CN114775279B - Antistatic flame-retardant polyester material - Google Patents

Antistatic flame-retardant polyester material Download PDF

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CN114775279B
CN114775279B CN202210695898.3A CN202210695898A CN114775279B CN 114775279 B CN114775279 B CN 114775279B CN 202210695898 A CN202210695898 A CN 202210695898A CN 114775279 B CN114775279 B CN 114775279B
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monomer
fluorine
polyester material
terephthalic acid
hydrophilic monomer
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CN114775279A (en
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李沅鸿
王洋
郭文光
朱亚凯
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Henan Yuanhong Polymer New Materials Co ltd
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Henan Yuanhong Polymer New Materials Co ltd
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M14/00Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
    • D06M14/18Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation
    • D06M14/26Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of synthetic origin
    • D06M14/30Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of synthetic origin of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M14/32Polyesters
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/02Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
    • C08G63/12Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
    • C08G63/16Dicarboxylic acids and dihydroxy compounds
    • C08G63/18Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
    • C08G63/181Acids containing aromatic rings
    • C08G63/183Terephthalic acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/78Preparation processes
    • C08G63/82Preparation processes characterised by the catalyst used
    • C08G63/83Alkali metals, alkaline earth metals, beryllium, magnesium, copper, silver, gold, zinc, cadmium, mercury, manganese, or compounds thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/78Preparation processes
    • C08G63/82Preparation processes characterised by the catalyst used
    • C08G63/85Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/78Preparation processes
    • C08G63/82Preparation processes characterised by the catalyst used
    • C08G63/85Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof
    • C08G63/86Germanium, antimony, or compounds thereof
    • C08G63/866Antimony or compounds thereof

Abstract

The invention provides an antistatic flame-retardant polyester material, which comprises the raw materials of a solvent, terephthalic acid, ethylene glycol, an additive, a hydrophilic monomer, a fluorine-silicon monomer and a photoinitiator; wherein the molar ratio of terephthalic acid to ethylene glycol is (1-2) to (1.2-1.6), and the molar ratio of the hydrophilic monomer to the fluorosilicone monomer is 1 (0.5-3); the dosage of the additive is 0.25 wt% -0.70 wt% of the terephthalic acid; the dosage of the hydrophilic monomer is 10-20 wt% of the terephthalic acid; the dosage of the photoinitiator is 0.5-2 wt% of the sum of the mass of the hydrophilic monomer and the mass of the fluorosilicone monomer. The polyester material has excellent hydrophilic performance, antistatic performance and flame retardant performance, and has wider application range compared with the conventional PET polyester material.

Description

Antistatic flame-retardant polyester material
Technical Field
The invention relates to a high polymer material, in particular to an antistatic flame-retardant polyester material.
Background
Polyesters (polyesters) are a class of polymers that contain ester functional groups in their backbone. Polyesters are of a wide variety, natural compounds such as plant cutin, and synthetic fibers such as polycarbonate and poly (terephthalic acid/adipic acid) ethylene glycol, which are formed by stepwise condensation. Both natural polyesters and a portion of synthetic polyesters are biodegradable, but the vast majority of synthetic polyesters are not biodegradable. Meanwhile, the polyester can be divided into two categories, namely saturated polyester and unsaturated polyester, and is prepared by polycondensation of one or more polybasic acids (anhydrides) and one or more polyhydric alcohols.
At present, polyester materials can be used for preparing fibers, sheets or films and the like, and are widely applied to the fields of packaging industry, electronic and electric appliances, medical treatment and health, buildings, automobiles and the like. However, the pure polyester material has insufficient flame retardant property, which limits the application occasions of the polyester material, and on the other hand, macromolecules in the polyester material are mutually connected in a covalent bond form, which cannot conduct electricity and is not easy to be wetted by water, so that the polyester material is easy to form static electricity, which greatly limits the use performance of the polyester material.
In order to solve the above problems, people are always seeking an ideal technical solution.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides an antistatic flame-retardant polyester material.
