CN1322474A - Aggregation-preventing nanometer wide-spectrum antibacterial silve powder and its inductrial production process - Google Patents

Aggregation-preventing nanometer wide-spectrum antibacterial silve powder and its inductrial production process Download PDF

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CN1322474A
CN1322474A CN01110767A CN01110767A CN1322474A CN 1322474 A CN1322474 A CN 1322474A CN 01110767 A CN01110767 A CN 01110767A CN 01110767 A CN01110767 A CN 01110767A CN 1322474 A CN1322474 A CN 1322474A
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silver
aggregation
nano
spectrum antibacterial
broad
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CN1179646C (en
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朱红军
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Shenzhen Yuanxing Nano-Pharmaceutical Co., Ltd.
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朱红军
朱骊
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Priority to CNB011107677A priority Critical patent/CN1179646C/en
Priority to CN01223000U priority patent/CN2479952Y/en
Priority to CN01129505A priority patent/CN1328819A/en
Priority to CNB011295074A priority patent/CN1169529C/en
Publication of CN1322474A publication Critical patent/CN1322474A/en
Priority to CNB018231578A priority patent/CN1224479C/en
Priority to PCT/CN2001/001584 priority patent/WO2002090025A1/en
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
    • A61L2/16—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using chemical substances
    • A61L2/23—Solid substances, e.g. granules, powders, blocks, tablets
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
    • A61L2/16—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using chemical substances
    • A61L2/23—Solid substances, e.g. granules, powders, blocks, tablets
    • A61L2/238—Metals or alloys, e.g. oligodynamic metals
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P13/00—Drugs for disorders of the urinary system
    • A61P13/08—Drugs for disorders of the urinary system of the prostate
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P15/00—Drugs for genital or sexual disorders; Contraceptives
    • A61P15/02—Drugs for genital or sexual disorders; Contraceptives for disorders of the vagina
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
    • A61P31/04—Antibacterial agents
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P9/00—Drugs for disorders of the cardiovascular system
    • A61P9/14—Vasoprotectives; Antihaemorrhoidals; Drugs for varicose therapy; Capillary stabilisers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites

Abstract

Between fiber elements and on fiber of natural porous plant material, superfine silver particles of 1-100 nm size with a silver oxide surface layer are attached firmly. The method of the present invention can prevent aggregation of superfine silver particles with extremely strong activity. Nanometer silver powder has extremely antiseptic capacity; wide antibacterial spectrum; high bactericidal effect, especially while contacting with water; no toxicity; no irrigation, no pathergy and drug resistance and may also be used as medicinal material.

Description

Aggregation-preventing broad-spectrum antibacterial nano-silver micro-powder and industrialized production process thereof
The invention relates to a broad-spectrum antibacterial nano-silver material and an industrialized manufacturing process, in particular to anti-aggregation broad-spectrum antibacterial nano-silver micro-powder and an industrialized manufacturing process.
As is known, nanotechnology is a new subject of research and study on substances with particle sizes of1-100 nanometers, is one of three major technologies in economic development in the 21 st century, and is also a new technology which is most likely to generate breakthrough achievement. The countries in the world compete for huge investment, and the technology integrates the elegance of developing the nanotechnology and the application thereof, and the research institutions from the upper central level to the lower level to the colleges and universities and grass-roots in China have great investment in the development trend of the nanotechnology, and especially the application and industrialization of the nanotechnology are the important factors for the research and development in China.
Many examples of silver antibacterial are disclosed in the prior art, for example, in Japanese patent No. Sho 54-151669, a bactericidal cloth is disclosed, which is obtained by treating a yarn with a resin solution containing a compound of copper and silver (average particle diameter of 6 μm) alone or in combination, uniformly coating the solution on the surface of the yarn, and weaving the yarn into a bactericidal cloth, which can be used as a lining of rubber boots, canvas shoes and socks.
In the report of "processing technology" vol.17 No.7 in Japan, the acrylic fiber is treated with copper and sulfide to obtain an acrylic fiber-copper sulfide composite, which has bacteriostatic ability on staphylococcus aureus, escherichia coli, bacillus subtilis and dermatophytes.
