CN106719816B - Yttrium Oxide-Straw Cellulose Composite Nano Antibacterial Material - Google Patents

Abstract

The invention relates to an yttrium oxide-stalk cellulose composite nano antibacterial material. The method includes the following steps: uniformly dispersing the extracted straw cellulose into the yttrium oxide synthesis system, reacting in a high-pressure reactor, centrifuging and separating the precipitate and drying overnight to obtain the yttrium oxide-straw cellulose compound. After the nanomaterials are sterilized by absolute ethanol, centrifuge to remove the supernatant, then add water and mix well. Add yttrium oxide-straw cellulose composite materials with different concentrations into test tubes with certain concentrations of Escherichia coli and Staphylococcus, and place them under light and dark for a certain period of shaking culture; then use the plate counting method to analyze the effect of nanomaterials on leather. Inhibition efficiency of gram-negative and gram-positive bacteria. The yttrium oxide-straw cellulose composite material has a good inhibitory effect on Gram-negative and positive bacteria, especially very high inhibitory efficiency on Gram-negative bacteria, and is environmentally friendly without causing problems such as bacterial drug resistance.

Description

Yttrium Oxide-Straw Cellulose Composite Nano Antibacterial Material

technical field

The invention belongs to the technical field of preparation of antibacterial materials, and in particular relates to a composite nanometer antibacterial material of yttrium oxide-straw cellulose.

Background technique

Bacteria widely exist in the human living environment. Antibiotics can not only kill bacteria but also have a good inhibitory and killing effect on pathogenic microorganisms, so they are widely used. The abuse of antibiotics has led to the increasingly serious problem of bacterial resistance, threatening human health and the development of the environment. Finding alternatives to antibiotics has become one of the urgent problems to be solved. Studies have shown that antibacterial agents can effectively control infectious diseases caused by pathogenic bacteria. And some nanomaterials have very good bactericidal and antibacterial properties, which can not only avoid causing bacterial drug resistance, but also have low cost. Therefore, the use of nanomaterials as antibacterial agents has a good application prospect. At present, people have made great achievements in the research and development of nano-antibacterial materials, but it is still necessary to continuously develop more efficient and cheaper antibacterial agents.

Substituting non-antibiotic antibacterial agents for antibiotics can greatly reduce the harm of antibiotics to the environment and humans. Nowadays, light-enhanced antibacterial agents have attracted extensive attention of researchers due to their high-efficiency photocatalytic antibacterial properties and the advantages of no secondary pollution to the environment.

Straw is a common agricultural waste, and many documents have confirmed that it can be used as a template material; and cellulose can be separated from straw after proper refining. This can effectively increase the specific surface area of the template material. As a rare earth oxide, yttrium oxide has become a research hotspot in the field of photocatalysis.

Contents of the invention

In order to overcome the problems in the prior art, the invention provides an antibacterial agent with excellent antibacterial performance and light-enhanced antibacterial performance.

The technical solution for realizing the object of the present invention is: a kind of yttrium oxide-straw cellulose composite nano antibacterial material, which is composed of yttrium oxide and straw cellulose, wherein the mass ratio of yttrium: straw cellulose For (3.6～72):1.

Described antibacterial material is prepared by the following steps:

(1) placing yttrium nitrate, polyvinylpyrrolidone and straw cellulose in a mixed solution of water and ethanol, stirring evenly, and reacting hydrothermally at 150-200° C. for 10-20 hours;

(2) Centrifuge the reaction product of step (1), wash with ethanol, wash with water, and then dry at 60-80° C. to obtain the antibacterial material.

In the above preparation steps, the mass ratio of yttrium nitrate to polyvinylpyrrolidone is (2-6.25):1.

In the above preparation steps, the volume ratio of water and ethanol in the mixed solution of water and ethanol is (0.14-0.33):1.

The invention also provides the application of the yttrium oxide-stalk cellulose composite nano antibacterial material in inhibiting Gram-negative bacteria and Gram-positive bacteria.

In the described application, the Gram-negative bacteria are Escherichia coli, and the Gram-positive bacteria are Staphylococcus.