In order to achieve the purpose, the invention adopts the technical scheme that:
an antistatic flame-retardant polyester material comprises raw materials of a solvent, terephthalic acid, ethylene glycol, an additive, a hydrophilic monomer, a fluorine-silicon monomer and a photoinitiator; wherein, the molar ratio of terephthalic acid to ethylene glycol is (1-2) to (1.2-1.6), and the molar ratio of the hydrophilic monomer to the fluorine-silicon monomer is 1 (0.5-3); the dosage of the additive is 0.25 wt% -0.70 wt% of the terephthalic acid; the dosage of the hydrophilic monomer is 10-20 wt% of the terephthalic acid; the dosage of the photoinitiator is 0.5-2 wt% of the sum of the mass of the hydrophilic monomer and the mass of the fluorosilicone monomer.
Based on the above, the additive is a combination of at least two of titanium dioxide, lithium acetate, calcium acetate, zinc acetate, cobalt acetate, manganese acetate, antimony trioxide, ethylene glycol antimony, and diisopropylamine.
Based on the above, the solvent is one or a combination of at least two of trifluoroacetic acid, chloroform, phenol, tetrachloroethane, o-chlorophenol, benzene, chlorobenzene, trichloromethane, ethyl acetate, ethanol, acetone and diethyl ether.
Based on the above, the solvent comprises ethyl acetate and trifluoroacetic acid in a volume ratio of (3-10): 50; or ethyl acetate, chloroform and trifluoroacetic acid in a volume ratio of (3-10) to 40: 10.
Based on the above, the photoinitiator is one or the combination of at least two of alpha-hydroxyisobutyrophenone, diphenyl- (2,4, 6-trimethylbenzoyl) oxyphosphorus, 1-hydroxycyclohexyl phenyl ketone and 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-acetone.
Based on the above, the hydrophilic monomer is one or a combination of at least two of acrylic acid, butyl acrylate, N-isopropylacrylamide, itaconic acid and hydroxyethyl methacrylate.
Based on the above, the fluorine-silicon monomer is one or a mixture of two of vinyl dimethyl fluorine silane and (1-fluorine vinyl) methyl diphenyl silane, the chemical structural formula of the vinyl dimethyl fluorine silane is formula 1, and the chemical structural formula of the (1-fluorine vinyl) methyl diphenyl silane is formula 2;
formula 1
Figure DEST_PATH_IMAGE001
(ii) a Formula 2
Figure DEST_PATH_IMAGE002
Based on the above, the antistatic flame-retardant polyester material is prepared by the following preparation method:
uniformly mixing an additive, ethylene glycol and terephthalic acid, adding the mixture into an esterification reaction kettle, carrying out esterification reaction at the temperature of 250 ℃ and 0.2-0.4Mpa at 220 ℃, discharging water generated in the esterification reaction in time, transferring the mixture into a polycondensation reaction kettle when the water discharge reaches 96% of the theoretical value of the water generation amount, and reacting for 2-6h at 290 ℃ at 260-; transferring to a mixing kettle, cooling to 25-100 ℃, adding a solvent, and uniformly mixing; then adding hydrophilic monomer, fluorine silicon monomer and photoinitiator and mixing uniformly; and carrying out ultraviolet irradiation to obtain the product.
Based on the above, before the ultraviolet irradiation, the electrostatic spinning is performed to obtain the polyester fiber film, and then the ultraviolet irradiation is performed.