In Chinese invention patent CN-87100231A, entitled "antibacterial deodorant fiber yarn and manufacturing method", the disclosure date is: 18.11.1987, an antibacterial yarn is disclosed, which is prepared by carrying out composite crosslinking on acrylic yarn with copper and alkaline green-4 in sequence, and the product has antibacterial function on 10 strains such as staphylococcus aureus, MRSA, staphylococcus albus, candida albicans and the like, and can be used as antibacterial and deodorant underwear, socks, insoles and work clothes in the medical industry and the food industry.
An antibacterial cloth for preventing mastitis in a cow is disclosed in Japanese patent laid-open No. Hei 3-136649, application date "24/10 in 1989. The silver ion and polyacrylonitrile are compounded in a coordination bond form, the product has an inhibiting effect on 6 strains such as streptococcus, staphylococcus and the like, and can be used as an antibacterial wiper for wiping the mammilla of a cow to prevent mastitis of the cow.
However, none of the above documents or reports relate to the use of nano silver and a suitable carrier as an antibacterial material.
The above products all have antibacterial effects, but the antibacterial spectrum is not wide, the effects are not obvious, and the products are completely different from the invention.
The invention aims to provide broad-spectrum antibacterial nano-silver micro-powder and an industrialized manufacturing process thereof.
Another object of the present invention is to provide a process for preventing aggregation between ultrafine silver particles having a very high activity.
The invention also aims to provide an industrialized production process of the anti-aggregation broad-spectrum antibacterial nano-silver micro-powder.
These and other objects of the present invention will be further elucidated by the following detailed description and description.
In the invention, the aggregation-preventing broad-spectrum antibacterial nano-silver micro-powder is characterized in that ultrafine silver particles with the particle size of 1-100 nanometers are firmly attached among fiber elements and on fibers of a natural porous plant material, the surface layer of the ultrafine silver particles is silver oxide with the particle size of 2-8 nanometers, and the core of the ultrafine silver particles is elemental silver; the silver content of the nano silver attached between the fiber elements and on the fibers of the natural porous plant material is 0.1-200 mg/g; the natural porous plant material is fiber pulp of rush, cotton, wool, hemp, silk, bamboo and wood, stems of reed flowers and loofah sponge plants, activated carbon, chemical fiber, non-woven fabric, foamed plastic and the like.
The industrialized production process of the aggregation-preventing broad-spectrum antibacterial nano-silver micro-powder comprises the steps of vacuum pretreatment of a carrier material, preparation of a medicament, impregnation, pressurization homogenization, chemical and physical reaction, cleaning, drying and crushing.
Further, in the industrial production process of the aggregation-preventing broad-spectrum antibacterial nano-silver micro-powder, the vacuum pretreatment comprises the steps of immersing natural porous plant materials (particularly rush materials) in 1-20% (V/V) of medical alcohol (75-98%), and then extracting the solid natural porous plant materials without organic components in vacuum.
In the industrialized production process of the aggregation-preventing broad-spectrum antibacterial nano-silver micro-powder, the preparation formula of the medicament is as follows (calculated by 10 kilograms of carriers after extraction):
A. 0.01-1M silver nitrate, 0.05-0.5M ammonia water, 0.01-0.3M sodium hydroxide
Adding water to the mixture until the total volume is 500 liters;
B. 1-8M of glucose or ascorbic acid, 0.02-0.2M of nitric acid, 2-10M of ethanol,
adding water to the mixture until the total volume is 500 liters;
mixing 10 parts by volume of A and 1 part by volume of B uniformly, standing for 10-40 minutes, soaking the medicament into a carrier, pressurizing and homogenizing to be uniform, putting the mixture into a reaction kettle, and adding a dispersing agent to react until the product is brownish yellow.
In the anti-aggregation broad-spectrum antibacterial nano-silver micro-powder, the prepared nano-silver micro-powder is added with proper pharmaceutical auxiliary agents or excipients to prepare powder, tablets, paste, cream, film, gel, patches, injection, aqua, spray and biological medicine chips; the prepared silver powder can be used as a sterilization material for various purposes in the fields of field, battlefield, disaster area and spaceflight, and is used for killing pathogenic bacteria in bacteria-containing water.
In the present invention, if necessary, some conventional treatment methods in the industry may be added, and it is of course possible to omit one or more steps as the case may be, including combining conventional knowledge in the art, as long as the product is prepared.
