CN105350111B - A kind of Mesoporous zirconium phosphate loads the preparation method of nano cupric oxide antibacterial polyester fibre - Google Patents
A kind of Mesoporous zirconium phosphate loads the preparation method of nano cupric oxide antibacterial polyester fibre Download PDFInfo
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Abstract
The invention provides the preparation method that a kind of Mesoporous zirconium phosphate loads nano cupric oxide antibacterial polyester fibre, it is characterised in that specific steps include：The first step：Prepare cupric oxide@Mesoporous zirconium phosphate Gel Precursors；Second step：Granulation is blended in above-mentioned cupric oxide Mesoporous zirconium phosphate Gel Precursor and polyester at 180~270 DEG C, and is dried, most Mesoporous zirconium phosphate loaded copper oxide antibacterial polyester fibre is spun into through melt spinning method afterwards；Or, above-mentioned cupric oxide@Mesoporous zirconium phosphates Gel Precursor, terephthalic acid (TPA) (PTA), dihydric alcohol, stabilizer and catalyst by proportion, which are added in polyester reactor, uses in-situ polymerization to prepare nano cupric oxide@Mesoporous zirconium phosphates/polyester antimicrobial composite material using polymerization reaction heat one-step method, dry, Mesoporous zirconium phosphate load nano cupric oxide antibacterial polyester fibre is spun into through melt spinning method.The method of the present invention is simple to operate, efficient, and cost is low, and effectiveness persistently, has a extensive future.
Description
Technical field
The invention belongs to antiseptic and anti-bacterial fibre preparation field, especially a kind of Mesoporous zirconium phosphate load nano cupric oxide resists
The preparation method of bacterium polyester fiber.
Background technology
The ecology overall situation severe exacerbation such as today's society extreme environment, environmental pollution, the special existence micro-loop such as confined space
Border causes active demand of the people to function protecting textile.The fiber for preparing textile at present does not have antibacterial ability in itself,
The environment of existence and breeding can be provided to bacterium under certain condition, human health is threatened.Solve the problems, such as the main of fibre antibacterial
Method is that composite modified, preparation changing with antibacterial action is carried out using nano-particle and polymeric matrix with antibacterial action
Property fiber.Fiber is progressively discharged 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 many function ingredients additions, scattered hardly possible at present, high temperature process is unstable, connect
The continuous metaplasia production low problem of row yielding, and the color problem of copper system antiseptic can not be solved, cause anti-bacterial fibre effective
Form large-scale production, it is difficult to meet the widespread demand of existing market.
At present, realize that there is fiber the main method of antibacterial functions to be by process for modifying surface and blend modification technology.
The former is antibacterial components is attached to fiber or fabric by the effect of antibacterial components and fiber or fabric face formation chemical bond
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, by carrying out reducing the anti-bacterial fibre or fabric that obtain surface attachment silver to the fiber after 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 received
Meter Yin Wei antibacterial components, with one kind in terylene or polypropylene fibre or polyamide fibre for carrier slice, anti-bacterial fibre is prepared by Screw Extrusion.
But this method, addition is larger, antibacterial components skewness, is difficult to realize continuous production.
The content of the invention
It is an object of the invention to provide a kind of preparation method of antibacterial polyester fibre, antibacterial in described antibacterial polyester fibre
The addition of guest component is big, be uniformly dispersed, and can persistently discharge, anti-bacterial fibre product colour is good.
In order to achieve the above object, nano cupric oxide antibacterial polyester fibre is loaded the invention provides a kind of Mesoporous zirconium phosphate
Preparation method, it is characterised in that specific steps include：
The first step：Cupric compound is added in ethanol aqueous slkali and forms Cu (OH)2Gel, filtration washing is into
Property, add Mesoporous zirconium phosphate, using the suction-operated in Mesoporous zirconium phosphate duct by the gel adsorptions of Cu (OH) 2 into mesopore orbit,
Obtain cupric oxide@Mesoporous zirconium phosphate Gel Precursors；
Second step：Above-mentioned cupric oxide@Mesoporous zirconium phosphates Gel Precursor and polyester are blended at 180~270 DEG C and made
Grain, and dry, most it is spun into Mesoporous zirconium phosphate loaded copper oxide antibacterial polyester fibre through melt spinning method afterwards；Or, will be above-mentioned
Cupric oxide@Mesoporous zirconium phosphates Gel Precursor, terephthalic acid (TPA) (PTA), dihydric alcohol, stabilizer and catalyst by proportion are added
Nano cupric oxide@Mesoporous zirconium phosphates/polyester is prepared using polymerization reaction heat one-step method using in-situ polymerization into polyester reactor
Antimicrobial composite material, is dried, and Mesoporous zirconium phosphate load nano cupric oxide antibacterial polyester fibre is spun into through melt spinning method.