Based on the above, the ultraviolet light source is an ultraviolet LED area light source, the ultraviolet wavelength is 300-400 nm, the ultraviolet irradiation time is 60-600s,the light intensity of the ultraviolet irradiation is 120-5000 mW/cm 2
Compared with the prior art, the antistatic flame-retardant polyester material has outstanding substantive characteristics and remarkable progress, and particularly, the UL94 flame-retardant grade of the antistatic flame-retardant polyester material reaches UL94VTM-0 grade, and the mass specific resistance is (5-8) multiplied by 10 7 Ω∙g∙cm -2 The surface static water contact angle is 50-70 degrees, and the polyester material has excellent hydrophilic property, antistatic property and flame retardant property, and has wider application range compared with the conventional PET polyester material. Specifically, the polyester material disclosed by the invention combines a polyester material, a fluorine-silicon monomer and a hydrophilic monomer, the flame retardant property and the hydrophilic property of the polyester are improved through the hydrophilic monomer and the fluorine-silicon monomer, and meanwhile, the improvement of the hydrophilic property is also beneficial to the improvement of the antistatic property of the polyester material in the using process. In addition, in the preparation process of the polyester material, components such as titanium dioxide, lithium acetate and the like are added, so that not only is the smooth proceeding of esterification reaction and polycondensation reaction facilitated, but also the resistance of the polyester material is facilitated to be reduced, and the mixed solvent is added after the polycondensation is completed, so that the PET macromolecules, the hydrophilic monomer and the fluorine-silicon monomer are dissolved in the mixed solvent, then the electrostatic spinning is carried out to form a fiber film, and then the ultraviolet irradiation is carried out, so that the uniform occurrence of polymerization reaction in the polyester material is facilitated.
Detailed Description
The technical solution of the present invention is further described in detail by the following embodiments.
Example 1
The antistatic flame-retardant polyester material comprises the raw materials of a solvent, terephthalic acid, ethylene glycol, an additive, a hydrophilic monomer, a fluorine-silicon monomer and a photoinitiator; wherein the molar ratio of terephthalic acid to ethylene glycol is 1:1.3, and the molar ratio of the hydrophilic monomer to the fluorosilicone monomer is 1: 0.7; the dosage of the additive is 0.5 wt% of the terephthalic acid; the amount of the hydrophilic monomer is 12 wt% of the terephthalic acid; the dosage of the photoinitiator is 0.50 wt% of the sum of the mass of the hydrophilic monomer and the mass of the fluorosilicone monomer.
Wherein the additive comprises titanium dioxide, lithium acetate and antimony trioxide in a mass ratio of 3:3: 1; the solvent comprises ethyl acetate and trifluoroacetic acid in a volume ratio of 1: 5; the photoinitiator is alpha-hydroxyisobutyrophenone (1173); the hydrophilic monomer comprises acrylic acid and butyl acrylate in a mass ratio of 1: 1; the fluorine-silicon monomer is (1-fluorine vinyl) methyl diphenyl silane.
The antistatic flame-retardant polyester material is prepared by the following preparation method:
uniformly mixing an additive, ethylene glycol and terephthalic acid, adding the mixture into an esterification reaction kettle, carrying out esterification reaction at the temperature of 250 ℃ and 0.25 Mpa at 220 ℃, discharging water generated by the esterification reaction in time, transferring the mixture into a polycondensation reaction kettle after the water discharge reaches 96% of the theoretical value of the water generation amount, and reacting for 3 hours at 290 ℃ at 260-; transferring to a mixing kettle, cooling to 80 ℃, adding a solvent, and mixing uniformly; then adding the hydrophilic monomer, the fluorine-silicon monomer and the photoinitiator, and uniformly mixing; carrying out electrostatic spinning at room temperature to obtain a polyester fiber film with the film thickness of 36 microns, wherein the receiving distance of the electrostatic spinning is 15 cm, the spinning voltage is 15 kV, and the injection speed is 1 mL/h; irradiating the polyester fiber film with ultraviolet rays with the wavelength of 365 nm for 80 s at the intensity of 1000 mW/cm 2 . It is to be noted that the solvent is intended to dissolve the polycondensation product in an amount not critical, for example: the amount may be 1.5 to 2.5 times the amount of the polycondensation product.