The product of the invention can be used as a medical (external) material for treating burns and scalds, a material for treating skin infection of trauma patients, superficial skin fungal infection and incision infection prevention and treatment after surgical incision operation, can also be used as a daily product, has broad-spectrum antibacterial property, long-acting property, and can kill drug-resistant pathogenic bacteria, and has excellent performances of stronger hydrophilic-water sterilizing power, no toxicity, no irritation, no allergy, no drug resistance and the like. Can be used for treating skin infection and dermatophyte infection of trauma patients and surgical incision infection. Especially for the field prevention and treatment of trauma infection under adverse environmental conditions such as field operation, war wound of sea water polluted wound, flood, fire, earthquake, etc. More importantly, the product of the invention can be used for treating intractable bedsore infection, burn and scald wound infection, intractable ulcer of lower limbs after diabetes, bacterial, mycotic and mixed infection vaginitis of women, prostatitis of men and other difficult and complicated infections, and opens an industrial paradigm of applying nanotechnology in the field of human body infection resistance.
The technology of the present invention can prevent the aggregation of newly generated silver ultrafine particles with nanometer particle size and strong surface activity, thereby preventing the generation of silver particles with larger particle size. The production is successful after the laboratory production and pilot plant test, the production operation and the product quality are stable, and the annual output value is estimated to reach more than 10 hundred million yuan.
The invention will be further described by means of the figures and flow charts.
FIG. 1 is a photograph of a silver sample not using this technique observed under a microscope.
FIG. 2 is a photograph of a silver sample not using this technique observed under a microscope.
FIG. 3 is a photograph of a silver sample not using this technique observed under a microscope.
FIG. 4 is a photograph showing the microscopic observation of a silver sample using the technique of the present invention
FIG. 5 is a process flow diagram of the present invention.
The invention relates to an anti-aggregation broad-spectrum antibacterial nano silver micro powder (hereinafter referred to as PNSM) belonging to an organic-inorganic nano composite material in which inorganic nano particles are dispersed on a natural organic matrix in the nano material science. The carrier of the PNSM is selected from a plurality of materials which are mastered by people and can be used as the carrierIn (1), rush was taken as the carrier of pnsm. The organic carrier is rush, the inorganic nano is ultrafine silver with the grain diameter of 1-100 nanometers, and the silver can be used as a functional material and particularly applied to the field of human body infection resistance. As for the definition of the nano material, besides the particle size of 1-100 nm, the nano material also needs to have specific performance which is far superior to that of the homogeneous material with macroscopic size in certain important performance. That is, if the particle size is 1-100 nm and the specific property is required, the particle size is not limited to be 1-100 nm, otherwise the particle size cannot be defined as a nano material. The ultrafine nanoparticles having a particle size of 1 to 100 nm have a very large specific surface area and are inversely proportional to the particle size, as compared with homogeneous macro-particles. For example: 1 g of copper with a particle size of 5 nm and a specific surface of 130 m2Per gram; the particle diameter is 2 nanometers, and the specific surface area is 330 meters2Per gram; at the same time, the surface effect is added, namely the volume percentage distributed on the particle surface is 50% when the particle diameter is 5 nm, and the volume percentage on the surface is 80% when the particle diameter is 2 nm, at this time, the reduction of the particle diameter leads the atom number on the surface layer to be rapidly increased, thus leading to insufficient original coordination, increasing the exposure of unsaturated bonds and increasing the surface energy of atoms, thus leading to the chemical activity of the nano-scale ultrafine particlesThe property is very strong, therefore, when the superfine particles are just generated, the mutual collision inevitably occurs, and two or even a plurality of the collided superfine particles are aggregated, thereby generating large particles with larger particle size which is larger than the original particle size N, No and Noo times, and even becoming particles with macroscopic size due to the aggregation, the corresponding chemical activity is greatly reduced, and finally the property of the nano material is lost. It is understood that the present invention achieves the effect of preventing the aggregation of newly formed ultrafine particles by appropriate chemical and physical means. The aggregation prevention technology is important for the success of a method for manufacturing 1-100 nm ultrafine particles mainly by a chemical method and secondarily by a physical method. To confirm the effect of the anti-agglomeration technique, we examined silver samples with and without the technique by electron microscopy and photographed the images, and the effect is evident, please refer to fig. 1, fig. 2, fig. 3 and fig. 4.
