阅读说明：本技术 一种抗菌微晶玻璃粉末及其制备方法 (Antibacterial microcrystalline glass powder and preparation method thereof ) 是由 鲁建伟 丁林锋 徐亚楠 施王明 王海风 蒋伟忠 于 2021-08-25 设计创作，主要内容包括：本发明公开了一种抗菌微晶玻璃粉末,由以下重量比例的原料制成：二氧化硅42.0％、氧化铝2.0％、氧化铜3.7％、氧化亚铜24.4％、碳酸钠8.6％、五氧化二磷8.9％、硼酸10.4％。其制备方法,步骤如下：1)按组分比例称取二氧化硅、氧化铝、氧化铜、氧化亚铜、碳酸钠、五氧化二磷、硼酸；2)将称取的组分研磨混合均匀后,在1500℃的温度条件下,使其充分熔融,形成均匀的玻璃液；3)将得到的玻璃液浇注到提前预热的模具上成型,得到玻璃块；4)将玻璃块放入500℃的温度条件下,保温6小时进行微晶化处理,之后冷却,得到微晶玻璃块体；5)将微晶玻璃块体破碎,进行研磨,即得到抗菌微晶玻璃粉末。本发明制备方法工艺简单,产品成本低,抗菌效果优良。(The invention discloses antibacterial microcrystalline glass powder which is prepared from the following raw materials in parts by weight: 42.0 percent of silicon dioxide, 2.0 percent of aluminum oxide, 3.7 percent of copper oxide, 24.4 percent of cuprous oxide, 8.6 percent of sodium carbonate, 8.9 percent of phosphorus pentoxide and 10.4 percent of boric acid. The preparation method comprises the following steps: 1) weighing silicon dioxide, aluminum oxide, copper oxide, cuprous oxide, sodium carbonate, phosphorus pentoxide and boric acid according to the component proportion; 2) grinding and uniformly mixing the weighed components, and fully melting the components at the temperature of 1500 ℃ to form uniform glass liquid; 3) pouring the obtained molten glass on a preheated mold for molding to obtain a glass block; 4) putting the glass block into a temperature condition of 500 ℃, preserving heat for 6 hours, carrying out micro crystallization treatment, and then cooling to obtain a microcrystalline glass block body; 5) and (3) crushing the microcrystalline glass blocks, and grinding to obtain the antibacterial microcrystalline glass powder. The preparation method has the advantages of simple process, low product cost and excellent antibacterial effect.)

1. The antibacterial microcrystalline glass powder is characterized by being prepared from the following raw materials in parts by weight: 42.0 percent of silicon dioxide, 2.0 percent of aluminum oxide, 3.7 percent of copper oxide, 24.4 percent of cuprous oxide, 8.6 percent of sodium carbonate, 8.9 percent of phosphorus pentoxide and 10.4 percent of boric acid.

2. The method for preparing the antibacterial microcrystalline glass powder according to claim 1, characterized by comprising the following steps:

1) weighing silicon dioxide, aluminum oxide, copper oxide, cuprous oxide, sodium carbonate, phosphorus pentoxide and boric acid according to the component proportion;

2) grinding and uniformly mixing the weighed components, and fully melting the components at the temperature of 1500 ℃ to form uniform glass liquid;

3) pouring the obtained molten glass on a preheated mold for molding to obtain a glass block;

4) putting the glass block into a temperature condition of 500 ℃, preserving heat for 6 hours, carrying out micro crystallization treatment, and then cooling to obtain a microcrystalline glass block body;

5) and (3) crushing the microcrystalline glass blocks, and grinding to obtain the antibacterial microcrystalline glass powder.

3. The method for preparing the antibacterial microcrystalline glass powder as claimed in claim 2, wherein the fineness of the antibacterial microcrystalline glass powder in step 5) is 250-350 meshes.

Technical Field

The invention belongs to the technical field related to glass manufacturing, and particularly relates to antibacterial microcrystalline glass powder and a preparation method thereof.

Background

In recent years, inorganic antibacterial materials have become a research and development hotspot in the field of antibacterial materials due to the characteristics of high safety, good heat resistance, excellent antibacterial effect and the like.

The antibacterial microcrystalline glass powder is a product of application and development of inorganic antibacterial materials, and can be added into base materials such as paint, coating, enamel, adhesive and the like to be coated on the surfaces of various products such as vessels, building materials and the like, so that the slow-release antibacterial effect is achieved.

However, the traditional antibacterial microcrystalline glass powder has a complex preparation process, the base glass needs to be reheated, and the antibacterial glass product can be obtained after one-step or even multi-step heat treatment process, so that not only is the energy consumption increased, but also the process flow is complex, the microcrystallization time is long, the manufacturing cost is increased, and the large-scale production and application of the antibacterial microcrystalline glass powder are limited.

In addition, silver-based antibacterial agents are commonly used in the antibacterial glass powder on the market at present, and the antibacterial agents are expensive, silver ions are easy to reduce, the antibacterial effect is reduced, and the defect that the antibacterial effect is not durable exists.

Therefore, it is very important to develop a microcrystalline glass powder with simple preparation process and good antibacterial property.

Disclosure of Invention

Aiming at the problems, the invention provides the antibacterial microcrystalline glass powder with simple process, low cost and excellent antibacterial effect and the preparation method thereof.

In order to achieve the purpose, the invention adopts the following technical scheme that the antibacterial microcrystalline glass powder is characterized by being prepared from the following raw materials in parts by weight: 42.0 percent of silicon dioxide, 2.0 percent of aluminum oxide, 3.7 percent of copper oxide, 24.4 percent of cuprous oxide, 8.6 percent of sodium carbonate, 8.9 percent of phosphorus pentoxide and 10.4 percent of boric acid.

