CA2283620A1 - Microbiocidal materials and method for manufacturing thereof - Google Patents
Microbiocidal materials and method for manufacturing thereof Download PDFInfo
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- CA2283620A1 CA2283620A1 CA 2283620 CA2283620A CA2283620A1 CA 2283620 A1 CA2283620 A1 CA 2283620A1 CA 2283620 CA2283620 CA 2283620 CA 2283620 A CA2283620 A CA 2283620A CA 2283620 A1 CA2283620 A1 CA 2283620A1
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- 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
- A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
- A01N33/02—Amines; Quaternary ammonium compounds
- A01N33/12—Quaternary ammonium compounds
-
- 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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/46—Compounds containing quaternary nitrogen atoms
- D06M13/463—Compounds containing quaternary nitrogen atoms derived from monoamines
-
- 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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
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- Life Sciences & Earth Sciences (AREA)
- Textile Engineering (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Agronomy & Crop Science (AREA)
- Dentistry (AREA)
- General Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Health & Medical Sciences (AREA)
- Microbiology (AREA)
- General Health & Medical Sciences (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
A composition for treating a material, such as a textile, to impart microbiocidal properties to the material. The composition includes a polysiloxane and quaternary ammonium compound. Methods for applying and fastening the composition to the material are included.
Description
MICROBIOCIDAL MATERIALS ~ METHODS FOR MANUFACTURE THEREOF
This invention relates to a process for preparing a process for preparing a microbiocidal material, such as a fabric, and the material prepared according to the process.
FIELD OF THE INVENTION
This invention concerns a microbiocidal material, for use in clothing, bedding, etc. and a method of manufacturing the material.
BACKGROUND OF THE INVENTION
Microbiocidal properties of quaternary ammonium compounds have been known for quite some time. United States patent No. 5,359,104, which issued to Higgs et al on October 25, 1994 provides an extensive list of patent references exemplifying microbiocidal properties of silicone quaternary ammonium salt compounds and the various uses to which such compounds have been put over the years. Higgs et all also proffer an explanation for the microbiocidal activity of the compounds.
~s United States Patent No. 5,091,102, which issued to Sheridan on February 25, 1992, describes the use of water-soluble quaternary ammonium compounds, such as C8-C18 alkyl dimethyl ammonium chlorides as caticnic surfactants in the preparation of a flexible matrix which may be used as garment material.
United States Patent No. 5,319,093, which issued to Huth et al on June 7, 1994, describes the 2o use of quaternized cationic monomers in the preparation of biocidal polymers, stated to be useful for textile finishing agents. United States Patent No. 5,336,305, which issued to Staats on August 9, 1994, describes biocidal activity of quaternary ammonium compounds, including [C,2 H25 - N (CH3)2 - CH2 - CsHs]+CI-, and use thereof in disposable medical gowns and the like.
2s Many approaches have been taken in obtaining textiles, and related types of materials, that have microbiocidal properties. Examples from the patent literature include: United States Patent No. 3,794,736, which issued to Abbott et al on February 26, 1974; United States Patent No. 3,811,932, which issued to Hubele on May 21, 1974; United States Patent No. 3,860,709, which issued to Abbott et al. on January 14, 1975; United States Patent No. 4,307,109, which issued to Arbir et al on December 22, 1981; United States Patent No. 4,401,712, which issued to Morrison on August 30, 1983; United States Patent No. 4,417,895, which issued to Hennemann et al on Nov.
29, 1983; United States Patent No. 4,443,222, which issued to Morris et al on April 17, 1984; United States Patent No. 4,496,363, which issued to De Filippi on January 29, 1985; United States Patent No. 4,810,567 which issued to Calcaterra et al on March 7, 1989; United States Patent No. 4,842,932, which issued to Burton on June 27, 1989;
United States Patent No. 5,027,438, which issued to Scwharze et al on July 2, 1991;
United States Patent No. 5,069,907 which issued to Mixan et al on December 3, 1991;
United States Patent No. 5,024,851, which issued to Good et al on June 18, 1991;
United States Patent No. 5,024,875, which issued to Hill et al on June 18, 1991; United States Patent No. 5,565,265, which issued to Rubin et al. on October 15, 1976;
United States Patent No. 5,643,971, which issued to Roenigk on July 1, 1997;
United ~s States Patent No. 5,662,991, which issued to Smolik et al. on Sept. 2, 1997; United States Patent No. 5,700,742, which issued to Payne on December 23, 1997;
United States Patent No. 5,830,526, which issued to Wilson et al. on November, 1998;
United States Patent No. 5,856,005, which issued to Gurian on January 5, 1999; United States Patent No. 5,874,164, which issued to Caldwell on February 23, 1999; United States 2o Patent No. 5,882,357, which issued to Sun et al. on March 16, 1999; United States Patent No. 5,889,130, which issued to Worley et al. on March 30, 1999; United States Patent No. 5,399,737, which issued to Park et al. on March 21, 1995; describes quaternary ammonium siioxane compounds for use in ophthalmic formulations for contact lens disinfecting solutions.
2s United States Patent No. 3,794,736, which issued to Abbott et al on February 26, 1974, describes a method of inhibiting the growth of bacteria and fungi on fabrics using organosilicon amines.
This invention relates to a process for preparing a process for preparing a microbiocidal material, such as a fabric, and the material prepared according to the process.
FIELD OF THE INVENTION
This invention concerns a microbiocidal material, for use in clothing, bedding, etc. and a method of manufacturing the material.
BACKGROUND OF THE INVENTION
Microbiocidal properties of quaternary ammonium compounds have been known for quite some time. United States patent No. 5,359,104, which issued to Higgs et al on October 25, 1994 provides an extensive list of patent references exemplifying microbiocidal properties of silicone quaternary ammonium salt compounds and the various uses to which such compounds have been put over the years. Higgs et all also proffer an explanation for the microbiocidal activity of the compounds.
~s United States Patent No. 5,091,102, which issued to Sheridan on February 25, 1992, describes the use of water-soluble quaternary ammonium compounds, such as C8-C18 alkyl dimethyl ammonium chlorides as caticnic surfactants in the preparation of a flexible matrix which may be used as garment material.
United States Patent No. 5,319,093, which issued to Huth et al on June 7, 1994, describes the 2o use of quaternized cationic monomers in the preparation of biocidal polymers, stated to be useful for textile finishing agents. United States Patent No. 5,336,305, which issued to Staats on August 9, 1994, describes biocidal activity of quaternary ammonium compounds, including [C,2 H25 - N (CH3)2 - CH2 - CsHs]+CI-, and use thereof in disposable medical gowns and the like.
2s Many approaches have been taken in obtaining textiles, and related types of materials, that have microbiocidal properties. Examples from the patent literature include: United States Patent No. 3,794,736, which issued to Abbott et al on February 26, 1974; United States Patent No. 3,811,932, which issued to Hubele on May 21, 1974; United States Patent No. 3,860,709, which issued to Abbott et al. on January 14, 1975; United States Patent No. 4,307,109, which issued to Arbir et al on December 22, 1981; United States Patent No. 4,401,712, which issued to Morrison on August 30, 1983; United States Patent No. 4,417,895, which issued to Hennemann et al on Nov.
