CN113564748A - Multifunctional anti-aging polycarbonate fiber membrane material and preparation method thereof - Google Patents
Multifunctional anti-aging polycarbonate fiber membrane material and preparation method thereof Download PDFInfo
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- CN113564748A CN113564748A CN202110934512.5A CN202110934512A CN113564748A CN 113564748 A CN113564748 A CN 113564748A CN 202110934512 A CN202110934512 A CN 202110934512A CN 113564748 A CN113564748 A CN 113564748A
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- zinc oxide
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- cyanuric chloride
- aging
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- 239000004417 polycarbonate Substances 0.000 title claims abstract description 55
- 229920000515 polycarbonate Polymers 0.000 title claims abstract description 55
- 239000000835 fiber Substances 0.000 title claims abstract description 42
- 239000012528 membrane Substances 0.000 title claims abstract description 41
- 239000000463 material Substances 0.000 title claims abstract description 33
- 230000003712 anti-aging effect Effects 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 99
- 239000011787 zinc oxide Substances 0.000 claims abstract description 50
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000009987 spinning Methods 0.000 claims abstract description 31
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 30
- 229920000642 polymer Polymers 0.000 claims abstract description 19
- 239000000243 solution Substances 0.000 claims abstract description 18
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 15
- 238000011065 in-situ storage Methods 0.000 claims abstract description 12
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 12
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000006467 substitution reaction Methods 0.000 claims abstract description 10
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical class [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 30
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 21
- 238000001914 filtration Methods 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 14
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 9
- 229910052782 aluminium Inorganic materials 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 239000011888 foil Substances 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000011858 nanopowder Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 6
- HHGHHFLQHHSCNW-UHFFFAOYSA-N N1=NN=CC=C1.C(CN)N Chemical compound N1=NN=CC=C1.C(CN)N HHGHHFLQHHSCNW-UHFFFAOYSA-N 0.000 claims description 5
- 239000002131 composite material Substances 0.000 claims description 2
- 229910000000 metal hydroxide Inorganic materials 0.000 claims description 2
- 150000004692 metal hydroxides Chemical class 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims description 2
- -1 zinc amide Chemical class 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims 1
- 239000011701 zinc Substances 0.000 claims 1
- 230000006750 UV protection Effects 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 229920006289 polycarbonate film Polymers 0.000 description 9
- 230000032683 aging Effects 0.000 description 7
- 239000011159 matrix material Substances 0.000 description 6
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000004033 plastic Substances 0.000 description 5
- 239000002250 absorbent Substances 0.000 description 4
- 230000002745 absorbent Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000009210 therapy by ultrasound Methods 0.000 description 4
- 238000000967 suction filtration Methods 0.000 description 3
- 125000003277 amino group Chemical group 0.000 description 2
- 239000013522 chelant Substances 0.000 description 2
- 239000005022 packaging material Substances 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 239000002985 plastic film Substances 0.000 description 2
- 229920006255 plastic film Polymers 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical group [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229920000587 hyperbranched polymer Polymers 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000002984 plastic foam Substances 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- 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
- D01F6/94—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 other polycondensation products
-
- 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
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention particularly discloses a multifunctional anti-aging polycarbonate fiber membrane material and a preparation method thereof. The method relates to a method for producing cyanuric chloride grafted zinc oxide through substitution reaction of aminated zinc oxide and cyanuric chloride, the cyanuric chloride grafted zinc oxide is obtained through in-situ polymerization reaction of the aminated zinc oxide and cyanuric chloride and ethylenediamine in a sodium carbonate aqueous solution, amino-terminated hyperbranched ethylenediamine-triazine polymer grafted zinc oxide is obtained, silanized LDHs is prepared at the same time, then the amino-terminated hyperbranched ethylenediamine-triazine polymer grafted zinc oxide, silanized LDHs and polycarbonate are mixed to obtain a uniformly dispersed spinning solution, and finally the anti-aging polycarbonate fiber membrane material is obtained through electrostatic spinning. The multifunctional anti-aging polycarbonate fiber membrane material provided by the invention has higher ultraviolet resistance and toughness performance.