Preferably, described cupric compound is at least one of copper chloride, copper sulphate and copper nitrate.
Preferably, described cupric oxide@Mesoporous zirconium phosphates Gel Precursor intermediary hole basic zirconium phosphate and Cu (OH)2Quality
Than for 90~99.5: 0.5~10.
Preferably, the dihydric alcohol in described second step be ethylene glycol, propane diols, butanediol and isobide at least
It is a kind of.
Preferably, the mass fraction of the cupric oxide@Mesoporous zirconium phosphate Gel Precursors in described second step is 0.1%
~10%, the mol ratio of terephthalic acid (TPA) and dihydric alcohol is 1: 1~1.5, and the mass fraction of stabilizer is 50ppm, catalyst
Mass fraction is 300ppm, cupric oxide@Mesoporous zirconium phosphates Gel Precursor, terephthalic acid (TPA) (PTA), dihydric alcohol, stabilizer and
The mass fraction sum of catalyst is 100%.
Preferably, described Mesoporous zirconium phosphate load nano cupric oxide antibacterial polyester fibre includes polymeric matrix and divided
It is dispersed in the Mesoporous zirconium phosphate load nano cupric oxide in polymeric matrix.
It is highly preferred that the size of the described Mesoporous zirconium phosphate being dispersed in polymeric matrix load nano cupric oxide exists
100~700nm.
It is highly preferred that described polymer substrate be PET, polybutylene terephthalate, poly- pair
One kind in phthalic acid propylene diester.
Preferably, the course of reaction of described in-situ polymerization is in 180~240 DEG C, 300Kpa, N2Under atmosphere reaction 2~
5h, at 260~285 DEG C, less than 2~6h of reaction under conditions of 150pa.
Preferably, the fabric whiteness value that the Mesoporous zirconium phosphate load nano cupric oxide antibacterial polyester fibre of gained is formed >=
60。
Preferably, the cupric oxide in described Mesoporous zirconium phosphate loaded copper oxide antibacterial polyester fibre is changed by Kocide SD
, its transition temperature is 180~270 DEG C.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) bivalent cupric ion is changed into Kocide SD gel in the present invention, using the suction-operated of mesopore orbit, by hydrogen-oxygen
Change copper to load in basic zirconium phosphate mesopore orbit, so as to realize high capacity of the Kocide SD in mesoporous；
(2) method that the present invention is combined using the assembling of antibacterial functions medium, functional polyester in-situ polymerization, Mesoporous zirconium phosphate
Load Kocide SD directly generates nano cupric oxide in the course of the polymerization process, while being supported in mesopore orbit, the effect with sustained release
Really；
(3) anti-bacterial fibre that the present invention is obtained can be effectively improved the color problem of copper system Antibacterial Products；
(4) method of the invention is simple to operate, efficient, and cost is low, and effectiveness persistently, has a extensive future.It is prepared by the present invention
Anti-bacterial fibre can effectively strengthen functional fiber, can effectively apply in mouth mask, household textiles, clothes, big aircraft, high ferro
Deng interior trim, spacefarer's dress ornament, military battle-dress uniform decorations etc. can effectively fill up domestic by the industrialization of anti-bacterial fibre of the present invention
Anti-bacterial fibre technology of preparing blank.
