CN105332077B - Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol fiber and preparation method thereof - Google Patents

Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol fiber and preparation method thereof Download PDF

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CN105332077B
CN105332077B CN201510866590.0A CN201510866590A CN105332077B CN 105332077 B CN105332077 B CN 105332077B CN 201510866590 A CN201510866590 A CN 201510866590A CN 105332077 B CN105332077 B CN 105332077B
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zirconium phosphate
mesoporous zirconium
loading nano
silver
mesoporous
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CN105332077A (en
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朱美芳
周家良
孟思
夏维
孙宾
江晓泽
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Donghua University
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/44Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/50Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyalcohols, polyacetals or polyketals
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/08Melt spinning methods
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • D01F1/103Agents inhibiting growth of microorganisms

Abstract

The invention provides a kind of Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol fiber and preparation method thereof.Described Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol fiber, it is characterised in that including polyvinyl alcohol matrix, Mesoporous zirconium phosphate loading nano silvery antimicrobial powder is dispersed with described polyvinyl alcohol matrix.The preparation method of Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol fiber, including:Described surface is added in the colloidal sol containing silver ion with sulfonic Mesoporous zirconium phosphate, 1~3h is stirred at 20~100 DEG C, obtain silver@Mesoporous zirconium phosphate sol precursors, 2~5h is heated at 200~550 DEG C under nitrogen atmosphere in tube furnace, Ag@Mesoporous zirconium phosphate antimicrobial powders are prepared;By Ag Mesoporous zirconium phosphates antimicrobial powder and polyvinyl alcohol, melt blending, drying at 180~260 DEG C, are most spun into Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol fiber through melt spinning method afterwards.The method of the present invention is simple to operate, efficient, low cost, and effectiveness persistently, has a extensive future.

Description

Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol fiber and preparation method thereof
Technical field
The invention belongs to the preparation field of anti-bacterial fibre, especially a kind of Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol The preparation method of fiber.
Background technology
The special existence micro-loops such as the ecology overall situation severe exacerbation such as today's society extreme environment, environmental pollution, confined space Border causes active demand of the people to function protecting textile.The fiber of textile is prepared at present in itself without antibacterial ability, The environment of existence and breeding is provided back to bacterium under certain condition, human health is threatened.Solve the problems, such as the main of fibre antibacterial Method is to carry out composite modified, preparation changing with antibacterial action with polymeric matrix using the nano-particle with antibacterial action Property fiber.The fiber can progressively discharge antimicrobial component in use, reach the purpose of antibacterial.Current anti-bacterial fibre application is wide General, demand is big, but technology can not effectively solve that function ingredients addition is more, dispersion is difficult, high temperature process is unstable at present, connect Continuous metaplasia produces the low problem of row yielding, causes anti-bacterial fibre to effectively form large-scale production, it is difficult to meet existing market Widespread demand.
At present, realize fiber to have the main method of antibacterial functions is by process for modifying surface and blend modification technology. The former is that the effect for forming chemical bond by antibacterial components and fiber or fabric face makes antibacterial components be attached to fiber or fabric Surface, so as to reach antibacterial action.Patent CN101942759A is that fiber is added in the solution containing silver nitrate to adsorb Silver nitrate in solution, carries out reducing the anti-bacterial fibre or fabric for obtaining surface attachment silver in the fiber after to absorption.Should Method can not form the antimicrobial coating of stable homogeneous, and antibacterial time is limited, it is impossible to reach durable antibiotic.Whole process is excessively multiple It is miscellaneous that pollution easily is produced to environment.The latter be then by antibacterial components it is direct or it is modified be added in polymer, by screw rod squeeze Go out to prepare antibacterial matrices, anti-bacterial fibre is being prepared by melt spinning technology.Patent CN101440533 is by bamboo charcoal nano and receives Meter Yin Wei antibacterial components, with the one kind in terylene or polypropylene fibre or polyamide fibre as carrier slice, anti-bacterial fibre are prepared by Screw Extrusion. But the method, addition is larger, antibacterial components skewness, is difficult to realize continuous prodution.
