CN118561268A

CN118561268A - Preparation method and application of macadamia shell antibacterial agent

Info

Publication number: CN118561268A
Application number: CN202411040011.2A
Authority: CN
Inventors: 张彬; 王清; 王琪盛; 杨正芳; 郭倩倩; 文官彬
Original assignee: Kunming University of Science and Technology
Current assignee: Kunming University of Science and Technology
Priority date: 2024-07-31
Filing date: 2024-07-31
Publication date: 2024-08-30

Abstract

The invention relates to a preparation method and application of an Australian nut shell antibacterial agent, wherein the preparation method of the Australian nut shell antibacterial agent comprises the following steps: step 1) selecting a material which is macadamia nut shells; step 2), dispersing the crushed materials into water according to a certain proportion to form a solution A; step 3) placing the solution A in a reaction kettle for reaction; and 4) filtering the product obtained after the reaction in the step 3), and collecting filtrate to obtain a solution B, wherein the solution B is the macadamia shell antibacterial agent. The invention adopts simple methods such as ultrasonic treatment method, hydrothermal reaction method, separation and impurity removal method and the like to prepare the macadimia shell antibacterial agent with excellent antibacterial performance. The work provides a hint for preparing the novel antibacterial material with excellent performance by taking the macadimia nut shells as the main raw material. The macadamia shell antibacterial agent prepared by the method has remarkable effects of resisting escherichia coli or staphylococcus aureus, and some mould and other miscellaneous bacteria in the sewage treatment process, and has broad-spectrum antibacterial effect.

Description

Preparation method and application of macadamia shell antibacterial agent

Technical Field

The invention belongs to the technical field of preparation methods and application of antibacterial agents, and particularly relates to the technical field of preparation methods of an Australian nut shell antibacterial agent.

Background

Macadamia nut (latin brand name: MACADAMIA INTEGRIFOLIAMAIDEN & Betche), alias: the kunshima chestnut, the macadamia nut, the hawaii nut and the kunshima nut are native to the macadamia. Is now widely planted in Yunnan province of China. At present, the development and utilization of macadimia nut shells mainly have the following aspects: firstly, backfilling fruit shells, burying the fruit shells in soil under fruit trees, and taking the fruit shells as fruit tree fertilizers; then the nut shell is calcined and the like to prepare the porous structure active carbon or is used for preparing adsorbents, water purifying agents and the like. Besides, the spice substances in the shells are extracted for preparing perfumes and cosmetics, preparing biomass charcoal from the shells, preparing liqueur and the like. No report on preparation of macadimia nut shell antibacterial agent by taking macadimia nut shells as main raw materials exists, and a large gap exists in the deep processing, development and utilization of the macadimia nut shells.

Disclosure of Invention

In order to solve the problems and defects, the invention provides a preparation method of an African nut shell antibacterial agent.

The invention is realized by adopting the following technical scheme.

The macadamia nut shells used in the invention are raw macadamia nut hard shells from a prandial tree planting demonstration base in the banum of Yunnan province, and the nut shells are dried in the shade and stored for later use.

A preparation method of an African nut shell antibacterial agent comprises the following steps:

Step 1) selecting macadamia shells as raw materials;

Step 2) crushing the macadamia nut shells, and dispersing the crushed macadamia nut shells in water according to a certain proportion to form a solution A;

step 3), placing the solution A in a reaction kettle for heating reaction;

And 4) filtering the product obtained after the reaction in the step 3), and collecting filtrate to obtain a solution B, wherein the solution B is the macadamia shell antibacterial agent.

Further, in the preparation method of the invention, the step 2) is specifically that the shell of the macadamia nut is crushed, and the crushed shell powder is dispersed in a container filled with distilled water to form a solution A; the weight ratio of the crushed shell powder to distilled water is 0.1-10g, and distilled water is 10-100 ml.

Further, the preparation method of the invention comprises the step 2), wherein the weight ratio of the shell powder of crushed macadimia nut shells to distilled water is 1g, and the distilled water is 20 ml.

Further, step 3) of the preparation method of the invention comprises the following steps: carrying out hydrothermal reaction for 5-24 hours at 100-400 ℃, and naturally cooling to room temperature.

Further, step 3) of the preparation method of the invention comprises the following steps: the hydrothermal reaction is carried out at 200 ℃ for 14 hours, and the mixture is naturally cooled to room temperature.