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 of the invention lectured has been read, 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 loads the preparation method of nano cupric oxide antibacterial polyester fibre, concretely comprises the following steps：
The first step：1.35g copper chlorides are added to the sodium hydroxide ethanol solution that 100ml mass fractions are 10%, middle shape
Into glaucous Cu (OH)2Gel, filtering is washed with absolute ethyl alcohol to neutrality, is added Mesoporous zirconium phosphate 19.5g, is utilized mesoporous phosphorus
The suction-operated in sour zirconium duct is by Cu (OH)2Gel adsorption is obtained before cupric oxide@Mesoporous zirconium phosphate gels into mesopore orbit
Drive body, described cupric oxide@Mesoporous zirconium phosphates Gel Precursor intermediary hole basic zirconium phosphate and Cu (OH)2Mass ratio be 99.5:
0.5；
Second step：By above-mentioned cupric oxide@Mesoporous zirconium phosphates Gel Precursor (mass fraction is 5%), p-phthalic acid
(PTA), ethylene glycol (PTA and EG mol ratios are 1: 1.2), stabilizer (dimethyl phosphate, mass fraction is 50ppm) and catalyst
(antimony glycol, mass fraction is 300ppm), cupric oxide@Mesoporous zirconium phosphates Gel Precursor, terephthalic acid (TPA) (PTA), binary
The mass fraction sum of alcohol, stabilizer and catalyst is 100%, is added in polyester reactor and (was reacted using in-situ polymerization
Journey be 230 DEG C, 300Kpa, reaction 3h, 275 DEG C, 150pa, reaction 3h)) using polymerization reaction heat one-step method prepare it is nano oxidized
Copper@Mesoporous zirconium phosphates/polyester antibacterial compound slice, are dried, and control moisture content is at 50~100ppm (mass content), through molten
Melt spin processes (spinning temperature is 270~285 DEG C) and be spun into Mesoporous zirconium phosphate load nano cupric oxide antibacterial polyester fibre, it is described
Mesoporous zirconium phosphate load nano cupric oxide antibacterial polyester fibre include polymeric matrix and be dispersed in polymeric matrix
Mesoporous zirconium phosphate loads nano cupric oxide, Cu (OH)2@Mesoporous zirconium phosphates are 5: 95 in mass ratio with polymeric matrix.Described
The size of Mesoporous zirconium phosphate load nano cupric oxide is in 100~300mm.
Fabric whiteness value >=75 of described Mesoporous zirconium phosphate load nano cupric oxide antibacterial polyester fibre formation.The fiber
To the antibiotic rate ＞ 95% of Escherichia coli, to the antibiotic rate ＞ 90% of staphylococcus aureus, to the antibiotic rate of Candida albicans
＞ 60%.The water-fastness number of times ＞ of fabric 100 times.
Embodiment 2
A kind of Mesoporous zirconium phosphate loads the preparation method of nano cupric oxide antibacterial polyester fibre, concretely comprises the following steps：
The first step：3.2g copper sulphate is added to the ethanol solution for the sodium hydroxide that 100ml mass fractions are 8%, middle shape
Into glaucous Cu (OH)2Gel, filtering is washed with absolute ethyl alcohol to neutrality, is added Mesoporous zirconium phosphate 39g, is utilized mesoporous phosphoric acid
The suction-operated in zirconium duct is by Cu (OH)2Gel adsorption obtains cupric oxide@Mesoporous zirconium phosphate gel forerunners into mesopore orbit
Body, described cupric oxide@Mesoporous zirconium phosphates Gel Precursor intermediary hole basic zirconium phosphate and Cu (OH)2Mass ratio be 99.5: 0.5；
Second step：By above-mentioned cupric oxide@Mesoporous zirconium phosphates Gel Precursor (mass fraction is 8%), p-phthalic acid
(PTA), ethylene glycol (mol ratio of PTA and ethylene glycol is 1: 1.3), trimethyl phosphate (mass fraction is 50ppm) and catalyst
(antimony glycol, mass fraction is 300ppm), cupric oxide@Mesoporous zirconium phosphates Gel Precursor, terephthalic acid (TPA) (PTA), binary
The mass fraction sum of alcohol, stabilizer and catalyst is 100%, is proportionally added into polyester reactor and uses in-situ polymerization
(course of reaction is 220 DEG C, 300kpa reactions 3h；280 DEG C, 130pa reactions 2h) prepare nanometer using polymerization reaction heat one-step method
Cupric oxide@Mesoporous zirconium phosphates/polyester antibacterial compound slice, are dried, and control moisture content at 50~100ppm (mass content),
Mesoporous zirconium phosphate load nano cupric oxide antibacterial polyester fibre is spun into through melt spinning method (spinning temperature is 240~260 DEG C),
Described Mesoporous zirconium phosphate load nano cupric oxide antibacterial polyester fibre includes polymeric matrix and is dispersed in polymeric matrix
In Mesoporous zirconium phosphate load nano cupric oxide, Cu (OH)2@Mesoporous zirconium phosphates are 8: 92 in mass ratio with polymeric matrix.Institute
The size for the Mesoporous zirconium phosphate load nano cupric oxide stated is in 300-700nm.
