CN105350111A - Method for preparing mesoporous zirconium phosphate supported nano copper oxide antibacterial polyester fibers - Google Patents
Method for preparing mesoporous zirconium phosphate supported nano copper oxide antibacterial polyester fibers Download PDFInfo
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- CN105350111A CN105350111A CN201510866915.5A CN201510866915A CN105350111A CN 105350111 A CN105350111 A CN 105350111A CN 201510866915 A CN201510866915 A CN 201510866915A CN 105350111 A CN105350111 A CN 105350111A
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Abstract
The invention provides a method for preparing mesoporous zirconium phosphate supported nano copper oxide antibacterial polyester fibers. The method is characterized by including the specific steps that firstly, a copper oxide @ mesoporous zirconium phosphate gel precursor is prepared; secondly, the copper oxide @ mesoporous zirconium phosphate gel precursor and polyester are mixed and granulated at the temperature of 180-270 DEG C, dried and then spun into the mesoporous zirconium phosphate supported nano copper oxide antibacterial polyester fibers through a melt spinning method, or the copper oxide @ mesoporous zirconium phosphate gel precursor, terephthalic acid (PTA), dihydric alcohol, stabilizer and a catalyst are added into a polyester reactor according to a proportion, and a nano copper oxide @ mesoporous zirconium phosphate/polyester antibacterial composite material is prepared by means of in situ polymerization through a polymerization reaction thermal one-step method, dried and spun into the mesoporous zirconium phosphate supported nano copper oxide antibacterial polyester fibers through the melt spinning method. The method is simple in operation, efficient, low in cost, lasting in effect and wide in application prospect.
Description
Technical field
The invention belongs to antiseptic and anti-bacterial fibre preparation field, a kind of especially preparation method of Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre.
Background technology
The ecological overall situation severe exacerbations such as society extreme environment, environmental pollution, the special existence microenvironment such as confined space causes people to the active demand of function protecting textiles.The fiber itself preparing textiles does not at present have antibacterial ability, can provide the environment of existence and breeding under certain condition, threaten human health to bacterium.The main method solving fibre antibacterial problem utilizes the nano particle with antibacterial action to carry out composite modified with polymeric matrix, prepares the modified fibre with antibacterial action.Make fiber in use progressively can discharge antimicrobial component, reach antibacterial object.Current anti-bacterial fibre is widely used; demand is large; but technology effectively can not solve the difficult problems such as function ingredients addition is many, dispersion is difficult, high temperature process is unstable, continuous prodution row yielding is low at present; and the color problem of copper series antibacterial agent cannot be solved; cause anti-bacterial fibre effectively can not form large-scale production, be difficult to the widespread demand meeting existing market.
At present, realizing the main method that fiber has an antibacterial functions is by process for modifying surface and blend modification technology.The former is that the effect forming chemical bond by antibacterial components and fiber or fabric face makes antibacterial components be attached to the surface of fiber or fabric, thus reaches antibacterial action.Fiber is joined the silver nitrate in the solution containing silver nitrate in adsorbent solution by patent CN101942759A, by reducing to the fiber after absorption the anti-bacterial fibre or fabric that obtain surface attachment silver.The method can not form the antimicrobial coating of stable homogeneous, and antibacterial time is limited, can not reach durable antibiotic.Whole process too complexity very easily produces pollution to environment.Latter antibacterial components is direct or modified joins in polymer, prepares antibacterial matrices, preparing anti-bacterial fibre through melt spinning technology by Screw Extrusion.Patent CN101440533 is antibacterial components by bamboo charcoal nano and Nano Silver, with the one in terylene or polypropylene fibre or polyamide fibre for carrier slice, prepares anti-bacterial fibre by Screw Extrusion.But the method, addition is comparatively large, antibacterial components skewness, not easily realizes continuous prodution.
Summary of the invention
The object of this invention is to provide a kind of preparation method of antibacterial polyester fibre, in described antibacterial polyester fibre the addition of antibacterial guest component large, be uniformly dispersed, can discharge lastingly, anti-bacterial fibre product colour is good.