The content of the invention
And the antibacterial polyethylene alcohol fiber that is evenly distributed small it is an object of the invention to provide a kind of antibacterial components addition and Its preparation method.
In order to achieve the above object, it is fine the invention provides a kind of Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol Dimension, it is characterised in that including polyvinyl alcohol matrix, Mesoporous zirconium phosphate loading nano silvery is dispersed with described polyvinyl alcohol matrix Antimicrobial powder.
Preferably, size of the described Mesoporous zirconium phosphate loading nano silvery antimicrobial powder in polyvinyl alcohol matrix be 200~700nm.
Preferably, described Mesoporous zirconium phosphate loading nano silvery antimicrobial powder and the mass ratio 0.5 of polyvinyl alcohol matrix: 99.5~3: 97.
Present invention also offers the preparation method of above-mentioned Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol fiber, its It is characterised by, specific steps include:
The first step:Surface is obtained with sulfonic Mesoporous zirconium phosphate using oleum treatment Mesoporous zirconium phosphate, by silver Ionic compound and dihydroxylic alcohols stirring ultrasound, obtain the colloidal sol containing silver ion, by described surface with sulfonic mesoporous Basic zirconium phosphate is added in the colloidal sol containing silver ion, and 1~3h is stirred at 20~100 DEG C, before obtaining silver@Mesoporous zirconium phosphate colloidal sols Body is driven, 2~5h is heated at 200~550 DEG C under nitrogen atmosphere in tube furnace, Ag@Mesoporous zirconium phosphate antimicrobial powders are prepared;
Second step:By Ag@Mesoporous zirconium phosphates antimicrobial powders and polyvinyl alcohol at 180~260 DEG C melt blending, dry, Most it is spun into Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol fiber through melt spinning method afterwards.
Preferably, described utilization oleum processes concretely comprising the following steps for Mesoporous zirconium phosphate:The quality of oleum point Number is 50%~98%, and reaction temperature is 40~80 DEG C, 20~80min of reaction time..
Preferably, the size of described Ag@Mesoporous zirconium phosphate antimicrobial powders is in 200~700nm.
Preferably, described surface is with sulfonic Mesoporous zirconium phosphate, silver iron compound and dihydroxylic alcohols mass ratio 60~90: 0.5~5: 5~39.5.
Preferably, described silver iron compound is silver chlorate, silver bromide, silver iodide, silver hydroxide, silver sulfide and sulfuric acid One or more in silver.
Preferably, described dihydroxylic alcohols is one or more in ethylene glycol, propane diols, butanediol and isobide.
The present invention forms colloidal sol by the use of the compound containing silver as antibacterial components presoma by with dihydroxylic alcohols, utilizes The duct suction-operated of sulfonated Mesoporous zirconium phosphate and sulfonic group are acted on the ionic bond of silver ion, make Mesoporous zirconium phosphate duct With the equal load silver ion in surface, Ag@Mesoporous zirconium phosphate antimicrobial powders are obtained after tube furnace, by organic inorganic hybridization technology system Standby polyvinyl alcohol antimicrobial composite material.
Compared with prior art, the beneficial effects of the invention are as follows:
(1) the duct suction-operated of the Mesoporous zirconium phosphate of sulfonation and sulfonic group are made with the ionic bond of silver ion in the present invention With, make Mesoporous zirconium phosphate duct and the equal load silver ion in surface, realize pay(useful) load of the silver ion in Mesoporous zirconium phosphate.
(2) intermediary hole basic zirconium phosphate load silver ion of the present invention, Nano Silver Mesoporous zirconium phosphate is generated after being acted on through thermal reduction, is led to Crossing mesoporous suction-operated can effectively realize the sustained release of function ingredients, and effectiveness is lasting.