Furthermore, in the preparation method of the invention, an ultrasonic link is arranged between the step 2) and the step 3), namely, the solution A is stirred and dispersed and then is put into an ultrasonic cleaner to be subjected to ultrasonic treatment for a certain time (such as 1-60min, preferably 10 min) at room temperature.

Further, in the preparation method of the invention, the filtration in the step 4) is carried out by a water system microporous filter membrane with the size of 0.1-0.5 mu m.

Further, the filtration in step 4) in the preparation method of the invention is filtration through a water system microporous filter membrane of 0.1 mu m.

As a product, the invention protects the antibacterial agent obtained by the preparation method.

As an application, the invention protects the application of the antibacterial agent as a sterilization additive or a sewage treatment agent.

The application of the invention comprises the preparation of a microbial agent or medicament for resisting escherichia coli or staphylococcus aureus.

The beneficial effects of the invention are as follows:

1) The invention adopts simple methods such as ultrasonic treatment method, hydrothermal reaction method, separation and impurity removal method and the like to prepare the macadimia nut shell antibacterial agent, and has low raw material cost, simple preparation method and excellent antibacterial effect.

2) The macadamia shell antibacterial agent prepared by the method has broad-spectrum antibacterial effect and is excellent in effect on coliform bacteria or staphylococcus aureus, some mould and other miscellaneous bacteria in the sewage treatment process.

3) The macadamia shell antibacterial agent prepared by the invention has stronger compatibility, can be used as a sewage treatment agent for bacterial treatment in the water pollution process, and can be added into various daily life products needing to be antibacterial, such as antibacterial fabrics, antibacterial sponges and the like.

The invention is further explained below with reference to the drawings and the specific embodiments.

Drawings

FIG. 1 is a diagram of the macadamia shell antimicrobial composition of the present invention.

Figure 2 is a topographical view of the macadamia shell antimicrobial agent of the present invention. FIG. 2A is a transmission electron microscope image of the macadamia shell antimicrobial agent; b is the particle size distribution diagram of the macadamia shell antibacterial agent; c is a high resolution transmission electron microscope image of the macadamia shell antibacterial agent.

FIG. 3 is a graph showing the antimicrobial activity of the macadamia shell antimicrobial of the present invention against the gram negative bacteria E.coli. A in fig. 3 is blank; b is the preparation proportion of 1g/20ml (ultrasonic for 30min at room temperature, other conditions are unchanged); c is the preparation proportion of 1g/20ml (100 ml hydrothermal reaction kettle reacts for 20 hours, and other reaction conditions are unchanged); d is the preparation ratio of 5g/100ml (150 ml hydrothermal reaction kettle is used for reacting for 14 hours, and other reaction conditions are unchanged); e is the preparation ratio of 1g/20ml (ultrasonic 0min at room temperature, reaction at 180 ℃ for 24 hours, other reaction conditions are unchanged); f is the preparation ratio of 0.1g/20ml (hydrothermal reaction at 50 ℃ C. For 2 hours, other reaction conditions are unchanged).

FIG. 4 is a bar graph of the antibacterial rate of the macadamia shell antibacterial agent of the present invention against gram negative bacteria E.coli. FIG. 4B shows the preparation ratio of 1g/20ml (ultrasonic at room temperature for 30min, other conditions are unchanged); c is the preparation proportion of 1g/20ml (100 ml hydrothermal reaction kettle reacts for 20 hours, and other reaction conditions are unchanged); d is the preparation ratio of 5g/100ml (150 ml hydrothermal reaction kettle is used for reacting for 14 hours, and other reaction conditions are unchanged); e is the preparation ratio of 1g/20ml (ultrasonic 0min at room temperature, reaction at 180 ℃ for 24 hours, other reaction conditions are unchanged); f is the preparation ratio of 0.1g/20ml (hydrothermal reaction at 50 ℃ C. For 2 hours, other reaction conditions are unchanged).