Compared with the prior art, the present invention has achieved the following beneficial effects:

①The purpose of adding straw to the yttrium oxide synthesis system is to adjust the structure of yttrium oxide, so that the yttrium oxide compound has a larger specific surface area and better dispersion performance. The synergistic effect of straw and yttrium oxide can effectively reduce the band gap of yttrium oxide width, thus ensuring better antibacterial properties of the resulting composites as well as light-enhanced antibacterial properties.

②In the preparation process, the unreacted polyvinylpyrrolidone was washed with ethanol, and then the unreacted inorganic ions were washed with deionized water to obtain pure yttrium oxide-straw cellulose composite nanomaterials.

③In the yttrium oxide-straw cellulose composite material prepared by the present invention, the mass ratio of yttrium: straw is about (3.6～72): 1, has excellent antibacterial performance and light-enhanced antibacterial performance, and the cost is low, and it is used for bacteria Contaminated wastewater has a high removal rate and has high potential industrial application value. For water with an initial bacterial concentration of 0.5 to 1.0×10 ⁷ CFU/mL, according to 60 mg/L yttrium oxide-straw cellulose, after 30 minutes (large intestine) or 60 minutes (staphylococcus) of light irradiation, the bacteria removal rate can reach 90 %above.

Description of drawings

Fig. 1 is an electron micrograph of the yttrium oxide-straw cellulose composite of Example 1 of the present invention.

Fig. 2 is the antibacterial rate of yttrium oxide-straw cellulose in the present invention to Escherichia coli after dark and light treatment at different working concentrations.

Fig. 3 is the antibacterial rate of yttrium oxide-straw cellulose in the present invention to Staphylococcus after dark and light treatment at different working concentrations.

Detailed ways

The present invention will be further described in detail below in conjunction with the accompanying drawings and specific embodiments. The accompanying drawings are provided for reference and illustration only, and are not intended to limit the present invention.

The preparation and application steps of the yttrium oxide-stalk cellulose composite nano antibacterial material of the present invention are as follows:

(1) Weigh 5-10 g of straw slurry and suspend it with 1 L of aqueous solution containing 0.12-0.16 TEMPO and 0.8-1 g NaBr;

(2) Utilize 0.1mol/L HCl to adjust the pH of the 5wt% NaClO solution to 10;

(3) Add the product of step (2) to the product of step (1) according to the ratio of 1.3-5mmol NaClO: 1g of straw slurry, and stir vigorously for 2 hours, during which the pH of the solution is adjusted with 0.3-1mol/L NaOH to keep it pH=10;

(4) After stirring, fully wash with deionized water, then filter, after stirring, fully wash with deionized water, then filter, then place it in an oven at 60-80°C for 8-16 hours , so as to obtain straw cellulose;

(5) Weigh 1.0-2.5g of yttrium nitrate hexahydrate, 0.4-0.5g of polyvinylpyrrolidone and 3-100mg of the product of step (4) into a system containing 14mL of water and 66mL of ethanol and stir evenly, then transfer the solution to the high pressure reaction In the kettle, react at 180°C for 10-20 hours;

(6) After centrifuging the reaction product of step (5) to remove water, the centrifuge speed is 2000-6000 rpm, first wash it with ethanol for 3-6 times to remove unreacted polyvinylpyrrolidone, and then wash it with deionized water for 3-6 times. Remove the unreacted inorganic ions once, put the cleaned reaction product in an oven and dry overnight at 60-80°C, so as to obtain the yttrium oxide-straw cellulose composite antibacterial material;

(7) Take 2-40 mg of the product of step (6) in a 1.5 mL test tube, add 1-1.5 ml of absolute ethanol to sterilize for 5-20 minutes, then centrifuge to remove the alcohol, add 0.5-1.5 ml of sterilized water to fully suspend;

(8) Weigh 20-50 g of tryptone soybean broth medium, stir and dissolve it in 0.5-2.0 L of water to obtain tryptone soybean broth, which is equally divided into two parts. Add 5 to 10 g of agar powder to one of the tryptone soybean broths, that is, tryptone soybean agar medium, and then sterilize them in an autoclave at 120 to 125° C. for 10 to 30 minutes. Plate the sterilized tryptone soy agar medium for later use.