(3) method of the present invention is simple to operate, efficient, low cost, and effectiveness persistently, has a extensive future.It is prepared by the present invention Anti-bacterial fibre can effectively apply in mouth mask, the interior trim such as household textiles, clothes, big aircraft, high ferro, spacefarer's dress ornament, army With fields such as fighting uniform decorations.Domestic anti-bacterial fibre technology of preparing can effectively be filled up by the industrialization of anti-bacterial fibre of the present invention Blank.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content for having read instruction of the present invention, people in the art Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited Scope.Mesoporous zirconium phosphate nano-powder in various embodiments of the present invention is commercially available prod, and particle diameter is 100-700nm, and aperture is 10-60nm。
Embodiment 1
A kind of Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol fiber, including polyvinyl alcohol matrix, described poly- second Mesoporous zirconium phosphate loading nano silvery antimicrobial powder is dispersed with enol matrix.
The preparation method of above-mentioned Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol fiber, concretely comprises the following steps:
(1) surface is obtained with sulfonic Mesoporous zirconium phosphate using oleum treatment Mesoporous zirconium phosphate, using smoke Sulfuric acid treatment Mesoporous zirconium phosphate is concretely comprised the following steps:Mass fraction is 98% oleum and Mesoporous zirconium phosphate mass ratio is 10 : 1,40 DEG C of reaction temperature reacts 20min.
(2) silver nitrate, ethylene glycol and surface that mass ratio is 0.5: 39.5: 60 are taken with sulfonic Mesoporous zirconium phosphate, It is 400rpm, ultrasonic (frequency 35KHZ, power output 80%) first to add silver nitrate and the ultrasonic rotating speed of ethylene glycol stirring at normal temperatures 2h, obtains the colloidal sol containing silver ion, described surface is added to sulfonic Mesoporous zirconium phosphate and contains silver ion In colloidal sol, 2h is stirred at 30 DEG C, silver@Mesoporous zirconium phosphate sol precursors are obtained, at 500 DEG C under nitrogen atmosphere in tube furnace Lower heating 3h, prepares Ag@Mesoporous zirconium phosphate antimicrobial powders, and size is in 200~700nm;
(3) by Ag@Mesoporous zirconium phosphates antimicrobial powders and polyvinyl alcohol (alcoholysis degree be 88%, intrinsic viscosity be 0.36dl/g, The degree of polymerization be 450) in mass ratio for 3: 97 at 200 DEG C melt blending prepare Ag@Mesoporous zirconium phosphate antibacterial compound slices, do Dry, control moisture content, through melt spinning method, at 205~215 DEG C, is spun into Mesoporous zirconium phosphate load in 50~100ppm Nanometer silver antimicrobial vinal.The fiber to the antibiotic rate > 90% of Escherichia coli, to the antibacterial of staphylococcus aureus Rate > 90%, to the antibiotic rate > 65% of Candida albicans.The water-fastness number of times > of fabric 100 times.
Embodiment 2
A kind of Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol fiber, including polyvinyl alcohol matrix, described poly- second Mesoporous zirconium phosphate loading nano silvery antimicrobial powder is dispersed with enol matrix.
The preparation method of above-mentioned Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol fiber, concretely comprises the following steps:
(1) surface is obtained with sulfonic Mesoporous zirconium phosphate using oleum treatment Mesoporous zirconium phosphate, using smoke Sulfuric acid treatment Mesoporous zirconium phosphate is concretely comprised the following steps:Mass fraction is 50% oleum and Mesoporous zirconium phosphate mass ratio is 10 : 1,40 DEG C of reaction temperature reacts 80min.