The resistance of 15 g of polyester fiber was measured using a fiber specific resistance meter according to the formula: mass specific resistance ρ = Rm/L 2 Wherein R is average resistance, m fiber mass, and L is the distance (2 cm) between the two polar plates. The measured mass specific resistance was 8.0X 10 7 Ω∙g∙cm -2 . The polyester fiber film had a UL94 flame retardancy rating of UL94VTM-0 rating according to Underwriters Laboratories Subject 94(UL94), and the surface static water contact angle of the polyester fiber film was measured to be 63 DEG by a contact angle measuring instrument
Comparative test
The polyester material comprises the raw materials of a solvent, terephthalic acid, ethylene glycol and an additive; wherein the molar ratio of terephthalic acid to ethylene glycol is 1:1.3, and the dosage of the additive is 0.5 wt% of the terephthalic acid; wherein the solvent comprises ethyl acetate and trifluoroacetic acid in a volume ratio of 1: 5; the additive comprises titanium dioxide, lithium acetate and antimony trioxide in a mass ratio of 3:3: 1.
The polyester material is prepared by the following preparation method:
uniformly mixing an additive, ethylene glycol and terephthalic acid, adding the mixture into an esterification reaction kettle, carrying out esterification reaction at the temperature of 250 ℃ and 0.25 Mpa at 220 ℃, discharging water generated by the esterification reaction in time, transferring the mixture into a polycondensation reaction kettle after the water discharge reaches 96% of the theoretical value of the water generation amount, and reacting for 3 hours at 290 ℃ at 260-; transferring to a mixing kettle, cooling to room temperature, adding a solvent, and uniformly mixing; carrying out electrostatic spinning at room temperature to obtain a polyester fiber film, wherein the receiving distance of the electrostatic spinning is 15 cm, the spinning voltage is 15 kV, and the injection speed is 1 mL/h; irradiating the polyester fiber film with ultraviolet rays with the wavelength of 365 nm for 80 s at the intensity of 1000 mW/cm 2
The resistance of 15 g of polyester fiber was measured using a fiber specific resistance meter according to the formula: mass specific resistance ρ = Rm/L 2 Wherein R is average resistance, m fiber mass, and L is the distance (2 cm) between the two polar plates. The measured mass specific resistance was 2.1X 10 12 Ω∙g∙cm -2 . The polyester fiber film had a UL94 flame retardancy rating of UL94VTM-2 rating according to Underwriters Laboratories Subject 94(UL94), and the surface static water contact angle of the polyester fiber film was measured to be 132 DEG by a contact angle measuring instrument
Example 2
An antistatic flame-retardant polyester material comprises raw materials of a solvent, terephthalic acid, ethylene glycol, an additive, a hydrophilic monomer, a fluorine-silicon monomer and a photoinitiator; wherein the molar ratio of terephthalic acid to ethylene glycol is 1: 1.6, and the molar ratio of the hydrophilic monomer to the fluorosilicone monomer is 1: 1; the dosage of the additive is 0.70 wt% of the terephthalic acid; the amount of the hydrophilic monomer is 15 wt% of the terephthalic acid; the dosage of the photoinitiator is 0.5 wt% of the sum of the mass of the hydrophilic monomer and the mass of the fluorosilicone monomer.
Wherein the additive comprises titanium dioxide, calcium acetate and ethylene glycol antimony in a mass ratio of 4:2: 4; the solvent comprises ethyl acetate, chloroform and trifluoroacetic acid in a volume ratio of 10:40: 10. The photoinitiator is diphenyl- (2,4, 6-trimethylbenzoyl) oxyphosphorus (TPO); the hydrophilic monomer comprises N-isopropyl acrylamide and itaconic acid in a mass ratio of 1: 2; the fluorine-silicon monomer comprises vinyl dimethyl fluorine silane and (1-fluorine vinyl) methyl diphenyl silane in a mass ratio of 1: 4.