29, 1983; United States Patent No. 4,443,222, which issued to Morris et al on April 17, 1984; United States Patent No. 4,496,363, which issued to De Filippi on January 29, 1985; United States Patent No. 4,810,567 which issued to Calcaterra et al on March 7, 1989; United States Patent No. 4,842,932, which issued to Burton on June 27, 1989;
United States Patent No. 5,027,438, which issued to Scwharze et al on July 2, 1991;
United States Patent No. 5,069,907 which issued to Mixan et al on December 3, 1991;
United States Patent No. 5,024,851, which issued to Good et al on June 18, 1991;
United States Patent No. 5,024,875, which issued to Hill et al on June 18, 1991; United States Patent No. 5,565,265, which issued to Rubin et al. on October 15, 1976;
United States Patent No. 5,643,971, which issued to Roenigk on July 1, 1997;
United ~s States Patent No. 5,662,991, which issued to Smolik et al. on Sept. 2, 1997; United States Patent No. 5,700,742, which issued to Payne on December 23, 1997;
United States Patent No. 5,830,526, which issued to Wilson et al. on November, 1998;
United States Patent No. 5,856,005, which issued to Gurian on January 5, 1999; United States Patent No. 5,874,164, which issued to Caldwell on February 23, 1999; United States 2o Patent No. 5,882,357, which issued to Sun et al. on March 16, 1999; United States Patent No. 5,889,130, which issued to Worley et al. on March 30, 1999; United States Patent No. 5,399,737, which issued to Park et al. on March 21, 1995; describes quaternary ammonium siioxane compounds for use in ophthalmic formulations for contact lens disinfecting solutions.
2s United States Patent No. 3,794,736, which issued to Abbott et al on February 26, 1974, describes a method of inhibiting the growth of bacteria and fungi on fabrics using organosilicon amines.
United States Patent No. 3, 817,739, which issued to Abbott et al on June 18, 1974, describes a method of inhibiting the growth of algae using quaternary ammonium siloxane compounds.
United States Patent No. 4,504,51, which issued to Yasuda et al on s March 12, 1985, describes antimicrobial fabric treated with a quaternary ammonium base-containing organosilicone.
United States Patent No. 3,730,701, which issued to Isquith et al on May 1, 1973, describes an early use of a silyl quaternary amine for controlling growth of algae.
United States Patent No. 4,282,366, which issued to Eudy on August 4, 1981, describes organosilicon quaternary ammonium antimicrobial compounds for treating a substrate, such as a cellulose fabric.
United States Patent No. 5,254,134, which issued to Zhao et al. on October 19, 1993, describes a textile finishing agent which includes a polysiloxane 15 having the formula Me3 Si0[SiMe20]m SiOMeR'SiOMeR"SiOMeR"' SiMe3. R' is a polyether residue, R" is an epoxy polyether residue, R'° is a polyethoxy residue and m is between 1,000 and 3,000. The foregoing compound is combined, in water, with a quaternary ammonium compound such as dodecyl-dimethyl-benzyl ammonium chloride, a crosslinking agent such as an a, w-bisepoxypropyl-hexamethylene diamine, 2o and catalysts such as acetic acid and magnesium chloride. A textile is soaked in the solution, excess solution removed, and the textile dried, e.g. at 70°C
for 5 to 15 minutes, and then e.g., at 110°C to 120°C for 20 to 90 seconds.
With the rapid development of social civilization, people become more and more concerned with the environment in which they are living. At the same time, 2s they begin to realize that textile is an important type of media for virus and microbe promulgation. For this reason, I began my research on the development of textile hygiene finishing technology. This new technology is named 'MX-08' textile hygiene finishing technology.
United States Patent No. 4,504,51, which issued to Yasuda et al on s March 12, 1985, describes antimicrobial fabric treated with a quaternary ammonium base-containing organosilicone.
United States Patent No. 3,730,701, which issued to Isquith et al on May 1, 1973, describes an early use of a silyl quaternary amine for controlling growth of algae.
United States Patent No. 4,282,366, which issued to Eudy on August 4, 1981, describes organosilicon quaternary ammonium antimicrobial compounds for treating a substrate, such as a cellulose fabric.
United States Patent No. 5,254,134, which issued to Zhao et al. on October 19, 1993, describes a textile finishing agent which includes a polysiloxane 15 having the formula Me3 Si0[SiMe20]m SiOMeR'SiOMeR"SiOMeR"' SiMe3. R' is a polyether residue, R" is an epoxy polyether residue, R'° is a polyethoxy residue and m is between 1,000 and 3,000. The foregoing compound is combined, in water, with a quaternary ammonium compound such as dodecyl-dimethyl-benzyl ammonium chloride, a crosslinking agent such as an a, w-bisepoxypropyl-hexamethylene diamine, 2o and catalysts such as acetic acid and magnesium chloride. A textile is soaked in the solution, excess solution removed, and the textile dried, e.g. at 70°C
for 5 to 15 minutes, and then e.g., at 110°C to 120°C for 20 to 90 seconds.
With the rapid development of social civilization, people become more and more concerned with the environment in which they are living. At the same time, 2s they begin to realize that textile is an important type of media for virus and microbe promulgation. For this reason, I began my research on the development of textile hygiene finishing technology. This new technology is named 'MX-08' textile hygiene finishing technology.
SUMMARY OF THE INVENTION
The invention is summarized in the claims, which are incorporated herein.
DESCRIPTION TO DETAILED OF PREFERRED EMBODIMENT
It is possible to obtain microbiocidal textiles and non-woven cloth by manufacturing the according to methods of the present invention. Microbiocidal characteristics obtainable are described below.
In a preferred embodiment, a microbiocidal textile is manufactured as follows.
Dodecanyl-dimethyl-benzyl-ammonium chloride (I) and a to poly(dimethylsiloxane) {II) are mixed in water in which NaOH has been dissolved and the reaction product diluted with water with the ratio of 1:20-25. For example, 0.2 gm of NaOH pellets were dissolved in 83 ml of water. 15 ml of I and 2ml of II were added to the solution with mixing and the solution was mixed for about 1 minute. In this step, NaCI can be substituted for NaOH. The amount of base (or NaCI) can be varied to a total of about 0.1 to 0.5 mass percent. The ratio of I:II can be varied between about 1:1 and about 1:12.5 (vol:vol). The reaction is generally carried out at room temperature, but the temperature can be between about 1 and 40°C.
Component I was obtained from the China Hangzhou ErQiao Washing Agent Factory located at QianJiang Bridge 2, HangHai Road, Hangzhou, Zhejiang, 2o China, 310021. Component 1 is synthesized by a two step process: C,2H250H
and HN(CH3)2 are reacted in the presence of AI203 to obtain C~2H25N{CH3)2 and water.
C,2H25N(CH3)2 and CsHSCI are reacted to obtain I as a colorless or light-yellow transparent liquid. The content of active material is about 40-45°~.
The ammonium salt concentration is about 4% (by weight), pH between about 6 and 8.
Component II was obtained from Hangzhou ZhaoHui Organic Silicon Factory located at 3,3rd Area, ZhaoHuiXinCun, Hangzhou, Zhejiang, China, Component II is obtained according to the reaction:
The invention is summarized in the claims, which are incorporated herein.
DESCRIPTION TO DETAILED OF PREFERRED EMBODIMENT
It is possible to obtain microbiocidal textiles and non-woven cloth by manufacturing the according to methods of the present invention. Microbiocidal characteristics obtainable are described below.
In a preferred embodiment, a microbiocidal textile is manufactured as follows.
Dodecanyl-dimethyl-benzyl-ammonium chloride (I) and a to poly(dimethylsiloxane) {II) are mixed in water in which NaOH has been dissolved and the reaction product diluted with water with the ratio of 1:20-25. For example, 0.2 gm of NaOH pellets were dissolved in 83 ml of water. 15 ml of I and 2ml of II were added to the solution with mixing and the solution was mixed for about 1 minute. In this step, NaCI can be substituted for NaOH. The amount of base (or NaCI) can be varied to a total of about 0.1 to 0.5 mass percent. The ratio of I:II can be varied between about 1:1 and about 1:12.5 (vol:vol). The reaction is generally carried out at room temperature, but the temperature can be between about 1 and 40°C.
