CN105386147B - A kind of Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro and preparation method thereof - Google Patents
A kind of Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro and preparation method thereof Download PDFInfo
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- CN105386147B CN105386147B CN201510866530.9A CN201510866530A CN105386147B CN 105386147 B CN105386147 B CN 105386147B CN 201510866530 A CN201510866530 A CN 201510866530A CN 105386147 B CN105386147 B CN 105386147B
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- zirconium phosphate
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- Chemical Or Physical Treatment Of Fibers (AREA)
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Abstract
The invention provides a kind of Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro and preparation method thereof.Described Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro, it is characterised in that including polyamide substrate, is dispersed with Ag@Mesoporous zirconium phosphate antimicrobial powders in described polyamide substrate.Its preparation method includes：Prepare Ag@Mesoporous zirconium phosphate antimicrobial powders；The raw material for including above-mentioned Ag@Mesoporous zirconium phosphates antimicrobial powders and polyamide reaction monomer is added in polyamide reaction device to carry out in-situ polymerization and prepares Mesoporous zirconium phosphate nanometer silver antimicrobial composite, dry, be most spun into Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro 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
Technical field
The invention belongs to the preparation field of anti-bacterial fibre, especially a kind of Mesoporous zirconium phosphate loading nano silvery antibacterial polyamide is fine
Dimension and preparation method thereof.
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 Fypro 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, the invention provides a kind of Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro,
It is characterised in that it includes polyamide substrate, is dispersed with Ag@Mesoporous zirconium phosphate antimicrobial powders in described polyamide substrate.
Preferably, the size of described Ag@Mesoporous zirconium phosphate antimicrobial powders is 200~700nm.
Preferably, described Ag@Mesoporous zirconium phosphates antimicrobial powders are 0.5 with the mass ratio of polyamide substrate:99.5~3:
97。
Preferably, described polyamide substrate is polycaprolactam, PA 66, poly- 11 lactams, poly- ten
Two lactams, polyhexamethylene sebacamide, the formyl hexamethylene diamine of poly- dodecane two, nylon 1010 and poly hexamethylene adipamide isophthalic diformazan
One kind in amine.
Present invention also offers the preparation method of above-mentioned Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro, it is special
Levy and be, including：
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：The raw material for including above-mentioned Ag@Mesoporous zirconium phosphates antimicrobial powders and polyamide reaction monomer is added to
In-situ polymerization is carried out in polyamide reaction device and prepares Mesoporous zirconium phosphate-nanometer silver antimicrobial composite, dried, most spun through melting afterwards
Silk method is spun into Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro.
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, 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.
Preferably, the course of reaction of described home position polymerization reaction be 220~240 DEG C, 1~3h of open loop under 0.5Mpa,
250~280 DEG C of 3~6h of polycondensation reaction；Or reacted under 230~270 DEG C, the protection of 1.70Mpa nitrogen into salt at 50~90 DEG C
2~6h.
Anti-bacterial fibre prepared by the inventive method is on the basis of being polymerized based on conventional polyamide, using the compound for containing silver
As antibacterial components presoma, colloidal sol is formed by with dihydroxylic alcohols, using the duct suction-operated of sulfonated Mesoporous zirconium phosphate
Ionic bond with sulfonic group and silver ion is acted on, and makes Mesoporous zirconium phosphate duct and the equal load silver ion in surface, is obtained after tube furnace
Ag@Mesoporous zirconium phosphate antimicrobial powders are obtained, is added in polymerization system, it is mesoporous to prepare Ag@in polymerization process situ
Basic zirconium phosphate/nylon 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 loading nano silvery of the present invention, addition in situ, realizes antibacterial functions component in the course of the polymerization process
Fine dispersion in the base.
(3) present invention prepares the section of silver-loaded zirconium phosphate antibacterial polyamide, function nano particle by the way of in-situ polymerization
In polymerization and processing link, stable performance nondiscolouring.
(4) 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 Fypro, including polyamide substrate (polycaprolactam), institute
Ag@Mesoporous zirconium phosphate antimicrobial powders are dispersed with the polyamide substrate stated.The size of described Ag@Mesoporous zirconium phosphate antimicrobial powders
Size is 200~400nm.Described Ag@Mesoporous zirconium phosphates antimicrobial powders are 3 with the mass ratio of polyamide substrate:97.