In order to achieve the above object, the invention provides a kind of preparation method of Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre, it is characterized in that, concrete steps comprise:
The first step: cupric compound is joined in ethanol aqueous slkali and form Cu (OH)
2gel, filtration washing, to neutral, adds Mesoporous zirconium phosphate, utilizes the suction-operated in Mesoporous zirconium phosphate duct by Cu (OH) 2 gel adsorption in mesopore orbit, obtains cupric oxide@Mesoporous zirconium phosphate Gel Precursor;
Second step: the blended granulation at 180 ~ 270 DEG C by above-mentioned cupric oxide@Mesoporous zirconium phosphate Gel Precursor and polyester, and dry, be spun into Mesoporous zirconium phosphate loaded copper oxide antibacterial polyester fibre finally by melt spinning method; Or, above-mentioned cupric oxide@Mesoporous zirconium phosphate Gel Precursor, terephthalic acid (TPA) (PTA), dihydroxylic alcohols, stabilizing agent and catalyst by proportion being joined in polyester reactor adopts in-situ polymerization to utilize polymerization reaction heat one-step method to prepare nano cupric oxide@Mesoporous zirconium phosphate/polyester antimicrobial composite material, drying, is spun into Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre through melt spinning method.
Preferably, described cupric compound is at least one in copper chloride, copper sulphate and copper nitrate.
Preferably, described cupric oxide@Mesoporous zirconium phosphate Gel Precursor intermediary hole basic zirconium phosphate and Cu (OH)
2mass ratio be 90 ~ 99.5: 0.5 ~ 10.
Preferably, the dihydroxylic alcohols in described second step is at least one in ethylene glycol, propylene glycol, butanediol and isobide.
Preferably, the mass fraction of the cupric oxide@Mesoporous zirconium phosphate Gel Precursor in described second step is 0.1% ~ 10%, the mol ratio of terephthalic acid (TPA) and dihydroxylic alcohols is 1: 1 ~ 1.5, the mass fraction of stabilizing agent is 50ppm, the mass fraction of catalyst is 300ppm, and the mass fraction sum of cupric oxide@Mesoporous zirconium phosphate Gel Precursor, terephthalic acid (TPA) (PTA), dihydroxylic alcohols, stabilizing agent and catalyst is 100%.
Preferably, described Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre comprises polymeric matrix and is dispersed in the Mesoporous zirconium phosphate loaded with nano cupric oxide in polymeric matrix.
More preferably, the described size being dispersed in the Mesoporous zirconium phosphate loaded with nano cupric oxide in polymeric matrix is at 100 ~ 700nm.
More preferably, described polymer substrate is the one in polyethylene terephthalate, polybutylene terephthalate, polytrimethylene terephthalate.
Preferably, the course of reaction of described in-situ polymerization is at 180 ~ 240 DEG C, 300Kpa, N
2react 2 ~ 5h under atmosphere, at 260 ~ 285 DEG C, react 2 ~ 6h lower than under the condition of 150pa.
Preferably, fabric whiteness value >=60 of the Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre formation of gained.
Preferably, the cupric oxide in described Mesoporous zirconium phosphate loaded copper oxide antibacterial polyester fibre is changed by Kocide SD, and its transition temperature is 180 ~ 270 DEG C.
Compared with prior art, the invention has the beneficial effects as follows:
(1) in the present invention, bivalent cupric ion is become Kocide SD gel, utilize the suction-operated of mesopore orbit, Kocide SD is loaded in basic zirconium phosphate mesopore orbit, thus realize the high capacity of Kocide SD in mesoporous;
(2) the present invention adopts the method that antibacterial functions medium is assembled, functional polyester in-situ polymerization combines, and Mesoporous zirconium phosphate load hydrogen cupric oxide directly generates nano cupric oxide in the course of the polymerization process, and load simultaneously, in mesopore orbit, has the effect of slowly-releasing;
(3) anti-bacterial fibre that the present invention obtains effectively can improve the color problem of copper series antibacterial agent product;
(4) method of the present invention is simple to operate, efficient, and cost is low, and effectiveness is lasting, has a extensive future.Anti-bacterial fibre prepared by the present invention effectively can strengthen functional fiber, effectively can be applied in mouth mask, household textiles, clothes, the large interior trim such as aircraft, high ferro, spacefarer's dress ornament, military battle-dress uniform decorations etc., effectively can fill up domestic anti-bacterial fibre technology of preparing blank by the industrialization of anti-bacterial fibre of the present invention.
