CN117304661B - Polyester composition, preparation method and application thereof - Google Patents

Polyester composition, preparation method and application thereof Download PDF

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CN117304661B
CN117304661B CN202311258846.0A CN202311258846A CN117304661B CN 117304661 B CN117304661 B CN 117304661B CN 202311258846 A CN202311258846 A CN 202311258846A CN 117304661 B CN117304661 B CN 117304661B
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reaction
titanium dioxide
carrying
nano titanium
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CN117304661A (en
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孟洪量
张园园
吴炎
王维
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Hunan Xinjiyuan New Material Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2237—Oxides; Hydroxides of metals of titanium
    • C08K2003/2241—Titanium dioxide
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/02—Flame or fire retardant/resistant

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses a polyester composition, a preparation method and application thereof, which are prepared from the following raw materials in parts by weight: 60-90 parts of polyethylene terephthalate, 5-10 parts of plasticizer, 5-15 parts of modified nano titanium dioxide, 0.5-1 part of talcum powder, 0.5-1 part of lubricant and 0.1-0.5 part of antioxidant.

Description

Polyester composition, preparation method and application thereof
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a polyester composition, a preparation method and application thereof.
Background
With the progress of social development, the demands of people on clothes are not only reflected in the attractive appearance, but also more new fabric clothes with comfort and various functionalities are needed. The polyester fiber is an important variety in the synthetic fiber, has the greatest advantages of good crease resistance and shape retention, but is not easy to sweat, has the feeling of thorn and is easy to generate static electricity, the use of the polyester fiber is always limited, the antibacterial performance of the conventional cotton fiber and polyester fiber blended fabric is insufficient to meet the demands of consumers on the functionality of the fabric, and with the social progress and the time development, the danger of fire occurrence is increased, and the fireproof textile and the flame retardant performance are also more and more concerned by people, so that under the condition of keeping the original performance of the polyester fiber, the novel polyester composition fiber fabric is developed, the problems are solved, and the consumption demands of the market can be better met.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a polyester composition, a preparation method and application thereof.
According to the invention, modified nano titanium dioxide is used as a filler, the nano titanium dioxide is easy to agglomerate, the performance of each property of the titanium dioxide is influenced, an organic molecular chain is grafted on the surface of the nano titanium dioxide, the polarity and agglomeration phenomenon of the nano titanium dioxide are improved, meanwhile, the nano titanium dioxide has ultraviolet absorption capacity, the grafted Schiff base and furan ring have better color generation, the ultraviolet absorption capacity of the titanium dioxide can be enhanced, meanwhile, ether oxygen bonds on the furan ring carry lone pair electrons, the antistatic property is realized, and when the titanium dioxide is irradiated by ultraviolet light, the sterilization effect of the Schiff base and the furan ring can be improved, the nitrogen-containing group and the phosphate group belong to P-N synergistic flame retardant components, flame retardance can be realized from condensed phases and multiple layers of gas phases, and the introduced ester group has good compatibility with a polyester matrix, so that uniform dispersion in polyester can be realized, and a better flame retardant effect is obtained.
The aim of the invention can be achieved by the following technical scheme:
a polyester composition is prepared from the following raw materials in parts by weight: 60-90 parts of polyethylene terephthalate, 5-10 parts of plasticizer, 5-15 parts of modified nano titanium dioxide, 0.5-1 part of talcum powder, 0.5-1 part of lubricant and 0.1-0.5 part of antioxidant.
Further, the plasticizer is one or more of benzoate, terephthalate and citrate.
Further, the lubricant is one or more than two of zinc stearate, calcium stearate, stearic acid and oleamide.
Further, the antioxidant is one of an antioxidant 1010, an antioxidant 1076 and an antioxidant 626.