Fabric whiteness value >=70 of described Mesoporous zirconium phosphate load nano cupric oxide antibacterial polyester fibre formation.The fiber
To the antibiotic rate ＞ 95% of Escherichia coli, to the antibiotic rate ＞ 92% of staphylococcus aureus, to the antibiotic rate of Candida albicans
＞ 70%.Water-fastness number of times ＞ 100 times.
Embodiment 3
A kind of Mesoporous zirconium phosphate loads the preparation method of nano cupric oxide antibacterial polyester fibre, concretely comprises the following steps：
The first step：1.88g copper nitrates are added in the ethanol solution for the ammoniacal liquor that 100ml mass fractions are 15% and form blue
The Cu (OH) of green2Gel, filtering is washed with absolute ethyl alcohol to neutrality, is added Mesoporous zirconium phosphate 18.62g, is utilized mesoporous phosphoric acid
The suction-operated in zirconium duct is by Cu (OH)2Gel adsorption obtains cupric oxide@Mesoporous zirconium phosphate gel forerunners into mesopore orbit
Body, described cupric oxide@Mesoporous zirconium phosphates Gel Precursor intermediary hole basic zirconium phosphate and Cu (OH)2Mass ratio be 95: 5；
Second step：By above-mentioned cupric oxide@Mesoporous zirconium phosphates Gel Precursor (mass fraction is 1%), p-phthalic acid
(PTA), ethylene glycol (mol ratio of PTA and ethylene glycol be 1: 1.2, stabilizer (dimethyl phosphate, mass fraction is 50ppm) and
Catalyst (antimony glycol, mass fraction is 300ppm), cupric oxide@Mesoporous zirconium phosphates Gel Precursor, terephthalic acid (TPA)
(PTA), the mass fraction sum of dihydric alcohol, stabilizer and catalyst is 100%, is proportionally added into polyester reactor and uses
(reaction condition is 225 DEG C to in-situ polymerization, 300kpa reactions 2h；280 DEG C, 100pa reactions 1.5h) utilize the step of polymerization reaction heat one
Method prepares nano cupric oxide Mesoporous zirconium phosphate/polyester antibacterial compound slice, dries, and control moisture content is in 50~100ppm (matter
Measure content) when, it is spun into Mesoporous zirconium phosphate load nano cupric oxide through melt spinning method (spinning temperature is 275~290 DEG C) and resists
Bacterium polyester fiber, described Mesoporous zirconium phosphate load nano cupric oxide antibacterial polyester fibre includes polymeric matrix and is dispersed in
Mesoporous zirconium phosphate load nano cupric oxide in polymeric matrix, Cu (OH)2@Mesoporous zirconium phosphates press quality with polymeric matrix
Than for 1: 99.The size of described Mesoporous zirconium phosphate load nano cupric oxide is in 100-300nm.
Fabric whiteness value >=75 of described Mesoporous zirconium phosphate load nano cupric oxide antibacterial polyester fibre formation.The fiber
To the antibiotic rate ＞ 97% of Escherichia coli, to the antibiotic rate ＞ 93% of staphylococcus aureus, to the antibiotic rate of Candida albicans
＞ 70%.The washable number of times ＞ of fabric 80 times.