FIG. 5 is a graph of an antimicrobial experiment of the macadamia shell antimicrobial of the present invention against the gram positive bacteria Staphylococcus aureus. In fig. 5a is blank; b is the preparation proportion of 1g/20ml (ultrasonic for 30min at room temperature, other conditions are unchanged); c is the preparation proportion of 1g/20ml (100 ml hydrothermal reaction kettle reacts for 20 hours, and other reaction conditions are unchanged); d is the preparation ratio of 5g/100ml (150 ml hydrothermal reaction kettle is used for reacting for 14 hours, and other reaction conditions are unchanged); e is the preparation ratio of 1g/20ml (ultrasonic 0min at room temperature, reaction at 180 ℃ for 24 hours, other reaction conditions are unchanged); f is the preparation ratio of 0.1g/20ml (hydrothermal reaction at 50 ℃ C. For 2 hours, other reaction conditions are unchanged).

FIG. 6 is a bar graph of the antimicrobial ratio of the macadamia shell antimicrobial of the present invention against the gram positive bacteria Staphylococcus aureus. FIG. 6B shows the preparation ratio of 1g/20ml (ultrasonic at room temperature for 30min, other conditions are unchanged); c is the preparation proportion of 1g/20ml (100 ml hydrothermal reaction kettle reacts for 20 hours, and other reaction conditions are unchanged); d is the preparation ratio of 5g/100ml (150 ml hydrothermal reaction kettle is used for reacting for 14 hours, and other reaction conditions are unchanged); e is the preparation ratio of 1g/20ml (ultrasonic 0min at room temperature, reaction at 180 ℃ for 24 hours, other reaction conditions are unchanged); f is the preparation ratio of 0.1g/20ml (hydrothermal reaction at 50 ℃ C. For 2 hours, other reaction conditions are unchanged).

FIG. 7 shows an experimental graph of different amounts of macadamia shell antimicrobial (preparation ratio of 1g/20 ml), 0.05g residue powder, 0.05g shell powder, 0.05g macadamia shell activated carbon (Ac), 0.05gCe doped activated carbon against gram-negative bacteria E.coli. ( The Australian nutshell activated carbon is prepared by taking Australian nutshell as a raw material and adopting a phosphoric acid activation method by the university of Yunnan national institute of chemistry and biotechnology Liu Xiaofang, wang Ruyang and the like, and the proper conditions for preparing the Australian nutshell activated carbon are that the phosphoric acid concentration is 50%, the soaking time is 20 and h and the activation temperature is 600 ℃. The specific method comprises the following steps: firstly, mashing macadimia nut shells, then carrying out carbonization, weighing 16g of the carbonized macadimia nut shells, placing the macadimia nut shells in a beaker, soaking the macadimia nut shells in phosphoric acid with the concentration of 50% for 20 hours, placing the macadimia nut shells in a porcelain crucible, placing the porcelain crucible in a muffle furnace for high-temperature calcination for 2 hours, cooling the porcelain crucible to room temperature, carrying out acid washing, washing the porcelain crucible with distilled water to be neutral, and placing the porcelain crucible in a baking oven for baking to obtain the macadimia nut shell activated carbon. )

In fig. 7 a is blank; b is 500 mu L; c is 450 mu L; d is 400 mu L; e is 350 mu L; f is 300 mu L; g is 250 mu L; h is 200 mu L; i is 150 mu L; j is 100 mu L; k is 50 mu L; l is residue powder; m is shell powder; n is Ac; o is Ac-Ce.

The residue powder is the residue powder which is filtered and treated after preparing the macadamia shell antibacterial agent solution, and is used for antibacterial test without antibacterial effect.

The shell powder is obtained by grinding hard shell of macadamia nut (also called hawaii fruit) from the Linum usitatissimum, and is used for antibacterial test without antibacterial effect.

Ac refers to Australian nut shell activated carbon obtained by calcining Australian nut shell powder and has little antibacterial effect when used for antibacterial test.

Ac-Ce refers to Australian nut shell activated carbon obtained by calcining Australian nut shell powder and the like, and is added with Ce to be doped with the activated carbon to obtain a composite antibacterial material, so that the composite antibacterial material has poor antibacterial effect when being used for antibacterial tests.

FIG. 8 is a bar graph of antibacterial activity against gram negative E.coli for varying amounts of macadamia shell antibacterial agent (preparation ratio 1g/20 ml), 0.05g residue powder, 0.05g shell powder, 0.05g macadamia shell activated carbon (Ac), 0.05gCe doped activated carbon. B in fig. 8 is 500 μl; c is 450 mu L; d is 400 mu L; e is 350 mu L; f is 300 mu L; g is 250 mu L; h is 200 mu L; i is 150 mu L; j is 100 mu L; k is 50 mu L; l is residue powder; m is shell powder; n is Ac; o is Ac-Ce.