Detailed description of the invention
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
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 preparation method for Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre, concrete steps are:
The first step: 1.35g copper chloride is joined the NaOH ethanolic solution that 100ml mass fraction is 10%, the glaucous Cu of middle formation (OH)
2gel, filtration to neutral with absolute ethanol washing, add Mesoporous zirconium phosphate 19.5g, utilizes the suction-operated in Mesoporous zirconium phosphate duct by Cu (OH)
2gel adsorption, in mesopore orbit, obtains cupric oxide@Mesoporous zirconium phosphate Gel Precursor, described cupric oxide@Mesoporous zirconium phosphate 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 phosphate Gel Precursor (mass fraction is 5%), p-phthalic acid (PTA), ethylene glycol (PTA and EG mol ratio is 1: 1.2), stabilizing agent (dimethyl phosphate, mass fraction is 50ppm) and catalyst (antimony glycol, mass fraction is 300ppm), cupric oxide@Mesoporous zirconium phosphate Gel Precursor, terephthalic acid (TPA) (PTA), dihydroxylic alcohols, the mass fraction sum of stabilizing agent and catalyst is 100%, join in polyester reactor and adopt in-situ polymerization (course of reaction is 230 DEG C, 300Kpa, reaction 3h, 275 DEG C, 150pa, reaction 3h)) utilize polymerization reaction heat one-step method to prepare the antibacterial compound slice of nano cupric oxide@Mesoporous zirconium phosphate/polyester, dry, control moisture content when 50 ~ 100ppm (mass content), Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre is spun into through melt spinning method (spinning temperature is 270 ~ 285 DEG C), described Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre comprises polymeric matrix and is dispersed in the Mesoporous zirconium phosphate loaded with nano cupric oxide in polymeric matrix, Cu (OH)
2@Mesoporous zirconium phosphate and polymeric matrix are 5: 95 in mass ratio.The size of described Mesoporous zirconium phosphate loaded with nano cupric oxide is at 100 ~ 300mm.
Fabric whiteness value >=75 that described Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre is formed.This fiber to colibacillary antibiotic rate > 95%, to the antibiotic rate > 90% of staphylococcus aureus, to the antibiotic rate > 60% of Candida albicans.The water-fastness number of times > of fabric 100 times.
Embodiment 2
A preparation method for Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre, concrete steps are:
The first step: 3.2g copper sulphate is joined the ethanolic solution that 100ml mass fraction is the NaOH of 8%, the glaucous Cu of middle formation (OH)
2gel, filtration to neutral with absolute ethanol washing, add Mesoporous zirconium phosphate 39g, utilizes the suction-operated in Mesoporous zirconium phosphate duct by Cu (OH)
2gel adsorption, in mesopore orbit, obtains cupric oxide@Mesoporous zirconium phosphate Gel Precursor, described cupric oxide@Mesoporous zirconium phosphate 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 phosphate 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 phosphate Gel Precursor, terephthalic acid (TPA) (PTA), dihydroxylic alcohols, the mass fraction sum of stabilizing agent and catalyst is 100%, join in proportion in polyester reactor and adopt in-situ polymerization (course of reaction is 220 DEG C, 300kpa reacts 3h, 280 DEG C, 130pa reacts 2h) utilize polymerization reaction heat one-step method to prepare the antibacterial compound slice of nano cupric oxide@Mesoporous zirconium phosphate/polyester, dry, control moisture content when 50 ~ 100ppm (mass content), Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre is spun into through melt spinning method (spinning temperature is 240 ~ 260 DEG C), described Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre comprises polymeric matrix and is dispersed in the Mesoporous zirconium phosphate loaded with nano cupric oxide in polymeric matrix, Cu (OH)
2@Mesoporous zirconium phosphate and polymeric matrix are 8: 92 in mass ratio.The size of described Mesoporous zirconium phosphate loaded with nano cupric oxide is at 300-700nm.
Fabric whiteness value >=70 that described Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre is formed.This fiber to colibacillary antibiotic rate > 95%, to the antibiotic rate > 92% of staphylococcus aureus, to the antibiotic rate > 70% of Candida albicans.Water-fastness number of times > 100 times.