Description
Technical Field
The invention relates to the field of Polycarbonate (PC) films, in particular to a multifunctional anti-aging fiber film material.
Background
The plastic products show a steady growth trend in the world economic development growth trend, the application field of the plastic products is continuously expanded, wherein the plastic packaging material is developed more and more rapidly in the globalization process, the status and the function of the plastic packaging industry in life and production are more and more obvious, the social demand is increased, the requirements on the quality and the quantity of the packaging plastic are greatly improved, and the polycarbonate plastic film is a green and environment-friendly packaging material due to the fact that the polycarbonate plastic film is non-toxic and harmless and is easy to recycle.
Polycarbonate films have many advantages and are widely used, but polycarbonate films have poor ultraviolet resistance, high tensile strength and poor toughness, and need to be modified correspondingly to improve the comprehensive performance.
Disclosure of Invention
Technical problem to be solved
In order to solve the problems, the invention aims to provide a multifunctional anti-aging polycarbonate fiber membrane material and a preparation method thereof, and solves the problems of poor ultraviolet resistance and poor toughness of the traditional aging fiber membrane material.
(II) technical scheme
In order to realize the aim, the invention provides a preparation method of a multifunctional anti-aging polycarbonate fiber membrane material, which comprises the following steps:
(1) ultrasonically dispersing a certain amount of aminated zinc oxide in a tetrahydrofuran solvent, adding cyanuric chloride and triethylamine, stirring and mixing uniformly to generate substitution reaction, and then filtering, washing and drying to obtain cyanuric chloride grafted zinc oxide;
(2) adding cyanuric chloride grafted zinc oxide into an acetone solvent for ultrasonic dispersion, simultaneously adding cyanuric chloride and ethylenediamine into a certain amount of sodium carbonate aqueous solution to form a mixed solution, slowly adding the mixed solution into the cyanuric chloride grafted zinc oxide solution, stirring and mixing uniformly to perform in-situ polymerization, and then filtering, washing and drying to obtain amino-terminated hyperbranched ethylenediamine-triazine polymer grafted zinc oxide;
(3) adding layered double-hydroxyl composite metal hydroxide LDHs nano powder into deionized water for ultrasonic dispersion, then adding a certain amount of water-soluble silane coupling agent for stirring reaction, then standing for reaction, filtering and drying to obtain silanized LDHs;
(4) dispersing the amino-terminated hyperbranched ethylenediamine triazine polymer grafted zinc oxide, silanized LDHs and polycarbonate in N-N-dimethylformamide, magnetically stirring for 12 hours at the temperature of 8 ℃ by using a constant-temperature magnetic stirrer, and then performing ultrasound for 3 hours by using a numerical control ultrasonic cleaner to obtain a uniformly dispersed spinning solution. And (3) obtaining a polycarbonate fiber membrane through electrostatic spinning, and finally, performing vacuum drying to obtain the anti-aging polycarbonate fiber membrane material.
Preferably, the mass ratio of the zinc oxide amide, the cyanuric chloride and the triethylamine in the step (1) is 10:4.5-5.5: 3-4.
Preferably, the temperature of the substitution reaction in the step (1) is 0-5 ℃, and the reaction time is 4-6 h.
Preferably, the mass ratio of the cyanuric chloride grafted zinc oxide to the cyanuric chloride to the ethylenediamine to the sodium carbonate in the step (2) is 2:5-7:4-6: 2-3.
Preferably, the temperature of the in-situ polymerization reaction in the step (2) is 15-40 ℃, and the time of the in-situ polymerization reaction is 6-12 h.
Preferably, the mass ratio of the LDHs to the silane coupling agent in the step (3) is 5: 2-4.
Preferably, in the step (3), the stirring reaction temperature is 20-30 ℃, the stirring reaction time is 10-15min, and the standing reaction time is 30-60 min.