In FIGS. 1 to 3, the deposition of spherical particles in the image is much larger than the size of the spherical particles because of the absence of the agglomeration preventing technique of the present invention.
FIG. 4 is an electron micrograph of PNSM using anti-agglomeration technique, clearly showing that the majority of the nanoparticles on PNSM have a particle size of 5-40 nm and are distributed uniformly and regularly, and a stripe-like ridge is formed in the middle of the photograph, but it can be clearly seen that it is not a spherical nanoparticle pile, and it may be a minute ridge on the surface of cilia in the carrier. In addition, in order to determine the composition of the ultrafine particles on the PNSM,the surface layer of the spherical ultrafine particles is silver oxide with the thickness of 2-8 nanometers, the core of the spherical ultrafine particles is element silver, and the silver content of the nano silver on the PNSM is determined to be 0.1-200 mg/g by a method of United states pharmacopoeia and British pharmacopoeia.
The functions and detection tests of the PNSM provided by the invention are as follows:
the PNSM of the invention is determined by an electron microscope and a photoelectron spectrometer, and most of the silver particles of the PNSM can be seen to be ultrafine particles with the particle size of 5-40 nanometers, and the composition of the ultrafine particles is Ag2O + Ag, the surface layer of the particles is Ag2O, whose core is elemental silver and can be clearly defined as sodiumThe silver particles having a particle diameter of a meter order were confirmed to have excellent specific properties by the following tests, and the test results are shown in tables 1 and 2.
Table 1 shows the results of the microbiological laboratory tests conducted by the general medicine test center of the people's liberation force of China.
Table 2 is a test conducted in the bacterial laboratory of Huashan Hospital, Shanghai medical university.
The antibacterial mechanism of the PNSM is a classical antibacterial mechanism:
as can be seen from the above, PNSM is the most classical antibacterial mechanism in which-SH groups in enzymes living in cells are replaced with-SAg to inactivate the enzymes and cause the death of germs, and its products are enzymes 2SAg and H2And O, no secondary pathogenic factor exists.
From the experimental results shown in tables 1 and 2, it can be seen that the PNSM of the present invention has the following excellent specific functions.
1. Broad spectrum of antibacterial:
the strains shown in tables 1 and 2 include gram-positive bacteria, gram-negative bacteria, fungi, spores and anaerobic bacteria, and the broad antimicrobial spectrum is very rare in the existing antimicrobial drugs. The number of strains counted in the strain removal repeat referred to in tables 1 and 2 was 38, and most of the strains were isolated from the secretions of the drug-resistant clinical patients.
2. Long-lasting property:
table 1, 50 and 20 washes as shown in table 2 are 50 and 20 rinses of PNSM with clean water for each hand scrub of soap. The 100 times of washing is 100 times of scrubbing with clean water each time, and the antibacterial performance of the washed PNSM is not obviously reduced.
3. Comparison of bacteriostatic effects of PNSM and 8 antibacterial agents on pathogenic bacteria:
table 1 shows that 8 antibacterial drugs of PNSM (28), cefuroxime (4), ceftazidime (15), oxacillin (2), gentamicin (6) and ciprofloxacin (14) were subjected to in vitro bacteriostasis tests simultaneously. The number in parentheses after the name of each drug is the number of bacteria that the drug is able to inhibit. It can be seen that PNSM is much superior in resistance to drug-resistant pathogenic bacteria than the 8 antibacterial agents. This may be desirable to break the current growth in bacterial resistance, which has made the development of antibiotics unable to keep up with the embarrassing situation of bacterial resistance growth. It is anticipated from the above that the PNSM of the presentinvention will likely become an alternative drug to antibiotics.