(9) Take the Escherichia coli (Gram-negative bacteria) and Staphylococcus (Gram-positive bacteria) stored at -80°C, draw plates on the tryptone soybean agar medium plate, and invert at 32-38°C The activation culture was overnight. Then pick a single clone in a test tube containing 3-6mL tryptone soybean broth medium, cultivate overnight on a shaker at 32-38°C, take 0.5-1.5ml of bacteria and centrifuge at 150-220 rpm to remove the culture base, and then dilute the bacteria to 0.5-1.0× ¹⁰⁷ CFU/mL with sterilized water containing 5-15g of sodium chloride to obtain the test bacteria of Escherichia coli and Staphylococcus;

(10) Add different amounts of the product in step ⑺ to 2-8 mL of the product in step ⑼, so as to prepare the product in step ⑺ to a working concentration of 10-100 mg/L. Then place these solutions separately in the dark and light for 0.5-2 hours, the temperature during treatment is 32-38°C, the rotation speed is not lower than 150-220 rpm, and the light power is 300-500 watts;

(11) Dilute the product of step ⑽ to 10 ^-1 ~ 10 ^-4 , and then take 50 ~ 200ul each to evenly spread on the tryptone soybean agar medium plate, incubate overnight at 32 ~ 38°C and count.

(12) Calculation of bacteria removal rate or bacteriostasis rate = (C ₀ -C ₁ )/C ₀ ×100% (CFU after treatment without material in C ₀ bacterial solution, CFU after treatment with material in C1 bacterial solution) .

Example 1

The preparation and application of a novel yttrium oxide-stalk cellulose composite nano antibacterial material of the present invention comprises the following steps in turn:

(1) Weigh 10 g of straw slurry and suspend it with 1 L of aqueous solution containing 0.16 TEMPO and 1 g of NaBr;

(2) Utilize 0.1mol/L HCl to adjust the pH of the 5wt% NaClO solution to 10;

(3) Add the product of step (2) to the product of step (1) according to the ratio of 2.5mmol NaClO:1g straw slurry, and stir vigorously for 2 hours, during which the pH of the solution is adjusted with 0.5mol/L NaOH to keep the pH = 10;

(4) After the stirring is completed, fully wash with deionized water, then filter, after the stirring is completed, fully wash with deionized water, then filter, and then place it in an oven to dry, thereby obtaining straw cellulose;

(5) Weigh 1.552g of yttrium nitrate hexahydrate, 0.5g of polyvinylpyrrolidone and 10mg of the product of step (4) into a system containing 14mL of water and 66mL of ethanol and stir evenly, then transfer the solution to an autoclave, Down reaction 16 hours;

(6) After centrifuging the reaction product of step (5) to remove water, first wash with ethanol to remove unreacted polyvinylpyrrolidone, then wash with deionized water to remove unreacted inorganic ions, and place the cleaned reaction product in an oven Dry overnight at 60°C to obtain the yttrium oxide-stalk cellulose composite bacteriostatic material, as shown in Figure 1;

(7) Take 4 mg of the product of step (6) in a 1.5 mL test tube, add 1 mL of absolute ethanol to sterilize for 10 minutes, then centrifuge to remove the alcohol, add 1 mL of sterilized water to fully suspend;

(8) Weigh 30 g of tryptone soybean broth medium, stir and dissolve it in 1000 mL of water to obtain tryptone soybean broth, which is evenly divided into two parts. Add 7.5g of agar powder to one of the tryptone soybean broths, that is, tryptone soybean agar medium, and then place them in an autoclave and sterilize at 121° C. for 15 minutes. Plate the sterilized tryptone soy agar medium for later use.

(9) Take the Escherichia coli stored at -80°C, draw a plate on a tryptone soybean agar medium plate, and culture it upside down at 37°C for overnight activation. Then pick a single clone in a test tube containing 5mL of tryptone soybean broth medium, culture it overnight on a shaker at 37°C at a speed of 180rpm/min, take 1mL of the bacteria and centrifuge to remove the medium, and then incinerate with 8.5g NaCl Bacteria were diluted to 0.5-1.0×10 ⁷ CFU/mL with bacterial water to prepare E. coli test bacteria;

(10) Add different amounts of the product in step ⑺ to 5 mL of the product in step ⑼ to prepare the product in step ⑺ to a working concentration of 30 mg/L. These solutions were then placed in the dark and under light for 0.5 hours;

(11) Dilute the product from step ⑽ to 10 ^-1 , 10 ^-2 , 10 ^-3 , 10 ^-4 , and then take 100ul of each to evenly spread on the tryptone soybean agar medium plate, incubate overnight at 37°C upside down and count.

