CN111269538B - Preparation method of barium sulfate polyethylene glycol terephthalate composite material - Google Patents
Preparation method of barium sulfate polyethylene glycol terephthalate composite material Download PDFInfo
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- 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
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- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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- 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
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- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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Abstract
The invention relates to a preparation method of a barium sulfate polyethylene glycol terephthalate composite material, which comprises the following steps of 1) adding ethylenediamine and phthalic anhydride into benzene, stirring, heating for reaction, cooling, adding deionized water, stirring, dispersing and performing rotary evaporation to obtain a modifier; 2): dispersing a modifier in ethanol, adding micron-sized barium sulfate particles, performing ultrasonic dispersion, and performing heating reaction to obtain modified barium sulfate; 3) premixing modified barium sulfate and polyethylene glycol terephthalate, melting and blending the mixture with an antioxidant, cooling extrudate by water, granulating and drying; 4) and injection molding to obtain the barium sulfate polyethylene glycol terephthalate composite material. The method can improve the compatibility of the inorganic nano particles and the polyethylene glycol terephthalate, so that the inorganic particles are uniformly dispersed in the polyethylene glycol terephthalate, and the transparency of the polyethylene glycol terephthalate is maintained and even improved while the mechanical properties such as tensile strength and the like of the polyethylene glycol terephthalate are improved.
Description
Technical Field
The application relates to a preparation method of a transparent plastic material, in particular to a preparation method of a barium sulfate polyethylene glycol terephthalate composite material.
Background
Polyethylene terephthalate is a thermoplastic saturated ester which is a condensation polymer made by the direct ester process of ethylene terephthalate or by the cross-linking process of polyethylene terephthalate and ethylene glycol. Non-toxic, odorless and tasteless crystalline linear polymer, and translucent milky white or colorless transparent particles. The flame-retardant polyester film has the characteristics of good temperature resistance, high mechanical strength, excellent electrical insulation, good chemical resistance and good flame retardance, and is widely applied to the packaging industry, and the preparation of films and containers. Common inorganic nano materials for modifying polyethylene terephthalate comprise silicon oxide, titanium oxide, zinc oxide, montmorillonite and the like, but because the interface bonding force between the inorganic material and a polymer is weak, the compatibility after compounding is extremely poor, the inorganic material is easy to exist in the polymer in a state of being agglomerated into particles, and the mechanical property of the composite material is reduced. In addition, when the inorganic material is compounded, the light transmittance of the polymer is easily lowered. How to improve the compatibility of the inorganic nanoparticles and the polyethylene terephthalate, so that the inorganic particles are uniformly dispersed in the polyethylene terephthalate, and the transparency of the polyethylene terephthalate is maintained or even improved while the mechanical properties such as tensile strength are improved, remains a problem to be solved.
Disclosure of Invention
The invention relates to a preparation method of a barium sulfate polyethylene terephthalate composite material, aiming at solving the technical problem of how to improve the compatibility of inorganic nano particles and polyethylene terephthalate, so that the inorganic particles are uniformly dispersed in the polyethylene terephthalate, and the transparency of the polyethylene terephthalate is maintained and even improved while the mechanical properties such as tensile strength and the like of the polyethylene terephthalate are improved.
A preparation method of a barium sulfate polyethylene terephthalate composite material comprises the following steps:
1) preparing a modifier: adding ethylenediamine into benzene, stirring and dispersing, adding phthalic anhydride, heating to 50-60 ℃ under rapid stirring, reacting for 30-40min, cooling, adding deionized water, stirring and dispersing, performing rotary evaporation at 70-75 ℃, and collecting a product at the bottom of a rotary evaporation bottle after most of the solvent is volatilized;
2) modification of barium sulfate: dispersing the product obtained in the step 1) in ethanol, adding micron-sized barium sulfate particles, performing ultrasonic dispersion uniformly, reacting at 40-50 ℃ for 2-3h, filtering, washing, and drying to obtain modified barium sulfate;
3) preparing a composite material: premixing the modified barium sulfate obtained in the step 2) with the dried polyethylene glycol terephthalate, adding the premixed material and an antioxidant into a double-screw extruder together for melt blending, wherein the melt blending temperature is 160-;
4) and 3) injection molding the blending product obtained in the step 3) to obtain the barium sulfate polyethylene terephthalate composite material.