4. Has stronger hydrophilic-water sterilizing power
From tables 1 and 2, it can be seen that the bacteriostatic ability of PNSM has no obvious decline after multiple rubbing, and the main mechanism is Ag on PNSM2O has slow release property, and the water content is enough to make Ag under the condition of water existence, even the humidity of human body surface or the moisture state when in application+When [ Ag]is released+]Up to 0, n-5ppm 10-6]Can reach Ag+Dynamic equilibrium of (1), and Ag+Has a minimum inhibitory concentration of 2 × 10-11M, the antibacterial mechanism and the absence of secondary pathogenic factors during the antibacterial process for pnsm have been elucidated in the section "antibacterial mechanism" above. In addition, the following test is also carried out, 0.5 g of PNSM coarse powder is soaked in 500 ml of water every day, the water is changed once every day, and the bacteriostatic ability of the PNSM coarse powder is not obviously reduced after 45 days. Therefore, the external medicine prepared by using PNSM as the raw material medicine has stronger antibacterial power when meeting water. This is very advantageous for current burn and scald moistening therapy. The clinical verification of the Nanjing general Hospital of the Chinese people's liberation army shows that the PNSM has good curative effect, and the fourth military medical university of the Chinese people's liberation army and the subsidiary Cijing Hospital thereof are used for on-site treatment of war wounds polluted by seawater.
5. Pharmacokinetic Studies
Through the national Beijing New drug safety evaluation research center and the general Hospital pharmacology department of the Nanjing military region, mice, guinea pigs and white big-ear rabbits are used as test objects. PNSM is used as an experimental medicine and is subjected to skin acute toxicity test, irritation test, allergy test and mouse acute toxicity test, maximum tolerance amount determination test and accumulative toxicity test, particularly, the PNSM amount is 925 mg/kg of the maximum tolerance amount after single gastric lavage administration of mice (9 mice) and is equivalent to 4625 times of the clinical dose of human beings, and after administration, 14 days of continuous observation are carried out, toxic symptoms and death are not found, and the growth condition is better. Thus, it was confirmed that PNSM was non-toxic, non-irritant, non-allergic, and non-drug resistant.
6. Comparison of PNSM with in vitro bacteriostasis of silver particles of homogeneous macroscopic particle size
Small circles with the diameter of 6 mm are respectively placed with PNSM and silver micro powder with the grain diameter of micron, the silver content of the PNSM is only 10 of the silver content of the silver micro powder-3-10-4. Agar MH Ping, which is bacteriostatic in vitro, howeverOn the plate, the former has an antibacterial ring of 12-20 mm, and the latter has no antibacterial ring. It can be seen that macroscopically sized, homogenous silver particles are not comparable to PNSM in terms of bacteriostatic ability.
In conclusion, the functions of the PNSM provided by the invention include broad-spectrum antibacterial property, long-acting property, stronger antibacterial ability to pathogenic bacteria with drug resistance, stronger hydrophilicity-water sterilizing ability, no toxicity (including no accumulated toxicity), no irritation, no allergy, no drug resistance and the like, which are far superior to the current commonly used antibacterial drugs and are also far superior to the homogeneous silver micro powder with macroscopic size, so that the silver particles on the PNSM provided by the invention not only meet the requirement of the particle size of 1-100 nanometers, but also show special superior antibacterial performance. The silver particles on the PNSM of the present invention can be defined without any problem as nano silver.
The essence of PNSM is that the anti-aggregation technology of the present invention is adopted to produce silver (Ag) with ultrafine particles of 1-100 nm in diameter uniformly and firmly adhered to natural light and porous rush2O + Ag) particles. And finally crushing into micron-sized micro powder to obtain the PNSM.
The manufacturing process of the invention comprises the following steps: selecting carrier raw materials, adding the preparation agent 1 in vacuum pretreatment, carrying out vacuum extraction and impregnation, adding the preparation agent 2 and the preparation agent 3 while carrying out impregnation, pressurizing and homogenizing, carrying out chemical and physical reaction, adding the dispersing agent in the chemical and physical reaction, and then carrying out cleaning, drying, crushing and refining to obtain a finished product.
In the present invention, all the raw materials, adjuvants and additives are commercially available, the dispersant is a general anti-agglomeration agent in the industry, and the specific species can be found in handbooks, for example, isopropyl alcohol, sodium dodecylbenzene sulfonate, sodium sulfosuccinate sulfonate, colloidal palladium or colloidal palladium, OP-10, trialkyl phosphates such as tributyl phosphate, trioctyl phosphate, triisopentyl phosphate, triisooctyl thiophosphate, etc. can be used, or refer to the statement on page 49-57 of silicate report on 2 in 1986, Shen 'preparation of fine ceramic fine powder'.
The present invention is further illustrated by the following specific examples, which are intended to be illustrative only and not to limit the scope of the invention.
In the present invention, unless otherwise specified, all parts and amounts are by weight based on total weight and "M" is the molar concentration.