(2) silver sulfate, propane diols and surface that mass ratio is 0.5: 5: 94.5 are taken with sulfonic Mesoporous zirconium phosphate, It is 300rpm, ultrasonic (frequency 35KHZ, power output 100%) that silver sulfate and the ultrasonic rotating speed of propane diols stirring are first added under normal temperature 1h, obtains the colloidal sol containing silver ion, described surface is added to sulfonic Mesoporous zirconium phosphate and contains silver ion In colloidal sol, 1h is stirred at 80 DEG C, silver@Mesoporous zirconium phosphate sol precursors are obtained, at 550 DEG C under nitrogen atmosphere in tube furnace Lower heating 2h, prepares Ag@Mesoporous zirconium phosphate antimicrobial powders, and size is in 200~700nm;
(3) by Ag@Mesoporous zirconium phosphates antimicrobial powders and polyvinyl alcohol, (alcoholysis degree is that 88.5%, intrinsic viscosity is 0.53dl/ G, the degree of polymerization for 780) in mass ratio for 3: 97 at 220 DEG C melt blending prepare Ag@Mesoporous zirconium phosphate antibacterial compound slices, do Dry, control moisture content, through melt spinning method, at 215~230 DEG C, is spun into Mesoporous zirconium phosphate load in 50~100ppm Nanometer silver antimicrobial vinal.The fiber to the antibiotic rate > 90% of Escherichia coli, to the antibacterial of staphylococcus aureus Rate > 90%, to the antibiotic rate > 65% of Candida albicans.The water-fastness number of times > of fabric 100 times.
Embodiment 3
A kind of Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol fiber, including polyvinyl alcohol matrix, described poly- second Mesoporous zirconium phosphate loading nano silvery antimicrobial powder is dispersed with enol matrix.
The preparation method of above-mentioned Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol fiber, concretely comprises the following steps:
(1) surface is obtained with sulfonic Mesoporous zirconium phosphate using oleum treatment Mesoporous zirconium phosphate, using smoke Sulfuric acid treatment Mesoporous zirconium phosphate is concretely comprised the following steps:Mass fraction is 80% oleum and Mesoporous zirconium phosphate mass ratio is 20 : 1,50 DEG C of reaction temperature reacts 60min.
(2) silver nitrate, isobide and surface that mass ratio is 5: 39.5: 54.5 are taken and carries sulfonic mesoporous phosphoric acid Zirconium, it is 300rpm that silver nitrate and the ultrasonic rotating speed of isobide stirring are first added at normal temperatures, ultrasonic (frequency 53KHZ, power output 50%) 1h, obtains the colloidal sol containing silver ion, by described surface with sulfonic Mesoporous zirconium phosphate be added to containing silver from In the colloidal sol of son, stir 3h at 40 DEG C, obtain silver@Mesoporous zirconium phosphate sol precursors, under nitrogen atmosphere in tube furnace 4h is heated at 300 DEG C, Ag@Mesoporous zirconium phosphate antimicrobial powders are prepared, size is in 200~700nm;
(3) by Ag@Mesoporous zirconium phosphates antimicrobial powders and polyvinyl alcohol, (alcoholysis degree is that 95.5%, intrinsic viscosity is 0.84dl/ G, the degree of polymerization for 1550) in mass ratio for 0.5: 99.5 at 210 DEG C melt blending prepare that Ag@Mesoporous zirconium phosphates antibacterials is compound to cut Piece, dries, and control moisture content, through melt spinning method, at 220~230 DEG C, is spun into Mesoporous zirconium phosphate in 50~100ppm Loading nano silvery antibacterial polyethylene alcohol fiber.The fiber to the antibiotic rate > 95% of Escherichia coli, to staphylococcus aureus Antibiotic rate > 95%, to the antibiotic rate > 75% of Candida albicans.The water-fastness number of times > of fabric 80 times.
Embodiment 4
A kind of Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol fiber, including polyvinyl alcohol matrix, described poly- second Mesoporous zirconium phosphate loading nano silvery antimicrobial powder is dispersed with enol matrix.
The preparation method of above-mentioned Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol fiber, concretely comprises the following steps:
(1) surface is obtained with sulfonic Mesoporous zirconium phosphate using oleum treatment Mesoporous zirconium phosphate, using smoke Sulfuric acid treatment Mesoporous zirconium phosphate is concretely comprised the following steps:Mass fraction is 98% oleum and Mesoporous zirconium phosphate mass ratio is 10 : 1,80 DEG C of reaction temperature reacts 40min.