Further, the modified nano titanium dioxide is prepared by the following steps:
s1, adding 5-hydroxymethylfurfural into a three-neck flask, adding absolute ethyl alcohol as a solvent, then adding glacial acetic acid as a catalyst, controlling the heating temperature to be 80 ℃, slowly dropwise adding diethylenetriamine into the three-neck flask by dissolving the diethylenetriamine in the ethanol, carrying out reflux reaction for 5 hours after the addition, carrying out reduced pressure rotary evaporation after the reaction is finished, washing a product with saturated NaCl solution for multiple times, and then carrying out vacuum drying to obtain an intermediate 1; the dosage ratio of the 5-hydroxymethylfurfural to the glacial acetic acid to the diethylenetriamine is 12.2g to 0.3mL to 5g;
under the condition of glacial acetic acid as a catalyst, the-CHO on 5-hydroxymethylfurfural molecules and the-NH on diethylenetriamine molecules 2 Chemical reaction is carried out to form-C=N-bond, the mol ratio of 5-hydroxymethylfurfural to diethylenetriamine is controlled to be 2:1, and an intermediate 1 is obtained, wherein the reaction process is as follows:
s2, placing triethylamine and the intermediate 1 into a three-neck flask, adding cyclohexane as a solvent, dissolving dimethyl phosphonochloride in the cyclohexane, slowly dropwise adding the solution into the three-neck flask at room temperature, controlling the heating temperature to be 85 ℃ after dropwise adding, carrying out reflux reaction for 5 hours, carrying out reduced pressure rotary evaporation after the reaction is finished, washing a product with saturated saline water for multiple times, and then placing the product into a vacuum drying box at 50 ℃ for drying for 6 hours to obtain the intermediate 2; the dosage ratio of triethylamine, intermediate 1 and dimethyl phosphonochloride is 3.1g:10g:7g;
under the catalysis of triethylamine, reacting-OH on the intermediate 1 molecule with-Cl on the dimethylphosphonyl chloride molecule, controlling the molar ratio of the two to be 1:2, and carrying out the following reaction process to obtain an intermediate 2;
s3, adding the intermediate 2 into a three-neck flask, then adding acetone as a solvent, stirring and dissolving, then adding anhydrous potassium carbonate, controlling the heating temperature to be 60 ℃ and refluxing for 1h, then slowly dropwise adding 2-chloroethanol, refluxing for reaction for 10h after the dropwise adding is finished, cooling to room temperature after the reaction is finished, filtering, collecting filtrate, performing reduced pressure rotary evaporation, recrystallizing a product by using acetone, and finally drying in a vacuum drying oven at 60 ℃ for 5h to obtain an intermediate 3; the dosage ratio of the intermediate 2, the acetone, the anhydrous potassium carbonate and the 2-chloroethanol is 10g to 120mL to 10g to 1.7g;
under the action of potassium carbonate, the intermediate 2 reacts with 2-chloroethanol to obtain an intermediate 3, and the specific reaction process is as follows:
s4, sequentially adding toluene, an intermediate 3, p-toluenesulfonic acid and phenylmalonic acid into a three-necked flask with a thermometer, a condenser pipe and a water separator, controlling the heating temperature to be 120 ℃ under the protection of nitrogen, carrying out reflux reaction for 8 hours, cooling to room temperature after the reaction is finished, adding a certain amount of distilled water, adding ethyl acetate for extraction for three times, collecting an organic phase, sequentially washing with a 5% sodium bicarbonate solution and a NaCl solution, and carrying out reduced pressure rotary evaporation to obtain a modifier; toluene, intermediate 3, p-toluene sulfonic acid, phenylmalonic acid in a ratio of 100mL:10g:0.4g:2.5g;
the mol ratio of the intermediate 3 to the phenylmalonic acid is controlled to be 1:1, and the p-toluenesulfonic acid is used as a catalyst to carry out esterification reaction to obtain a modifier, wherein the specific reaction process is as follows:
s5, adding a modifier, triethylamine and DMF into a flask, adding aminated titanium dioxide and N, N-diisopropylcarbodiimide, introducing nitrogen for protection, performing ultrasonic treatment for 30min, performing room temperature reaction for 6h, performing centrifugal separation on the reaction solution after the reaction is finished, washing 2-3 times by using DMF and ethanol water solution in sequence, and finally putting the product into a vacuum oven at 50 ℃ for drying for 3h to obtain modified nano titanium dioxide; the dosage ratio of the modifier, the triethylamine, the DMF, the aminated nano titanium dioxide and the N, N-diisopropylcarbodiimide is 10g to 2.7g to 100mL to 2.7g to 3.3g;
aminated titanium dioxide surface grafted-NH under the action of triethylamine and N, N-diisopropylcarbodiimide 2 Carrying out amidation reaction with-COOH on the modifier molecule to obtain the modified nano titanium dioxide.