Example 1
The following liquid medicines (calculated according to 10 kg carrier)
A、AgNO30.5M,NH3·H2O 0.3M,NaOH 0.1M,
Adding water to the mixture until the total volume is 500 liters;
B. glucose 4M, HNO30.1M, boiling for 1-5 minutes, cooling, and adding ethanol to obtain 10M solution with a volume of 50 liters.
Cleaning carrier (medulla Junci), adding 98% medical alcohol and distilled water (ratio of 1: 15), immersing carrier, and vacuum extracting until the carrier is free of organic components and impurities.
Mixing 10 parts of B (V/V) and 1 part of B (V/V) uniformly, standing for 10-40 minutes for impregnation, and adding 10 kilograms of treated carrier (rush). After dipping, pressurizing and homogenizing to evenly mix the liquid medicine and the carrier, continuously adding a dispersing agent-OP-10 (under ventilation condition and proper stirring condition) in the chemical and physical treatment of the mixture in a reaction kettle until the rush is brownish yellow, and then cleaning, drying and crushing the mixture to obtain the aggregation-preventing broad-spectrum antibacterial nano silver micro powder.
Example 2
The following liquid medicines (calculated according to 10 kg carrier)
A、AgNO30.3M,NH3·H2O 0.2M,NaOH 0.07M，
Adding water to the mixture until the total volume is 500 liters;
B. ascorbic acid 3M, HNO30.1M, boiling for 1-5 minutes, cooling, and adding ethanol to obtain 10M solution with a volume of 50 liters.
Cleaning carrier (medulla Junci), adding 75% medical alcohol and distilled water (ratio of 1: 10), soaking the carrier, and vacuum extracting until the carrier is free of organic components and impurities.
Mixing 10 parts of B (V/V) and 1 part of B (V/V) uniformly, standing for 10-40 minutes for impregnation, and adding 10 kilograms of treated carrier (rush). After dipping, pressurizing and homogenizing to mix the liquid medicine and the carrier evenly, putting the mixture into a reaction kettle for chemical and physical treatment, adding sodium dodecyl benzene sulfonate as a dispersing agent (under the conditions of ventilation and proper stirring) until the rush is brownish yellow, and then cleaning, drying and crushing the mixture to obtain the aggregation-preventing broad-spectrum antibacterial nano silver micro powder.
The aggregation-preventing broad-spectrum antibacterial nano-silver micro-powder is mainly used for developing medical products, and can be used for external antibacterial drugs to develop into internal antibacterial drugs after clinical verification, thereby partially replacing antibiotics. Meanwhile, the textile fabric can also relate to other industries, such as bedding, shoes, socks and clothes in the textile industry; can be used as antibacterial detergent, antibacterial shampoo, toothpaste, cosmetics and acne-treating facial mask in daily chemical industry; the paper can be used as paper for printing money, paper tableware, books, documents and paper in the paper industry; can be used as a sterilizing, antiseptic and preservative agent for fruits and vegetables in the food industry; can be used as mildew-proof antibacterial coating in the building material industry, etc.; can be used as water disinfectant, antibacterial towel and disinfectant for food service industry in tourism industry; can be used as antibacterial material in antibacterial sanitary towel, antibacterial baby diaper, air conditioner, and air freshener in health promotion industry.TABLE 1 inhibition results of PNSM and 8 antibacterial agents
Source of bacterial name PNSM and control bacteriostatic diameter (mm) Result of drug sensitivity of antibacterial drug canthus C method
Final washing Washing machine 50 times Washing machine 100 times (twice) Negative of Control Erythromycin Benzoxazole Penicillin Fluorobenzyl Penicillin Cephalosporin Azoline Cephalosporin Furoxime Cephalosporin Tadin derivatives Qingda (celebration) Mycin Cyclopropan Floxacin hydrate