Wherein the molar ratio of ethylenediamine to phthalic anhydride is about 1: 1.1-1.3.
Wherein the molar ratio of phthalic anhydride to barium sulfate is 1: 0.7-0.9.
Wherein, the barium sulfate accounts for 10-30% of the weight of the polyethylene glycol terephthalate.
Wherein the washing in the step 2) is washing by absolute ethyl alcohol, and the drying is vacuum drying for 10min at the temperature of 60 ℃.
Wherein the particle size of the barium sulfate is 0.08-0.2 micron.
Has the advantages that:
the invention utilizes the reaction of ethylenediamine and phthalic anhydride to open the ring of the anhydride, one carboxyl group is reserved, and the other carboxyl group reacts with one amido group of the ethylenediamine, thus preparing the modifier with the amido group and the carboxyl group. The carboxyl of the modifier can be adsorbed on the surface of barium sulfate particles, the hydrophilicity of barium sulfate is reduced, the hydrophobicity of barium sulfate is improved, when the modifier is blended with polyethylene terephthalate, the amido of the modifier can form a certain hydrogen bond effect with the polyethylene terephthalate, so that the compatibility of inorganic particles and the polyethylene terephthalate is enhanced, the barium sulfate can be uniformly dispersed in a polymer, the agglomeration is avoided, the mechanical property of the polymer is improved, and meanwhile, the dispersibility is good, the combination is sufficient, and the transparency of the polyethylene terephthalate is not reduced.
Detailed Description
Using polyethylene terephthalate having an intrinsic viscosity of 0.85dL/g, the tensile strength was 51.7MPa and the light transmittance was 90.2%.
The tensile strength of the composite was determined using GB/T1040-1992, with a sample size of 250mm 25mm 3 mm.
And (3) testing light transmittance, preparing 50mm by 50mm samples according to the GB/T2410-2008 standard, testing 5 samples, and taking the average value of the samples.
Example 1
1) Preparing a modifier: adding ethylenediamine into benzene, stirring and dispersing, then adding phthalic anhydride, heating to 60 ℃ under rapid stirring, reacting for 30min, cooling, then adding deionized water, stirring and dispersing, then carrying out rotary evaporation at 72 ℃, and collecting a product at the bottom of a rotary evaporation bottle after most of a solvent is volatilized;
2) modification of barium sulfate: dispersing the product obtained in the step 1) in ethanol, adding 0.08-micron barium sulfate particles, wherein the molar ratio of phthalic anhydride to barium sulfate is 1: 0.8, performing ultrasonic dispersion uniformly, reacting at 40 ℃ for 3h, filtering, washing with absolute ethanol, and performing vacuum drying at 60 ℃ for 10min to obtain modified barium sulfate;
3) preparing a composite material: premixing the modified barium sulfate obtained in the step 2) with dried polyethylene terephthalate, wherein the barium sulfate accounts for 10% of the weight of the polyethylene terephthalate, adding the barium sulfate and an antioxidant into a double-screw extruder together for melt blending, wherein the melt blending temperature is 160 ℃, the screw rotating speed is 160rpm, the feeding screw rotating speed is 30rpm, cooling extrudate by water, granulating and drying;
4) and 3) injection molding the blending product obtained in the step 3) to obtain the barium sulfate polyethylene terephthalate composite material.
The test shows that the tensile strength of the composite material is 65.1MPa, and the light transmittance is 92.7%.
