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WO2008011748A1 - Procédé d'obtention de textiles contenant de l'argent de valence élevée et produits ainsi obtenus - Google Patents

Procédé d'obtention de textiles contenant de l'argent de valence élevée et produits ainsi obtenus Download PDF

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Publication number
WO2008011748A1
WO2008011748A1 PCT/CN2006/001441 CN2006001441W WO2008011748A1 WO 2008011748 A1 WO2008011748 A1 WO 2008011748A1 CN 2006001441 W CN2006001441 W CN 2006001441W WO 2008011748 A1 WO2008011748 A1 WO 2008011748A1
Authority
WO
WIPO (PCT)
Prior art keywords
textile
silver
fabric
solution
minutes
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/CN2006/001441
Other languages
English (en)
Chinese (zh)
Inventor
Rongyu Zheng
Huade Jiang
Xiaoming Luo
Yong Sun
Dongzhao Qiu
Yiduan Zheng
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shenzhen Yuanxing Bio-Pharm Science & Technology Co Ltd
Original Assignee
Shenzhen Yuanxing Bio-Pharm Science & Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shenzhen Yuanxing Bio-Pharm Science & Technology Co Ltd filed Critical Shenzhen Yuanxing Bio-Pharm Science & Technology Co Ltd
Priority to PCT/CN2006/001441 priority Critical patent/WO2008011748A1/fr
Publication of WO2008011748A1 publication Critical patent/WO2008011748A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/34—Shaped forms, e.g. sheets, not provided for in any other sub-group of this main group
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A01N59/16—Heavy metals; Compounds thereof
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising

Definitions

  • the present invention relates to an antibacterial textile and a preparation method thereof, and more particularly to a high-priced silver antibacterial textile and a preparation method thereof. Background technique
  • the antibacterial fabric is directly used with a strong alkali and a strong oxidant in the production process, and silver nitrate is directly used as a raw material. Some of them are made by directly depositing Ag 4 0 4 produced by the reaction on the fabric, and the uniformity and color of the silver distribution are relatively poor.
  • the silver-containing fabric prepared by CN1241662 is characterized in that ultrafine silver adheres to the fibers of the fabric, so the firmness is poor, and the folding or kneading causes the silver particles to fall off, affecting the antibacterial effect, and at the same time forming uneven color.
  • the preparation of the antibacterial fabric is carried out simultaneously in the preparation of the finishing agent (the solution containing the silver particles), so that the strong alkali, the strong oxidizing agent and the salt produced in the reaction are present in the finishing agent, so that the fabric has more impurities, and the preparation process is more complex.
  • U.S. Patent No. 6,436,420 discloses a method for preparing a fabric containing high-priced silver, but the fabric is The preparation is deposited on the fabric in the presence of a strong base and a strong oxidant, so the process is complicated, the content is difficult to control, and the uniformity is also poor.
  • the Chinese patent application CN1214867 which has been assigned to the present applicant, discloses a preparation method of a silver-containing bactericide, which comprises the following steps: 1) taking an oxide of silver and adding distilled water; 2) after stirring for 15 to 60 minutes, was added dropwise concentrated acid to make a pH of 2-3.5; 3) clarification of at least 2 hours, the supernatant was decanted; 4) was added to the supernatant liquid hydrogen peroxide sterilant is obtained containing H 4 Ag 2 0 6 in.
  • the method is characterized by the use of silver oxides, such as silver oxide or silver peroxide, rather than the commonly used silver nitrate, thus avoiding the step of reducing silver ions to elemental silver.
  • the applicant's Chinese patent application CN1605676 discloses a method which is prepared as described above. H 4 Ag 2 0 6 fungicide applied on the fabric method, comprising the steps of: 1) ⁇ solution containing Preparation 11 ⁇ 2 0 6; 2) was impregnated with the resultant 3 ⁇ 4Ag 206, rinsed injection Or coating the textile; then 3) drying the wet textile. Summary of the invention
  • the present invention proposes a method for producing a high-priced silver antibacterial textile comprising the following steps:
  • step (3) The textile of step (3) is baked in a pre-drying room at 50-120 ° C for 1-5 minutes, and then baked in a main baking oven at a temperature of 100 to 190 ° C for 5-10 minutes.
  • the present invention utilizes a high-valent silver (H 4 Ag 2 0 6 ) solution prepared by the method disclosed in Chinese Patent Application No. CN1214867, soaks various fabrics, and obtains the fabric by a specific condition such as silver content control and color reaction.
  • the silver Ag3d5 in the fabric obtained by the present invention was determined by the XPS method to be 367 ⁇ (Kumar Kaushik V., J. Electron. Spectrosc. Relat. Phenom. 1991, 56, 273; the metal form of Ag was 368 ⁇ , Ag in Ag 2 0 is 367* 7 ev, Ag is 367* 3 ev in Ag 2 0 2 .
  • the concentration of the H 4 Ag 2 0 6 solution used in the present invention is 0.002-1.0 w/v%, more preferably 0.01-0.6 w/v%, as needed.
  • the soaking time is more preferably from 10 seconds to 5 minutes.
  • the pre-drying chamber temperature described in the step (4) is more preferably from 70 to 120 ° C, and the main drying chamber temperature is more preferably from 130 to 190 °C.
  • the fabric of the present invention may be a natural textile, a synthetic textile, or a mixture thereof.
  • the natural textile which can be used in the present invention may be cotton, wool, hemp, silk, chitosan, or a mixture thereof, preferably cotton, such as gauze, yarn, cotton nonwoven fabric, chitosan nonwoven fabric or the like.
  • Synthetic textiles which can be used in the present invention are synthetic fibers, that is, a rayon fiber, including but not limited to polyester, nylon, polyethylene, and acetate fibers, etc. One of them can be used alone, and a mixed textile of the above products can also be used.
  • the fabric of the present invention may be in the form of a knitted fabric, a woven fabric, a nonwoven fabric, a yarn or a perforated film.
  • the invention can be made into different silver-containing fabrics according to different uses, and has good stability and strong bactericidal ability, no strong alkali in the production process, no nitrate ions, and no strong oxidant. More specifically, the high-priced silver antibacterial textile prepared according to the method of the present invention has the following characteristics:
  • the silver content of the fabric can be selected according to the requirements of the application. detailed description
  • the stability of the high-priced silver antibacterial textile of the present invention was evaluated by the following method.
  • the cotton non-woven fabric was immersed in a silver (H 4 Ag 2 0 6 ) solution having a concentration of 0.40 ⁇ 0.01 w/v% for 1 minute, and then the drum was controlled to have a gap of 1.0 mm and the rotation speed of the drum was 4 m/sec.
  • the non-woven fabric is run at a constant speed in the immersion liquid, and the liquid absorption amount is kept consistent, and the fresh liquid is continuously replenished to ensure that the adsorbed amount and concentration of the silver solution remain unchanged. It was then baked in a pre-drying oven at 80 ° C for 5 minutes and then in a main oven at a temperature of 180 ° for 5 minutes.
  • the cotton nonwoven fabric thus prepared was stirred in water for 72 hours, the silver content was detected to be 47%, and the sterilization rate was still 99.99% by the AATCC test method 100-1999; the fabric was boiled 10 times in water, each time 10 Minutes (each time changing water), the silver content is still 49.7%, and the sterilization rate is still 99.96%.