(12) Calculation of bacteria removal rate or bacteriostasis rate = (C ₀ -C ₁ )/C ₀ ×100% (CFU after treatment without material in C ₀ bacterial solution, CFU after treatment with material in C1 bacterial solution) .

Dark treatment bacteriostasis rate=(C ₀ -C ₁ )/C ₀ ×100%=93.12%.

Antibacterial rate of light treatment=(C ₀ -C ₁ )/C ₀ ×100%=99.23%.

Example 2

The preparation and application of a novel yttrium oxide-stalk cellulose composite nano antibacterial material of the present invention comprises the following steps in turn:

(1) Weigh 10 g of straw slurry and suspend it with 1 L of aqueous solution containing 0.16 TEMPO and 1 g of NaBr;

(2) Utilize 0.1mol/L HCl to adjust the pH of the 5wt% NaClO solution to 10;

(3) Add the product of step (2) to the product of step (1) according to the ratio of 2.5mmol NaClO:1g straw slurry, and stir vigorously for 2 hours, during which the pH of the solution is adjusted with 0.5mol/L NaOH to keep the pH = 10;

(4) After the stirring is completed, fully wash with deionized water, then filter, after the stirring is completed, fully wash with deionized water, then filter, and then place it in an oven to dry, thereby obtaining straw cellulose;

(5) Weigh 1.552g of yttrium nitrate hexahydrate, 0.5g of polyvinylpyrrolidone and 10mg of the product of step (4) into a system containing 14mL of water and 66mL of ethanol and stir evenly, then transfer the solution to an autoclave, Down reaction 16 hours;

(6) After centrifuging the reaction product of step (5) to remove water, first wash with ethanol to remove unreacted polyvinylpyrrolidone, then wash with deionized water to remove unreacted inorganic ions, and place the cleaned reaction product in an oven Dry overnight at 60°C to obtain the yttrium oxide-straw cellulose composite antibacterial material;

(7) Take 4 mg of the product of step (6) in a 1.5 mL test tube, add 1 mL of absolute ethanol to sterilize for 10 minutes, then centrifuge to remove the alcohol, add 1 mL of sterilized water to fully suspend;

(8) Weigh 30 g of tryptone soybean broth medium, stir and dissolve it in 1000 mL of water to obtain tryptone soybean broth, which is evenly divided into two parts. Add 7.5g of agar powder to one of the tryptone soybean broths, that is, tryptone soybean agar medium, and then place them in an autoclave and sterilize at 121° C. for 15 minutes. Plate the sterilized tryptone soy agar medium for later use.

(9) Take the Escherichia coli stored at -80°C, draw a plate on a tryptone soybean agar medium plate, and culture it upside down at 37°C for overnight activation. Then pick a single clone in a test tube containing 5mL of tryptone soybean broth medium, culture it overnight on a shaker at 37°C at a speed of 180rpm/min, take 1mL of the bacteria and centrifuge to remove the medium, and then incinerate with 8.5g NaCl Bacteria were diluted to 0.5-1.0×10 ⁷ CFU/mL with bacterial water to prepare E. coli test bacteria;

(10) Add different amounts of the product in step ⑺ to 5 mL of the product in step ⑼ to prepare the product in step ⑺ to a working concentration of 60 mg/L. These solutions were then placed in the dark and under light for 0.5 hours;

(11) Dilute the product from step ⑽ to 10 ^-1 , 10 ^-2 , 10 ^-3 , 10 ^-4 , and then take 100ul of each to evenly spread on the tryptone soybean agar medium plate, incubate overnight at 37°C upside down and count.

(12) Calculation of bacteria removal rate or bacteriostasis rate = (C ₀ -C ₁ )/C ₀ ×100% (CFU after treatment without material in C ₀ bacterial solution, CFU after treatment with material in C1 bacterial solution) .

Dark treatment bacteriostasis rate=(C ₀ -C ₁ )/C ₀ ×100%=98.91%.