Component I was obtained from the China Hangzhou ErQiao Washing Agent Factory located at QianJiang Bridge 2, HangHai Road, Hangzhou, Zhejiang, 2o China, 310021. Component 1 is synthesized by a two step process: C,2H250H
and HN(CH3)2 are reacted in the presence of AI203 to obtain C~2H25N{CH3)2 and water.
C,2H25N(CH3)2 and CsHSCI are reacted to obtain I as a colorless or light-yellow transparent liquid. The content of active material is about 40-45°~.
The ammonium salt concentration is about 4% (by weight), pH between about 6 and 8.
Component II was obtained from Hangzhou ZhaoHui Organic Silicon Factory located at 3,3rd Area, ZhaoHuiXinCun, Hangzhou, Zhejiang, China, Component II is obtained according to the reaction:
t ~ ~ c~3 ~~~ cN
s c~~
! r~'~. a ~ ~ ~, ~i ~ ,, ~ a C~°~ '~ ~; ~' o ~- sr.~- ~~~
The product is obtained as an white liquid, pH between about 5 and 7. The content of non-volatile substance is 28 to 32%, content of extraction grease is about 26 to 30, viscosity of extraction grease is about mpa.s 2.0x103 to about 3.0 x 105, the acentric s stability is about 3000 turns/min, and after 60 minutes there is no delamination or floating grease.
The above mixture of I and II is diluted with water by about the ratio of 1:20-25 (vollvol), water in excess.
The textile is exposed to the diluted working solution by soaking and 1o rolling for a time sufficient to thoroughly soak the textile, usually between about 30 and 60 seconds.
The textile is pre-dried at 100°C for 2-3 minutes.
This is followed by drying at 120°C -140°C for 20-30 seconds.
The above drying times and temperatures can be varied, the relationship ~s between temperature and time required, being a generally inverse one. The weightier the textile, the longer the time needed in each step.
In the case of a non-woven material, the mixture of I and II, prepared as above, is diluted with water at a ratio of about 1:50 to about 1:100 (vol/vol), water in excess. The non-woven material is exposed to the working solution, to soak it as much as possible. The material is dried at 80°C-100°C.
Microbiocidal materials suitable for the below-listed items can be made by textile and non-woven cloth obtained using the foregoing method:
- underwear, shirts, socks - medical, sanitation, food processing and cosmetology industry, bathroom and related textiles.
- bedding, such as sheets, bedspreads, towels, pillowcases.
- women's sanitation napkins, sanitation pads, napkins, nappies for adults ~o and children.
- single use non-woven items used in medical, sanitation, food processing and beverage industries.
In addition to variations described above, it is contemplated that the long side chain of compound I, can be varied according to the formula C~H~2~+,~
wlth n having ~ 5 a value of anywhere from 8 to 18. The best known compound found to date, however, is compound I itself. As well, microbiocidal materials can also be obtained with the bromide analogues of the chloride compounds disclosed herein.
In the context of this invention, a "textile" is a woven material that can be natural or synthetic. Preferred materials are cotton terylene, acrylic and silk.
2o A "non-woven" material is, for example, an extruded material and can be one that sets upon application of heat.
Experiments have been performed to demonstrate the biocidal properties (anti-bacterial and anti-viral activities) of materials prepared according to the foregoing procedures.
25 It has been shown that use of this approach can effectively eliminate 99.9% of Staphylococcus aureus within 10 minutes, Escherichia coli, 94.87%, and for Candida albicans, 88.19%. It is able to destroy HBsAg (hepatitis B surface antigen) in about six hours. Products include anti-bacterial and anti-viral working clothes for medical workers, clothes for patients as well as anti-bacterial and anti-viral.
s c~~
! r~'~. a ~ ~ ~, ~i ~ ,, ~ a C~°~ '~ ~; ~' o ~- sr.~- ~~~
The product is obtained as an white liquid, pH between about 5 and 7. The content of non-volatile substance is 28 to 32%, content of extraction grease is about 26 to 30, viscosity of extraction grease is about mpa.s 2.0x103 to about 3.0 x 105, the acentric s stability is about 3000 turns/min, and after 60 minutes there is no delamination or floating grease.
The above mixture of I and II is diluted with water by about the ratio of 1:20-25 (vollvol), water in excess.
The textile is exposed to the diluted working solution by soaking and 1o rolling for a time sufficient to thoroughly soak the textile, usually between about 30 and 60 seconds.
The textile is pre-dried at 100°C for 2-3 minutes.
This is followed by drying at 120°C -140°C for 20-30 seconds.
The above drying times and temperatures can be varied, the relationship ~s between temperature and time required, being a generally inverse one. The weightier the textile, the longer the time needed in each step.
In the case of a non-woven material, the mixture of I and II, prepared as above, is diluted with water at a ratio of about 1:50 to about 1:100 (vol/vol), water in excess. The non-woven material is exposed to the working solution, to soak it as much as possible. The material is dried at 80°C-100°C.
Microbiocidal materials suitable for the below-listed items can be made by textile and non-woven cloth obtained using the foregoing method:
- underwear, shirts, socks - medical, sanitation, food processing and cosmetology industry, bathroom and related textiles.
- bedding, such as sheets, bedspreads, towels, pillowcases.
- women's sanitation napkins, sanitation pads, napkins, nappies for adults ~o and children.
- single use non-woven items used in medical, sanitation, food processing and beverage industries.
In addition to variations described above, it is contemplated that the long side chain of compound I, can be varied according to the formula C~H~2~+,~
wlth n having ~ 5 a value of anywhere from 8 to 18. The best known compound found to date, however, is compound I itself. As well, microbiocidal materials can also be obtained with the bromide analogues of the chloride compounds disclosed herein.
In the context of this invention, a "textile" is a woven material that can be natural or synthetic. Preferred materials are cotton terylene, acrylic and silk.
2o A "non-woven" material is, for example, an extruded material and can be one that sets upon application of heat.
Experiments have been performed to demonstrate the biocidal properties (anti-bacterial and anti-viral activities) of materials prepared according to the foregoing procedures.
25 It has been shown that use of this approach can effectively eliminate 99.9% of Staphylococcus aureus within 10 minutes, Escherichia coli, 94.87%, and for Candida albicans, 88.19%. It is able to destroy HBsAg (hepatitis B surface antigen) in about six hours. Products include anti-bacterial and anti-viral working clothes for medical workers, clothes for patients as well as anti-bacterial and anti-viral.
Experimental results of the research show that textile treated in accordance with the invention can effectively prevent the reproduction of microbes so as to reduce the threat of textiles contaminated by microbes on people's health. A
preferred application is thus in providing anti-bacterial and anti-viral materials and textiles in medical clinics and hospitals.
Anti-bacterial effect test shows that textile treated according to the present invention has anti-bacterial effect for both Staphylococcus aureus and Escherichia coli, with bacteria inhibition rate of 100% after 30 minutes. For Candida albicans, the percentage was close to 90% after 30 minutes. See Table 1 for results obtained with cotton material. Bacterial inhibition was determined according to the equation rate(%)=(A-B)/Ax100 where A is (non-antibacterial fabric) control sample average return amount of bacteria and B is (anti-bacterial fabric) sample average return amount of bacteria.
Table 1 Result of anti-bacterial effect test for textile treated with composition of the invention Bacteria strains Bacteria inhibition rate (%) for assay 10min 30min 60min 120min Staphylococcus aureus 97.97 100 100 100 (ATCC6538) Escherichia coli (ATCC25922) 94.87 100 100 100 Candida albicans (ATCC10231) 86.49 88.19 90.21 92.29 2o Anti-viral test shows that a textile treated with can have an anti-viral effect. It can completely destroy HBsAg in about six hours. See Table 2 for results obtained with towel. (A negative control optical density (OD) value is 0.03, positive control OD value is 1.40, and blank control OD value is 1.32-1.37 (1-6h).) A
sample is 0.3 x 1 cm.