Preferably, the mass ratio of the amine-terminated hyperbranched ethylenediamine-triazine polymer grafted zinc oxide, the silanized LDHs, the polycarbonate and the N-N-dimethylformamide in the step (4) is 1-2:1-2:20: 100.
Preferably, the spinning voltage in the step (4) is +20.5kV, the distance from the needle to the receiving plate is 15cm, the surface of the receiving plate is coated with aluminum foil, the ambient room temperature is 25 ℃, the relative humidity is 30%, and the spinning time is 60-90 min.
The invention also provides a multifunctional anti-aging polycarbonate fiber membrane material prepared by the method.
(III) advantageous technical effects
Compared with the prior art, the invention has the beneficial technical effects that:
a multifunctional anti-ageing polycarbonate fibre membrane material is prepared from the hyperbranched polymer (such as hyperbranched polyamine) containing a lot of flexible long chains for effectively improving the toughness of matrix, and the polycarbonate membrane obtained by mixing it with it has high anti-ultraviolet power and toughness. The hyperbranched ethylenediamine-triazine polymer has a three-dimensional network structure, the three-dimensional network structure contains a large number of flexible long chains, the toughness of a polycarbonate film of a matrix can be effectively improved, meanwhile, the tail end contains a large number of terminal amine groups with high activity, the mechanical property and compatibility of the matrix can be effectively improved, chemical micro-crosslinking is generated between the terminal amine groups and the matrix, and the hyperbranched triazine grafted zinc oxide modified polycarbonate film obtained after mixing has excellent ultraviolet resistance and toughness.
The zinc oxide is used as a third-generation semiconductor material, has a series of advantages of forbidden bandwidth, low price, environmental friendliness and the like, has good ultraviolet absorption capacity, and can improve the ultraviolet resistance of the polycarbonate film by using an organic ultraviolet absorbent triazine ultraviolet absorbent. The polycarbonate film can age under the irradiation of ultraviolet light to influence the performance of the polycarbonate film, the nano zinc oxide has the characteristic of forbidden bandwidth, electrons on a valence band of the nano zinc oxide can absorb the ultraviolet light and are excited on a conduction band to generate electron-hole pairs, the nano zinc oxide has scattering capacity on the ultraviolet light due to a nano size effect and plays an anti-ultraviolet role, the anti-ultraviolet capacity of a polycarbonate film matrix can be effectively enhanced due to the addition of a triazine ultraviolet absorbent, six-membered chelate rings are formed between hydroxyl groups on a benzene ring of the triazine ultraviolet absorbent and nitrogen atoms on adjacent triazine rings, and when the polycarbonate film is irradiated by the ultraviolet light, the chelate rings are opened and electrons jump to absorb a large amount of ultraviolet light.
Layered Double Hydroxide (LDHs) is an inorganic supramolecular material. The LDHs belongs to an anionic layered structure, and is a supermolecular material assembled by a main body laminate with positive charges and interlayer anions through the interaction of non-covalent bonds, the unique layered structure has a good shielding effect on ultraviolet light, and meanwhile, a hydrotalcite structure can form a penetrating cross-linked network with organic groups to shield ultraviolet light and improve the toughness and strength of a matrix.
A multifunctional anti-aging polycarbonate fiber membrane material is prepared by blending a functional liquid into a membrane by an electrostatic spinning method, and forming the membrane by blended polycarbonate fibers, so that the toughness and tensile strength of the membrane are integrally improved.
Detailed Description
In order to make the technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are fully described below, and the described embodiments are some, but not all, embodiments of the present invention; unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood in the art to which this invention belongs.
The terminology used in the description is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
In this example, unless otherwise specified, commercially available products were generally used for each component.