Embodiment 3
A preparation method for Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre, concrete steps are:
The first step: 1.88g copper nitrate being joined 100ml mass fraction is form glaucous Cu (OH) in the ethanolic solution of the ammoniacal liquor of 15%
2gel, filtration to neutral with absolute ethanol washing, add Mesoporous zirconium phosphate 18.62g, utilizes the suction-operated in Mesoporous zirconium phosphate duct by Cu (OH)
2gel adsorption, in mesopore orbit, obtains cupric oxide@Mesoporous zirconium phosphate Gel Precursor, described cupric oxide@Mesoporous zirconium phosphate Gel Precursor intermediary hole basic zirconium phosphate and Cu (OH)
2mass ratio be 95: 5;
Second step: by above-mentioned cupric oxide@Mesoporous zirconium phosphate Gel Precursor (mass fraction is 1%), p-phthalic acid (PTA), (mol ratio of PTA and ethylene glycol is 1: 1.2 to ethylene glycol, stabilizing agent (dimethyl phosphate, mass fraction is 50ppm) and catalyst (antimony glycol, mass fraction is 300ppm), cupric oxide@Mesoporous zirconium phosphate Gel Precursor, terephthalic acid (TPA) (PTA), dihydroxylic alcohols, the mass fraction sum of stabilizing agent and catalyst is 100%, join in proportion in polyester reactor and adopt in-situ polymerization (reaction condition is 225 DEG C, 300kpa reacts 2h, 280 DEG C, 100pa reacts 1.5h) utilize polymerization reaction heat one-step method to prepare the antibacterial compound slice of nano cupric oxide@Mesoporous zirconium phosphate/polyester, dry, control moisture content when 50 ~ 100ppm (mass content), Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre is spun into through melt spinning method (spinning temperature is 275 ~ 290 DEG C), described Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre comprises polymeric matrix and is dispersed in the Mesoporous zirconium phosphate loaded with nano cupric oxide in polymeric matrix, Cu (OH)
2@Mesoporous zirconium phosphate and polymeric matrix are 1: 99 in mass ratio.The size of described Mesoporous zirconium phosphate loaded with nano cupric oxide is at 100-300nm.
Fabric whiteness value >=75 that described Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre is formed.This fiber to colibacillary antibiotic rate > 97%, to the antibiotic rate > 93% of staphylococcus aureus, to the antibiotic rate > 70% of Candida albicans.The washable number of times > of fabric 80 times.
Embodiment 4
A preparation method for Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre, concrete steps are:
The first step: 3.2g copper sulphate being joined 100ml mass fraction is form glaucous Cu (OH) in the NaOH ethanolic solution of 5%
2gel, filtration to neutral with absolute ethanol washing, add Mesoporous zirconium phosphate 37.24g, utilizes the suction-operated in Mesoporous zirconium phosphate duct by Cu (OH)
2gel adsorption, in mesopore orbit, obtains cupric oxide@Mesoporous zirconium phosphate Gel Precursor, described cupric oxide@Mesoporous zirconium phosphate Gel Precursor intermediary hole basic zirconium phosphate and Cu (OH)
2mass ratio be 95: 5;
Second step: by above-mentioned cupric oxide@Mesoporous zirconium phosphate Gel Precursor (mass fraction is 5%), p-phthalic acid (PTA), propylene glycol (mol ratio of PTA and propylene glycol is 1: 1.3), stabilizing agent (dimethyl phosphate, mass fraction is 50ppm) and catalyst (antimony glycol, mass fraction is 300ppm), cupric oxide@Mesoporous zirconium phosphate Gel Precursor, terephthalic acid (TPA) (PTA), dihydroxylic alcohols, the mass fraction sum of stabilizing agent and catalyst is 100%, join in proportion in polyester reactor and adopt in-situ polymerization (reaction condition is 210 DEG C, 300kpa reacts 3h, 285 DEG C, 150pa reacts 3h) utilize polymerization reaction heat one-step method to prepare the antibacterial compound slice of nano cupric oxide@Mesoporous zirconium phosphate/polyester, dry, control moisture content when 50 ~ 100ppm (mass content), Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre is spun into through melt spinning method (spinning temperature is 235 ~ 255 DEG C), described Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre comprises polymeric matrix and is dispersed in the Mesoporous zirconium phosphate loaded with nano cupric oxide in polymeric matrix, Cu (OH)
2@Mesoporous zirconium phosphate and polymeric matrix are 5: 95 in mass ratio.The size of described Mesoporous zirconium phosphate loaded with nano cupric oxide is at 300-700nm.
Fabric whiteness value >=65 that described Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre is formed.This fiber to colibacillary antibiotic rate > 99%, to the antibiotic rate > 97% of staphylococcus aureus, to the antibiotic rate > 80% of Candida albicans.The washable number of times > of fabric 100 times.