  • the fabric prepared by the method of the present invention is irradiated by ultraviolet light for 30 hours and X-ray (25 GY), and sunlight for 25 hours, and its color is stable and the sterilization rate is unchanged.
  • the fabric is boiled or stirred with water, and the pH of the solution is 6-7, which is neutral.
  • the present invention adds the step of rolling.
  • the rotation speed of the drum is strictly controlled, the original cloth is operated at a constant speed during the immersion process, the liquid absorption amount is kept consistent, and the fresh liquid is continuously replenished to ensure the silver.
  • the adsorbed amount and concentration of the solution remain unchanged.
  • Silver fabrics have a stable silver content.
  • Table 3 shows the effect of the concentration of the original solution on the silver content of the fabric under other conditions (roller gap 1.0 mm, pressure equalization 2 times, pressure 0.3 mpa speed 0.3 m/min).
  • a plurality of points are randomly selected on the high-priced silver antibacterial fabric cotton non-woven fabric prepared by the above method of the present invention and the high-priced silver antibacterial fabric cotton non-woven fabric prepared by the impregnation method described in CN1605676, and the points are measured multiple times.
  • the silver content, the results are shown in Tables 4 and 5, respectively, and the concentration of the silver (3 ⁇ 4 Ag 2 0 6 ) solution used in the test was 0.40 ⁇ 0.01 w/v%.
  • the inventors Using the same batch of cotton non-woven fabric, the inventors also compared the antibacterial properties of the silver-containing non-woven fabrics prepared by different methods, using USP27 to measure the silver content, and the bactericidal ability of the fabric antibacterial property test method FZ/ The sterilization rate was measured by T01021-92, and the results are shown in Table 6 below:
  • the silver-containing textile prepared by the method of the present invention can achieve a very good bactericidal effect at a low silver content.
  • the inventors have further compared the bactericidal effect of the present invention with the different silver content of the fabric prepared in the prior application CN1605676 for 1 hour.
  • the silver-containing nonwoven fabric of Table 7 was prepared by the following method:
  • the textile of the step (3) was baked in a 100-inch pre-drying oven for 5 minutes, and then baked in a main baking oven at a temperature of 170 ° C for 5 minutes.
  • the silver-containing nonwoven fabric of Table 8 was prepared by the method of the prior application CN1605676:
  • a solution containing Ag 2 0 6 was prepared; and a silver solution of 20 ppm, 50 ppm, 200 ppm, 600 ppm series concentration was prepared.
  • the inhibition rate was evaluated in accordance with AATCC Test Method 100-1999.
  • the bacteria used for detection are Staphylococcus aureus.
  • the calculation method of the inhibition rate is as follows:
  • A represents the number of bacteria after 1 hour of inoculation of the drug-containing sample
  • C represents the number of viable cells of the blank sample after "0" contact time.
  • Table 7 Antibacterial effects of silver-containing fabrics prepared by the method of the invention
  • the textile is subjected to high temperature treatment in order to prevent recoloration.
  • the invention has strict and uniform temperature control in production, adopts oil conduction heating, multi-point temperature measuring device, and is controlled within a range of ⁇ 2 °C of the selected temperature.
  • the temperature of the main oven (second bake) is selected to be constant, and the time of the selected fabric staying in the main oven is closely related to the uniformity of the color of the silver-containing fabric, the maintenance of the silver valence state and the stability of the physical properties. , but does not affect the amount of silver in the fabric.
  • the silver ion concentration was formulated to be 1000 ppm. Soak the cotton non-woven fabric in this solution for 5 minutes, adjust the roller spacing of the rolling device to 0.5 mm, roll, and then enter the drying room (temperature set at 50 ° C). After 1 minute, enter the main temperature of 100 ⁇ . Drying room for 5 minutes. The silver content on the cotton nonwoven fabric was measured to be 36.5 g/cm 2 .
  • the silver ion concentration was formulated to be 3000 ppm.
  • the chitosan non-woven fabric was immersed in this solution for 25 minutes, the roller spacing of the roller unit was adjusted to 2.0 mm, rolled, and then entered into the drying room (temperature set at 80 ° C). After 1 minute, the temperature was 150 ° C. The main drying room is 10 minutes. Chitosan non-woven fabric was measured on a silver content of 75.8 g / C m 2.
  • the silver ion concentration was formulated to be 4000 ppm.
  • the woven polyester cloth was immersed in this solution for 4 minutes, the roller spacing of the rolling device was adjusted to 1.5 mm, rolled, and then entered into the drying room (temperature set at 50 ° C), and after 1 minute, the temperature was 175 ° C. The main drying room is 3 minutes.
  • the silver content of the woven polyester cloth was measured to be 86.8 g/cm 2 .
  • the silver ion concentration was formulated to be 500 ppm. Soak the leech viscose non-woven fabric in this solution 5 Minutes, the roller spacing of the rolling mill was adjusted to 1.2 mm, rolled, and then entered the drying room (temperature set at 100 ° C), and after 1 minute, the main drying room was heated to 150 ° C for 4 minutes. The silver content of the leech viscose nonwoven fabric was measured to be 16.7 g/cm 2 .
  • the silver ion concentration was prepared to be 20 ppm.
  • Nylon cloth was immersed in this solution for 5 minutes, the roller spacing of the rolling equipment was adjusted to 0.5 mm, rolled, and then entered into the drying room (temperature set at 50 °C). After 1 minute, the main drying room was introduced at a temperature of 120 °C. 2 minutes. The nylon cloth was found to have a silver content of 3.0 g/cm 2 .
  • the bacteriostatic rate experiment was carried out using the samples of Examples 2-6 in accordance with AATCC Test Method 100-1999.
  • the bacteria used for detection were Staphylococcus aureus.
  • the calculation method of the inhibition rate is as follows:
  • Inhibition rate [(c a Aye] 1 oo%
  • A indicates the number of bacteria after 24 hours of inoculation of the drug-containing sample
  • C indicates the number of viable cells in the blank sample after "0" contact time.