FIG. 9 is a graph of antibacterial experiments against gram negative E.coli with varying amounts of macadamia shell antibacterial agent (preparation ratio 1g/20 ml). In fig. 9 a is blank; b is 40 mu L; c is 30 mu L; d is 20 mu L; e is 10 mu L.

FIG. 10 is a bar graph of antibacterial ratio of different amounts of macadamia shell antibacterial agent (preparation ratio 1g/20 ml) against gram negative E.coli. B in fig. 10 is 40 μl; c is 30 mu L; d is 20 mu L; e is 10 mu L.

Fig. 11 shows an experimental graph of antibacterial agents of macadamia shells prepared according to different raw material ratios against gram-negative bacteria such as escherichia coli (the antibacterial experimental dosage is 10 mu L). In fig. 11a is blank; b is 0.1g/20ml; c is 0.5g/100ml; d is 0.1g/60ml; e is 1g/100ml; f is 0.01g/60ml.

Fig. 12 is a bar graph of antibacterial ratio (10 μl of antibacterial experimental dose) of the macadamia shell antibacterial agent prepared with different raw material ratios against gram negative bacteria escherichia coli. FIG. 12B is 0.1g/20ml; c is 0.5g/100ml; d is 0.1g/60ml; e is 1g/100ml; f is 0.01g/60ml.

FIG. 13 shows an antimicrobial experimental graph of varying amounts of macadamia shell antimicrobial (preparation ratio 1g/20 ml) against the gram positive bacteria Staphylococcus aureus. A in fig. 13 is blank; b is 500 mu L; c is 400 mu L; d is 300 mu L; e is 200 mu L; f is 100 mu L; g is 40 mu L; h is 30 mu L; i is 20 mu L; j is 10 mu L.

FIG. 14 is a bar graph of antibacterial ratio of varying amounts of macadamia shell antibacterial agent (preparation ratio 1g/20 ml) against the gram positive bacteria Staphylococcus aureus. B in fig. 14 is 500 μl; c is 400 mu L; d is 300 mu L; e is 200 mu L; f is 100 mu L; g is 40 mu L; h is 30 mu L; i is 20 mu L; j is 10 mu L.

Fig. 15 shows an antimicrobial experimental diagram (the antimicrobial experimental dose is 10 μl) of the macadamia shell antimicrobial agent prepared with different raw material ratios against the gram positive bacteria staphylococcus aureus. A in fig. 15 is blank; b is 0.1g/20ml; c is 0.5g/100ml; d is 0.1g/60ml; e is 1g/100ml; f is 0.01g/60ml.

Fig. 16 is a bar graph of the antibacterial ratio of the macadamia shell antibacterial agent prepared with different raw material ratios to the gram positive bacteria staphylococcus aureus (the antibacterial experimental dose is 10 mul). FIG. 16B is 0.1g/20ml; c is 0.5g/100ml; d is 0.1g/60 ml; e is 1g/100ml; f is 0.01g/60ml.

Fig. 17 shows an experimental graph of the antibacterial effect of escherichia coli (the antibacterial experimental dose is 10 mu L) of the shell antibacterial agent prepared from different raw materials (the preparation ratio is 1g/20 ml). In fig. 17 a is blank; b is an macadamia shell antibacterial agent; c is a melon seed shell antibacterial agent; d is peanut shell antibacterial agent; e is an antibacterial agent of the almond shell.

Fig. 18 shows a graph of an antimicrobial experiment against staphylococcus aureus (antimicrobial experimental dose 10 μl) of a shell antimicrobial (preparation ratio 1g/20 ml) prepared from different raw materials. A in fig. 18 is blank; b is an macadamia shell antibacterial agent; c is a melon seed shell antibacterial agent; d is peanut shell antibacterial agent; e is an antibacterial agent of the almond shell.

Fig. 19 is a physical view of the sponge and fabric used to conduct the experiment. Fig. 19 a is a sponge; b is fabric.

FIG. 20 shows an experimental graph of the antibacterial effect of sponges and fabrics not treated with the macadamia shell antibacterial agent and sponges and fabrics treated with the macadamia shell antibacterial agent on gram negative bacteria E.coli. In fig. 20 a is blank; b is sponge which is not treated by the Australian nut shell antibacterial agent; c is sponge treated by Australian nut shell antibacterial agent; d is a fabric not treated with an australian nut shell antibacterial agent; e is a fabric treated with an antimicrobial agent of the macadamia nut shell.