Embodiment 5
A preparation method for Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre, concrete steps are:
The first step: 8g copper sulphate being joined 500ml mass fraction is form glaucous Cu (OH) in the ethanol containing ammonia of 5%
2gel, filtration to neutral with absolute ethanol washing, add Mesoporous zirconium phosphate 93.1g, utilizes the suction-operated in Mesoporous zirconium phosphate duct by Cu (OH)
2gel adsorption, in mesopore orbit, obtains cupric oxide@Mesoporous zirconium phosphate Gel Precursor, described cupric oxide@Mesoporous zirconium phosphate Gel Precursor intermediary hole basic zirconium phosphate and Cu (OH)
2mass ratio be 95: 5;
Second step: by above-mentioned cupric oxide@Mesoporous zirconium phosphate Gel Precursor (mass fraction is 0.5%), p-phthalic acid (PTA), propylene glycol (mol ratio of PTA and propylene glycol is 1: 1.2), stabilizing agent (trimethyl phosphate, mass fraction is 50ppm) and catalyst (antimony glycol, mass fraction is 300ppm), cupric oxide@Mesoporous zirconium phosphate Gel Precursor, terephthalic acid (TPA) (PTA), dihydroxylic alcohols, the mass fraction sum of stabilizing agent and catalyst is 100%, join in proportion in polyester reactor and adopt in-situ polymerization (course of reaction is 210 DEG C, 300kpa reacts 3h, 285 DEG C, 150pa reacts 3h) utilize polymerization reaction heat one-step method to prepare the antibacterial compound slice of nano cupric oxide@Mesoporous zirconium phosphate/polyester, dry, control moisture content when 50 ~ 100ppm (mass content), Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre is spun into through melt spinning method (spinning temperature is 235 ~ 255 DEG C), described Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre comprises polymeric matrix and is dispersed in the Mesoporous zirconium phosphate loaded with nano cupric oxide in polymeric matrix, Cu (OH)
2@Mesoporous zirconium phosphate and polymeric matrix are 0.5: 99.5 in mass ratio.The size of described Mesoporous zirconium phosphate loaded with nano cupric oxide is at 100-300nm.
Fabric whiteness value >=75 that described Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre is formed.This fiber to colibacillary antibiotic rate > 90%, to the antibiotic rate > 88% of staphylococcus aureus, to the antibiotic rate > 65% of Candida albicans.Water-fastness number of times > 80 times.
Embodiment 6
A preparation method for Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre, concrete steps are:
(1) 9.4g copper nitrate is joined the NaOH ethanolic solution that 500ml mass fraction is 8%, the glaucous Cu of middle formation (OH) 2 gel, filtration is extremely neutral with absolute ethanol washing, 93.1g Mesoporous zirconium phosphate is joined in neutral Cu (OH) 2 gel, the physisorption in Mesoporous zirconium phosphate duct is utilized to be loaded in the duct of Mesoporous zirconium phosphate by Cu (OH) 2 gel, obtain cupric oxide@Mesoporous zirconium phosphate presoma, described cupric oxide@Mesoporous zirconium phosphate presoma intermediary hole basic zirconium phosphate and the mass ratio of Cu (OH) 2 are 99.5: 0.5, at 200 DEG C, 4h is heated under nitrogen atmosphere in tube furnace, obtain cupric oxide@Mesoporous zirconium phosphate antimicrobial powder, the size of described cupric oxide@Mesoporous zirconium phosphate antimicrobial powder is at 100-300nm.