Embodiment 4
A kind of Mesoporous zirconium phosphate loads the preparation method of nano cupric oxide antibacterial polyester fibre, concretely comprises the following steps：
The first step：3.2g copper sulphate is added in the sodium hydroxide ethanol solution that 100ml mass fractions are 5% and forms blue
The Cu (OH) of green2Gel, filtering is washed with absolute ethyl alcohol to neutrality, is added Mesoporous zirconium phosphate 37.24g, is utilized mesoporous phosphoric acid
The suction-operated in zirconium duct is by Cu (OH)2Gel adsorption obtains cupric oxide@Mesoporous zirconium phosphate gel forerunners into mesopore orbit
Body, described cupric oxide@Mesoporous zirconium phosphates Gel Precursor intermediary hole basic zirconium phosphate and Cu (OH)2Mass ratio be 95: 5；
Second step：By above-mentioned cupric oxide@Mesoporous zirconium phosphates Gel Precursor (mass fraction is 5%), p-phthalic acid
(PTA), propane diols (mol ratio of PTA and propane diols be 1: 1.3), stabilizer (dimethyl phosphate, mass fraction is 50ppm) and
Catalyst (antimony glycol, mass fraction is 300ppm), cupric oxide@Mesoporous zirconium phosphates Gel Precursor, terephthalic acid (TPA)
(PTA), the mass fraction sum of dihydric alcohol, stabilizer and catalyst is 100%, is proportionally added into polyester reactor and uses
(reaction condition is 210 DEG C to in-situ polymerization, 300kpa reactions 3h；285 DEG C, 150pa reactions 3h) utilize polymerization reaction heat one-step method
Nano cupric oxide@Mesoporous zirconium phosphates/polyester antibacterial compound slice is prepared, is dried, control moisture content is in 50~100ppm (quality
Content) when, it is spun into Mesoporous zirconium phosphate load nano cupric oxide antibacterial through melt spinning method (spinning temperature is 235~255 DEG C)
Polyester fiber, described Mesoporous zirconium phosphate load nano cupric oxide antibacterial polyester fibre includes polymeric matrix and is dispersed in poly-
Mesoporous zirconium phosphate load nano cupric oxide in compound matrix, Cu (OH)2@Mesoporous zirconium phosphates and polymeric matrix are in mass ratio
For 5: 95.The size of described Mesoporous zirconium phosphate load nano cupric oxide is in 300-700nm.
Fabric whiteness value >=65 of described Mesoporous zirconium phosphate load nano cupric oxide antibacterial polyester fibre formation.The fiber
To the antibiotic rate ＞ 99% of Escherichia coli, to the antibiotic rate ＞ 97% of staphylococcus aureus, to the antibiotic rate of Candida albicans
＞ 80%.The washable number of times ＞ of fabric 100 times.
Embodiment 5
A kind of Mesoporous zirconium phosphate loads the preparation method of nano cupric oxide antibacterial polyester fibre, concretely comprises the following steps：
The first step：8g copper sulphate is added in the ethanol containing ammonia that 500ml mass fractions are 5% and forms glaucous
Cu(OH)2Gel, filtering is washed with absolute ethyl alcohol to neutrality, is added Mesoporous zirconium phosphate 93.1g, is utilized Mesoporous zirconium phosphate duct
Suction-operated is by Cu (OH)2Gel adsorption obtains cupric oxide@Mesoporous zirconium phosphate Gel Precursors into mesopore orbit, described
Cupric oxide@Mesoporous zirconium phosphates Gel Precursor intermediary hole basic zirconium phosphate and Cu (OH)2Mass ratio be 95: 5；
Second step：By above-mentioned cupric oxide@Mesoporous zirconium phosphates Gel Precursor (mass fraction is 0.5%), smart terephthaldehyde
Sour (PTA), propane diols (mol ratio of PTA and propane diols is 1: 1.2), stabilizer (trimethyl phosphate, mass fraction is 50ppm)
With catalyst (antimony glycol, mass fraction is 300ppm), cupric oxide@Mesoporous zirconium phosphates Gel Precursor, terephthalic acid (TPA)
(PTA), the mass fraction sum of dihydric alcohol, stabilizer and catalyst is 100%, is proportionally added into polyester reactor and uses
(course of reaction is 210 DEG C to in-situ polymerization, 300kpa reactions 3h；285 DEG C, 150pa reactions 3h) utilize polymerization reaction heat one-step method
Nano cupric oxide@Mesoporous zirconium phosphates/polyester antibacterial compound slice is prepared, is dried, control moisture content is in 50~100ppm (quality
Content) when, it is spun into Mesoporous zirconium phosphate load nano cupric oxide antibacterial through melt spinning method (spinning temperature is 235~255 DEG C)
Polyester fiber, described Mesoporous zirconium phosphate load nano cupric oxide antibacterial polyester fibre includes polymeric matrix and is dispersed in poly-
Mesoporous zirconium phosphate load nano cupric oxide in compound matrix, Cu (OH)2@Mesoporous zirconium phosphates and polymeric matrix are in mass ratio
For 0.5: 99.5.The size of described Mesoporous zirconium phosphate load nano cupric oxide is in 100-300nm.