Figure 21 shows a graph of antimicrobial activity against gram positive bacteria staphylococcus aureus for sponges and fabrics not treated with macadamia shell antimicrobial agent and sponges and fabrics treated with macadamia shell antimicrobial agent. A in fig. 21 is blank; b is sponge which is not treated by the Australian nut shell antibacterial agent; c is sponge treated by Australian nut shell antibacterial agent; d is a fabric not treated with an australian nut shell antibacterial agent; e is a fabric treated with an antimicrobial agent of the macadamia nut shell.

Fig. 22 shows a graph of a bacterial experiment in yunnan water culture and a graph of a bacterial experiment in yunnan water culture after treatment with an antimicrobial agent of macadamia nutshell. Fig. 22 a is the yunnan pond water; b is Dian pond water treated by Australian nut shell antibacterial agent.

Detailed Description

The following examples are only a part of the technical solutions of the present invention, but are not limiting to the whole technical solutions of the present invention, and the present examples are provided for further explanation and explanation of the technical solution details of the present invention. Example 1

The macadamia shell antibacterial agent prepared by the invention is shown in fig. 1, which is a physical diagram of the macadamia shell antibacterial agent, and is a light yellow clear transparent liquid solution, the pH is acidic, and the macadamia shell antibacterial agent contains carbon dots and possibly salicylic acid and other effective bactericidal components, so that when the antibacterial usage amount is 10 mu L, the antibacterial effect is obviously better than that of carbon dots prepared by other shells.

The morphology of the macadamia shell antimicrobial agent was studied using a Transmission Electron Microscope (TEM) (see figure 2). A transmission electron microscopy image of the macadamia shell antimicrobial (fig. 2A), a particle size distribution image of the macadamia shell antimicrobial (fig. 2B), and a high resolution transmission electron microscopy image of the macadamia shell antimicrobial (fig. 2C). In TEM image FIG. 2A, the macadamia shell antimicrobial agent exhibits regular spherical particles, which have a mean diameter of about 4.25 nm spheres shown in particle size distribution chart 2B, ranging from 1 to 9nm. High Resolution TEM (HRTEM) images showed that the macadamia shell antimicrobial had a good lattice spacing of 0.21 nm (fig. 2C), corresponding to the (100) plane of graphitic carbon.

Example two

A preparation method of an Australian nut shell antibacterial agent comprises the following steps:

1) 1.0g of macadamia shell brown powder was weighed out and dispersed in a small beaker with 20ml distilled water (solution A).

2) The solution A is stirred and dispersed, and then is put into an ultrasonic cleaner for ultrasonic treatment at room temperature for 10 min.

3) The solution A after ultrasonic treatment is transferred into a 50ml polytetrafluoroethylene lining high-pressure reaction kettle, and is subjected to hydrothermal reaction at 200 ℃ for 14 hours, and naturally cooled to room temperature.

4) The large particulate material was filtered through a 0.1 μm aqueous microporous filter and the product sample solution B, was the macadamia shell antimicrobial. The solution B was stored in a refrigerator at 4℃until use.

5) Antibacterial: coli and staphylococcus aureus are used as experimental bacteria, and a coating plate method is adopted to examine the antibacterial performance of the material.

Gram negative bacteria escherichia coli (e.coli, cctccc 204033) and gram positive bacteria staphylococcus aureus (s.aureus, ATCC 25723) were experimentally selected as experimental species for antibacterial detection.

Firstly preparing LB agar medium (tryptone 5g, yeast powder 2.5 g, sodium chloride 5g, distilled water 500mL, agar 7.5 g), and pouring into a plate for later use; LB liquid culture medium (tryptone 5g, yeast powder 2.5 g, sodium chloride 5g, distilled water 500 mL) was prepared again, the strain was added to a sterile liquid culture medium of appropriate content, and cultured to prepare a bacterial suspension, which was diluted to 5X 10 ⁶ CFU/mL with sterile water. The sample solution B and the diluted bacterial solution are mixed and placed in a sterile test tube to prepare a suspension. All test tubes are placed on a shaking table at 37 ℃ and 200rpm for incubation for 15min so that the effect is even, then the test tubes are taken out, 100 mu L of upper liquid is sucked and dropped into a culture dish, and a coating flat plate method is adopted to uniformly coat bacterial liquid on a culture medium. Placing the culture dish in a constant temperature incubator for culturing 18-24 h.