(2) silver sulfate, isobide and surface that mass ratio is 5: 5: 90 are taken with sulfonic Mesoporous zirconium phosphate, normal It is 200rpm, ultrasonic (frequency 53KHZ, power output 70%) that silver sulfate and the ultrasonic rotating speed of isobide stirring are first added under temperature 1.5h, obtains the colloidal sol containing silver ion, described surface is added to sulfonic Mesoporous zirconium phosphate and contains silver ion Colloidal sol in, stir 2h at 50 DEG C, silver@Mesoporous zirconium phosphate sol precursors are obtained, 300 under nitrogen atmosphere in tube furnace 4h is heated at DEG C, Ag@Mesoporous zirconium phosphate antimicrobial powders are prepared, size is in 200~700nm;
(3) by Ag@Mesoporous zirconium phosphates antimicrobial powders and polyvinyl alcohol, (alcoholysis degree is that 98.3%, intrinsic viscosity is 0.50dl/ G, the degree of polymerization for 750) in mass ratio for 0.5: 99.5 at 230 DEG C melt blending prepare that Ag@Mesoporous zirconium phosphates antibacterials is compound to cut Piece, dries, and control moisture content, through melt spinning method, at 225~240 DEG C, is spun into Mesoporous zirconium phosphate in 50~100ppm Loading nano silvery antibacterial polyethylene alcohol fiber.The fiber to the antibiotic rate > 98% of Escherichia coli, to staphylococcus aureus Antibiotic rate > 95%, to the antibiotic rate > 75% of Candida albicans.The water-fastness number of times > of fabric 80 times.
Embodiment 5
A kind of Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol fiber, including polyvinyl alcohol matrix, described poly- second Mesoporous zirconium phosphate loading nano silvery antimicrobial powder is dispersed with enol matrix.
The preparation method of above-mentioned Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol fiber, concretely comprises the following steps:
(1) surface is obtained with sulfonic Mesoporous zirconium phosphate using oleum treatment Mesoporous zirconium phosphate, using smoke Sulfuric acid treatment Mesoporous zirconium phosphate is concretely comprised the following steps:Mass fraction is 75% oleum and Mesoporous zirconium phosphate mass ratio is 20 : 1,40 DEG C of reaction temperature reacts 80min.
(2) silver chlorate, ethylene glycol and surface that mass ratio is 0.5: 39.5: 60 are taken with sulfonic Mesoporous zirconium phosphate, It is 400rpm first to add silver chlorate and the ultrasonic rotating speed of ethylene glycol stirring at normal temperatures, ultrasonic (frequency 53KHZ, power output 100%) 2h, obtains the colloidal sol containing silver ion, described surface is added to sulfonic Mesoporous zirconium phosphate and contains silver In the colloidal sol of ion, 2h is stirred at 75 DEG C, silver@Mesoporous zirconium phosphate sol precursors are obtained, under nitrogen atmosphere in tube furnace 5h is heated at 250 DEG C, Ag@Mesoporous zirconium phosphate antimicrobial powders are prepared, size is in 200~700nm;
(3) by Ag@Mesoporous zirconium phosphates antimicrobial powders and polyvinyl alcohol, (alcoholysis degree is that 99.7%, intrinsic viscosity is 0.71dl/ G, the degree of polymerization for 1210) in mass ratio for 2: 98 at 230 DEG C melt blending prepare Ag@Mesoporous zirconium phosphate antibacterial compound slices, Dry, control moisture content, through melt spinning method, at 230~245 DEG C, is spun into Mesoporous zirconium phosphate and bears in 50~100ppm Carrying nano silver antibacterial polyethylene alcohol fiber.The fiber resists to the antibiotic rate > 95% of Escherichia coli to staphylococcus aureus Bacterium rate > 92%, to the antibiotic rate > 70% of Candida albicans.The water-fastness number of times > of fabric 100 times.

