CN111732819B - Polyester resin composition and preparation method and application thereof - Google Patents
Polyester resin composition and preparation method and application thereof Download PDFInfo
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- CN111732819B CN111732819B CN202010452425.1A CN202010452425A CN111732819B CN 111732819 B CN111732819 B CN 111732819B CN 202010452425 A CN202010452425 A CN 202010452425A CN 111732819 B CN111732819 B CN 111732819B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/52—Encapsulations
- H01L33/56—Materials, e.g. epoxy or silicone resin
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/58—Optical field-shaping elements
- H01L33/60—Reflective elements
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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
- 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
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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
- 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
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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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
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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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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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
- C08K2201/00—Specific properties of additives
- C08K2201/016—Additives defined by their aspect ratio
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
Abstract
The invention discloses a polyester resin composition, a preparation method and application thereof, wherein the polyester resin composition comprises polyester resin and white pigment; the polyester resin comprises PCT resin and hyperbranched polyester; the molecular weight of the hyperbranched polyester is 900-15000 g/mol, and the acid value is 100-400 mg KOH/g; the weight ratio of the hyperbranched polyester to the polyester resin is (0.5-10) to 60. According to the invention, the hyperbranched polyester with specific molecular weight and carboxyl content and the PCT resin are used together, and the addition amount of the hyperbranched polyester is controlled to obtain the polyester resin composition with excellent fluidity, so that the bonding force between a molded product prepared from the polyester resin composition and silica gel can be effectively improved, the molded product and the silica gel are not easy to separate, the reflectivity is excellent, and the luminosity retention rate of a light-emitting device assembled by an LED reflector plate prepared from the polyester resin composition is effectively improved.
Description
Technical Field
The invention relates to the technical field of thermoplastic resin compositions, in particular to a polyester resin composition and a preparation method and application thereof.
Background
The advent of Light Emitting Diodes (LEDs) has brought the lighting industry into the semiconductor lighting era. The LED light source has the advantages of high reliability, high luminous power, low power consumption, high corresponding speed, long service life, low price, rich colors and the like. Following gas lighting, incandescent and fluorescent lamps, LEDs are becoming a new generation of mainstream lighting technology. With the development of the times and the advancement of science and technology, LEDs have been widely applied to various fields such as street lamps, indoor lighting, backlight display screens, automobile headlamps, landscape lamps, and the like.
The LED bracket is used as a chip carrier, has both the electric conduction function and the heat conduction function, and is an indispensable key auxiliary material for LED devices. The materials used as LED support are mainly high temperature resistant polyamide (PPA) and high temperature resistant polyester (cyclohexyldimethyl terephthalamide, PCT). The high-temperature resistant polyamide (mainly comprising PA46, PA6T and PA9T) has high initial whiteness, good heat resistance, high fluidity, low cost and suitability for injection molding process, and is the mainstream material of the LED bracket at present. However, the photo-thermal aging of the PPA material is relatively fast, and the PPA material can only be used for low-power products at present. With the introduction of high-voltage LEDs, PCT has great advantages in application to medium and high power LED reflecting plates due to excellent high-temperature discoloration resistance.
The LED packaging adhesive mainly comprises epoxy resin and silica gel, the silica gel has the remarkable characteristics of excellent mechanical property, ageing resistance, good thermal stability, weather resistance, flexibility, high light transmittance, small internal stress, low hygroscopicity and the like, and compared with the epoxy resin, the performance of the silica gel can better meet the packaging requirement of high-power and high-brightness LED products. Therefore, silica gel is rapidly replacing epoxy resin, and becomes a new generation of more ideal LED packaging material.
However, the bonding force between the LED reflecting plate made of the PCT material and the silica gel is poor, the problem that the LED reflecting plate is separated from the silica gel can occur in the aging and actual use processes, oxygen and water vapor in the air invade the inside of an LED lamp bead through a gap generated by separation, so that the lamp bead is dead, the lamp is invalid, and the service life is reduced.
The prior art improves the reflectivity, the aging resistance and the light stability of the PCT material, but reports for improving the binding force between an LED reflecting plate made of the PCT material and silica gel are not found. For example: prior art CN105531319A discloses a thermoplastic resin composition which is imparted with discoloration resistance and impact resistance by the addition of a reactive polysiloxane. Prior art CN105849190A discloses a thermoplastic resin composition which has excellent light efficiency, discoloration resistance and light stability, while maintaining impact strength and molding processability, by adding a silicon-containing graft copolymer. The prior art CN106084672A discloses a thermoplastic resin composition, which has high reflectivity and light efficiency and excellent discoloration resistance by adding sodium phosphate. Prior art CN103849126A mentions improving the heat and light aging properties of polyester compositions by adding metal oxides. The LED reflecting plate made of the PCT material in the prior art is insufficient in binding force with silica gel, so that the LED reflecting plate and the silica gel are separated, and the service life of an LED lamp bead is influenced.