The specific implementation mode is as follows:
example 1
(1) Ultrasonically dispersing 10g of aminated zinc oxide in 40g of tetrahydrofuran solvent, adding 4.5g of cyanuric chloride and 3g of triethylamine, stirring and mixing uniformly, carrying out substitution reaction at 0 ℃ for 4 hours, filtering, washing and drying to obtain cyanuric chloride grafted zinc oxide;
(2) adding 10g of cyanuric chloride grafted zinc oxide into 30g of acetone solvent for ultrasonic dispersion, simultaneously adding 25g of cyanuric chloride and 20g of ethylenediamine into 80g of sodium carbonate aqueous solution (wherein the mass of the sodium carbonate is 10g) to form a mixed solution, slowly adding the mixed solution into the cyanuric chloride grafted zinc oxide solution, stirring and mixing uniformly, carrying out in-situ polymerization reaction at 15 ℃ for 6h, filtering, washing and drying after the reaction is finished, thus obtaining the amino-terminated hyperbranched ethylenediamine-triazine polymer grafted zinc oxide;
(3) adding 5g of LDHs nano powder into 100g of deionized water for ultrasonic dispersion, then adding 2g of water-soluble silane coupling agent, stirring and reacting at 20 ℃ for 10min, standing and reacting for 30min, then filtering and drying to obtain silanized LDHs;
(4) 1g of amino-terminated hyperbranched ethylenediamine-triazine polymer grafted zinc oxide, 1g of silanized LDHs and 20g of polycarbonate are dispersed in 100g of N-N-dimethylformamide, magnetically stirred for 12h at 8 ℃ by a constant-temperature magnetic stirrer, and then subjected to ultrasonic treatment for 3h by a numerical control ultrasonic cleaner to obtain a uniformly dispersed spinning solution. Setting the spinning voltage to be +20.5kV, setting the distance between a needle head and a receiving plate to be 15cm, covering aluminum foil on the surface of the receiving plate, enabling the ambient room temperature to be 25 ℃, the relative humidity to be 30%, spinning for 60min, obtaining a polycarbonate fiber membrane through a spinning machine, and finally performing vacuum drying to obtain the anti-aging polycarbonate fiber membrane material.
Example 2
(1) Ultrasonically dispersing 10g of aminated zinc oxide in 40g of tetrahydrofuran solvent, adding 4.8g of cyanuric chloride and 3.4g of triethylamine, stirring and mixing uniformly, carrying out substitution reaction for 4 hours at 2 ℃, and then filtering, washing and drying to obtain cyanuric chloride grafted zinc oxide;
(2) adding 10g of cyanuric chloride grafted zinc oxide into 30g of acetone solvent for ultrasonic dispersion, simultaneously adding 28g of cyanuric chloride and 24g of ethylenediamine into 80g of sodium carbonate aqueous solution (wherein the mass of the sodium carbonate is 13g) to form a mixed solution, slowly adding the mixed solution into the cyanuric chloride grafted zinc oxide solution, stirring and mixing uniformly, carrying out in-situ polymerization reaction at 20 ℃ for 8h, filtering, washing and drying to obtain amino-terminated hyperbranched ethylenediamine-triazine polymer grafted zinc oxide;
(3) adding 5g of LDHs nano powder into 100g of deionized water for ultrasonic dispersion, then adding 3g of water-soluble silane coupling agent, stirring and reacting for 10min at 20 ℃, standing and reacting for 30min, filtering and drying to obtain silanized LDHs;
(4) dispersing 2g of amino-terminated hyperbranched ethylenediamine triazine polymer grafted zinc oxide, 1g of silanized LDHs and 20g of polycarbonate in 100g of N-N-dimethylformamide, magnetically stirring for 12h at 8 ℃ by using a constant-temperature magnetic stirrer, and then performing ultrasonic treatment for 3h by using a numerical control ultrasonic cleaner to obtain a uniformly dispersed spinning solution. Setting the spinning voltage to be +20.5kV, setting the distance between a needle head and a receiving plate to be 15cm, covering aluminum foil on the surface of the receiving plate, enabling the ambient room temperature to be 25 ℃, the relative humidity to be 30%, spinning for 70min, obtaining a polycarbonate fiber membrane through a spinning machine, and finally performing vacuum drying to obtain the anti-aging polycarbonate fiber membrane material.