The Ti-O bond in the nano titanium dioxide has larger specific surface area, water molecules are easy to absorb, a large number of hydroxyl groups in different bonding states are easy to form on the surface after the water molecules are polarized, so that particles are mutually contacted to form aggregation, each performance of the titanium dioxide is influenced, an organic molecular chain is grafted on the surface of the titanium dioxide, the polarity and aggregation phenomenon of the nano titanium dioxide are improved, meanwhile, the nano titanium dioxide has ultraviolet absorption capacity, the grafted Schiff base and the furan ring both contain O and N atoms with coordination capacity, a larger conjugated system exists, the color generation rate is better, the photoelectron generation rate of the titanium dioxide is improved, the light conversion rate is improved, the light response wave band is widened, the ultraviolet light is further absorbed by the ether-oxygen bond on the furan ring, the lone pair electrons are carried by the ether-oxygen bond on the furan ring, the capability of accepting protons is realized, the electrostatic dissipation effect can be realized through the transfer of internal protons, the antistatic property is realized, the electron cloud density of Schiff base and the furan ring can be improved when the titanium dioxide is irradiated by ultraviolet light, the polar absorption capacity is improved, the adsorption capacity with cells is improved, the nitrogen-containing groups and the nitrogen-containing groups are well dispersed, the flame retardant groups are well-dispersed with the flame retardant polyester can be better, and the flame retardant polyester is better in the flame retardant phase is better, and the flame retardant phase is better compatible with the flame retardant polyester is realized.
Further, the aminated nano titanium dioxide is prepared by the following steps:
adding a silane coupling agent KH550 into a three-neck flask, adding an ethanol aqueous solution with the volume ratio of 50% as a solvent, stirring for 20min at room temperature, adding nano titanium dioxide, controlling the heating temperature to be 70 ℃, carrying out reflux reaction for 1.5h, centrifuging after the reaction is finished, washing with the ethanol aqueous solution for three times, drying, and grinding to obtain the aminated nano titanium dioxide; the dosage ratio of the silane coupling agent KH550 to the ethanol aqueous solution to the nano-titania is 23g:230mL:10g.
It is another object of the present invention to provide a process for the preparation of a polyester composition comprising the steps of;
according to the proportion, polyethylene terephthalate, plasticizer, talcum powder, lubricant, antioxidant and modified nano titanium dioxide are put into a kneader to be evenly mixed, and then the mixture is put into a double screw for plasticizing, extrusion and granulation, thus obtaining the polyester composition.
Another object of the invention is to provide the use of such a polyester composition in the preparation of a fabric, a method of preparing a fabric comprising: slicing and melt spinning the polyester composition to obtain polyester fibers, and blending the polyester fibers and cotton fibers according to the mass ratio of 100:35-50 to obtain the fabric.