Staphylococcus aureus ATCC25923 Escherichia coli ATCC25922 Pseudomonas aeruginosa ATCC27853 Clostridium perfringens CMCC (B)64606 Staphylococcus Aureus (MRSA) secretion Staphylococcus Epidermidis (MRSE) secretion Secretion of streptococcus pyogenes Neisseria gonorrhoeae secretion Secretion of Escherichia coli Secretion of enterobacter cloacae Enterobacter aerogenesSecretion material Secretion of pseudomonas aeruginosa Secretion of stenotrophomonas maltophilia Acinetobacter baumannii secretion Klebsiella pneumoniae secretion Serratia marcescens secretion Secretion of Citrobacter freudenreichii Secretion of Rauverdenum Repentium Hydrophilic aeromonas secretion Aeromonas sobria secretion Vibrio vulnificus secretion Proteus mirabilis secretion Secretion of Proteus vulgaris Proteus pennisatus secretion Candida albicans secretion Candida tropicalis secretion Candida parapsilosis secretion Glomus saccharomycete secretion 18 13 12 10 17 18 9 10 17 9 14 15 14 13 15 16 11 15 13 14 17 11 11 10 21 18 20 27 15 13 12 15 15 8 10 14 8 12 15 13 12 14 13 10 13 11 12 15 10 9 9 20 17 19 26 5 12 12 15 16 8 10 14 8 13 15 14 12 14 14 11 13 13 12 15 10 11 10 20 18 20 26 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 24 10 6 6 6 6 31 6 11 6 6 6 19 6 6 6 6 16 17 6 9 6 6 6 6 6 6 S R R S S S R R S S R R R R R R R R R R R R R R R R S S R R S S R R R R R R R R R R R I R R R R S S R R S S R R R R R R R R R R R I R R R I S S S R R S S R R R R S S S R R S S S S S S S S S S R R S S R R R R R S R R R R R R I R R R S S S R R S S R R R R S S S S R S S S S R R S
Note: s: sensitivity I: an intermediate R: drug resistanceTABLE 2
Strain blank AB fabric PNSM
20 times of no-washing of fabrics, 20 times of high-pressure no-washing and 20 times of high-pressure no-washing of 50 times of pseudomonas aeruginosa, 15131616 staphylococcus aureus, 15171515 escherichia coli, 13141815 MRSA, 14141715 bacillus cereus, 1113131515 vibrio vulnificus, 16161617 candida albicans, 21 11111111B group hemolytic streptococcus, 11111211 pseudomonas maltophilia, 12121514 nitrate negative bacillus, 14141315 salmonella paratyphi, 12, 12141914 salmonella alimentarius, 14141514 citrobacter, 14141513 pneumobacillus, 13131713 bacillus subtilis, 12121212 rhizogenes, 1012121212 alcaligenes faecalis, 14121616 pseudomonas stutzeri 12121413 Enterobacter cloacae-13131313 gonococcus-11111111
The results show that PNSM has inhibition effect on 20 strains of bacteria, and on bacteria which are easy to generate drug resistance, such as staphylococcus aureus drug-resistant strains (MRSA), pseudomonas aeruginosa, pseudomonas maltophilia, nitrate negative bacillus and the like, the inhibition effect on the bacteria is not obviously affected after high pressure and washing for 20 times and 50 times, and the bacteria cannot be inhibited after the AB fabric is washed for 20 times, so that the inhibition range of PNSM is wider than that of the AB fabric, and the inhibition effect cannot be affected by washing.

Claims (11)

1. An aggregation-preventing broad-spectrum antibacterial nano-silver micropowder is characterized in that ultrafine silver particles with the particle size of 1-100 nm are firmly attached among and on fiber elements of a natural porous plant material, the surface layer of the ultrafine silver particles is silver oxide with the particle size of 2-8 nm, and the core of the ultrafine silver particles is elemental silver.
2. The aggregation-preventing broad-spectrum antibacterial nano-silver micropowder as claimed in claim 1, wherein the silver content of nano-silver attached to the inter-fiberelements and the fibers of the natural porous plant material is 0.1 to 200 mg/g.
3. The aggregation-preventing broad-spectrum antibacterial nano-silver micropowder as claimed in claim 1, wherein the natural porous plant material is fiber pulp of rush, cotton, wool, hemp, silk, bamboo and wood, stem of reed flower and loofah sponge plant, activated carbon and chemical fiber, non-woven fabric, foam plastic.
4. The industrial process for producing an aggregation-preventing broad-spectrum antibacterial silver nanoparticle as claimed in claim 1 to 3, wherein a method for preventing aggregation between silver ultrafine particles having a very strong activity is employed.