Example 3
(1) Ultrasonically dispersing 10g of aminated zinc oxide in 40g of tetrahydrofuran solvent, adding 5g of cyanuric chloride and 3.6g of triethylamine, stirring and mixing uniformly, carrying out substitution reaction at 4 ℃ for 3h, filtering, washing and drying to obtain cyanuric chloride grafted zinc oxide;
(2) adding 10g of cyanuric chloride grafted zinc oxide into 30g of acetone solvent for ultrasonic dispersion, simultaneously adding 33g of cyanuric chloride and 28g of ethylenediamine into 80g of sodium carbonate aqueous solution (wherein the mass of the sodium carbonate is 14g) to form a mixed solution, slowly adding the mixed solution into the cyanuric chloride grafted zinc oxide solution, stirring and mixing uniformly, carrying out in-situ polymerization reaction at 30 ℃ for 10 hours, and after the reaction is finished, carrying out suction filtration, washing and drying to obtain the amino-terminated hyperbranched ethylenediamine-triazine polymer grafted zinc oxide;
(3) adding 5g of LDHs nano powder into 100g of deionized water for ultrasonic dispersion, then adding 3g of water-soluble silane coupling agent, stirring and reacting for 10min at 30 ℃, standing and reacting for 30min, filtering and drying to obtain silanized LDHs;
(4) 1g of amino-terminated hyperbranched ethylenediamine-triazine polymer grafted zinc oxide, 2g of silanized LDHs and 20g of polycarbonate are dispersed in 100g of N-N-dimethylformamide, magnetically stirred for 12h at 8 ℃ by a constant-temperature magnetic stirrer, and then ultrasonically treated for 3h by a numerical control ultrasonic cleaner to obtain a uniformly dispersed spinning solution. Setting the spinning voltage to be +20.5kV, setting the distance between a needle head and a receiving plate to be 15cm, covering aluminum foil on the surface of the receiving plate, enabling the ambient room temperature to be 25 ℃, the relative humidity to be 30%, spinning for 80min, obtaining a polycarbonate fiber membrane through a spinning machine, and finally performing vacuum drying to obtain the anti-aging polycarbonate fiber membrane material.
Example 4
(1) Ultrasonically dispersing 10g of aminated zinc oxide in 40g of tetrahydrofuran solvent, adding 5.5g of cyanuric chloride and 4.0g of triethylamine, stirring and mixing uniformly, carrying out substitution reaction at 5 ℃ for 6 hours, and then filtering, washing and drying to obtain cyanuric chloride grafted zinc oxide;
(2) adding 10g of cyanuric chloride grafted zinc oxide into 30g of acetone solvent for ultrasonic dispersion, simultaneously adding 35g of cyanuric chloride and 30g of ethylenediamine into 80g of sodium carbonate aqueous solution (wherein the mass of the sodium carbonate is 15g) to form a mixed solution, slowly adding the mixed solution into the cyanuric chloride grafted zinc oxide solution, stirring and mixing uniformly, carrying out in-situ polymerization reaction at 40 ℃ for 12h, after the reaction is finished, carrying out suction filtration, washing and drying to obtain the amino-terminated hyperbranched ethylenediamine-triazine polymer grafted zinc oxide;
(3) adding 5g of LDHs nano powder into 100g of deionized water for ultrasonic dispersion, then adding 4g of water-soluble silane coupling agent, stirring and reacting for 15min at 30 ℃, standing and reacting for 60min, filtering and drying to obtain silanized LDHs;
(4) dispersing 2g of amino-terminated hyperbranched ethylenediamine triazine polymer grafted zinc oxide, 2g of silanized LDHs and 20g of polycarbonate in 100g of N-N-dimethylformamide, magnetically stirring for 12h at 8 ℃ by using a constant-temperature magnetic stirrer, and then performing ultrasonic treatment for 3h by using a numerical control ultrasonic cleaner to obtain a uniformly dispersed spinning solution. Setting the spinning voltage to be +20.5kV, setting the distance between a needle head and a receiving plate to be 15cm, covering aluminum foil on the surface of the receiving plate, enabling the ambient room temperature to be 25 ℃, the relative humidity to be 30%, spinning for 90min, obtaining a polycarbonate fiber membrane through a spinning machine, and finally performing vacuum drying to obtain the anti-aging polycarbonate fiber membrane material.