The antistatic flame-retardant polyester material is prepared by the following preparation method:
uniformly mixing an additive, ethylene glycol and terephthalic acid, adding the mixture into an esterification reaction kettle, carrying out esterification reaction at the temperature of 220-290 ℃ and under the pressure of 0.4Mpa, discharging water generated in the esterification reaction in time, transferring the mixture into a polycondensation reaction kettle when the water discharge reaches 96 percent of the theoretical value of the water generation amount, and reacting for 4 hours at the temperature of 260-290 ℃; transferring to a mixing kettle, cooling to room temperature, adding a solvent, and uniformly mixing; then adding the hydrophilic monomer, the fluorine-silicon monomer and the photoinitiator, and uniformly mixing; carrying out electrostatic spinning to obtain a polyester fiber film; wherein the receiving distance of electrostatic spinning is 15 cm, the spinning voltage is 15 kV, and the injection speed is 1 mL/h; the polyester fiber film is subjected to ultraviolet irradiation, the wavelength of the ultraviolet is 366 nm, the time of the ultraviolet irradiation is 100 s, and the light intensity of the ultraviolet irradiation is 2000 mW/cm 2
The resistance of 15 g of polyester fiber was measured using a fiber specific resistance meter according to the formula: mass specific resistance ρ = Rm/L 2 Wherein R is average resistance, m fiber mass, and L is the distance (2 cm) between the two polar plates. The measured mass specific resistance was 5.4X 10 7 Ω∙g∙cm -2 . The polyester fiber film had a UL94 flame retardancy rating of UL94VTM-0 rating according to Underwriters Laboratories Subject 94(UL94), and the surface static water contact angle of the polyester fiber film was measured to be 67 DEG by a contact angle measuring instrument
Example 3
An antistatic flame-retardant polyester material comprises raw materials of a solvent, terephthalic acid, ethylene glycol, an additive, a hydrophilic monomer, a fluorine-silicon monomer and a photoinitiator; wherein the molar ratio of terephthalic acid to ethylene glycol is 1:1.2, and the molar ratio of the hydrophilic monomer to the fluorosilicone monomer is 1: 2; the dosage of the additive is 0.25 wt% of the terephthalic acid; the amount of the hydrophilic monomer is 18 wt% of that of the terephthalic acid; the dosage of the photoinitiator is 1.5 wt% of the sum of the mass of the hydrophilic monomer and the mass of the fluorosilicone monomer.
The additive comprises titanium dioxide, zinc acetate and antimony trioxide in a mass ratio of 4:4: 2; the solvent comprises ethyl acetate, chloroform and trifluoroacetic acid in a volume ratio of 7:40: 10; the photoinitiator is 1-hydroxycyclohexyl phenyl ketone (184); the hydrophilic monomer comprises acrylic acid and N-isopropyl acrylamide in a mass ratio of 1: 3; the fluorine-silicon monomer is (1-fluorine vinyl) methyl diphenyl silane.
The antistatic flame-retardant polyester material is prepared by the following preparation method:
uniformly mixing an additive, ethylene glycol and terephthalic acid, adding the mixture into an esterification reaction kettle, carrying out esterification reaction at the temperature of 220-250 ℃ and under the pressure of 0.2-0.4Mpa, discharging water generated in the esterification reaction in time, transferring the discharged water to a polycondensation reaction kettle when the discharged water reaches 96% of a theoretical value of the water generation amount, and reacting for 6 hours at the temperature of 260-290 ℃; transferring to a mixing kettle, cooling to room temperature, adding a solvent, and uniformly mixing; then adding hydrophilic monomer, fluorine silicon monomer and photoinitiator and mixing uniformly; carrying out electrostatic spinning to obtain a polyester fiber film, and carrying out ultraviolet irradiation on the polyester fiber film to obtain the polyester fiber film; wherein the ultraviolet wavelength is 333 nm, the ultraviolet irradiation time is 120 s, and the ultraviolet irradiation light intensity is 1000 mW/cm 2
The resistance of 15 g of polyester fiber was measured using a fiber specific resistance meter according to the formula: mass specific resistance ρ = Rm/L 2 Wherein R is average resistance, m fiber mass, and L is the distance (2 cm) between the two polar plates. The measured mass specific resistance was 5.9X 10 7 Ω∙g∙cm -2 . The polyester fiber film had a UL94 flame retardancy rating of UL94VTM-0 rating according to Underwriters Laboratories Subject 94(UL94), and the surface static water contact angle of the polyester fiber film was measured to be 69 DEG by a contact angle measuring instrument
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention and not to limit it; although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art will understand that: modifications to the specific embodiments of the invention or equivalent substitutions for parts of the technical features may be made; without departing from the spirit of the present invention, it is intended to cover all aspects of the invention as defined by the appended claims.