Example 2
1) Preparing a modifier: adding ethylenediamine into benzene, stirring and dispersing, then adding phthalic anhydride, heating to 60 ℃ under rapid stirring, reacting for 30min, cooling, then adding deionized water, stirring and dispersing, then carrying out rotary evaporation at 72 ℃, and collecting a product at the bottom of a rotary evaporation bottle after most of the solvent is volatilized;
2) modification of barium sulfate: dispersing the product obtained in the step 1) in ethanol, adding 0.08-micron barium sulfate particles, wherein the molar ratio of phthalic anhydride to barium sulfate is 1: 0.8, performing ultrasonic dispersion uniformly, reacting at 40 ℃ for 3h, filtering, washing with absolute ethanol, and performing vacuum drying at 60 ℃ for 10min to obtain modified barium sulfate;
3) preparing a composite material: premixing the modified barium sulfate obtained in the step 2) with the dried polyethylene glycol terephthalate, wherein the barium sulfate accounts for 30% of the weight of the polyethylene glycol terephthalate, adding the barium sulfate and an antioxidant into a double-screw extruder together for melt blending, wherein the melt blending temperature is 160 ℃, the screw rotating speed is 160rpm, the feeding screw rotating speed is 30rpm, cooling an extrudate by water, granulating and drying;
4) and 3) injection molding the blending product obtained in the step 3) to obtain the barium sulfate polyethylene terephthalate composite material.
The test shows that the tensile strength of the composite material is 68.9MPa, and the light transmittance is 91.3%.
Example 3
1) Modification of barium sulfate: dispersing stearic acid in ethanol, adding 0.08-micron barium sulfate particles according to the molar ratio of stearic acid to barium sulfate of 1: 0.8, ultrasonically dispersing uniformly, reacting for 3h at 40 ℃, filtering, washing with absolute ethanol, and vacuum drying for 10min at 60 ℃ to obtain modified barium sulfate;
2) preparing a composite material: premixing the modified barium sulfate obtained in the step 2) with dried polyethylene glycol terephthalate, wherein the barium sulfate accounts for 10% of the weight of the polyethylene glycol terephthalate, adding the barium sulfate and an antioxidant into a double-screw extruder together for melt blending, wherein the melt blending temperature is 160 ℃, the screw rotating speed is 160rpm, the feeding screw rotating speed is 30rpm, cooling an extrudate by water, granulating and drying;
3) and 2) injection molding the blending product obtained in the step 2) to obtain the barium sulfate polyethylene terephthalate composite material.
The test shows that the tensile strength of the composite material is 53.6MPa, and the light transmittance is 88.5%.
Example 4
1) Preparing a modifier: adding ethylenediamine into benzene, stirring and dispersing, then adding phthalic anhydride, heating to 60 ℃ under rapid stirring, reacting for 30min, cooling, then adding deionized water, stirring and dispersing, then carrying out rotary evaporation at 72 ℃, and collecting a product at the bottom of a rotary evaporation bottle after most of the solvent is volatilized;
2) modification of barium sulfate: dispersing the product obtained in the step 1) in ethanol, adding 0.08-micron barium sulfate particles, wherein the molar ratio of phthalic anhydride to barium sulfate is 1: 0.8, performing ultrasonic dispersion uniformly, reacting at 40 ℃ for 3h, filtering, washing with absolute ethanol, and performing vacuum drying at 60 ℃ for 10min to obtain modified barium sulfate;
3) preparing a composite material: premixing the modified barium sulfate obtained in the step 2) with dried polyethylene terephthalate, wherein the barium sulfate accounts for 10% of the weight of the polyethylene terephthalate, adding the barium sulfate and an antioxidant into a double-screw extruder together for melt blending, wherein the melt blending temperature is 160 ℃, the screw rotating speed is 160rpm, the feeding screw rotating speed is 30rpm, cooling extrudate by water, granulating and drying;
4) and 3) injection molding the blending product obtained in the step 3) to obtain the barium sulfate polyethylene terephthalate composite material.
In the obtained composite material, the dispersibility of barium sulfate is not ideal, and the test shows that the tensile strength of the composite material is 43.4MPa, and the light transmittance is 86.9%.