The preparation method of above-mentioned Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro is：
(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) it is 0.5 to take mass ratio:39.5:60 silver nitrate, ethylene glycol and surface carry 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, obtain silver@Mesoporous zirconium phosphate sol precursors；At 500 DEG C under nitrogen atmosphere in tube furnace
Lower heating 3h, prepares Ag@Mesoporous zirconium phosphate antimicrobial powders, and size is in 200~400nm；
(3) by above-mentioned cupric oxide@Mesoporous zirconium phosphates Gel Precursor and caprolactam in mass ratio 3:97 are added to polyamides
Using in-situ polymerization, (220~240 DEG C, open loop 3h under 0.5Mpa, polycondensation reaction react 3h at 280 DEG C in amine reactor.) prepare
Mesoporous zirconium phosphate-nanometer silver antimicrobial compound slice, dries, and controls moisture content at 50~100ppm (mass content), through melting
Spin processes, at 250~275 DEG C, are spun into Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro.The fiber is to large intestine bar
The antibiotic rate ＞ 95% of bacterium, to the antibiotic rate ＞ 90% of staphylococcus aureus, to the antibiotic rate ＞ 60% of Candida albicans.Knit
The water-fastness number of times ＞ of thing 100 times.
Embodiment 2
A kind of Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro, including polyamide substrate (polycaprolactam), institute
Ag@Mesoporous zirconium phosphate antimicrobial powders are dispersed with the polyamide substrate stated.The size of described Ag@Mesoporous zirconium phosphate antimicrobial powders
Size is 400~700nm.Described Ag@Mesoporous zirconium phosphates antimicrobial powders are 3 with the mass ratio of polyamide substrate:97.
The preparation method of above-mentioned Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro is：
(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) it is 0.5 to take mass ratio:5:94.5 silver sulfate, propane diols and surface carry 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, obtain silver@Mesoporous zirconium phosphate sol precursors；At 550 DEG C under nitrogen atmosphere in tube furnace
Lower heating 2h, prepares Ag@Mesoporous zirconium phosphate antimicrobial powders, and size is in 400~700nm；
(3) in mass ratio it is 5 by above-mentioned cupric oxide@Mesoporous zirconium phosphates Gel Precursor and caprolactam:95 be added to it is poly-
Using in-situ polymerization, (220~240 DEG C, open loop 3h under 0.5Mpa, polycondensation reaction react 3h at 280 DEG C in acid amides reactor.) system
Standby Mesoporous zirconium phosphate-nanometer silver antimicrobial compound slice, dries, and controls moisture content at 50~100ppm (mass content), through molten
Melt spin processes (spinning temperature is 260~285 DEG C) and be spun into Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro.The fiber
To the antibiotic rate ＞ 98% of Escherichia coli, to the antibiotic rate ＞ 91% of staphylococcus aureus, to the antibiotic rate of Candida albicans
＞ 70%.The water-fastness number of times ＞ of fabric 100 times.
Embodiment 3
A kind of Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro, including polyamide substrate (polyadipate oneself two
Amine), Ag@Mesoporous zirconium phosphate antimicrobial powders are dispersed with described polyamide substrate.Described Ag@Mesoporous zirconium phosphate antimicrobial powders
Size be 500~700nm.Described Ag@Mesoporous zirconium phosphates antimicrobial powders are 0.5 with the mass ratio of polyamide substrate:
99.5。
The preparation method of above-mentioned Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro is：
(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) it is 5 to take mass ratio:39.5:54.5 silver nitrate, isobide and surface carry 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, 2h is stirred at 80 DEG C, obtain silver@Mesoporous zirconium phosphate sol precursors；Under nitrogen atmosphere in tube furnace
2h is heated at 500 DEG C, Ag@Mesoporous zirconium phosphate antimicrobial powders are prepared, size is in 500~700nm；
(3) in mass ratio it is 2 by above-mentioned cupric oxide@Mesoporous zirconium phosphates Gel Precursor, adipic acid and hexamethylene diamine:49:49
It is proportionally added into (into salt at 75~80 DEG C, being protected in 240 DEG C, 1.70Mpa nitrogen using in-situ polymerization in polyamide reaction device
The lower reaction 3h of shield) Mesoporous zirconium phosphate-nanometer silver antimicrobial compound slice is prepared, dry, control moisture content is in 50~100ppm (quality
Content) when, Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro is spun at 275~290 DEG C through melt spinning method.Should
Fiber, to the antibiotic rate ＞ 88% of staphylococcus aureus, resists to the antibiotic rate ＞ 90% of Escherichia coli to Candida albicans
Bacterium rate ＞ 65%.The water-fastness number of times ＞ of fabric 100 times.