After culturing, the antibacterial rate of each sample was calculated by colony counting. The calculation formula is as follows:

within the above interval, as shown in fig. 3,4,5,6, for gram-negative bacteria escherichia coli (e.coli, cctccc 204033) and gram-positive bacteria staphylococcus aureus (s.aureus, ATCC 25723), B: the preparation ratio is 1g/20ml, but in the step S2, the ultrasonic treatment is carried out for 30min at room temperature, and other conditions are unchanged; c: the preparation ratio is 1g/20ml, but in the step S3, the reaction is carried out for 20 hours in a 100ml hydrothermal reaction kettle, and other reaction conditions are unchanged; d: the preparation ratio was 5g/100ml, but in step S3, the reaction was carried out in a 150ml hydrothermal reaction vessel for 14 hours, and the other reaction conditions were unchanged. B. C, D has very remarkable antibacterial effect.

E outside the above interval: preparing 1g/20ml of the solution, wherein the solution is subjected to ultrasonic treatment at room temperature for 0min in the step S2, and the solution is subjected to reaction at 180 ℃ for 24 hours in the step S3, and other reaction conditions are unchanged; f: the preparation ratio was 0.1g/20ml but the reaction was carried out in step S3 at 50℃for 2 hours under the same conditions as the other reaction conditions. E. F has quite unsatisfactory antibacterial effect.

Therefore, the macadamia shell antibacterial agent prepared in the range of the interval has excellent antibacterial effect.

A in fig. 3, 4: blank;

b: the preparation ratio is 1g/20ml (ultrasonic for 30min at room temperature, other conditions are unchanged);

c: preparation ratio 1g/20 ml (100 ml hydrothermal reaction kettle for 20 hours, other reaction conditions are unchanged);

d: the preparation ratio is 5g/100ml (150 ml hydrothermal reaction kettle reacts for 14 hours, and other reaction conditions are unchanged);

E: preparation ratio 1g/20ml (ultrasonic 0min at room temperature, reaction at 180 ℃ C. For 24 hours, other reaction conditions are unchanged); f: an E.coli antibacterial experiment chart and an antibacterial ratio bar chart with a ratio of 0.1g/20ml (hydrothermal reaction at 50 ℃ for 2 hours and other reaction conditions unchanged) were prepared.

Fig. 5,6 a: blank;

C: the preparation ratio is 1g/20ml (100 ml hydrothermal reaction kettle reacts for 20 hours, and other reaction conditions are unchanged);

e: preparation ratio 1g/20ml (ultrasonic 0min at room temperature, reaction at 180 ℃ C. For 24 hours, other reaction conditions are unchanged); f: an antibacterial experiment graph and an antibacterial ratio bar graph of staphylococcus aureus with a ratio of 0.1g/20ml (hydrothermal reaction at 50 ℃ for 2 hours and other reaction conditions unchanged) were prepared.

Example III

See fig. 7, 8, 9, 10. FIG. 7 shows an E.coli antimicrobial assay of different amounts of macadamia shell antimicrobial (preparation ratio 1g/20 ml), 0.05g residue powder, 0.05g shell powder, 0.05g macadamia shell activated carbon (Ac), 0.05gCe doped with activated carbon. FIG. 8 is a bar graph of E.coli antibacterial rates for different amounts of macadamia shell antibacterial agent (preparation ratio of 1g/20 ml), 0.05g residue powder, 0.05g shell powder, 0.05g macadamia shell activated carbon (Ac), 0.05gCe doped miscellaneous activated carbon. FIGS. 9 and 10 are graphs of E.coli antibacterial experiments and antibacterial rate bars for different amounts of macadamia shell antibacterial agent (preparation ratio 1g/20 ml).

Fig. 7,8 a: blank; b, 500 [ mu ] L; 450 mu L; d, 400 mu L; e, 350 mu L; f, 300 mu L; g, 250 [ mu ] L; h, 200 mu L; i, 150 [ mu ] L; j, 100 mu L; k is 50 mu L; l is residue powder; m is shell powder; ac; o is Ac-Ce.