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Environmental Sciences (AREA)
  • Zoology (AREA)
  • Textile Engineering (AREA)
  • Agronomy & Crop Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Dentistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Biochemistry (AREA)
  • Inorganic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Microbiology (AREA)
  • Toxicology (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

La présente invention concerne un procédé d'obtention de textile antibactérien contenant de l'argent à valence élevée. Ce procédé comporte plusieurs étapes. 1°) On prépare une solution de H4Ag2O6. 2°) On imprègne un textile dans la solution de la première étape pendant 10 s à 30 mn. 3°) On calandre le textile obtenu dans un intervalle entre cylindre de 0,01 à 2 mm pour réguler la quantité d'argent portée par le textile. 4°) On soumet à un pré-séchage le textile de l'étape précédente dans un four de pré-séchage pendant 1 à 5 minutes à une température de 50 à 120°C, puis à une cuisson dans le four principal pendant 5 à 10 minutes à une température de 100 à 190°C. L'invention concerne également les produits selon ce procédé.
PCT/CN2006/001441 2006-06-26 2006-06-26 Procédé d'obtention de textiles contenant de l'argent de valence élevée et produits ainsi obtenus Ceased WO2008011748A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/CN2006/001441 WO2008011748A1 (fr) 2006-06-26 2006-06-26 Procédé d'obtention de textiles contenant de l'argent de valence élevée et produits ainsi obtenus

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/CN2006/001441 WO2008011748A1 (fr) 2006-06-26 2006-06-26 Procédé d'obtention de textiles contenant de l'argent de valence élevée et produits ainsi obtenus

Publications (1)

Publication Number Publication Date
WO2008011748A1 true WO2008011748A1 (fr) 2008-01-31

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PCT/CN2006/001441 Ceased WO2008011748A1 (fr) 2006-06-26 2006-06-26 Procédé d'obtention de textiles contenant de l'argent de valence élevée et produits ainsi obtenus

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07109672A (ja) * 1993-10-08 1995-04-25 Toagosei Co Ltd 抗菌性繊維製品の製造方法
CN1214867A (zh) * 1997-10-21 1999-04-28 蒋华德 含银杀菌剂的制备方法
CN1432084A (zh) * 2000-06-02 2003-07-23 美利肯公司 局部施加金属基整理剂的耐洗非导电性纱线和织物
CN1605676A (zh) * 2003-10-09 2005-04-13 深圳市清华源兴生物医药科技有限公司 含银纺织品的制备方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07109672A (ja) * 1993-10-08 1995-04-25 Toagosei Co Ltd 抗菌性繊維製品の製造方法
CN1214867A (zh) * 1997-10-21 1999-04-28 蒋华德 含银杀菌剂的制备方法
CN1432084A (zh) * 2000-06-02 2003-07-23 美利肯公司 局部施加金属基整理剂的耐洗非导电性纱线和织物
CN1605676A (zh) * 2003-10-09 2005-04-13 深圳市清华源兴生物医药科技有限公司 含银纺织品的制备方法

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