The invention has the beneficial effects that:
according to the invention, modified nano titanium dioxide is used as a filler, the nano titanium dioxide is easy to agglomerate, the performance of each property of the titanium dioxide is influenced, an organic molecular chain is grafted on the surface of the nano titanium dioxide, the polarity and agglomeration phenomenon of the nano titanium dioxide are improved, meanwhile, the nano titanium dioxide has ultraviolet absorption capacity, the grafted Schiff base and furan ring have better color generation, the ultraviolet absorption capacity of the titanium dioxide can be enhanced, meanwhile, ether oxygen bonds on the furan ring carry lone pair electrons, the antistatic property is realized, and when the titanium dioxide is irradiated by ultraviolet light, the sterilization effect of the Schiff base and the furan ring can be improved, the nitrogen-containing group and the phosphate group belong to P-N synergistic flame retardant components, flame retardance can be realized from condensed phases and multiple layers of gas phases, and the introduced ester group has good compatibility with a polyester matrix, so that uniform dispersion in polyester can be realized, and a better flame retardant effect is obtained.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Preparing aminated nano titanium dioxide:
23g of silane coupling agent KH550 is added into a three-neck flask, then 230mL of ethanol aqueous solution with the volume ratio of 50% is added as a solvent, stirring is carried out for 20min at room temperature, then 10g of nano titanium dioxide is added, the heating temperature is controlled to be 70 ℃, the reflux reaction is carried out for 1.5h, centrifugal separation is carried out after the reaction is finished, the three times of washing with the ethanol aqueous solution are carried out, and the amination nano titanium dioxide is obtained after drying and grinding.
Example 2
Preparing aminated nano titanium dioxide:
adding 46g of a silane coupling agent KH550 into a three-necked flask, adding 460mL of an ethanol water solution with the volume ratio of 50% as a solvent, stirring for 20min at room temperature, adding 20g of nano titanium dioxide, controlling the heating temperature to be 70 ℃, carrying out reflux reaction for 1.5h, centrifuging after the reaction is finished, washing with the ethanol water solution for three times, drying, and grinding to obtain the aminated nano titanium dioxide.
Example 3
Preparing modified nano titanium dioxide:
s1, adding 12.2g of 5-hydroxymethylfurfural into a three-neck flask, adding absolute ethyl alcohol as a solvent, then adding 0.3g of glacial acetic acid as a catalyst, controlling the heating temperature to be 80 ℃, slowly dropwise adding 5g of diethylenetriamine into the three-neck flask by dissolving the diethylenetriamine into the ethanol, carrying out reflux reaction for 5 hours after the addition, carrying out reduced pressure rotary evaporation after the reaction is finished, washing a product with saturated NaCl solution for multiple times, and then carrying out vacuum drying to obtain an intermediate 1;
s2, placing 3.1g of triethylamine and 10g of intermediate 1 into a three-neck flask, adding cyclohexane as a solvent, dissolving 7g of dimethyl phosphono chloride into the cyclohexane, slowly dropwise adding the mixture into the three-neck flask at room temperature, controlling the heating temperature to be 85 ℃ after the dropwise adding is finished, carrying out reflux reaction for 5 hours, carrying out reduced pressure rotary evaporation after the reaction is finished, washing a product with saturated saline for multiple times, and then placing the product into a vacuum drying box at 50 ℃ for drying for 6 hours to obtain an intermediate 2;
s3, adding 10g of intermediate 2 into a three-neck flask, then adding 120mL of acetone as a solvent, stirring and dissolving, then adding 10g of anhydrous potassium carbonate, controlling the heating temperature to be 60 ℃ and refluxing for 1h, then slowly dropwise adding 1.7g of 2-chloroethanol, after the dropwise adding is completed, carrying out reflux reaction for 10h, cooling to room temperature after the reaction is completed, then filtering, collecting filtrate, carrying out reduced pressure rotary evaporation, recrystallizing a product with acetone, and finally putting into a vacuum drying box at 60 ℃ and drying for 5h to obtain an intermediate 3;
s4, sequentially adding 100mL of toluene, 10g of intermediate 3, 0.4g of p-toluenesulfonic acid and 2.5g of phenylmalonic acid into a three-necked flask with a thermometer, a condenser and a water separator, controlling the heating temperature to 120 ℃ under the protection of nitrogen, carrying out reflux reaction for 8 hours, cooling to room temperature after the reaction is finished, adding a certain amount of distilled water, then adding ethyl acetate for extraction for three times, collecting an organic phase, sequentially washing with 5% sodium bicarbonate solution and NaCl solution, and then carrying out reduced pressure rotary evaporation to obtain a modifier;
s5, adding 10g of modifier, 2.7g of triethylamine and 100mL of DMF into a flask, adding 2.7g of the aminated nano titanium dioxide prepared in the example 1 and 3.3g of N, N-diisopropylcarbodiimide, introducing nitrogen for protection, performing ultrasonic treatment for 30min, reacting at room temperature for 6h, centrifugally separating reaction liquid after the reaction is finished, washing the reaction liquid with DMF and ethanol water solution for 2-3 times in sequence, and finally drying the product in a vacuum oven at 50 ℃ for 3h to obtain the modified nano titanium dioxide.