Antibacterial rate of light treatment=(C ₀ -C ₁ )/C ₀ ×100%=99.72%.

Example 3

The preparation and application of a novel yttrium oxide-stalk cellulose composite nano antibacterial material of the present invention comprises the following steps in turn:

(1) Weigh 10 g of straw slurry and suspend it with 1 L of aqueous solution containing 0.16 TEMPO and 1 g of NaBr;

(2) Utilize 0.1mol/L HCl to adjust the pH of the 5wt% NaClO solution to 10;

(3) Add the product of step (2) to the product of step (1) according to the ratio of 2.5mmol NaClO:1g straw slurry, and stir vigorously for 2 hours, during which the pH of the solution is adjusted with 0.5mol/L NaOH to keep the pH = 10;

(4) After the stirring is completed, fully wash with deionized water, then filter, after the stirring is completed, fully wash with deionized water, then filter, and then place it in an oven to dry, thereby obtaining straw cellulose;

(5) Weigh 1.552g of yttrium nitrate hexahydrate, 0.5g of polyvinylpyrrolidone and 10mg of the product of step (4) into a system containing 14mL of water and 66mL of ethanol and stir evenly, then transfer the solution to an autoclave, Down reaction 16 hours;

(6) After centrifuging the reaction product of step (5) to remove water, first wash with ethanol to remove unreacted polyvinylpyrrolidone, then wash with deionized water to remove unreacted inorganic ions, and place the cleaned reaction product in an oven Dry overnight at 60°C to obtain the yttrium oxide-straw cellulose composite antibacterial material;

(7) Take 4 mg of the product of step (6) in a 1.5 mL test tube, add 1 mL of absolute ethanol to sterilize for 10 minutes, then centrifuge to remove the alcohol, add 1 mL of sterilized water to fully suspend;

(8) Weigh 30 g of tryptone soybean broth medium, stir and dissolve it in 1000 mL of water to obtain tryptone soybean broth, which is evenly divided into two parts. Add 7.5g of agar powder to one of the tryptone soybean broths, that is, tryptone soybean agar medium, and then place them in an autoclave and sterilize at 121° C. for 15 minutes. Plate the sterilized tryptone soy agar medium for later use.

(9) Take the Escherichia coli stored at -80°C, draw a plate on a tryptone soybean agar medium plate, and culture it upside down at 37°C for overnight activation. Then pick a single clone in a test tube containing 5mL of tryptone soybean broth medium, culture it overnight on a shaker at 37°C at a speed of 180rpm/min, take 1mL of the bacteria and centrifuge to remove the medium, and then incinerate with 8.5g NaCl Bacteria were diluted to 0.5-1.0×10 ⁷ CFU/mL with bacterial water to prepare E. coli test bacteria;

(10) Add different amounts of the product in step ⑺ to 5 mL of the product in step ⑼ to prepare the product in step ⑺ to a working concentration of 100 mg/L. These solutions were then placed in the dark and under light for 0.5 hours;

(11) Dilute the product from step ⑽ to 10 ^-1 , 10 ^-2 , 10 ^-3 , 10 ^-4 , and then take 100ul of each to evenly spread on the tryptone soybean agar medium plate, incubate overnight at 37°C upside down and count.

(12) Calculation of bacteria removal rate or bacteriostasis rate = (C ₀ -C ₁ )/C ₀ ×100% (CFU after treatment without material in C ₀ bacterial solution, CFU after treatment with material in C1 bacterial solution) .

Dark treatment bacteriostasis rate=(C ₀ -C ₁ )/C ₀ ×100%=99.98%.

Antibacterial rate of light treatment=(C ₀ -C ₁ )/C ₀ ×100%=99.99%.