Table 2 Results of anti-viral test for textile treated with composition of the invention The amount of HBsAg dyed S/N average value (Ng/piece) 60min 180min 240min 300min 360min 2.0 6.9 4.1 3.0 2.6 <2.1 _8_ Washing fastness tests were also performed. The anti-bacterial effect of a textile treated according to the invention was thus found to be fast to washing over many washings. The bacteria inhibition rate within 10 minutes for Staphylococcus aureus remains over 96% after the textile was washed 50 times. See Table 3 obtained with towel.
Table 3 Results of fast-to-washing test for textile treated with composition of the invention Bacteria Times of Bacteria inhibition rate (%) strains washing for assay 10min 30min 60min 180min 240min Staphylococcu 0 99.97 100 100 100 100 s 10 98.50 98.75 98.87 99.15 99.50 Aureus 20 97.94 98.06 98.50 98.68 98.84 40 97.29 98.36 98.50 98.85 98.70 50 96.16 97.23 98.14 98.48 98.51 Tests shows have also shown that products treated according to the invention have stability over time. An accelerating test showed that the products retain 1s anti-bacterial properties after one year of storage, with only 3%
decreasing in bacteria inhibition rate. See Table 4 for results obtained with cotton material.
Table 4 Stability of the textile's bacteria inhibition rate under 54°C
for 2 weeks Bacteria strains Temperature Bacteria inhibition rate (°~) for assay Processing 10min 30min 60min 120min Candida albicans (-) 88.19 89.49 91.42 92.29 (ATCC10231) (+) 85.71 87.42 89.41 89.74 Note: (-) means with no temperature processing, and (+) means under 54°C for 2 weeks Acute oral toxicities of the agents used to create materials according to the invention (under the working concentration of 1:25) were tested on male and female _g_ mice. The tests indicated an LDP of greater than 15.Og/kg indicating that the material is not toxic to the animals.
A skin irritation test on Chinese white rabbits obtained a mean integral value of zero. According to the criteria for skin irritating grade, this shows that the sample is not irritating to the skin of the animals.
A micronucleus test was performed on mice. The results showed that each group of the animals with different doses of the agent had a statistically negative result in comparison to the negative control groups and treated, that is, there was no generation induced under the conditions of the experiment.
1o Anti-bacterial and anti-viral tests were also performed on non-woven cloth prepared according to the invention. Table 5 demonstrates that non-woven cloth of the invention has similar anti-bacterial and anti-viral properties to textiles. In the HBsAg test, the negative control OD value was 0.03; positive control OD value was 1.38; and the blank control OD value was 1.38-1.40.
Table 5 Result of anti-viral effect test for non-woven cloth treated with composition of the invention Bacteria strains Bacteria inhibifion rate (%) for assay 10min 30min 60min 120min Escherichia coli (ATCC:25922) 96.14 100 100 Staphylococcus aureus (ATCC6538) 100 100 100 Candida albicans (ATCC10231) 86.49 88.19 90.21 92.29 Candida albicans (54°C 2 weeks) 86.31 87.11 88.81 91.00 HBsAg Completely destroyed after 360 minutes' action The tests of color fastness, rupture strength and capillarity on the a towel created according to the invention showed the following results:
- there is little difference in the color fastness when washed or rubbed between the sample of the invention and an ordinary sample;
- the warp rupture strength of the anti-bacterial towel, though 4.06% lower than that of the ordinary towel, doesn't exceed the allowance of rupture strength for grade A towel in Standards FZIT62006-93 'Towel';
- the capillarity of both anti-bacterial and ordinary towels were very similar.
See Table 6 for a summary of the results using towel.
Table 6 Results of color fastness, rupture strength 8 capillarity tests for the towel treated with composition of the invention Item Ordinary towelAnti-bacteria towel Color fastness to washingColor change 4-5 4-5 (degree) Color attach 4-5 4-5 Color fastness to rubbingDry rubbing 4-5 4-5 (degree) Web rubbing 4-5 4-5 Rupture strength (N/5'20cm)Vertical 236.4 226.8 Horizontal / /
Capillarity (cm/30 min)Vertical 9.1 9.5 Horizontal 8.7 8.1 Tests for color fastness and rupture strength on sweat cloth treated with compositions of the invention showed the following:
- there was little difference in the color fastness to washing and color fastness to rubbing between the sample of the invention and the untreated sample;
- the warp rupture strength of the anti-bacterial sweat cloth, though 10.75%
lower 2o than that of the ordinary sample, does not exceed the allowance of rupture strength for grade A cloth.
See Table 7 for a summary of the results.
Table 7 Results of color fastness and rupture strength tests for sweat cloth treated with composition of the invention Item Ordinary clothAnti-bacteria cloth Color fastness to washingColor change4-5 4 (degree) Color attach4-5 4-5 Color fastness to sweat Color change4-5 4 (degree) Color attach4-5 4-5 Color fastness to rubbingDry rubbing 4-5 4-5 (degree) Wet rubbing 4-5 4-5 Rupture strength (N) 623.2 556.2 Clinical experiments were performed on products created from materials of the invention. The research was performed under the inspection of Special Committee of Chinese Hospital Infection Management, PLA General Hospital (301 Hospital) and Hangzhou Hygiene and Anti-Epidemic Station. The results show that medical textiles of the invention have anti-bacterial ability and is suitable for an application in reducing infection in hospitals.
Results obtained with 100% cotton material are summarized in Tables 8, ~ 5 9, 10 and 11.
Table 8 Experiment operation Item Working Clothes Sheets clothes for for patients medical workers Anti- Non- Anti- Non- Anti- Non-bacteria antibacteribacteriaantibacteribacteriaantibacteri group a group group a group group a group Number 30 30 30 30 30 30 of textile departureRespiratio10 10 10 10 10 10 nt n Digestion- - 20 20 20 20 Ordinary20 20 - - - -surgery Time 7 days 3 days 7 days for using Sampling 10 cm 10 cm Midpoint place left left of the and 10 and midline, cm 10 cm right right 30 cm to 3rd to 2nd left button button and in the in 30 cam front the front right and in and to the the suture in the midpoint.
of left suture Totally lap. of left 3 places.
Totally lap.
places. Totally 3 places.
Sampling 5'S=25cm2 area Sampling The textile method in the corresponding places is cut off by sterilizing scissors.
After broken into pieces, the textile is emerged into 5ml sterilizing salt water, which is contained in test tubes of 1 Oml.
Each sample is put into a different tube.
Cultivation Shake method the samples by the oscillator for 1 min, then extract 0.1 ml with sampling sucker from each tube and cover it uniformly on the blood flat plate which contains 5% sheep blood.
Put the plate in an incubator of 37C
for 24h.
Counting Amount of bacteria of bacteria on textile N (cfu/cm~=[(amount of bacteria on plate n10.1 )'S]/25=2n Results Statistics processing processing by means of't-test' with pairs of data Table 9 Experiment results with working clothes for medical workers in 301 Hospital No. Mean amount of bacteria on the clothes (cfu/cm~
Respiration Ordinary Ordinary department surgery surgery (group (group I) II) An>i- Non- Anti- Non- Anti- Non-bacteria antibacteriabacteria antibacteriabacteria antibacteria group group group group grou p group I 1.3 54.0 0.6 30.0 0.6 153.3 II 0.6 36.7 0.6 105.3 0 44.0 III 0 49.3 0 192.0 0 102.7 IV 0 65.3 0 56.0 0 142.0 V 0 54.0 0 99.3 0 208.7 VI 0 82.0 0 36.0 0 64.7 VII 0 52.0 0 36.0 0 44.7 VIII 0 74.0 0 23.3 0 72.7 IX 0 112.7 0 55.3 0 26.7 X 0 59.3 0 109.3 0 45.3 P value <0.01 <0.01 <0.01 Note: After t-test, on the working clothes for medical workers, the amount of bacteria in anti-bacteria group is greatly lower than that of non-antibacteria group.