Example 4
Preparing modified nano titanium dioxide:
s1, adding 24.4g of 5-hydroxymethylfurfural into a three-neck flask, adding absolute ethyl alcohol as a solvent, then adding 0.6g of glacial acetic acid as a catalyst, controlling the heating temperature to be 80 ℃, slowly dropwise adding 10g of diethylenetriamine into the three-neck flask by dissolving the diethylenetriamine into the ethanol, carrying out reflux reaction for 5 hours after the addition, carrying out reduced pressure rotary evaporation after the reaction is finished, washing a product with saturated NaCl solution for multiple times, and then carrying out vacuum drying to obtain an intermediate 1;
s2, placing 6.2g of triethylamine and 20g of intermediate 1 into a three-neck flask, adding cyclohexane as a solvent, dissolving 14g of dimethyl phosphono chloride into the cyclohexane, slowly dropwise adding the mixture into the three-neck flask at room temperature, controlling the heating temperature to be 85 ℃ after the dropwise adding is finished, carrying out reflux reaction for 5 hours, carrying out reduced pressure rotary evaporation after the reaction is finished, washing a product with saturated saline for multiple times, and then placing the product into a vacuum drying box at 50 ℃ for drying for 6 hours to obtain an intermediate 2;
s3, adding 20g of intermediate 2 into a three-neck flask, then adding 240mL of acetone as a solvent, stirring and dissolving, then adding 20g of anhydrous potassium carbonate, controlling the heating temperature to be 60 ℃ and refluxing for 1h, then slowly dropwise adding 3.4g of 2-chloroethanol, after the dropwise adding is completed, carrying out reflux reaction for 10h, cooling to room temperature after the reaction is completed, then filtering, collecting filtrate, carrying out reduced pressure rotary evaporation, recrystallizing a product by acetone, and finally putting into a vacuum drying box at 60 ℃ and drying for 5h to obtain an intermediate 3;
s4, sequentially adding 200mL of toluene, 20g of intermediate 3, 0.8g of p-toluenesulfonic acid and 5g of phenylmalonic acid into a three-necked flask with a thermometer, a condenser pipe and a water separator, controlling the heating temperature to 120 ℃ under the protection of nitrogen, carrying out reflux reaction for 8 hours, cooling to room temperature after the reaction is finished, adding a certain amount of distilled water, then adding ethyl acetate for extraction for three times, collecting an organic phase, sequentially washing with 5% sodium bicarbonate solution and NaCl solution, and then carrying out reduced pressure rotary evaporation to obtain a modifier;
s5, adding 20g of modifier, 5.4g of triethylamine and 200mL of DMF into a flask, adding 5.4g of the aminated nano titanium dioxide prepared in the example 2 and 6.6g of N, N-diisopropylcarbodiimide, introducing nitrogen for protection, performing ultrasonic treatment for 30min, reacting at room temperature for 6h, centrifuging the reaction solution after the reaction is finished, washing the reaction solution with DMF and ethanol water solution for 2-3 times in sequence, and finally drying the product in a vacuum oven at 50 ℃ for 3h to obtain the modified nano titanium dioxide.
Example 5
6kg of polyethylene terephthalate, 500g of benzoate, 50g of talcum powder, 50g of zinc stearate, 10g of antioxidant 1010 and 500g of modified nano titanium dioxide prepared in example 3 are placed in a kneader to be uniformly mixed, and then the mixture is put into a double screw for plasticizing, extrusion and granulation, thus obtaining the polyester composition.