The shell powder is obtained by drying hard shells of raw fruits of macadimia nuts (also called macadimia nuts) from the cloud of the cloud, grinding the shells into powder by a shell crusher, and using the powder for antibacterial test, wherein the powder has no antibacterial effect.

Fig. 9, 10 a: blank; b, 40 mu L; c, 30 mu L; d, 20 mu L; e, 10 mu L.

Along with the continuous reduction of the use amount of the Australian nut shell antibacterial agent in an escherichia coli antibacterial experiment, the antibacterial effect is still quite excellent compared with the use amount of 0.05g of high-dose shell powder and the use amount of 0.05g of high-dose residue powder. (the usage amount of the solid powder antibacterial agent in the antibacterial experiment is generally 0.005g at ordinary times) and the antibacterial effect of the solid powder antibacterial agent is quite remarkable even when the low-dose antibacterial agent of the macadamia shell is 10 mu L compared with 0.05g of activated carbon prepared from the macadamia shell. Although the antibacterial effect of the composite material is further improved after the activated carbon is doped with metal ions, the effect of the composite material is still not good as that of the macadamia shell antibacterial agent.

Example IV

See the escherichia coli antibacterial experiment graph (the antibacterial experiment dosage is 10 mu L) of the macadamia shell antibacterial agent prepared by different raw material ratios in the figure 11. Fig. 12 is a bar graph of the escherichia coli antibacterial rate (10 μl of antibacterial experimental dose) of the macadamia shell antibacterial agent prepared from different raw material ratios.

Meanwhile, compared with the Australian nut shell antibacterial agent with different raw material preparation ratios, the Australian nut shell antibacterial agent with different raw material preparation ratios in figures 11 and 12 has poor escherichia coli antibacterial effect, and the Australian nut shell antibacterial agent with the raw material preparation ratio of 1g/20ml is the best antibacterial effect when 10 mu L of antibacterial experiment is taken.

Fig. 11, 12 a: blank; b, 0.1g/20ml; c, 0.5g/100ml; d, 0.1g/60ml; e, 1g/100ml; f, 0.01g/60ml.

Example five

See FIG. 13 for a graph of Staphylococcus aureus antimicrobial experiments with varying amounts of macadamia shell antimicrobial (preparation ratio 1g/20 ml). FIG. 14 is a bar graph of the antibacterial rate of Staphylococcus aureus for different amounts of the macadamia shell antibacterial agent (preparation ratio 1g/20 ml).

As can be seen from fig. 13 and 14, the macadamia shell antibacterial agent has a better antibacterial effect against staphylococcus aureus. With the continuous reduction of the dosage, the antibacterial rate is still more than ninety percent.

Fig. 13, 14 a: blank; b, 500 [ mu ] L; c, 400 mu L; d, 300 mu L; e, 200 mu L; f, 100 mu L; g is 40 mu L; h, 30 mu L; i, 20 mu L; j, 10 mu L.

Example six

See fig. 15 for an antibacterial experiment graph of staphylococcus aureus of the macadamia shell antibacterial agent prepared by different raw material ratios (the antibacterial experiment dosage is 10 mu L). Fig. 16 is a bar graph of the antibacterial rate against staphylococcus aureus for macadamia shell antibacterial agents prepared at different raw material ratios (antibacterial experimental dose 10 μl).

As can be seen from fig. 15 and 16, when the antibacterial experiment using 10 μl of the antibacterial agent is used, the antibacterial effect of staphylococcus aureus of the macadamia shell antibacterial agent prepared by different raw materials in a ratio of 1g/20ml is not very good, and the antibacterial effect of the macadamia shell antibacterial agent prepared by the raw materials in a ratio of 1g/20ml is the best.

Fig. 15, 16 a: blank; b, 0.1g/20ml; c, 0.5g/100ml; d, 0.1g/60ml; e, 1g/100ml; f, 0.01g/60ml.

Example seven

See an escherichia coli antibacterial experiment chart (the antibacterial experiment dosage is 10 mu L) of the shell antibacterial agent (the preparation ratio is 1g/20 ml) prepared by different raw materials in the figure 17. Fig. 18 shows a graph of an antimicrobial experiment against staphylococcus aureus (antimicrobial experimental dose 10 μl) of a shell antimicrobial (preparation ratio 1g/20 ml) prepared from different raw materials.