Comparative example 1
(1) Adding 5g of LDHs nano powder into 100g of deionized water for ultrasonic dispersion, then adding 2g of water-soluble silane coupling agent, stirring and reacting for 10min at 20 ℃, standing and reacting for 30min, then filtering and drying to obtain silanized LDHs;
(2) dispersing 1g of zinc oxide, 1g of silanized LDHs and 20g of polycarbonate in 100g N-N-dimethylformamide, magnetically stirring for 12h at 8 ℃ by using a constant-temperature magnetic stirrer, and then performing ultrasonic treatment for 3h by using a numerical control ultrasonic cleaner to obtain a uniformly dispersed spinning solution. Setting the spinning voltage to be +20.5kV, setting the distance between a needle head and a receiving plate to be 15cm, covering aluminum foil on the surface of the receiving plate, enabling the ambient room temperature to be 25 ℃, the relative humidity to be 30%, spinning for 60min, obtaining a polycarbonate fiber membrane through a spinning machine, and finally performing vacuum drying to obtain the anti-aging polycarbonate fiber membrane material.
Comparative example 2
(1) Ultrasonically dispersing 10g of aminated zinc oxide in 40g of tetrahydrofuran solvent, adding 4.5g of cyanuric chloride and 3g of triethylamine, stirring and mixing uniformly, carrying out substitution reaction at 0 ℃ for 4 hours, filtering, washing and drying after the reaction is finished, thus obtaining cyanuric chloride grafted zinc oxide;
(2) adding 10g of cyanuric chloride grafted zinc oxide into 30g of acetone solvent for ultrasonic dispersion, simultaneously adding 25g of cyanuric chloride and 20g of ethylenediamine into 80g of sodium carbonate (wherein the mass of the sodium carbonate is 10g) aqueous solution to form a mixed solution, slowly adding the mixed solution into the cyanuric chloride grafted zinc oxide solution, stirring and mixing uniformly, carrying out in-situ polymerization reaction at 15 ℃ for 6 hours, after the reaction is finished, carrying out suction filtration, washing and drying to obtain amino-terminated hyperbranched ethylenediamine triazine polymer grafted zinc oxide;
(3) 1g of amino-terminated hyperbranched ethylenediamine-triazine polymer grafted zinc oxide and 20g of polycarbonate are dispersed in 100g N-N-dimethylformamide, magnetically stirred for 12 hours at the temperature of 8 ℃ by a constant-temperature magnetic stirrer, and then ultrasonically treated for 3 hours by a numerical control ultrasonic cleaner to obtain a uniformly dispersed spinning solution. Setting the spinning voltage to be +20.5kV, setting the distance between a needle head and a receiving plate to be 15cm, covering aluminum foil on the surface of the receiving plate, enabling the ambient room temperature to be 25 ℃, the relative humidity to be 30%, spinning for 60min, obtaining a polycarbonate fiber membrane through a spinning machine, and finally performing vacuum drying to obtain the anti-aging polycarbonate fiber membrane material.
The polycarbonate fiber films applied to ultraviolet aging resistance obtained in examples 1 to 4 and comparative examples 1 to 2 were placed in an ultraviolet aging box of 128W and irradiated for 30 days, and the aged wood plastic foam board was photographed under natural light by using a digital camera of 2000 ten thousand pixels, and the results were as follows.