Table 10 Experiment results with clothes for patients in 301 Hospital No. Mean amount of bacteria on the clothes (cfu/cm~
Respiratory Digestion Digestion department dept. dept.
(group (group I) II) Anti- Non- Anti- Non- Anti- Non-bacteria antibacteriabacteria antibacteriabacteria antibacteria group group group group group group I 0.6 134.0 3.3 28.0 0.6 104.7 II 0 167.3 0 18.0 0.6 17.3 III 0 64.0 0 29.3 0.6 40.0 IV 0 44.7 0 16.0 0.6 18.0 V 0 146.0 0 74.7 0 13.3 VI 0 90.7 0 14.0 0 18.0 VII 0 68.0 0 26.7 0 154.7 VIII 0 42.0 0 76.7 0 68.7 IX 0 26.7 0 6.7 0 81.3 X 0 185.3 0 18.7 0 44.7 P value <0.01 <0.01 <0.01 Note: After t-test, on the clothes for patients, the amount of bacteria in anti-bacteria group is greatly lower than that of non-antibacteria group.
Table 11 Experiment results with sheets in 301 Hospital No. Mean amount of bacteria on the sheets (cfu/cm~
Respiration Digestion Digestion,dept.
department dept.,(group (group I) II) Anti- Non- Anti- Non- Anti- Non-bacteria antibacteriabacteria antibacteriabacteria antibacteria grou p group group group group group I 0.6 135.3 0.6 48.0 0.6 58.7 I I 1.3 8.7 0.6 13.3 1.3 70.0 I I I 2.0 172.7 0 182.0 0.6 11.3 IV 1.3 80.7 0 28.7 1.3 46.0 V 2.0 12.7 0 192.0 0 4.7 VI 0 78.7 0 47.3 0 30.0 VII 0 8.0 0 23.3 0 163.3 VIII 0 14.7 0 200.0 0 56.0 IX 0 90.0 0 30.0 0 51.3 X 0 68.7 0 23.3 0 104.7 P value <0.01 <0.01 <0.01 Note: After t-test, the amount of bacteria on the sheets in anti-bacteria group is greatly lower than that of non-antibacteria group.
Tests were also performed using anti-bacterial and anti-viral gauze of the invention. Experiments were conducted in conjunction with Hangzhou Hygiene and Anti-Epidemic Station and the 2"d People's Hospital of Hangzhou. Sixty cases were randomly chosen in the surgery area of the hospital, with thirty cases using gauze 2o prepared according to the invention and the other thirty using ordinary gauze as a control. After 3 days, the gauze was sealed into sterilizing bags and sent to Hangzhou Hygiene and Anti-Epidemic Station for checking. Under sterilizing condition, 4 layers of gauze were cut open to check the total amount of bacteria. See Table 12. This indicated that on the test gauze twenty-five of thirty (83%) displayed no bacterial growth, in comparison to control gauze in which 10 (33%) displayed no bacterial growth.
Table 12 Bacteria growth on test gauze bearing composi~on of the invention and ordinary gauze Type of gauze Number of gauze Number of gauze Total with bacteria growth without bacteria (%0 growth (%) Test gauze 5 (16.67) 25 (83.33) 30 Ordinary gauze 20 (66.67) 10 (33.33) 30 Total 25 35 60 (XZ~H = 15.17, P«0.001) Materials of the invention can thus be used for anti-bacterial and anti-viral 1o working clothes for medical workers, patients' clothes, quilts, pillow covers and sheets, mattresses, medical masks and caps, gauze for medical uses, and towels, particularly towels for medical uses.
It is important to note the rate at which materials created according to the invention are effective in their anti-bacterial and anti-viral actions.
1s The anti-bacterial test for Staphylococcus aureus, Escherichia coli and Candida albicans shows that textile and non-woven cloth created according to the present invention have been shown to effectively eliminate bacteria within short period of time, i.e., 10-30 min. This appears to be marked advantage over previous materials produced for the same purpose.
2o Materials created according to the present invention appear to destroy HbsAg. This also, as far as reports known to the inventor are concerned, appears to be another advantage of materials of the present invention over previously known materials.
-17_ The capacity of materials of the present invention to retain their microbiocidal characteristics in the face or repeated washing and aging is also advantageous.
Further, the low toxicity of materials of the present invention, is an s advantage.
Also, materials of the present invention appear to be generally compatible with other aspects of treated materials, as far as strength, color fastness, softeness, absorption characteristics, etc.
In the context of this invention, sheet material includes textiles, which may synthetic or natural, cotton, wool, polyester, etc. and non-woven web-like material, such as extruded materials. It is understood, of course, that the "sheet" may have already been manufactured into an item for use, such as a doctor's smock, a towel, gloves, diapers, etc., prior to application of the antimicrobial composition of the present invention.
~s In the context of this invention, "consisting essentially of means that there are no other components present that markedly alter the desired effect of the required elements, i.e., that the desired role of the required elements is not adversely deprecated by other elements that may be added. References consulted in the preparation of this specification include Textile Technology Abroad,1998, 2:
29-31;
2o Zhang Ling et al . Magazine on Hospital Infection in China, 1997, 7(1 ) :
59; Liu Guangming et al . Chinese Sterilization Magazine, 1993, 10(2): 112-113; Xun Houqin et al. Chinese Sterilization Magazine,1994, 11(2) :126; Mo Zhanlan .Chinese Sterilization Magazine, 1994, 11 (3) : 194; Zhao Jin et al. Magazine on Hospital Infection in China, 1997, 7(1) : 1-3; Lu Xian'e. Magazine on Hospital Infection in China, 1997, 7{2) : 82-84;
2s Bossard CM. International Textile Bulletin, 1995, 41 (4) : 44-48; He Hebo.
Compilation of International Conference on Anti-bacterial Hygiene Finishing Technology, Beijing, 1995, 41 (4) :44-48; Yin Jinduo. Chinese Sterilization Magazine, 1994, 11 (3) :243-244;
Zhang Jie. Chinese Sterilization Magazine, 1994, 11 (4): 244-245; Ding Lanying et al., Chinese Sterilization Magazine, 1997, 14(2) : 84-86; International Textile Development, 1996, 4: 23-24; International Textile Development, 1992, 42(5): 58-61;
International Textile Development,1992, 43(6): 39-43.
All of the reference described in this specification are herein incorporated in their entirety.
The best method and composition of the invention known to the inventor having been described, the scope of protection to be sought for the invention is given below. Of course, a person skilled in the art would be readily capable, given the teachings of this specification to obtain embodiments not precisely described here, but which, nonetheless fall within the scope of the following claims.
preferred application is thus in providing anti-bacterial and anti-viral materials and textiles in medical clinics and hospitals.
Anti-bacterial effect test shows that textile treated according to the present invention has anti-bacterial effect for both Staphylococcus aureus and Escherichia coli, with bacteria inhibition rate of 100% after 30 minutes. For Candida albicans, the percentage was close to 90% after 30 minutes. See Table 1 for results obtained with cotton material. Bacterial inhibition was determined according to the equation rate(%)=(A-B)/Ax100 where A is (non-antibacterial fabric) control sample average return amount of bacteria and B is (anti-bacterial fabric) sample average return amount of bacteria.