(2) by above-mentioned cupric oxide@Mesoporous zirconium phosphate antimicrobial powder and polyester PET ([η]=6.2, Mw=2.0 × 104) 5: 95 blended granulations at 200 DEG C ~ 230 DEG C in mass ratio, and dry, be spun into Mesoporous zirconium phosphate loaded copper oxide antibacterial polyester fibre finally by melt spinning method (spinning temperature is 255 ~ 279 DEG C).In fiber, the size of cupric oxide@Mesoporous zirconium phosphate antimicrobial powder is at 100-300nm, fibroplastic fabric whiteness value >=75.This fiber to colibacillary antibiotic rate > 90%, to 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 (10)
1. a preparation method for Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre, it is characterized in that, concrete steps comprise:
The first step: cupric compound is joined in ethanol aqueous slkali and form Cu (OH) 2 gel, filtration washing is to neutral, add Mesoporous zirconium phosphate, utilize the suction-operated in Mesoporous zirconium phosphate duct by Cu (OH) 2 gel adsorption in mesopore orbit, obtain copper oxide meso-porous zirconium phosphate gel presoma;
Second step: the blended granulation at 180 ~ 270 DEG C by above-mentioned copper oxide meso-porous zirconium phosphate gel presoma and polyester, and dry, be spun into Mesoporous zirconium phosphate loaded copper oxide antibacterial polyester fibre finally by melt spinning method; Or, above-mentioned copper oxide meso-porous zirconium phosphate gel presoma, terephthalic acid (TPA) (PTA), dihydroxylic alcohols, stabilizing agent and catalyst by proportion being joined in polyester reactor adopts in-situ polymerization to utilize polymerization reaction heat one-step method to prepare nano copper oxide meso-porous basic zirconium phosphate/polyester antimicrobial composite material, drying, is spun into Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre through melt spinning method.
2. the preparation method of Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre as claimed in claim 1, it is characterized in that, described cupric compound is at least one in copper chloride, copper sulphate and copper nitrate.
3. the preparation method of Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre as claimed in claim 1, it is characterized in that, described copper oxide meso-porous zirconium phosphate gel presoma intermediary hole basic zirconium phosphate and the mass ratio of Cu (OH) 2 are 90 ~ 99.5: 0.5 ~ 10.
4. the preparation method of Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre as claimed in claim 1, it is characterized in that, the dihydroxylic alcohols in described second step is at least one in ethylene glycol, propylene glycol, butanediol and isobide.
5. the preparation method of Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre as claimed in claim 1, it is characterized in that, the mass fraction of the copper oxide meso-porous zirconium phosphate gel presoma in described second step is 0.1% ~ 10%, the mol ratio of terephthalic acid (TPA) and dihydroxylic alcohols is 1: 1 ~ 1.5, the mass fraction of stabilizing agent is 50ppm, the mass fraction of catalyst is 300ppm, and the mass fraction sum of copper oxide meso-porous zirconium phosphate gel presoma, terephthalic acid (TPA) (PTA), dihydroxylic alcohols, stabilizing agent and catalyst is 100%.
6. the preparation method of Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre as claimed in claim 1, it is characterized in that, described Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre comprises polymeric matrix and is dispersed in the Mesoporous zirconium phosphate loaded with nano cupric oxide in polymeric matrix.
7. the preparation method of Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre as claimed in claim 6, it is characterized in that, the size of described Mesoporous zirconium phosphate loaded with nano cupric oxide is at 100 ~ 700nm.
8. the preparation method of Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre as claimed in claim 6, it is characterized in that, described polymer substrate is the one in polyethylene terephthalate, polybutylene terephthalate, polytrimethylene terephthalate.
9. the preparation method of Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre as claimed in claim 6, it is characterized in that, the course of reaction of described in-situ polymerization is at 180 ~ 240 DEG C, 300KPa, 2 ~ 5h is reacted under N2 atmosphere, at 260 ~ 285 DEG C, react 2 ~ 6h lower than under the condition of 150Pa.
10. the preparation method of Mesoporous zirconium phosphate loaded with nano cupric oxide antibacterial polyester fibre as claimed in claim 6, is characterized in that, fabric whiteness value >=60 of the Mesoporous zirconium phosphate loaded with 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 |
| CN116535856A (en) * | 2023-06-14 | 2023-08-04 | 山东天合京工新材料科技有限公司 | Antibacterial PI composite material and preparation method thereof |
| CN116622231A (en) * | 2023-06-24 | 2023-08-22 | 山东天合京工新材料科技有限公司 | Antibacterial PI composite material and preparation method thereof |
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| CN116535856A (en) * | 2023-06-14 | 2023-08-04 | 山东天合京工新材料科技有限公司 | Antibacterial PI composite material and preparation method thereof |
| CN116535856B (en) * | 2023-06-14 | 2024-03-15 | 山东天合京工新材料科技有限公司 | Antibacterial PI composite material and preparation method thereof |
| CN116622231A (en) * | 2023-06-24 | 2023-08-22 | 山东天合京工新材料科技有限公司 | Antibacterial PI composite material and preparation method thereof |
| CN116622231B (en) * | 2023-06-24 | 2024-03-15 | 山东天合京工新材料科技有限公司 | Antibacterial PI composite material and preparation method thereof |
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