5. The industrial process for preparing the anti-aggregation broad-spectrum antibacterial nano-silver micro-powder as claimed in claim 4, which comprises the steps of vacuum pretreatment of carrier materials, preparation of medicament, impregnation, pressurizing homogenization, chemical and physical reaction, cleaning, drying and crushing.
6. The industrial process for preparing the aggregation-preventing broad-spectrum antibacterial nano-silver micro-powder as claimed in claim 4, wherein the vacuum pretreatment comprises immersing the natural porous plant material with 1-20% (V/V) medical alcohol, and then extracting the solid natural porous plant material without organic components in vacuum.
7. The industrial process for preparing nano silver micro powder with broad spectrum and antibacterial effect for preventing aggregation as claimed in claim 4, wherein the vacuum pretreatment comprises immersing the rush material in 1-20% (V/V) medical alcohol, andvacuum extracting to obtain rush material without organic component.
8. The industrial production process of the aggregation-preventing broad-spectrum antibacterial nano-silver micro-powder according to claims 1 to 7, characterized in that the formulation of the medicament is (based on 10 kg of the extracted carrier):
A. 0.01-1M of silver nitrate, 0.05-0.5M of ammonia water and 0.01-0.3M of sodium hydroxide are added with water until the total volume is 500 liters;
B. 1-8M of glucose or ascorbic acid, 0.02-0.2M of nitric acid and 2-10M of ethanol, and adding water until the total volume is 500 liters;
and (3) uniformly mixing 10 parts by volume of A and 1 part by volume of B, and standing for 10-40 minutes.
9. The industrial process for preparing the aggregation-preventing broad-spectrum antibacterial nano-silver micro-powder as claimed in claims 1 to 7, wherein the medicament is impregnated into the carrier, then pressurized and homogenized to be uniform, and then put into a reaction kettle for reaction, and a dispersant is added until the product is brownish yellow.
10. The aggregation-preventing broad-spectrum antibacterial nano-silver micropowder of claim 1, wherein the prepared nano-silver micropowder is added with appropriate pharmaceutical adjuvants or excipients to prepare powders, tablets, ointments, creams, films, gels, patches, injections, mists, sprays and biomedical chips.
11. The aggregation-preventing broad-spectrum antibacterial nano-silver micropowder as claimed in claim 1, wherein the prepared silver powder can be used as a bactericidal materialfor various uses in the fields of field, battlefield, disaster area and aerospace, for killing pathogenic bacteria in bacteria-containing water.
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CN01223000U CN2479952Y (en) 2001-04-20 2001-05-08 Nm silver plaster for trauma
CN01129505A CN1328819A (en) 2001-04-20 2001-06-22 Nanometer silver antimicrobial inflammation-relieving film for curing gynecopathy and its production process
CNB011295074A CN1169529C (en) 2001-04-20 2001-06-22 Nanometer silver antimicrobial inflammation-relieving gel for curing prostatitis and its industrial production process
CNB018231578A CN1224479C (en) 2001-04-20 2001-11-26 Mathod for preparing micro powder containing anti-agglomerated nanometer silver, micro powder produced by the mathod and its application
PCT/CN2001/001584 WO2002090025A1 (en) 2001-04-20 2001-11-26 Mathod for preparing micro powder containing anti-agglomerated nanometer silver, micro powder produced by the mathod and its application

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CN01223000U CN2479952Y (en) 2001-04-20 2001-05-08 Nm silver plaster for trauma
CN01129505A CN1328819A (en) 2001-04-20 2001-06-22 Nanometer silver antimicrobial inflammation-relieving film for curing gynecopathy and its production process
CNB011295074A CN1169529C (en) 2001-04-20 2001-06-22 Nanometer silver antimicrobial inflammation-relieving gel for curing prostatitis and its industrial production process

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CN01129505A Pending CN1328819A (en) 2001-04-20 2001-06-22 Nanometer silver antimicrobial inflammation-relieving film for curing gynecopathy and its production process
CNB011295074A Expired - Fee Related CN1169529C (en) 2001-04-20 2001-06-22 Nanometer silver antimicrobial inflammation-relieving gel for curing prostatitis and its industrial production process
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CNB011295074A Expired - Fee Related CN1169529C (en) 2001-04-20 2001-06-22 Nanometer silver antimicrobial inflammation-relieving gel for curing prostatitis and its industrial production process
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