Table 1 Result of anti-bacterial effect test for textile treated with composition of the invention Bacteria strains Bacteria inhibition rate (%) for assay 10min 30min 60min 120min Staphylococcus aureus 97.97 100 100 100 (ATCC6538) Escherichia coli (ATCC25922) 94.87 100 100 100 Candida albicans (ATCC10231) 86.49 88.19 90.21 92.29 2o Anti-viral test shows that a textile treated with can have an anti-viral effect. It can completely destroy HBsAg in about six hours. See Table 2 for results obtained with towel. (A negative control optical density (OD) value is 0.03, positive control OD value is 1.40, and blank control OD value is 1.32-1.37 (1-6h).) A
sample is 0.3 x 1 cm.
Table 2 Results of anti-viral test for textile treated with composition of the invention The amount of HBsAg dyed S/N average value (Ng/piece) 60min 180min 240min 300min 360min 2.0 6.9 4.1 3.0 2.6 <2.1 _8_ Washing fastness tests were also performed. The anti-bacterial effect of a textile treated according to the invention was thus found to be fast to washing over many washings. The bacteria inhibition rate within 10 minutes for Staphylococcus aureus remains over 96% after the textile was washed 50 times. See Table 3 obtained with towel.
Table 3 Results of fast-to-washing test for textile treated with composition of the invention Bacteria Times of Bacteria inhibition rate (%) strains washing for assay 10min 30min 60min 180min 240min Staphylococcu 0 99.97 100 100 100 100 s 10 98.50 98.75 98.87 99.15 99.50 Aureus 20 97.94 98.06 98.50 98.68 98.84 40 97.29 98.36 98.50 98.85 98.70 50 96.16 97.23 98.14 98.48 98.51 Tests shows have also shown that products treated according to the invention have stability over time. An accelerating test showed that the products retain 1s anti-bacterial properties after one year of storage, with only 3%
decreasing in bacteria inhibition rate. See Table 4 for results obtained with cotton material.
Table 4 Stability of the textile's bacteria inhibition rate under 54°C
for 2 weeks Bacteria strains Temperature Bacteria inhibition rate (°~) for assay Processing 10min 30min 60min 120min Candida albicans (-) 88.19 89.49 91.42 92.29 (ATCC10231) (+) 85.71 87.42 89.41 89.74 Note: (-) means with no temperature processing, and (+) means under 54°C for 2 weeks Acute oral toxicities of the agents used to create materials according to the invention (under the working concentration of 1:25) were tested on male and female _g_ mice. The tests indicated an LDP of greater than 15.Og/kg indicating that the material is not toxic to the animals.
A skin irritation test on Chinese white rabbits obtained a mean integral value of zero. According to the criteria for skin irritating grade, this shows that the sample is not irritating to the skin of the animals.
A micronucleus test was performed on mice. The results showed that each group of the animals with different doses of the agent had a statistically negative result in comparison to the negative control groups and treated, that is, there was no generation induced under the conditions of the experiment.
1o Anti-bacterial and anti-viral tests were also performed on non-woven cloth prepared according to the invention. Table 5 demonstrates that non-woven cloth of the invention has similar anti-bacterial and anti-viral properties to textiles. In the HBsAg test, the negative control OD value was 0.03; positive control OD value was 1.38; and the blank control OD value was 1.38-1.40.
Table 5 Result of anti-viral effect test for non-woven cloth treated with composition of the invention Bacteria strains Bacteria inhibifion rate (%) for assay 10min 30min 60min 120min Escherichia coli (ATCC:25922) 96.14 100 100 Staphylococcus aureus (ATCC6538) 100 100 100 Candida albicans (ATCC10231) 86.49 88.19 90.21 92.29 Candida albicans (54°C 2 weeks) 86.31 87.11 88.81 91.00 HBsAg Completely destroyed after 360 minutes' action The tests of color fastness, rupture strength and capillarity on the a towel created according to the invention showed the following results:
- there is little difference in the color fastness when washed or rubbed between the sample of the invention and an ordinary sample;
- the warp rupture strength of the anti-bacterial towel, though 4.06% lower than that of the ordinary towel, doesn't exceed the allowance of rupture strength for grade A towel in Standards FZIT62006-93 'Towel';
- the capillarity of both anti-bacterial and ordinary towels were very similar.
See Table 6 for a summary of the results using towel.
Table 6 Results of color fastness, rupture strength 8 capillarity tests for the towel treated with composition of the invention Item Ordinary towelAnti-bacteria towel Color fastness to washingColor change 4-5 4-5 (degree) Color attach 4-5 4-5 Color fastness to rubbingDry rubbing 4-5 4-5 (degree) Web rubbing 4-5 4-5 Rupture strength (N/5'20cm)Vertical 236.4 226.8 Horizontal / /
Capillarity (cm/30 min)Vertical 9.1 9.5 Horizontal 8.7 8.1 Tests for color fastness and rupture strength on sweat cloth treated with compositions of the invention showed the following:
- there was little difference in the color fastness to washing and color fastness to rubbing between the sample of the invention and the untreated sample;
- the warp rupture strength of the anti-bacterial sweat cloth, though 10.75%
lower 2o than that of the ordinary sample, does not exceed the allowance of rupture strength for grade A cloth.
See Table 7 for a summary of the results.
Table 7 Results of color fastness and rupture strength tests for sweat cloth treated with composition of the invention Item Ordinary clothAnti-bacteria cloth Color fastness to washingColor change4-5 4 (degree) Color attach4-5 4-5 Color fastness to sweat Color change4-5 4 (degree) Color attach4-5 4-5 Color fastness to rubbingDry rubbing 4-5 4-5 (degree) Wet rubbing 4-5 4-5 Rupture strength (N) 623.2 556.2 Clinical experiments were performed on products created from materials of the invention. The research was performed under the inspection of Special Committee of Chinese Hospital Infection Management, PLA General Hospital (301 Hospital) and Hangzhou Hygiene and Anti-Epidemic Station. The results show that medical textiles of the invention have anti-bacterial ability and is suitable for an application in reducing infection in hospitals.
Results obtained with 100% cotton material are summarized in Tables 8, ~ 5 9, 10 and 11.
Table 8 Experiment operation Item Working Clothes Sheets clothes for for patients medical workers Anti- Non- Anti- Non- Anti- Non-bacteria antibacteribacteriaantibacteribacteriaantibacteri group a group group a group group a group Number 30 30 30 30 30 30 of textile departureRespiratio10 10 10 10 10 10 nt n Digestion- - 20 20 20 20 Ordinary20 20 - - - -surgery Time 7 days 3 days 7 days for using Sampling 10 cm 10 cm Midpoint place left left of the and 10 and midline, cm 10 cm right right 30 cm to 3rd to 2nd left button button and in the in 30 cam front the front right and in and to the the suture in the midpoint.
of left suture Totally lap. of left 3 places.
Totally lap.
places. Totally 3 places.
Sampling 5'S=25cm2 area Sampling The textile method in the corresponding places is cut off by sterilizing scissors.
After broken into pieces, the textile is emerged into 5ml sterilizing salt water, which is contained in test tubes of 1 Oml.
Each sample is put into a different tube.
Cultivation Shake method the samples by the oscillator for 1 min, then extract 0.1 ml with sampling sucker from each tube and cover it uniformly on the blood flat plate which contains 5% sheep blood.
Put the plate in an incubator of 37C
for 24h.