Therefore, there is a need to improve the existing PCT materials to improve the adhesion of molded articles made from the PCT materials to silicone gels.
Disclosure of Invention
The invention provides a polyester resin composition for overcoming the defect of poor binding force between a molded product prepared from the PCT material and silica gel in the prior art, the provided polyester resin composition can be used for a molding composition, has excellent fluidity, and the prepared molded product has good binding force with the silica gel and excellent reflectivity.
Another object of the present invention is to provide a method for preparing the polyester resin composition.
The invention also aims to provide application of the polyester resin composition in preparing an LED reflecting plate.
It is still another object of the present invention to provide a molded article obtained from the above polyester resin composition.
Still another object of the present invention is to provide an LED reflector made of the polyester resin composition.
In order to solve the technical problems, the invention adopts the technical scheme that:
a polyester resin composition comprising a polyester resin and a white pigment;
the polyester resin comprises PCT resin and hyperbranched polyester; the number average molecular weight of the hyperbranched polyester is 900-15000 g/mol, and the acid value is 100-400 mg KOH/g; the weight ratio of the hyperbranched polyester to the polyester resin is (0.5-10) to 60.
PCT resins, i.e. polycyclohexylenedimethylene terephthalates, are commonly used in the art as high temperature resistant polyesters. PCT resins are commercially available and have the formula
Can be produced by the polycondensation of terephthalic acid and 1, 4-cyclohexanedimethanol.
The polyester resin composition taking PCT resin as a main resin can be used for preparing molded products, in particular for preparing LED reflecting plates, and the components of the polyester resin composition generally comprise polyester resin and white pigment. The amount of the white pigment added in the present application may be an amount conventionally added in the art.
The hyperbranched polyester can be divided into hydroxyl-terminated hyperbranched polyester and carboxyl-terminated hyperbranched polyester. The hyperbranched polyester used in the present application is a carboxyl-terminated hyperbranched polyester. For carboxyl-terminated hyperbranched polyesters, the carboxyl content is generally expressed in terms of acid number, which is relatively high. The hydroxyl value of the carboxyl-terminated hyperbranched polyester is lower, and is generally less than 15mg KOH/g.
The carboxyl-terminated hyperbranched polyester can be carboxyl-terminated aliphatic hyperbranched polyester and/or carboxyl-terminated aromatic hyperbranched polyester. The commercially available carboxyl-terminated hyperbranched polyesters are generally aromatic hyperbranched polyesters.
The inventor researches and discovers that when hyperbranched polyester with specific molecular weight and carboxyl content is used together with PCT resin, and the adding amount of the hyperbranched polyester is controlled, a polyester resin composition with excellent fluidity can be prepared, the binding force of a molded product prepared from the polyester resin composition and silica gel can be effectively improved, the molded product is not easy to separate from the silica gel, and the reflectivity is excellent.
When the hyperbranched polyester with specific molecular weight and carboxyl content is used together with the PCT resin, the hyperbranched polyester contains ester bonds and has good compatibility with the PCT matrix, and the hyperbranched polyester can migrate to the surface of the polyester resin composition in the injection molding process. When silica gel is packaged, carboxyl on the hyperbranched polyester can chemically react with hydroxyl groups on the surface of the silica gel, so that the binding force of the polyester resin composition and the silica gel is improved. The technology is applied to the field of LED reflecting plates, can improve the binding force between the LED reflecting plate made of a polyester resin composition (such as a PCT material) and silica gel, does not cause the problem of separation of the LED reflecting plate and the silica gel in a high-temperature and high-humidity environment, and prolongs the service life of LED lamp beads. In addition, the hyperbranched polyester is added, so that the fluidity of the polyester resin composition is remarkably improved, and the polyester resin composition is particularly suitable for the characteristic of multi-mode hole forming of an LED reflecting plate.
If the molecular weight of the hyperbranched polyester is less than 900g/mol, the molecular weight is too low, which can cause poor thermal stability of the hyperbranched polyester and degradation failure in the processing and forming processes; and if the molecular weight is too high and is more than 15000g/mol, the hyperbranched polyester has poor fluidity and can not migrate to the surface of a material during injection molding, so that the binding force with silica gel is improved. Also, the carboxyl group content is important. If the acid value is too low and is less than 100mg KOH/g, the binding force with silica gel is insufficient; if the acid value is too high, more than 400mg KOH/g, the hyperbranched polyester is discolored in a high-temperature and high-humidity environment, and the reflectivity of the polyester composition is affected.
In addition, if the usage amount of the hyperbranched polyester in the polyester resin is too low, namely the weight ratio of the hyperbranched polyester to the polyester resin is less than 0.5: 60, the bonding force between a molded product prepared from the polyester resin composition and silica gel cannot be effectively improved; if the amount is too high, the overall properties of the polyester resin composition are lowered.