Example 4

The preparation and application of a novel yttrium oxide-stalk cellulose composite nano antibacterial material of the present invention comprises the following steps in turn:

(1) Weigh 10 g of straw slurry and suspend it with 1 L of aqueous solution containing 0.16 TEMPO and 1 g of NaBr;

(2) Utilize 0.1mol/L HCl to adjust the pH of the 5wt% NaClO solution to 10;

(3) Add the product of step (2) to the product of step (1) according to the ratio of 2.5mmol NaClO:1g straw slurry, and stir vigorously for 2 hours, during which the pH of the solution is adjusted with 0.5mol/L NaOH to keep the pH = 10;

(4) After the stirring is completed, fully wash with deionized water, then filter, after the stirring is completed, fully wash with deionized water, then filter, and then place it in an oven to dry, thereby obtaining straw cellulose;

(5) Weigh 1.552g of yttrium nitrate hexahydrate, 0.5g of polyvinylpyrrolidone and 10mg of the product of step (4) into a system containing 14mL of water and 66mL of ethanol and stir evenly, then transfer the solution to an autoclave, Down reaction 16 hours;

(6) After centrifuging the reaction product of step (5) to remove water, first wash with ethanol to remove unreacted polyvinylpyrrolidone, then wash with deionized water to remove unreacted inorganic ions, and place the cleaned reaction product in an oven Dry overnight at 60°C to obtain the yttrium oxide-straw cellulose composite antibacterial material;

(7) Take 4 mg of the product of step (6) in a 1.5 mL test tube, add 1 mL of absolute ethanol to sterilize for 10 minutes, then centrifuge to remove the alcohol, add 1 mL of sterilized water to fully suspend;

(8) Weigh 30 g of tryptone soybean broth medium, stir and dissolve it in 1000 mL of water to obtain tryptone soybean broth, which is evenly divided into two parts. Add 7.5g of agar powder to one of the tryptone soybean broths, that is, tryptone soybean agar medium, and then place them in an autoclave and sterilize at 121° C. for 15 minutes. Plate the sterilized tryptone soy agar medium for later use.

(9) Staphylococci preserved at -80°C were drawn on a tryptone soybean agar medium plate, and cultured upside down at 37°C for overnight activation. Then pick a single clone in a test tube containing 5mL of tryptone soybean broth medium, culture it overnight on a shaker at 37°C at a speed of 180rpm/min, take 1mL of the bacteria and centrifuge to remove the medium, and then incinerate with 8.5g NaCl Bacteria were diluted to 0.5-1.0×10 ⁷ CFU/mL with bacterial water to prepare staphylococcus test bacteria;

(10) Add different amounts of the product in step ⑺ to 5 mL of the product in step ⑼ to prepare the product in step ⑺ to a working concentration of 30 mg/L. These solutions were then placed in the dark and light for 1 hour;

(11) Dilute the product from step ⑽ to 10 ^-1 , 10 ^-2 , 10 ^-3 , 10 ^-4 , and then take 100ul of each to evenly spread on the tryptone soybean agar medium plate, incubate overnight at 37°C upside down and count.

(12) Calculation of bacteria removal rate or bacteriostasis rate = (C ₀ -C ₁ )/C ₀ ×100% (CFU after treatment without material in C ₀ bacterial solution, CFU after treatment with material in C1 bacterial solution) .

Dark treatment bacteriostasis rate=(C ₀ -C ₁ )/C ₀ ×100%=48.96%.

Antibacterial rate of light treatment=(C ₀ -C ₁ )/C ₀ ×100%=88.22%.

Example 5

The preparation and application of a novel yttrium oxide-stalk cellulose composite nano antibacterial material of the present invention comprises the following steps in turn:

(1) Weigh 10 g of straw slurry and suspend it with 1 L of aqueous solution containing 0.16 TEMPO and 1 g of NaBr;

(2) Utilize 0.1mol/L HCl to adjust the pH of the 5wt% NaClO solution to 10;

(3) Add the product of step (2) to the product of step (1) according to the ratio of 2.5mmol NaClO:1g straw slurry, and stir vigorously for 2 hours, during which the pH of the solution is adjusted with 0.5mol/L NaOH to keep the pH = 10;

(4) After the stirring is completed, fully wash with deionized water, then filter, after the stirring is completed, fully wash with deionized water, then filter, and then place it in an oven to dry, thereby obtaining straw cellulose;

(5) Weigh 1.552g of yttrium nitrate hexahydrate, 0.5g of polyvinylpyrrolidone and 10mg of the product of step (4) into a system containing 14mL of water and 66mL of ethanol and stir evenly, then transfer the solution to an autoclave, Down reaction 16 hours;