The invention provides a preparation method of antibacterial microcrystalline glass powder, which is characterized by comprising the following steps:

1) weighing silicon dioxide, aluminum oxide, copper oxide, cuprous oxide, sodium carbonate, phosphorus pentoxide and boric acid according to the component proportion;

2) grinding and uniformly mixing the weighed components, and fully melting the components at the temperature of 1500 ℃ to form uniform glass liquid;

3) pouring the obtained molten glass on a preheated mold for molding to obtain a glass block;

4) putting the glass block into a temperature condition of 500 ℃, preserving heat for 6 hours, carrying out micro crystallization treatment, and then cooling to obtain a microcrystalline glass block body;

5) and (3) crushing the microcrystalline glass blocks, and grinding to obtain the antibacterial microcrystalline glass powder.

The fineness of the antibacterial microcrystalline glass powder in the step 5) is 250-350 meshes.

Compared with the prior art, the invention has the beneficial effects that:

1. the antibacterial microcrystalline glass powder does not contain silver components, so that the cost can be reduced, and the antibacterial effect can be effectively prolonged. The antibacterial microcrystalline glass powder is prepared into a sample solution with the concentration of 0.2mg/mL, and the inhibition rate of the sample solution on escherichia coli and staphylococcus aureus reaches 100%.

2. According to the invention, by selecting the components, the inorganic antibacterial agent containing copper ions is directly added into the batch of the aluminosilicate glass, and through melt molding and one-time microcrystallization treatment, the antibacterial microcrystalline glass powder with excellent performance is obtained, and the antibacterial microcrystalline glass powder can be obtained without complicated nucleation and crystallization heat treatment, so that the preparation process of the microcrystalline glass is simplified, the energy consumption and cost of reheating are reduced, and the industrial production is easy to carry out.

3. The antibacterial microcrystalline glass powder takes the cuprite as a main crystal phase, is not easy to crystallize in multiple phases, and is beneficial to enhancing the antibacterial effect.

Drawings

FIG. 1 is a Differential Scanning Calorimeter (DSC) analysis of the starting glass prepared in example 1.

Fig. 2 is an X-ray diffraction spectrum of the antibacterial microcrystalline glass powder prepared in example 1, which shows that the microcrystalline glass powder has cuprite as a main crystal phase by the analysis of the Jade software.

FIG. 3 is a graph showing the antibacterial effect of antibacterial sample solutions containing different concentrations on Escherichia coli.

Fig. 4 is a graph showing the antibacterial effect of antibacterial sample solutions containing different concentrations on staphylococcus aureus.

Detailed Description

The present invention will be described in further detail with reference to the accompanying drawings and examples.

Example 1:

preparation of copper-containing aluminosilicate antibacterial microcrystalline glass powder

1. Weighing the following raw materials in percentage by weight: 42.0% of silicon dioxide, 2.0% of aluminum oxide, 3.7% of copper oxide, 24.4% of cuprous oxide, 8.6% of sodium carbonate, 8.9% of phosphorus pentoxide and 10.4% of boric acid;

2. the raw materials are fully and uniformly mixed, then are placed in a crucible, and are kept warm for 6 hours in a high-temperature furnace at 1500 ℃ to obtain glass liquid;

3. injecting the glass liquid obtained in the step 2 into a mold preheated in advance for molding, rapidly cooling in air to form a glass block, and performing Differential Scanning Calorimeter (DSC) analysis on a 20mg glass sample, wherein the glass transition point of the glass is determined to be 458 ℃ and the crystallization peak is 554 ℃ as shown in figure 1;

4. then, the glass block obtained in the step 3 is moved into a muffle furnace at 500 ℃, heat preservation is carried out for 6 hours for micro crystallization treatment, and then the glass block is cooled to room temperature along with the furnace to obtain a microcrystalline glass block;

5. and (4) crushing the microcrystalline glass blocks in the step (4), and putting the crushed microcrystalline glass blocks into a ball mill for ball milling to obtain antibacterial microcrystalline glass powder with the fineness of 325 meshes.

As can be seen from the X-ray diffraction spectrum of the antibacterial microcrystalline glass powder shown in FIG. 2, the antibacterial microcrystalline glass powder takes the cuprite as a main crystal phase, is not easy to crystallize in multiple phases, and is beneficial to enhancing the antibacterial effect.

II, testing the antibacterial performance of the copper-containing aluminosilicate microcrystalline glass powder:

1. culturing of the microorganisms: inoculating escherichia coli and staphylococcus aureus into a liquid culture medium, culturing for 24-28 hours, and preparing 5-10 multiplied by 10⁵The concentration of diluted bacterium liquid of CFU/mL is for later use;

2. sterilization of the experimental tools: sterilizing the relevant experimental tools at 121 ℃ under high pressure for 40 minutes, and cooling and then operating on a super clean bench;

3. preparation of samples of different concentrations: preparing the microcrystalline glass powder into sample solutions of 0.2mg/mL and 0.02 mg/mL;

4. respectively mixing 1mL of sample solution with different concentrations obtained in the step 3, 1mL of diluted bacterial liquid obtained in the step 1 and 3mL of sterile physiological saline to obtain 5mL of mixed solution, and culturing for 24 hours;

5. the mixture obtained in step 4 was transferred to 200uL agar plates and cultured for 48 hours to obtain the results (see FIG. 3 and FIG. 4).

The result shows that the bacteriostasis performance is obviously improved along with the increase of the concentration of the antibacterial sample solution. The antibacterial microcrystalline glass powder is prepared into a sample solution with the concentration of 0.2mg/mL, and the inhibition rate of the sample solution on escherichia coli and staphylococcus aureus reaches 100%.

The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, but rather as the subject of the invention in all its modifications, substitutions and alterations all within the spirit and scope of the appended claims.