Example 6
7.5kg of polyethylene terephthalate, 750g of terephthalic acid ester, 75g of talcum powder, 75g of calcium stearate, 30g of antioxidant 1076 and 750g of modified nano titanium dioxide prepared in example 4 are placed in a kneader to be uniformly mixed, and then the mixture is put into a twin screw for plasticizing, extruding and granulating to obtain a polyester composition.
Example 7
9kg of polyethylene terephthalate, 1kg of citric acid ester, 100g of talcum powder, 100g of stearic acid, 50g of antioxidant 626 and 1kg of modified nano titanium dioxide prepared in example 3 are placed in a kneader for uniform mixing, and then the mixture is put into a double screw for plasticizing, extrusion granulation, thus obtaining a polyester composition.
Comparative example 1
Compared with example 5, the polyester composition is obtained by using nano titanium dioxide instead of modified nano titanium dioxide in the preparation process, and keeping the rest raw materials and the preparation process unchanged.
The materials prepared in examples 5 to 7 and comparative example 1 were extruded into standard plaques using an extruder, and the following performance tests were performed:
test item Test standard Example 5 Example 6 Example 7 Comparative example 1
Oxygen index/% GB/T2406 31.2 29.7 30.9 25.3
Maximum smoke density (flameless method) GB/T8323.1-2008 58.3 59.5 58.7 65.3
Tensile Strength/MPa ASTMD-412 33.9 34.5 33.6 26.5
Flexural Strength/MPa ASTMD-790 60.5 63.2 61.2 52.2
The materials prepared in examples 5-7 and comparative example 1 were respectively sliced and melt-spun to prepare polyester fibers, and then the polyester fibers and spandex fibers were blended at a mass ratio of 100:35 to obtain a fabric, and the following performance tests were performed:
test item Test standard Example 5 Example 6 Example 7 Comparative example 1
Charge area density/uC.m -2 GB/T12703.1-2008 0.074 0.075 0.073 0.084
Antibacterial rate GB/T20944.2-2007 97 97 96 86
Ultraviolet resistance (UPF) AS/NZS4399:1996 40 43 42 30
From the above table data, it can be seen that examples 5 to 7 have higher mechanical properties, better oxygen index and smoke density, and better flame retardant properties, and are more excellent in antistatic, antibacterial and ultraviolet-proof properties after being made into fabrics, compared with comparative example 1 in which nano titanium dioxide is not modified.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or in a similar manner, by those skilled in the art, without departing from the scope of the invention or exceeding the scope of the invention as defined in the claims.

Claims (5)

1. The polyester composition is characterized by being prepared from the following raw materials in parts by weight: 60-90 parts of polyethylene terephthalate, 5-10 parts of plasticizer, 5-15 parts of modified nano titanium dioxide, 0.5-1 part of talcum powder, 0.5-1 part of lubricant and 0.1-0.5 part of antioxidant;
the modified nano titanium dioxide is prepared by the following steps:
s1, adding 5-hydroxymethylfurfural into a three-neck flask, adding absolute ethyl alcohol as a solvent, then adding glacial acetic acid as a catalyst, controlling the heating temperature to be 80 ℃, slowly dropwise adding diethylenetriamine into the three-neck flask by dissolving the diethylenetriamine in the ethanol, carrying out reflux reaction for 5 hours after the addition, carrying out reduced pressure rotary evaporation after the reaction is finished, washing a product with saturated NaCl solution for multiple times, and then carrying out vacuum drying to obtain an intermediate 1; the dosage ratio of the 5-hydroxymethylfurfural to the glacial acetic acid to the diethylenetriamine is 12.2g to 0.3mL to 5g;
s2, placing triethylamine and the intermediate 1 into a three-neck flask, adding cyclohexane as a solvent, dissolving dimethyl phosphonochloride in the cyclohexane, slowly dropwise adding the solution into the three-neck flask at room temperature, controlling the heating temperature to be 85 ℃ after dropwise adding, carrying out reflux reaction for 5 hours, carrying out reduced pressure rotary evaporation after the reaction is finished, washing a product with saturated saline water for multiple times, and then placing the product into a vacuum drying box at 50 ℃ for drying for 6 hours to obtain the intermediate 2; the dosage ratio of triethylamine, intermediate 1 and dimethyl phosphonochloride is 3.1g:10g:7g;