The polycarbonate fiber films applied to ultraviolet aging resistance obtained in examples 1 to 4 and comparative examples 1 to 2 were placed in an ultraviolet aging oven of 128W and irradiated for 30 days, and the impact strength before and after aging of the polycarbonate fiber films applied to ultraviolet aging resistance obtained in examples and comparative examples was tested using a pendulum impact tester of type JB-300B, and the results are as follows.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. The preparation method of the multifunctional anti-aging polycarbonate fiber membrane material is characterized by comprising the following steps:
(1) ultrasonically dispersing a certain amount of aminated zinc oxide in a tetrahydrofuran solvent, adding cyanuric chloride and triethylamine, stirring and mixing uniformly to generate substitution reaction, and then filtering, washing and drying to obtain cyanuric chloride grafted zinc oxide;
(2) adding cyanuric chloride grafted zinc oxide into an acetone solvent for ultrasonic dispersion, simultaneously adding cyanuric chloride and ethylenediamine into a certain amount of sodium carbonate aqueous solution to form a mixed solution, slowly adding the mixed solution into the cyanuric chloride grafted zinc oxide solution, stirring and mixing uniformly to perform in-situ polymerization, and then filtering, washing and drying to obtain amino-terminated hyperbranched ethylenediamine-triazine polymer grafted zinc oxide;
(3) adding layered double-hydroxyl composite metal hydroxide LDHs nano powder into deionized water for ultrasonic dispersion, then adding a certain amount of water-soluble silane coupling agent for stirring reaction, then standing for reaction, filtering and drying to obtain silanized LDHs;
(4) dispersing amino-terminated hyperbranched ethylenediamine triazine polymer grafted zinc oxide, silanized LDHs and polycarbonate in N-N-dimethylformamide, magnetically stirring for 12 hours at the temperature of 8 ℃ by using a constant-temperature magnetic stirrer, then performing ultrasound for 3 hours in a numerical control ultrasonic cleaner to obtain a uniformly dispersed spinning solution, performing electrostatic spinning to obtain a polycarbonate fiber membrane, and finally performing vacuum drying to obtain the anti-aging polycarbonate fiber membrane material.
2. The preparation method of the multifunctional anti-aging polycarbonate fiber membrane material as claimed in claim 1, wherein the mass ratio of zinc amide, cyanuric chloride and triethylamine in step (1) is 10:4.5-5.5: 3-4.
3. The preparation method of the multifunctional anti-aging polycarbonate fiber membrane material as claimed in claim 1, wherein the temperature of the substitution reaction in the step (1) is 0-5 ℃ and the reaction time is 4-6 h.
4. The preparation method of the multifunctional anti-aging polycarbonate fiber membrane material as claimed in claim 1, wherein the mass ratio of the cyanuric chloride grafted zinc oxide to the cyanuric chloride to the ethylenediamine to the sodium carbonate in the step (2) is 2:5-7:4-6: 2-3.
5. The preparation method of the multifunctional anti-aging polycarbonate fiber membrane material as claimed in claim 1, wherein the temperature of the in-situ polymerization reaction in step (2) is 15-40 ℃, and the time of the in-situ polymerization reaction is 6-12 h.
6. The preparation method of the multifunctional anti-aging polycarbonate fiber membrane material as claimed in claim 1, wherein the mass ratio of the LDHs to the silane coupling agent in the step (3) is 5: 2-4.
7. The preparation method of the multifunctional anti-aging polycarbonate fiber membrane material as claimed in claim 1, wherein in the step (3), the stirring reaction temperature is 20-30 ℃, the stirring reaction time is 10-15min, and the standing reaction time is 30-60 min.
8. The preparation method of the multifunctional anti-aging polycarbonate fiber membrane material as claimed in claim 1, wherein the mass ratio of the amine-terminated hyperbranched ethylenediamine-triazine polymer grafted zinc oxide, the silanized LDHs, the polycarbonate and the N-N-dimethylformamide in the step (4) is 1-2:1-2:20: 100.
9. The preparation method of the multifunctional anti-aging polycarbonate fiber membrane material as claimed in claim 1, wherein the spinning voltage in the step (4) is +20.5kV, the distance from the needle to the receiving plate is 15cm, the surface of the receiving plate is coated with aluminum foil, the ambient room temperature is 25 ℃, the relative humidity is 30%, and the spinning time is 60-90 min.
10. A multifunctional anti-aging polycarbonate fiber membrane material, which is characterized by being prepared by the preparation method of any one of claims 1 to 9.
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