Claims (7)

1. a kind of preparation method of Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol fiber, described Mesoporous zirconium phosphate load Nanometer silver antimicrobial vinal, including polyvinyl alcohol matrix, Mesoporous zirconium phosphate is dispersed with described polyvinyl alcohol matrix Loading nano silvery antimicrobial powder, it is characterised in that specific steps include:
The first step:Surface is obtained with sulfonic Mesoporous zirconium phosphate using oleum treatment Mesoporous zirconium phosphate, by silver ion Compound and dihydroxylic alcohols stirring ultrasound, obtain the colloidal sol containing silver ion, and described surface is carried into sulfonic mesoporous phosphoric acid Zirconium is added in the colloidal sol containing silver ion, and 1~3h is stirred at 20 ~ 100 DEG C, obtains silver@Mesoporous zirconium phosphate sol precursors, 2 ~ 5h is heated at 200 ~ 550 DEG C under nitrogen atmosphere in tube furnace, Ag@Mesoporous zirconium phosphate antimicrobial powders are prepared;
Second step:By Ag Mesoporous zirconium phosphates antimicrobial powder and polyvinyl alcohol, melt blending, drying at 180 ~ 260 DEG C, most pass through afterwards Melt spinning method is spun into Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol fiber.
2. the preparation method of Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol fiber as claimed in claim 1, its feature It is, the mass ratio 0.5 of described Mesoporous zirconium phosphate loading nano silvery antimicrobial powder and polyvinyl alcohol matrix: 99.5~3 : 97。
3. the preparation method of Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol fiber as claimed in claim 1, its feature It is that described utilization oleum processes concretely comprising the following steps for Mesoporous zirconium phosphate:The mass fraction of oleum be 50% ~ 98%, reaction temperature is 40 ~ 80 DEG C, the min of reaction time 20 ~ 80.
4. the preparation method of Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol fiber as claimed in claim 1, its feature It is that the size of described Ag@Mesoporous zirconium phosphate antimicrobial powders is in 200 ~ 700 nm.
5. the preparation method of Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol fiber as claimed in claim 1, its feature It is that described surface is 60 ~ 90 with sulfonic Mesoporous zirconium phosphate, silver iron compound and dihydroxylic alcohols mass ratio: 0.5 ~ 5 : 5~39.5。
6. the preparation method of Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol fiber as claimed in claim 1, its feature It is that described silver iron compound is the one kind in silver chlorate, silver bromide, silver iodide, silver hydroxide, silver sulfide and silver sulfate Or it is several.
7. the preparation method of Mesoporous zirconium phosphate loading nano silvery antibacterial polyethylene alcohol fiber as claimed in claim 1, its feature It is that described dihydroxylic alcohols is one or more in ethylene glycol, propane diols, butanediol and isobide.
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Publication number Priority date Publication date Assignee Title
JP2007077519A (en) * 2005-09-13 2007-03-29 Mitsui Chemicals Inc Antimicrobial aggregate of fiber, method for producing the same and its application
CN101305735A (en) * 2007-05-16 2008-11-19 上海松明寄存设备有限公司 Ag-carrying nano antibiotic material and its preparation method and use
CN101363141A (en) * 2007-08-09 2009-02-11 太仓市金辉化纤实业有限公司 Full light extinction and antibiotic polyester fiber, preparation method and application thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007077519A (en) * 2005-09-13 2007-03-29 Mitsui Chemicals Inc Antimicrobial aggregate of fiber, method for producing the same and its application
CN101305735A (en) * 2007-05-16 2008-11-19 上海松明寄存设备有限公司 Ag-carrying nano antibiotic material and its preparation method and use
CN101363141A (en) * 2007-08-09 2009-02-11 太仓市金辉化纤实业有限公司 Full light extinction and antibiotic polyester fiber, preparation method and application thereof

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