s3, adding the intermediate 2 into a three-neck flask, then adding acetone as a solvent, stirring and dissolving, then adding anhydrous potassium carbonate, controlling the heating temperature to be 60 ℃ and refluxing for 1h, then slowly dropwise adding 2-chloroethanol, refluxing for reaction for 10h after the dropwise adding is finished, cooling to room temperature after the reaction is finished, filtering, collecting filtrate, performing reduced pressure rotary evaporation, recrystallizing a product by using acetone, and finally drying in a vacuum drying oven at 60 ℃ for 5h to obtain an intermediate 3; the dosage ratio of the intermediate 2, the acetone, the anhydrous potassium carbonate and the 2-chloroethanol is 10g to 120mL to 10g to 1.7g;
s4, sequentially adding toluene, an intermediate 3, p-toluenesulfonic acid and phenylmalonic acid into a three-necked flask with a thermometer, a condenser pipe and a water separator, controlling the heating temperature to be 120 ℃ under the protection of nitrogen, carrying out reflux reaction for 8 hours, cooling to room temperature after the reaction is finished, adding a certain amount of distilled water, adding ethyl acetate for extraction for three times, collecting an organic phase, sequentially washing with a 5% sodium bicarbonate solution and a NaCl solution, and carrying out reduced pressure rotary evaporation to obtain a modifier; toluene, intermediate 3, p-toluene sulfonic acid, phenylmalonic acid in a ratio of 100mL:10g:0.4g:2.5g;
s5, adding a modifier, triethylamine and DMF into a flask, adding aminated titanium dioxide and N, N-diisopropylcarbodiimide, introducing nitrogen for protection, performing ultrasonic treatment for 30min, performing room temperature reaction for 6h, performing centrifugal separation on the reaction solution after the reaction is finished, washing 2-3 times by using DMF and ethanol water solution in sequence, and finally putting the product into a vacuum oven at 50 ℃ for drying for 3h to obtain modified nano titanium dioxide; the dosage ratio of the modifier, the triethylamine, the DMF, the aminated nano titanium dioxide and the N, N-diisopropylcarbodiimide is 10g to 2.7g to 100mL to 2.7g to 3.3g;
the aminated titanium oxide in step S5 is prepared by the steps of:
adding a silane coupling agent KH550 into a three-neck flask, adding an ethanol aqueous solution with the volume ratio of 50% as a solvent, stirring for 20min at room temperature, adding nano titanium dioxide, controlling the heating temperature to be 70 ℃, carrying out reflux reaction for 1.5h, centrifuging after the reaction is finished, washing with the ethanol aqueous solution for three times, drying, and grinding to obtain the aminated titanium dioxide; the dosage ratio of the silane coupling agent KH550 to the ethanol aqueous solution to the nano-titania is 23g:230mL:10g.
2. The polyester composition according to claim 1, wherein the plasticizer is one or more of benzoate, terephthalate and citrate.
3. A polyester composition according to claim 1, wherein the lubricant is one or more of zinc stearate, calcium stearate, stearic acid, oleamide.
4. The method of preparing a polyester composition according to claim 1, comprising the steps of:
according to the proportion, polyethylene terephthalate, plasticizer, talcum powder, lubricant, antioxidant and modified nano titanium dioxide are put into a kneader to be evenly mixed, and then the mixture is put into a double screw for plasticizing, extrusion and granulation, thus obtaining the polyester composition.
5. Use of a polyester composition according to claim 1 in a textile fabric.
CN202311258846.0A 2023-09-27 2023-09-27 Polyester composition, preparation method and application thereof Active CN117304661B (en)

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