Embodiment 4
A kind of Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro, including polyamide substrate (polyadipate oneself two
Amine), Ag@Mesoporous zirconium phosphate antimicrobial powders are dispersed with described polyamide substrate.Described Ag@Mesoporous zirconium phosphate antimicrobial powders
Size be 200~450nm.Described Ag@Mesoporous zirconium phosphates antimicrobial powders are 0.5 with the mass ratio of polyamide substrate:
99.5。
The preparation method of above-mentioned Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro is：
(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) it is 5 to take mass ratio:39.5:54.5 silver sulfate, isobide and surface carry sulfonic mesoporous phosphoric acid
Zirconium, it is 200rpm that silver sulfate and the ultrasonic rotating speed of isobide stirring are first added at normal temperatures, ultrasonic (frequency 53KHZ, power output
70%) 1.5h, 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 50 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 200~450nm；
(3) in mass ratio it is 5 by above-mentioned cupric oxide@Mesoporous zirconium phosphates Gel Precursor, adipic acid and hexamethylene diamine:47.5:
47.5 are added in polyamide reaction device and (into salt at 75~80 DEG C, are protected in 250 DEG C, 1.70Mpa nitrogen using in-situ polymerization
Lower reaction 2h) Mesoporous zirconium phosphate-nanometer silver antimicrobial compound slice is prepared, dry, in 50~100ppm, (quality contains control moisture content
Amount) when, through melt spinning method, Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro is spun at 280~295 DEG C.Should
Fiber, to the antibiotic rate ＞ 90% of staphylococcus aureus, resists to the antibiotic rate ＞ 90% of Escherichia coli to Candida albicans
Bacterium rate ＞ 65%.The water-fastness number of times ＞ of fabric 100 times.
Embodiment 5
A kind of Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro, including polyamide substrate (polycaprolactam), institute
Ag@Mesoporous zirconium phosphate antimicrobial powders are dispersed with the polyamide substrate stated.The size of described Ag@Mesoporous zirconium phosphate antimicrobial powders
Size is 400~700nm.Described Ag@Mesoporous zirconium phosphates antimicrobial powders are 2 with the mass ratio of polyamide substrate:98.
The preparation method of above-mentioned Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro is：
(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) it is 0.5 to take mass ratio:39.5:60 silver nitrate, butanediol and surface carry sulfonic Mesoporous zirconium phosphate,
It is 400rpm first to add silver nitrate and the ultrasonic rotating speed of butanediol stirring at normal temperatures, ultrasonic (frequency 35KHZ, 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, obtain silver@Mesoporous zirconium phosphate sol precursors；Under nitrogen atmosphere in tube furnace
5h is heated at 250 DEG C, Ag@Mesoporous zirconium phosphate antimicrobial powders are prepared, size is in 400~700nm；
(3) in mass ratio it is 1 by above-mentioned cupric oxide@Mesoporous zirconium phosphates Gel Precursor and caprolactam:99 be added to it is poly-
Prepared using in-situ polymerization (230~245 DEG C, open loop 2h under 0.5Mpa, polycondensation reaction react 4h at 280 DEG C) in acid amides reactor
Mesoporous zirconium phosphate-nanometer silver antimicrobial compound slice, dries, and controls moisture content at 50~100ppm (mass content), through melting
Spin processes, at 250~265 DEG C, are spun into Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro.The fiber is to large intestine bar
The antibiotic rate ＞ 99% of bacterium, to the antibiotic rate ＞ 95% of staphylococcus aureus, to the antibiotic rate ＞ 70% of Candida albicans.Knit
The water-fastness number of times ＞ of thing 80 times.