Fabric whiteness value >=75 of described Mesoporous zirconium phosphate load nano cupric oxide antibacterial polyester fibre formation.The fiber
To the antibiotic rate ＞ 90% of Escherichia coli, to the antibiotic rate ＞ 88% of staphylococcus aureus, to the antibiotic rate of Candida albicans
＞ 65%.Water-fastness number of times ＞ 80 times.
Embodiment 6
A kind of Mesoporous zirconium phosphate loads the preparation method of nano cupric oxide antibacterial polyester fibre, concretely comprises the following steps：
(1) 9.4g copper nitrates are added to the sodium hydroxide ethanol solution that 500ml mass fractions are 8%, middle formation is bluish-green
The gels of Cu (OH) 2 of color, filtering is washed to neutrality with absolute ethyl alcohol, and 93.1g Mesoporous zirconium phosphates are added to the Cu (OH) 2 of neutrality
In gel, the gels of Cu (OH) 2 are loaded into the duct of Mesoporous zirconium phosphate using the physisorption in Mesoporous zirconium phosphate duct,
Obtain cupric oxide@Mesoporous zirconium phosphate presomas, described cupric oxide@Mesoporous zirconium phosphates presoma intermediary hole basic zirconium phosphate and Cu
(OH) 2 mass ratio is 99.5: 0.5, heats 4h at 200 DEG C under nitrogen atmosphere in tube furnace, obtains cupric oxide@mesoporous
Basic zirconium phosphate antimicrobial powder；The size of described cupric oxide@Mesoporous zirconium phosphate antimicrobial powders is in 100-300nm.
(2) by above-mentioned cupric oxide@Mesoporous zirconium phosphates antimicrobial powder and polyester PET ([η]=6.2, Mw=2.0 × 104) press
Granulation is blended in mass ratio 5: 95 at 200 DEG C~230 DEG C, and dries, and most through melt spinning method, (spinning temperature is 255~279 afterwards
DEG C) it is spun into Mesoporous zirconium phosphate loaded copper oxide antibacterial polyester fibre.Cupric oxide@Mesoporous zirconium phosphate antimicrobial powders in fiber
Size is in 100-300nm, fibroplastic fabric whiteness value >=75.The fiber is to the antibiotic rate ＞ 90% of Escherichia coli, to gold
The antibiotic rate ＞ 85% of staphylococcus aureus, to the antibiotic rate ＞ 60% of Candida albicans.The water-fastness number of times ＞ of fabric 80 times.