(6) After centrifuging the reaction product of step (5) to remove water, first wash with ethanol to remove unreacted polyvinylpyrrolidone, then wash with deionized water to remove unreacted inorganic ions, and place the cleaned reaction product in an oven Dry overnight at 60°C to obtain the yttrium oxide-straw cellulose composite antibacterial material;

(7) Take 4 mg of the product of step (6) in a 1.5 mL test tube, add 1 mL of absolute ethanol to sterilize for 10 minutes, then centrifuge to remove the alcohol, add 1 mL of sterilized water to fully suspend;

(8) Weigh 30 g of tryptone soybean broth medium, stir and dissolve it in 1000 mL of water to obtain tryptone soybean broth, which is evenly divided into two parts. Add 7.5g of agar powder to one of the tryptone soybean broths, that is, tryptone soybean agar medium, and then place them in an autoclave and sterilize at 121° C. for 15 minutes. Plate the sterilized tryptone soy agar medium for later use.

(9) Staphylococci preserved at -80°C were drawn on a tryptone soybean agar medium plate, and cultured upside down at 37°C for overnight activation. Then pick a single clone in a test tube containing 5mL of tryptone soybean broth medium, culture it overnight on a shaker at 37°C at a speed of 180rpm/min, take 1mL of the bacteria and centrifuge to remove the medium, and then incinerate with 8.5g NaCl Bacteria were diluted to 0.5-1.0×10 ⁷ CFU/mL with bacterial water to prepare staphylococcus test bacteria;

(10) Add different amounts of the product in step ⑺ to 5 mL of the product in step ⑼ to prepare the product in step ⑺ to a working concentration of 60 mg/L. These solutions were then placed in the dark and light for 1 hour;

(11) Dilute the product from step ⑽ to 10 ^-1 , 10 ^-2 , 10 ^-3 , 10 ^-4 , and then take 100ul of each to evenly spread on the tryptone soybean agar medium plate, incubate overnight at 37°C upside down and count.

(12) Calculation of bacteria removal rate or bacteriostasis rate = (C ₀ -C ₁ )/C ₀ ×100% (CFU after treatment without material in C ₀ bacterial solution, CFU after treatment with material in C1 bacterial solution) .

Dark treatment bacteriostasis rate=(C ₀ -C ₁ )/C ₀ ×100%=76.54%.

Light treatment bacteriostasis rate=(C ₀ -C ₁ )/C ₀ ×100%=99.51%.

Example 6

The preparation and application of a novel yttrium oxide-stalk cellulose composite nano antibacterial material of the present invention comprises the following steps in turn:

(1) Weigh 10 g of straw slurry and suspend it with 1 L of aqueous solution containing 0.16 TEMPO and 1 g of NaBr;

(2) Utilize 0.1mol/L HCl to adjust the pH of the 5wt% NaClO solution to 10;

(3) Add the product of step (2) to the product of step (1) according to the ratio of 2.5mmol NaClO:1g straw slurry, and stir vigorously for 2 hours, during which the pH of the solution is adjusted with 0.5mol/L NaOH to keep the pH = 10;

(4) After the stirring is completed, fully wash with deionized water, then filter, after the stirring is completed, fully wash with deionized water, then filter, and then place it in an oven to dry, thereby obtaining straw cellulose;

(5) Weigh 1.552g of yttrium nitrate hexahydrate, 0.5g of polyvinylpyrrolidone and 10mg of the product of step (4) into a system containing 14mL of water and 66mL of ethanol and stir evenly, then transfer the solution to an autoclave, Down reaction 16 hours;

(6) After centrifuging the reaction product of step (5) to remove water, first wash with ethanol to remove unreacted polyvinylpyrrolidone, then wash with deionized water to remove unreacted inorganic ions, and place the cleaned reaction product in an oven Dry overnight at 60°C to obtain the yttrium oxide-straw cellulose composite antibacterial material;

(7) Take 4 mg of the product of step (6) in a 1.5 mL test tube, add 1 mL of absolute ethanol to sterilize for 10 minutes, then centrifuge to remove the alcohol, add 1 mL of sterilized water to fully suspend;

(8) Weigh 30 g of tryptone soybean broth medium, stir and dissolve it in 1000 mL of water to obtain tryptone soybean broth, which is evenly divided into two parts. Add 7.5g of agar powder to one of the tryptone soybean broths, that is, tryptone soybean agar medium, and then place them in an autoclave and sterilize at 121° C. for 15 minutes. Plate the sterilized tryptone soy agar medium for later use.