Counting Amount of bacteria of bacteria on textile N (cfu/cm~=[(amount of bacteria on plate n10.1 )'S]/25=2n Results Statistics processing processing by means of't-test' with pairs of data Table 9 Experiment results with working clothes for medical workers in 301 Hospital No. Mean amount of bacteria on the clothes (cfu/cm~
Respiration Ordinary Ordinary department surgery surgery (group (group I) II) An>i- Non- Anti- Non- Anti- Non-bacteria antibacteriabacteria antibacteriabacteria antibacteria group group group group grou p group I 1.3 54.0 0.6 30.0 0.6 153.3 II 0.6 36.7 0.6 105.3 0 44.0 III 0 49.3 0 192.0 0 102.7 IV 0 65.3 0 56.0 0 142.0 V 0 54.0 0 99.3 0 208.7 VI 0 82.0 0 36.0 0 64.7 VII 0 52.0 0 36.0 0 44.7 VIII 0 74.0 0 23.3 0 72.7 IX 0 112.7 0 55.3 0 26.7 X 0 59.3 0 109.3 0 45.3 P value <0.01 <0.01 <0.01 Note: After t-test, on the working clothes for medical workers, the amount of bacteria in anti-bacteria group is greatly lower than that of non-antibacteria group.
Table 10 Experiment results with clothes for patients in 301 Hospital No. Mean amount of bacteria on the clothes (cfu/cm~
Respiratory Digestion Digestion department dept. dept.
(group (group I) II) Anti- Non- Anti- Non- Anti- Non-bacteria antibacteriabacteria antibacteriabacteria antibacteria group group group group group group I 0.6 134.0 3.3 28.0 0.6 104.7 II 0 167.3 0 18.0 0.6 17.3 III 0 64.0 0 29.3 0.6 40.0 IV 0 44.7 0 16.0 0.6 18.0 V 0 146.0 0 74.7 0 13.3 VI 0 90.7 0 14.0 0 18.0 VII 0 68.0 0 26.7 0 154.7 VIII 0 42.0 0 76.7 0 68.7 IX 0 26.7 0 6.7 0 81.3 X 0 185.3 0 18.7 0 44.7 P value <0.01 <0.01 <0.01 Note: After t-test, on the clothes for patients, the amount of bacteria in anti-bacteria group is greatly lower than that of non-antibacteria group.
Table 11 Experiment results with sheets in 301 Hospital No. Mean amount of bacteria on the sheets (cfu/cm~
Respiration Digestion Digestion,dept.
department dept.,(group (group I) II) Anti- Non- Anti- Non- Anti- Non-bacteria antibacteriabacteria antibacteriabacteria antibacteria grou p group group group group group I 0.6 135.3 0.6 48.0 0.6 58.7 I I 1.3 8.7 0.6 13.3 1.3 70.0 I I I 2.0 172.7 0 182.0 0.6 11.3 IV 1.3 80.7 0 28.7 1.3 46.0 V 2.0 12.7 0 192.0 0 4.7 VI 0 78.7 0 47.3 0 30.0 VII 0 8.0 0 23.3 0 163.3 VIII 0 14.7 0 200.0 0 56.0 IX 0 90.0 0 30.0 0 51.3 X 0 68.7 0 23.3 0 104.7 P value <0.01 <0.01 <0.01 Note: After t-test, the amount of bacteria on the sheets in anti-bacteria group is greatly lower than that of non-antibacteria group.
Tests were also performed using anti-bacterial and anti-viral gauze of the invention. Experiments were conducted in conjunction with Hangzhou Hygiene and Anti-Epidemic Station and the 2"d People's Hospital of Hangzhou. Sixty cases were randomly chosen in the surgery area of the hospital, with thirty cases using gauze 2o prepared according to the invention and the other thirty using ordinary gauze as a control. After 3 days, the gauze was sealed into sterilizing bags and sent to Hangzhou Hygiene and Anti-Epidemic Station for checking. Under sterilizing condition, 4 layers of gauze were cut open to check the total amount of bacteria. See Table 12. This indicated that on the test gauze twenty-five of thirty (83%) displayed no bacterial growth, in comparison to control gauze in which 10 (33%) displayed no bacterial growth.
Table 12 Bacteria growth on test gauze bearing composi~on of the invention and ordinary gauze Type of gauze Number of gauze Number of gauze Total with bacteria growth without bacteria (%0 growth (%) Test gauze 5 (16.67) 25 (83.33) 30 Ordinary gauze 20 (66.67) 10 (33.33) 30 Total 25 35 60 (XZ~H = 15.17, P«0.001) Materials of the invention can thus be used for anti-bacterial and anti-viral 1o working clothes for medical workers, patients' clothes, quilts, pillow covers and sheets, mattresses, medical masks and caps, gauze for medical uses, and towels, particularly towels for medical uses.
It is important to note the rate at which materials created according to the invention are effective in their anti-bacterial and anti-viral actions.
1s The anti-bacterial test for Staphylococcus aureus, Escherichia coli and Candida albicans shows that textile and non-woven cloth created according to the present invention have been shown to effectively eliminate bacteria within short period of time, i.e., 10-30 min. This appears to be marked advantage over previous materials produced for the same purpose.
2o Materials created according to the present invention appear to destroy HbsAg. This also, as far as reports known to the inventor are concerned, appears to be another advantage of materials of the present invention over previously known materials.
-17_ The capacity of materials of the present invention to retain their microbiocidal characteristics in the face or repeated washing and aging is also advantageous.
Further, the low toxicity of materials of the present invention, is an s advantage.
Also, materials of the present invention appear to be generally compatible with other aspects of treated materials, as far as strength, color fastness, softeness, absorption characteristics, etc.
In the context of this invention, sheet material includes textiles, which may synthetic or natural, cotton, wool, polyester, etc. and non-woven web-like material, such as extruded materials. It is understood, of course, that the "sheet" may have already been manufactured into an item for use, such as a doctor's smock, a towel, gloves, diapers, etc., prior to application of the antimicrobial composition of the present invention.
~s In the context of this invention, "consisting essentially of means that there are no other components present that markedly alter the desired effect of the required elements, i.e., that the desired role of the required elements is not adversely deprecated by other elements that may be added. References consulted in the preparation of this specification include Textile Technology Abroad,1998, 2:
29-31;
2o Zhang Ling et al . Magazine on Hospital Infection in China, 1997, 7(1 ) :
59; Liu Guangming et al . Chinese Sterilization Magazine, 1993, 10(2): 112-113; Xun Houqin et al. Chinese Sterilization Magazine,1994, 11(2) :126; Mo Zhanlan .Chinese Sterilization Magazine, 1994, 11 (3) : 194; Zhao Jin et al. Magazine on Hospital Infection in China, 1997, 7(1) : 1-3; Lu Xian'e. Magazine on Hospital Infection in China, 1997, 7{2) : 82-84;
2s Bossard CM. International Textile Bulletin, 1995, 41 (4) : 44-48; He Hebo.
Compilation of International Conference on Anti-bacterial Hygiene Finishing Technology, Beijing, 1995, 41 (4) :44-48; Yin Jinduo. Chinese Sterilization Magazine, 1994, 11 (3) :243-244;
Zhang Jie. Chinese Sterilization Magazine, 1994, 11 (4): 244-245; Ding Lanying et al., Chinese Sterilization Magazine, 1997, 14(2) : 84-86; International Textile Development, 1996, 4: 23-24; International Textile Development, 1992, 42(5): 58-61;
International Textile Development,1992, 43(6): 39-43.
All of the reference described in this specification are herein incorporated in their entirety.
The best method and composition of the invention known to the inventor having been described, the scope of protection to be sought for the invention is given below. Of course, a person skilled in the art would be readily capable, given the teachings of this specification to obtain embodiments not precisely described here, but which, nonetheless fall within the scope of the following claims.