Claims (7)
1. a kind of Mesoporous zirconium phosphate loads the preparation method of nano cupric oxide antibacterial polyester fibre, it is characterised in that specific steps
Including：
The first step：Cupric compound is added in ethanol aqueous slkali and forms Cu (OH)2Gel, filtration washing to neutrality is added
Mesoporous zirconium phosphate, using the suction-operated in Mesoporous zirconium phosphate duct by Cu (OH)2Gel adsorption obtains mesoporous into mesopore orbit
Basic zirconium phosphate loaded copper oxide Gel Precursor；Described Mesoporous zirconium phosphate loaded copper oxide Gel Precursor intermediary hole basic zirconium phosphate and
Cu(OH)2Mass ratio be 90 ~ 99.5：0.5~10；
Second step：Granulation is blended in above-mentioned Mesoporous zirconium phosphate loaded copper oxide Gel Precursor and polyester at 180 ~ 270 DEG C,
And dry, most it is spun into Mesoporous zirconium phosphate loaded copper oxide antibacterial polyester fibre through melt spinning method afterwards；Or, will be above-mentioned mesoporous
It is anti-that basic zirconium phosphate loaded copper oxide Gel Precursor, terephthalic acid (TPA), dihydric alcohol, stabilizer and catalyst by proportion are added to polyester
Answer in device using in-situ polymerization using polymerization reaction heat one-step method prepare mesoporous nano basic zirconium phosphate loaded copper oxide/polyester antibacterial answer
Condensation material, is dried, and Mesoporous zirconium phosphate load nano cupric oxide antibacterial polyester fibre is spun into through melt spinning method；Described is mesoporous
Basic zirconium phosphate load nano cupric oxide antibacterial polyester fibre includes polymeric matrix and the mesoporous phosphorus being dispersed in polymeric matrix
Sour zirconium loads nano cupric oxide；The size of described Mesoporous zirconium phosphate load nano cupric oxide is in 100 ~ 700 nm.
2. Mesoporous zirconium phosphate as claimed in claim 1 loads the preparation method of nano cupric oxide antibacterial polyester fibre, its feature
It is, described cupric compound is at least one of copper chloride, copper sulphate and copper nitrate.
3. Mesoporous zirconium phosphate as claimed in claim 1 loads the preparation method of nano cupric oxide antibacterial polyester fibre, its feature
It is, the dihydric alcohol in described second step is at least one of ethylene glycol, propane diols, butanediol and isobide.
4. Mesoporous zirconium phosphate as claimed in claim 1 loads the preparation method of nano cupric oxide antibacterial polyester fibre, its feature
It is, the mass fraction of the Mesoporous zirconium phosphate loaded copper oxide Gel Precursor in described second step is 0.1% ~ 10%, to benzene
The mol ratio of dioctyl phthalate and dihydric alcohol is 1：1~1.5, the mass fraction of stabilizer is 50ppm, and the mass fraction of catalyst is
300ppm, Mesoporous zirconium phosphate loaded copper oxide Gel Precursor, terephthalic acid (TPA), dihydric alcohol, the quality of stabilizer and catalyst
Fraction sum is 100%.
5. Mesoporous zirconium phosphate as claimed in claim 1 loads the preparation method of nano cupric oxide antibacterial polyester fibre, its feature
It is, described polymeric matrix is PET, polybutylene terephthalate, poly terephthalic acid the third two
One kind in ester.
6. Mesoporous zirconium phosphate as claimed in claim 1 loads the preparation method of nano cupric oxide antibacterial polyester fibre, its feature
It is, the course of reaction of described in-situ polymerization is in 180 ~ 240 DEG C, 300kPa, N22 ~ 5h is reacted under atmosphere, 260 ~ 285
DEG C, less than 2 ~ 6 h of reaction under conditions of 150Pa.
7. Mesoporous zirconium phosphate as claimed in claim 1 loads the preparation method of nano cupric oxide antibacterial polyester fibre, its feature
It is, fabric whiteness value >=60 of the Mesoporous zirconium phosphate load nano cupric oxide antibacterial polyester fibre formation of gained.
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| CN110294839A (en) * | 2019-06-29 | 2019-10-01 | 江苏鑫福纤维科技有限公司 | A method of the fiber polyester chip for textile processing |
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| CN104593897A (en) * | 2013-10-31 | 2015-05-06 | 上海环谷新材料科技发展有限公司 | Long-acting mildew-resistant odor-removing moisture-absorbing polyamide fiber and preparing method thereof |
| CN105040142A (en) * | 2015-08-17 | 2015-11-11 | 俞尧芳 | Antibacterial polyester fibers and preparation method thereof |
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