Claims (5)

1. An antistatic flame-retardant polyester material, which is characterized in that: the preparation method comprises the following steps:
uniformly mixing an additive, ethylene glycol and terephthalic acid, adding the mixture into an esterification reaction kettle, carrying out esterification reaction at the temperature of 250 ℃ and the pressure of 0.2-0.4MPa, discharging water generated in the esterification reaction in time, transferring the mixture into a polycondensation reaction kettle when the water discharge reaches 96% of the theoretical value of the water generation amount, and reacting for 2-6h at the temperature of 290 ℃ and 260 ℃; transferring to a mixing kettle, cooling to 25-100 ℃, adding a solvent, and uniformly mixing; then adding hydrophilic monomer, fluorine silicon monomer and photoinitiator and mixing uniformly; performing ultraviolet irradiation to obtain the product;
wherein, the molar ratio of terephthalic acid to ethylene glycol is (1-2) to (1.2-1.6), and the molar ratio of the hydrophilic monomer to the fluorine-silicon monomer is 1 (0.5-3); the dosage of the additive is 0.25 wt% -0.70 wt% of the terephthalic acid; the dosage of the hydrophilic monomer is 10-20 wt% of the terephthalic acid; the dosage of the photoinitiator is 0.5 to 2 weight percent of the sum of the mass of the hydrophilic monomer and the mass of the fluorosilicone monomer; the solvent is one or the combination of at least two of trifluoroacetic acid, chloroform, phenol, tetrachloroethane, o-chlorophenol, benzene, chlorobenzene, trichloromethane, ethyl acetate, ethanol, acetone and diethyl ether;
the hydrophilic monomer is one or the combination of at least two of acrylic acid, butyl acrylate, N-isopropyl acrylamide, itaconic acid and hydroxyethyl methacrylate; the fluorine-silicon monomer is one or a mixture of two of vinyl dimethyl fluorine silane and (1-fluorine vinyl) methyl diphenyl silane, the chemical structural formula of the vinyl dimethyl fluorine silane is shown as formula 1, and the chemical structural formula of the (1-fluorine vinyl) methyl diphenyl silane is shown as formula 2;
formula 1
Figure 985099DEST_PATH_IMAGE001
(ii) a Formula 2
Figure 233678DEST_PATH_IMAGE002
The additive is a combination of at least two of titanium dioxide, lithium acetate, calcium acetate, zinc acetate, cobalt acetate, manganese acetate, antimony trioxide, ethylene glycol antimony and diisopropylamine.
2. The antistatic flame retardant polyester material according to claim 1, characterized in that: the solvent comprises ethyl acetate and trifluoroacetic acid in a volume ratio of (3-10) to 50; or ethyl acetate, chloroform and trifluoroacetic acid in a volume ratio of (3-10) to 40: 10.
3. The antistatic flame retardant polyester material according to claim 1, characterized in that: the photoinitiator is one or the combination of at least two of alpha-hydroxyisobutyrophenone, diphenyl- (2,4, 6-trimethylbenzoyl) oxyphosphorus, 1-hydroxycyclohexyl phenyl ketone and 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-acetone.
4. The antistatic flame retardant polyester material according to claim 1, characterized in that: before ultraviolet irradiation, electrostatic spinning is carried out to obtain a polyester fiber film, and then ultraviolet irradiation is carried out.