As can be seen from fig. 17 and 18, when the antibacterial experiment using 10 μl was used, compared with the antibacterial agent of macadamia nutshell in fig. B, the antibacterial agent of different shell materials had poor antibacterial effects on escherichia coli and staphylococcus aureus, and the antibacterial rate of the antibacterial agent of melon seed shell, the antibacterial agent of peanut shell and the antibacterial agent of almond shell was almost zero, and no antibacterial effect was obtained. In contrast, the antimicrobial effect of the macadamia shell antimicrobial agent is best in a raw material preparation ratio of 1g/20 ml.

Fig. 17, 18 a: blank; b, an antimicrobial agent of macadamia shells; c, melon seed shell antibacterial agent; d, peanut shell antibacterial agent; e, an antibacterial agent with a badam shell.

Example eight

The macadamia shell antibacterial agent is added into products such as sponge and fabrics. As can be seen from figures 19, 20, 21, the sponge (panel B) and fabric (panel D) were compared to the blank (panel a) and the sponge without the macadamia shell antimicrobial treatment. The sponges (panel C) and fabrics (panel E) treated with the macadamia shell antimicrobial had a remarkable antimicrobial effect against both E.coli and Staphylococcus aureus.

Example nine

The macadamia shell antibacterial agent is applied to sewage antibacterial treatment. The Yunnan pond water is used for culturing bacteria, and as shown in figure 22A, various bacteria including mould and other miscellaneous bacteria can be seen to grow. After the treatment with the macadamia shell antibacterial agent, the bacterial colony count in the graph B is significantly reduced, indicating that the macadamia shell antibacterial agent can effectively kill various bacteria in a realistic sewage environment.

Fig. 22 a: water of Yunnan pond; b: dian pond water containing Australian nut shell antibacterial agent is provided.

The foregoing description is only a few specific embodiments of the present application (the embodiments are not intended to be exhaustive, and the scope of the application includes the scope of the application and other technical points), and the details or common sense of the present application are not described in any more detail herein (including but not limited to the shorthand, abbreviations, units commonly used in the art). It should be noted that the above embodiments do not limit the present application in any way, and it is within the scope of the present application for those skilled in the art to obtain the technical solution by equivalent substitution or equivalent transformation. The protection scope of the present application is subject to the content of the claims, and the description of the specific embodiments and the like in the specification can be used for explaining the content of the claims.

Claims

1. A method for preparing an antimicrobial agent from macadamia shells, comprising the steps of:

Step 1) selecting macadamia shells as raw materials;

step 3), placing the solution A in a reaction kettle for heating reaction;

2. The method of preparing an antimicrobial agent for macadamia shells according to claim 1, wherein step 2) of the preparation method comprises pulverizing the macadamia shells, and dispersing the pulverized powder in a container filled with distilled water to form a solution a; the material ratio of the crushed powder of the macadamia shell to distilled water is 0.1-10g:10-100 ml.

3. The method of preparing an antimicrobial agent for macadamia shells according to claim 2, wherein in the step 2), the ratio of the pulverized powder of the macadamia shells to distilled water is 1 g:20 ml.

4. The method for preparing the macadamia shell antibacterial agent according to claim 1, wherein in the step 3) of the preparation method, the reaction in the reaction kettle is as follows: carrying out hydrothermal reaction for 5-24 hours at 100-400 ℃, and then naturally cooling to room temperature.

5. The method for preparing the macadamia shell antibacterial agent according to claim 4, wherein in the step 3 of the preparation method, the reaction in the reaction kettle is as follows: the hydrothermal reaction is carried out at 200 ℃ for 14 hours, and the mixture is naturally cooled to room temperature.

6. The preparation method of the macadamia shell antibacterial agent according to claim 1, wherein an ultrasonic link is arranged between the step 2) and the step 3), and the ultrasonic link is that the solution A is stirred and dispersed and then put into an ultrasonic cleaner to be subjected to ultrasonic treatment at room temperature.

7. The method of preparing an antimicrobial agent for macadamia shells according to claim 1, wherein the filtration in step 4) of the preparation method is performed by a water-based microporous filter membrane of 0.1-0.5 μm.

8. The method of claim 7, wherein the filtration in step 4) is performed by a 0.1 μm aqueous microporous filter.

9. An antibacterial agent obtainable by the process of preparation of an antibacterial agent according to any one of claims 1 to 8.

10. The use of the antibacterial agent according to claim 9 as a bactericide additive or a sewage treatment agent.