Claims (9)
1. a kind of preparation method of Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro, described Mesoporous zirconium phosphate load is received
The silver-colored antibacterial Fypro of rice, including polyamide substrate, are dispersed with Ag@Mesoporous zirconium phosphate antibacterial powders in described polyamide substrate
Body, it is characterised in that including：
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：The raw material for including above-mentioned Ag@Mesoporous zirconium phosphates antimicrobial powders and polyamide reaction monomer is added to polyamides
In-situ polymerization is carried out in amine reactor and prepares Mesoporous zirconium phosphate-nanometer silver antimicrobial composite, dried, most afterwards through melt spinning method
It is spun into Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro.
2. the preparation method of Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro as claimed in claim 1, its feature exists
In the size of described Ag@Mesoporous zirconium phosphate antimicrobial powders is 200 ~ 700 nm.
3. the preparation method of Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro as claimed in claim 1, its feature exists
In described Ag@Mesoporous zirconium phosphates antimicrobial powders and the mass ratio of polyamide substrate is 0.5: 99.5~3 : 97.
4. the preparation method of Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro as claimed in claim 1, its feature exists
In described polyamide substrate is polycaprolactam, PA 66, poly- 11 lactams, nylon 12, the poly- last of the ten Heavenly stems
One kind in two acyl hexamethylene diamines, the formyl hexamethylene diamine of poly- dodecane two, nylon 1010 and poly-meta-xylylene adipamide.
5. the preparation method of Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro as claimed in claim 1, its feature exists
In described utilization oleum processes concretely comprising the following steps for Mesoporous zirconium phosphate：The mass fraction of oleum is 50% ~ 98%,
Reaction temperature is 40 ~ 80 DEG C, the min of reaction time 20 ~ 80.
6. the preparation method of Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro as claimed in claim 1, its feature exists
In described surface is 60 ~ 90 with sulfonic Mesoporous zirconium phosphate, silver iron compound and dihydroxylic alcohols mass ratio: 0.5 ~
5 : 5~39.5。
7. the preparation method of Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro as claimed in claim 1, its feature exists
In, described silver iron compound for the one kind in silver chlorate, silver bromide, silver iodide, silver hydroxide, silver sulfide and silver sulfate or
It is several.
8. the preparation method of Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro as claimed in claim 1, its feature exists
In described dihydroxylic alcohols is one or more in ethylene glycol, propane diols, butanediol and isobide.
9. the preparation method of Mesoporous zirconium phosphate loading nano silvery antibacterial Fypro as claimed in claim 1, its feature exists
In the course of reaction of, described home position polymerization reaction be 220 ~ 240 DEG C, 1 ~ 3h of open loop under 0.5Mpa, it is anti-in 250 ~ 280 DEG C of polycondensations
Answer 3 ~ 6h；Or react 2 ~ 6h under 230 ~ 270 DEG C, the protection of 1.70Mpa nitrogen into salt at 50 ~ 90 DEG C.
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| CN112704292A (en) * | 2021-02-01 | 2021-04-27 | 高守垒 | Preparation method of antibacterial breathable mask |
| CN113062005B (en) * | 2021-03-25 | 2022-11-25 | 嘉兴学院 | Method for preparing antibacterial polyamide fiber by in-situ polymerization |
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| JP2007077519A (en) * | 2005-09-13 | 2007-03-29 | Mitsui Chemicals Inc | Antimicrobial aggregate of fiber, method for producing the same and its application |
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| 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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Application publication date: 20160309 Assignee: Jiangsu Wenfeng Chemical Fiber Group Co., Ltd. Assignor: Donghua University Contract record no.: 2019310000032 Denomination of invention: Mesoporous zirconium phosphate-loaded nanosilver antibacterial polyamide fiber and preparation method thereof Granted publication date: 20170630 License type: Exclusive License Record date: 20190417 |
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