5. The antistatic flame retardant polyester material according to claim 1, characterized in that: the ultraviolet light source of the ultraviolet irradiation is an ultraviolet LED area light source, the ultraviolet wavelength is 300-400 nm, the ultraviolet irradiation time is 60-600s, and the light intensity of the ultraviolet irradiation is 120-5000 mW/cm 2
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2703436A1 (en) * 2012-08-28 2014-03-05 Ems-Patent Ag Polyamide moulding material and its application
CN105315864A (en) * 2014-07-04 2016-02-10 上海彩奇亮粉末涂料有限公司 Preparation method of aqueous double-component fluorosilicon acrylic acid polyurethane anti-corrosion coating
CN110128897A (en) * 2019-04-28 2019-08-16 湖南辰砾新材料有限公司 A kind of crosslinking with radiation cured flame-retardant coating and preparation method thereof
CN111088594A (en) * 2019-12-31 2020-05-01 常熟市欣鑫经纬编有限公司 Regenerated fiber fabric
CN111118724A (en) * 2019-12-31 2020-05-08 常熟市欣鑫经纬编有限公司 Preparation method of regenerated fiber fabric
CN111690171A (en) * 2020-07-10 2020-09-22 宁波保税区君一汽配科技有限公司 Flame retardant and flame-retardant PC plastic

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6036891A (en) * 1998-05-11 2000-03-14 Pharmacia & Upjohn Polymerizable hydrophilic ultraviolet light absorbing monomers
CN1763275A (en) * 2004-10-21 2006-04-26 天津石油化工公司化纤厂 Method for manufacturing fire retardant-antistatic polyester fiber
KR101418485B1 (en) * 2011-01-27 2014-07-10 에스케이이노베이션 주식회사 Polymer blend composition based on the carbon dioxide polymers and the environment friendly decorating materials using it
CN102391488B (en) * 2011-09-26 2013-06-05 四川东方绝缘材料股份有限公司 Preparation method for fluorine silicon phosphorus-containing anti-dropping flame-retardant polyethylene terephthalate
CN102926023B (en) * 2012-11-16 2014-07-23 东华大学 Preparation method of antistatic hydrophilic polyester fiber
CN103122583B (en) * 2013-01-31 2015-01-14 北京化工大学常州先进材料研究院 Preparation method of novel amphiphilic nano fiber having core-shell structure
CN105088770B (en) * 2015-08-12 2017-10-13 中国人民解放军总后勤部军需装备研究所 A kind of core-skin spins flame-retardant anti-dripping fibre and preparation method and application
CN107556463A (en) * 2017-10-08 2018-01-09 吉祥三宝高科纺织有限公司 A kind of preparation method of composite hydrophilic copolyesters
CN111171349A (en) * 2020-04-11 2020-05-19 李丹丹 Antistatic flame-retardant polyester film
CN111978522B (en) * 2020-09-08 2022-12-20 常州美胜生物材料有限公司 Preparation method of hydrophilic antistatic antibacterial copolyester master batch

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2703436A1 (en) * 2012-08-28 2014-03-05 Ems-Patent Ag Polyamide moulding material and its application
CN105315864A (en) * 2014-07-04 2016-02-10 上海彩奇亮粉末涂料有限公司 Preparation method of aqueous double-component fluorosilicon acrylic acid polyurethane anti-corrosion coating
CN110128897A (en) * 2019-04-28 2019-08-16 湖南辰砾新材料有限公司 A kind of crosslinking with radiation cured flame-retardant coating and preparation method thereof
CN111088594A (en) * 2019-12-31 2020-05-01 常熟市欣鑫经纬编有限公司 Regenerated fiber fabric
CN111118724A (en) * 2019-12-31 2020-05-08 常熟市欣鑫经纬编有限公司 Preparation method of regenerated fiber fabric
CN111690171A (en) * 2020-07-10 2020-09-22 宁波保税区君一汽配科技有限公司 Flame retardant and flame-retardant PC plastic

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
含氟硅丙烯酸酯乳液超疏水膜中疏水基团的梯度分布与表面微观结构研究;曲爱兰等;《高分子学报》;20071215(第12期);第1176-1182页 *
含氟聚丙烯酸酯防水易去污整理剂的合成与应用;田森等;《印染助剂》;20161020;第33卷(第10期);第9-14页 *

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