Claims (24)
1. A method of manufacturing a sheet of material having antimicrobial properties, which method comprises the steps of:
providing the sheet;
exposing the sheet to a liquid composition comprising a mixture of a quaternary ammonium compound and a polysiloxane;
heating the sheet to fasten an effective amount of the composition to the sheet to impart antimicrobial properties to the sheet.
providing the sheet;
exposing the sheet to a liquid composition comprising a mixture of a quaternary ammonium compound and a polysiloxane;
heating the sheet to fasten an effective amount of the composition to the sheet to impart antimicrobial properties to the sheet.
2. The method of claim 1 wherein the ammonium compound and the polysiloxane are provided separately as a first component and a second component and the components are mixed together just prior to the exposing step.
3. The method of claim 2 wherein the components are mixed together within about 1 hour prior to the exposing step, or within about 30 minutes, or within about 15 minutes, or within about 10 minutes, or within about 5 minutes, or within about 1 minute.
4. The method of any preceding claim wherein the mixture further comprises NaOH
and/or NaCI, wherein the total amount of NaOH and/or NaCI is preferably between about 0.1 and 0.5 percent by mass of the composition applied in the exposing step.
and/or NaCI, wherein the total amount of NaOH and/or NaCI is preferably between about 0.1 and 0.5 percent by mass of the composition applied in the exposing step.
5. The method of any preceding claim wherein the first component consists essentially of an aqueous mixture of said polysiloxane and the polysiloxane is a polyhydrocarbylpolysiloxane containing essentially no hydrolyzable radicals.
6. The method of any preceding claim wherein the polysiloxane is a polyhydrocarbylpolysiloxane that is a polydialkylsiloxane.
7. The method of claim 6 wherein the polydialkylsiloxane is a polydimethylsiloxane.
8. The method of claim 7 where the polydimethylsiloxane has the formula:
where n is between about 600 and about 1200.
where n is between about 600 and about 1200.
9. The method of claim any preceding claim wherein the second component consists essentially of a salt of a quaternary ammonium compound, R4N+, wherein each R
is a hydrocarbon radical.
is a hydrocarbon radical.
10. The method of claim 9 wherein said salt is a halide quaternary ammonium compound, R4N+.
11. The method of claim 10 wherein said quaternary ammonium compound, R4N+, has the formula:
wherein R' is C nH2n+1 for n being an integer of from about 8 to about 18.
wherein R' is C nH2n+1 for n being an integer of from about 8 to about 18.
12. The method of claim 8 wherein said quaternary ammonium compound, R4N+, is dodecyl-dimethyl-benzyl ammonium chloride.
13. The method of any preceding claim, wherein said liquid composition is an aqueous solution obtainable by combining between 0.1 and 0.5 gm of NaOH or NaCI, about ml of the dodecanyl-dimethyl-benzyl-ammonium chloride (I) of the preferred embodiment and 2 ml of the poly(dimethylsiloxane) (II) of the preferred embodiment, wherein the ratio of I:II can be varied between from between about 1:1 and about 1:12.5 (vol:vol) and wherein the composition includes those obtainable by diluting the foregoing solution by up to about 100 fold, or 50 fold, and including about 25 fold, 20 fold, 15 fold, 10 fold and about 5 fold.
14. The method of any preceding claim, wherein said sheet is selected from the group consisting of textiles and non-woven sheet materials.
15. The method of any preceding claim, wherein said sheet is a textile selected from the group consisting of cotton terylene, acrylic and silk.
16. The method of any of claims 1 to 14, wherein said sheet is polyester, cellulose, fabric, nylon, rayon, vinyl, acetate, acrylate, linen, and wool.
17. The method of any preceding claim, wherein said heating step includes a pre-drying in which the textile is exposed to a temperature of up to about 100°C for between about 2 and about 3 minutes.
18. The method of claim 17, wherein said heating step includes a drying step subsequent to the pre-drying step in which the textile is exposed to a temperature of between about 120° and 140°C for between about 20 and about 30 seconds.
19. The method of any preceding claim wherein the exposing step includes soaking the sheet in a reservoir of said liquid composition.
20. A method of manufacturing a sheet of material having antimicrobial properties, which method comprises the steps of:
(a) providing the sheet;
(b) providing a first component consisting essentially of a halide salt of a quaternary ammonium, R4N+, wherein each R is a hydrocarbon radical;
(c) providing a second component consisting essentially of an aqueous solution of a polyhydrocarbylpolysiloxane;
(d) mixing the first and second components such to the proportions set out in claim 13;
(e) providing the mixture of step (d), as needed, with NaCl and/or NaOH to bring the amount of NaCl and/or NaOH to between about 0.1 and about 0.5% of the mass percentage of the final mixture;
(f) providing sufficient water to the mixture, as needed, to bring the overall amount of amount of NaCl and/or NaOH to between about 0.1 and about 0.5% of the composition;
(g) heating the sheet to fasten an effective amount of the composition to the final mixture thereto so as to provide the sheet with antimicrobial properties.
(a) providing the sheet;
(b) providing a first component consisting essentially of a halide salt of a quaternary ammonium, R4N+, wherein each R is a hydrocarbon radical;
(c) providing a second component consisting essentially of an aqueous solution of a polyhydrocarbylpolysiloxane;
(d) mixing the first and second components such to the proportions set out in claim 13;
(e) providing the mixture of step (d), as needed, with NaCl and/or NaOH to bring the amount of NaCl and/or NaOH to between about 0.1 and about 0.5% of the mass percentage of the final mixture;
(f) providing sufficient water to the mixture, as needed, to bring the overall amount of amount of NaCl and/or NaOH to between about 0.1 and about 0.5% of the composition;
(g) heating the sheet to fasten an effective amount of the composition to the final mixture thereto so as to provide the sheet with antimicrobial properties.
21. The method of any preceding claim wherein the sheet is a flexible sheet.
22. A microbiocidal textile finishing composition, comprising:
(a) a first component consisting essentially of a quaternary ammonium compound, R4N+, wherein each R is a hydrocarbon radical;
(b) a second component consisting essentially of an aqueous solution of a polyhydrocarbylpolysiloxane; and (c) a third component selected from the group of NaOH and NaCl.
(a) a first component consisting essentially of a quaternary ammonium compound, R4N+, wherein each R is a hydrocarbon radical;
(b) a second component consisting essentially of an aqueous solution of a polyhydrocarbylpolysiloxane; and (c) a third component selected from the group of NaOH and NaCl.
23. A microbiocidal textile finishing composition comprising at least the components of any composition of defined in any preceding claim.
24. The composition of claim 22 wherein the polyhydrocarbylpolysiloxane contains essentially no hydrolyzable radicals.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA 2283620 CA2283620A1 (en) | 1999-09-27 | 1999-09-27 | Microbiocidal materials and method for manufacturing thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA 2283620 CA2283620A1 (en) | 1999-09-27 | 1999-09-27 | Microbiocidal materials and method for manufacturing thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA2283620A1 true CA2283620A1 (en) | 2001-03-27 |
Family
ID=4164228
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA 2283620 Abandoned CA2283620A1 (en) | 1999-09-27 | 1999-09-27 | Microbiocidal materials and method for manufacturing thereof |
Country Status (1)
| Country | Link |
|---|---|
| CA (1) | CA2283620A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106667164A (en) * | 2016-12-12 | 2017-05-17 | 广西凯喜雅丝绸有限公司 | Method for producing silk cotton quilt |
-
1999
- 1999-09-27 CA CA 2283620 patent/CA2283620A1/en not_active Abandoned
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106667164A (en) * | 2016-12-12 | 2017-05-17 | 广西凯喜雅丝绸有限公司 | Method for producing silk cotton quilt |
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