Example 5
1) Preparing a modifier: adding ethylenediamine into benzene, stirring and dispersing, then adding phthalic anhydride, heating to 60 ℃ under rapid stirring, reacting for 30min, cooling, then adding deionized water, stirring and dispersing, then carrying out rotary evaporation at 72 ℃, and collecting a product at the bottom of a rotary evaporation bottle after most of the solvent is volatilized;
2) modification of barium sulfate: dispersing the product obtained in the step 1) in ethanol, adding 0.08-micron barium sulfate particles, uniformly dispersing phthalic anhydride and barium sulfate at a molar ratio of 1: 1 by ultrasonic, reacting at 40 ℃ for 3h, filtering, washing with absolute ethanol, and vacuum-drying at 60 ℃ for 10min to obtain modified barium sulfate;
3) preparing a composite material: premixing the modified barium sulfate obtained in the step 2) with dried polyethylene glycol terephthalate, wherein the barium sulfate accounts for 10% of the weight of the polyethylene glycol terephthalate, adding the barium sulfate and an antioxidant into a double-screw extruder together for melt blending, wherein the melt blending temperature is 160 ℃, the screw rotating speed is 160rpm, the feeding screw rotating speed is 30rpm, cooling an extrudate by water, granulating and drying;
4) and 3) injection molding the blending product obtained in the step 3) to obtain the barium sulfate polyethylene terephthalate composite material.
In the obtained composite material, the dispersibility of the barium sulfate is not ideal, and the test shows that the tensile strength of the composite material is 51.2MPa, and the light transmittance is 83.4%.
Claims (2)
1. A preparation method of a barium sulfate polyethylene terephthalate composite material is characterized by comprising the following steps: the method comprises the following steps:
1) preparing a modifier: adding ethylenediamine into benzene, stirring and dispersing, adding phthalic anhydride, heating to 50-60 ℃ under rapid stirring, reacting for 30-40min, cooling, adding deionized water, stirring and dispersing, performing rotary evaporation at 70-75 ℃, and collecting a product at the bottom of a rotary evaporation bottle after most of the solvent is volatilized;
2) modification of barium sulfate: dispersing the product obtained in the step 1) in ethanol, adding barium sulfate particles with the particle size of 0.08-0.2 microns, ultrasonically dispersing uniformly, reacting for 2-3h at 40-50 ℃, filtering, washing and drying to obtain modified barium sulfate;
3) preparing a composite material: premixing the modified barium sulfate obtained in the step 2) with the dried polyethylene glycol terephthalate, adding the premixed material and an antioxidant into a double-screw extruder together for melt blending, wherein the melt blending temperature is 160-;
4) injection molding the blending product obtained in the step 3) to obtain a barium sulfate polyethylene glycol terephthalate composite material;
the molar ratio of the ethylenediamine to the phthalic anhydride is 1: 1.1-1.3;
the molar ratio of phthalic anhydride to barium sulfate is 1: 0.7-0.9;
the barium sulfate accounts for 10-30% of the weight of the polyethylene terephthalate.
2. The method of claim 1, wherein: and in the step 2), the washing is carried out by using absolute ethyl alcohol, and the drying is carried out for 10min in vacuum at the temperature of 60 ℃.
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| CN110041672A (en) * | 2019-04-28 | 2019-07-23 | 杭州大华塑业有限公司 | A kind of fire retardant mylar and preparation method thereof |
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| CN104861519A (en) * | 2014-10-14 | 2015-08-26 | 青岛欣展塑胶有限公司 | Antistatic color master batch based on PET blending modification |
| CN104845133A (en) * | 2014-12-11 | 2015-08-19 | 青岛佳亿阳工贸有限公司 | PET/PTT alloy with metallic luster and preparation method thereof |
| CN106832814A (en) * | 2017-01-24 | 2017-06-13 | 杭州科翼科技有限公司 | A kind of polyester material of antiultraviolet and blue light |
| CN110041672A (en) * | 2019-04-28 | 2019-07-23 | 杭州大华塑业有限公司 | A kind of fire retardant mylar and preparation method thereof |
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