mass percentage concentration of 80-90 wt.% and 10-80 wt.%, respectively;

(2) taking an aqueous solution of N-methylmorpholine-N-oxide with the concentration of 80-90 wt.%, adding cellulose fiber into the aqueous solution of N-methylmorpholine-N-oxide, adjusting the pH value to 10-12 by using a pH regulator, and heating and dissolving at the temperature of 100 ℃ and 110 ℃ to form a uniform transparent liquid to form a first mixed solution for later use; wherein the amount of cellulose fibers is 10-25 wt.% of the total mass of the first mixed solution;

(3) taking an N-methylmorpholine-N-oxide aqueous solution with the concentration of 10-80 wt.%, adding active zinc oxide powder into the N-methylmorpholine-N-oxide aqueous solution for mixing, adjusting the pH value to 10-12 by using a pH regulator, adding into a sand mill, and grinding until the particle size of the active zinc oxide powder is less than 1 mu m to form a second mixed solution for later use; wherein the dosage of the active zinc oxide powder accounts for 10-50 wt% of the total mass of the second mixed solution;

(4) pouring the first mixed solution into the second mixed solution in a continuous grinding state in a sand mill, continuously grinding for 5-10min, and discharging to form a zinc oxide powder dispersion liquid; wherein the mass ratio of the first mixed solution to the second mixed solution is 1 (9-99);

(5) and (3) spray-drying the zinc oxide powder dispersion liquid to form the zinc oxide powder for the antibacterial tencel, wherein the temperature of a spray-drying outlet is lower than 120 ℃.

The further technical scheme is as follows:

the cellulose fiber is one of natural wood pulp and raw wood pulp.

The zinc oxide powder is a zinc oxide powder aggregate with a micro-nano structure, the particle size of the zinc oxide powder aggregate is less than 5 mu m, and any one dimension of the powder surface in the zinc oxide powder aggregate is less than 100 nm.

The crystal shape of the zinc oxide powder in the zinc oxide powder aggregate is at least one of a rod shape, a sphere shape and a petal shape.

The pH regulator is sodium hydroxide, potassium hydroxide or ammonia water.

The invention also discloses the zinc oxide powder for the antibacterial tencel prepared by the preparation method.

The beneficial technical effects of the invention are as follows: according to the method, cellulose fibers are firstly dissolved in NMMO aqueous solution with a specific concentration and adjusted to be alkaline to form first mixed solution, then, active zinc oxide powder is placed in NMMO aqueous solution with another specific concentration and adjusted to be alkaline and then ground to form second mixed solution, the first mixed solution and the second mixed solution are mixed according to a certain proportion and then continuously ground to form zinc oxide powder dispersion liquid, and then, the zinc oxide powder is formed through spray drying. When the zinc oxide powder is applied to tencel fiber spinning as an antibacterial component, the tencel fiber can be kept white and not discolored all the time because the zinc oxide is not oxidized by alkaline NMMO; meanwhile, the zinc oxide powder only exists in the tencel, and cannot be dissolved out from the tencel in the water washing process to appear in a solvent, so that the impurity content in the solvent can be ensured to be low, and the recovery is convenient; the retention rate of the zinc oxide powder in the tencel fiber after washing is high, so that the fiber has excellent antibacterial performance, and the bacteriostasis rate of escherichia coli can reach 99.9 percent and is far higher than that of tencel when a conventional silver ion type antibacterial agent is used.

Drawings

FIG. 1 is a particle size distribution diagram of zinc oxide powder prepared in the specific example 1 of the present application;

FIG. 2 is an electron microscope picture of the zinc oxide powder dispersed in tencel prepared in example 1 of the present application.

Detailed Description

In order to clearly understand the technical means of the present invention and to implement the technical means according to the content of the specification, the following embodiments are further described in detail in the following with reference to the specific examples, which are used for illustrating the present invention and are not intended to limit the scope of the present invention.