(9) Staphylococci preserved at -80°C were drawn on a tryptone soybean agar medium plate, and cultured upside down at 37°C for overnight activation. Then pick a single clone in a test tube containing 5mL of tryptone soybean broth medium, culture it overnight on a shaker at 37°C at a speed of 180rpm/min, take 1mL of the bacteria and centrifuge to remove the medium, and then incinerate with 8.5g NaCl Bacteria were diluted to 0.5-1.0×10 ⁷ CFU/mL with bacterial water to prepare staphylococcus test bacteria;

(10) Add different amounts of the product in step ⑺ to 5 mL of the product in step ⑼ to prepare the product in step ⑺ to a working concentration of 100 mg/L. These solutions were then placed in the dark and light for 1 hour;

(11) Dilute the product from step ⑽ to 10 ^-1 , 10 ^-2 , 10 ^-3 , 10 ^-4 , and then take 100ul of each to evenly spread on the tryptone soybean agar medium plate, incubate overnight at 37°C upside down and count.

(12) Calculation of bacteria removal rate or bacteriostasis rate = (C ₀ -C ₁ )/C ₀ ×100% (CFU after treatment without material in C ₀ bacterial solution, CFU after treatment with material in C1 bacterial solution) .

Dark treatment bacteriostasis rate=(C ₀ -C ₁ )/C ₀ ×100%=99.94%.

Antibacterial rate of light treatment=(C ₀ -C ₁ )/C ₀ ×100%=99.99%.

The data of Examples 1 to 6 are summarized in the following table, and are drawn into Fig. 2 according to the data of Examples 1 to 3, root

Figure 3 is drawn according to the data of Examples 4-6.

The light treatment in this paper adopts the sh-yz-B photocatalytic reactor of Shanghai Bilang Experimental Instrument Co., Ltd.

The above descriptions are only preferred feasible embodiments of the present invention, and are not intended to limit the scope of patent protection of the present invention. In addition to the above-mentioned embodiments, the present invention can also have other implementations, for example, the mass and volume of each component can be enlarged several times in equal proportions. All technical solutions formed by equivalent replacement or equivalent transformation fall within the scope of protection required by the present invention. The undescribed technical features of the present invention can be realized by or adopting existing technologies, and will not be repeated here.

Claims (8)

1. A composite nanometer bacteriostatic material of yttrium oxide-stalk cellulose is characterized in that, the bacteriostatic material is compounded by yttrium oxide and straw cellulose, and wherein, yttrium: the mass ratio of straw cellulose is (3.6～ 72): 1. 2. antibacterial material as claimed in claim 1, is characterized in that, is prepared by the following steps: (1) Put yttrium nitrate, polyvinylpyrrolidone and straw cellulose in a mixed solution of water and ethanol, stir evenly, and conduct a hydrothermal reaction at 150-200°C for 10-20 hours; (2) The reaction product of step (1) is centrifuged, washed with ethanol, washed with water, and then dried at 60-80°C to obtain the antibacterial material. 3. The antibacterial material according to claim 2, wherein the mass ratio of yttrium nitrate to polyvinylpyrrolidone is (2~6.25):1. 4. The antibacterial material according to claim 2, wherein the volume ratio of water and ethanol in the mixed solution of water and ethanol is (0.14~0.33):1. 5. a preparation method of yttrium oxide-stalk cellulose composite nano antibacterial material as claimed in claim 1, is characterized in that, comprises the steps: (1) Put yttrium nitrate, polyvinylpyrrolidone and straw cellulose in a mixed solution of water and ethanol, stir evenly, and conduct a hydrothermal reaction at 150-200°C for 10-20 hours; (2) The reaction product of step (1) is centrifuged, washed with ethanol, washed with water, and then dried at 60-80°C to obtain the antibacterial material. 6. the application of bacteriostatic material as described in any one of claim 1-4 in suppressing Gram-negative bacteria and Gram-positive bacteria. 7. application as claimed in claim 6, is characterized in that, gram-negative bacterium is escherichia coli. 8. The application according to claim 6, characterized in that the gram-positive bacterium is staphylococcus.