In conclusion, the polyester resin composition of the present invention can be used for a molding composition, has excellent flowability, and can produce a molded article having good adhesion to silica gel and excellent reflectance.
Preferably, the molecular weight of the hyperbranched polyester is 1000-10000 g/mol, and the acid value is 200-350 mgKOH/g. When the molecular weight of the hyperbranched polyester is 1000-10000 g/mol and the acid value is 200-350 mg KOH/g, the bonding force between a molded product prepared from the polyester resin composition and silica gel is further improved.
Preferably, the weight ratio of the hyperbranched polyester to the polyester resin is (2-5) to 60. The bonding force between a molded product prepared from the polyester resin composition and silica gel can be adjusted by controlling the using amount of the hyperbranched polyester in the polyester resin. When the weight ratio of the hyperbranched polyester to the polyester resin is (2-5) to 60, the molded product prepared from the polyester resin composition has better bonding force with silica gel.
Preferably, the intrinsic viscosity of the PCT resin is 0.6-0.8 dL/g.
The white pigment may be a white pigment conventional in the art. The white pigment includes, but is not limited to, titanium dioxide, zinc oxide, zinc sulfide, white lead, zinc sulfate, barium sulfate, calcium carbonate, aluminum oxide, and the like, and mixtures thereof.
In the art, the white pigment is typically subjected to a surface modification treatment. In one embodiment, the white pigment is titanium dioxide, and the surface thereof is treated with a silicone compound. The white pigment has an average particle size of 0.2 to 0.4 μm.
Preferably, the weight ratio of the white pigment to the polyester resin is (1-4): 6.
Preferably, the polyester resin composition further comprises a reinforcing material.
More preferably, the reinforcing material is one or a combination of two or more of glass fiber, wollastonite, potassium titanate whisker, kaolin, talc or mica.
Glass fibers are common reinforcing materials in the art. Optionally, the glass fiber comprises the following components in percentage by weight: 60-67 wt% of silicon dioxide and 33-40 wt% of alumina.
Preferably, the weight percentage of the polyester resin is 50-60%, the weight percentage of the white pigment is 10-30%, and the weight percentage of the reinforcing material is 10-30%.
The polyester resin composition may further contain additives, if necessary. Additives include, without limitation, antioxidants, impact modifiers, flame retardants, optical brighteners, lubricants, plasticizers, thickeners, antistatic agents, nucleating agents, UV stabilizers, mold release agents, dyes, and the like, and mixtures thereof.
The invention also provides a preparation method of the polyester resin composition.
When no reinforcing material is added, the preparation method comprises the following steps: uniformly mixing the PCT resin and the hyperbranched polyester, then melting and blending the mixture with a white pigment, and extruding and granulating to obtain the polyester resin composition.
When the reinforcing material is added, the preparation method comprises the following steps: uniformly mixing the PCT resin and the hyperbranched polyester, then, carrying out melt blending on the mixture, the white pigment and the reinforcing material, and carrying out extrusion granulation to obtain the polyester resin composition.
Similarly, when additives are added, the preparation method comprises the following steps: uniformly mixing the PCT resin and the hyperbranched polyester, then carrying out melt blending, extrusion and granulation with the white pigment, the reinforcing material and the additive to obtain the polyester resin composition.
The mixing of the PCT resin with the hyperbranched polyester can be carried out by means of a high-speed stirrer.
The melt blending and the extrusion granulation can be carried out by a double-screw extruder, and the temperature of the double-screw extruder is set to be 230-300 ℃.
The application of the polyester resin composition in the preparation of the LED reflecting plate is also within the protection scope of the invention.
The present invention also provides a molded article prepared from the above polyester resin composition. Specifically, the above polyester composition is molded in a mold to obtain a molded article.
The invention also provides an LED reflecting plate, which is prepared from the polyester resin composition. The LED reflector belongs to a molded product and can be obtained by molding the polyester composition in a mold.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the hyperbranched polyester with specific molecular weight and carboxyl content and the PCT resin are used together, and the addition amount of the hyperbranched polyester is controlled to obtain the polyester resin composition with excellent fluidity, so that the bonding force between a molded product prepared from the polyester resin composition and silica gel can be effectively improved, the molded product and the silica gel are not easy to separate, the reflectivity is excellent, and the luminosity retention rate of a light-emitting device assembled by an LED reflecting plate prepared from the polyester resin composition is effectively improved.
Drawings
Fig. 1 is a schematic view of the structure of a light-emitting device in example 16 of the present invention and comparative example 4.
Detailed Description
The present invention will be further described with reference to the following embodiments.
The raw materials in the examples are all commercially available;
the polyester resin includes PCT resin and hyperbranched polyester.
PCT resin: from Eastman Chemical Products, PCT36296, intrinsic viscosity 0.719 dL/g.
Hyperbranched polyester: from Wuhan hyper branched resin Science, Inc. (Wuhan hyper branched Polymers Science & Technology Co., Ltd.). Structure of aromatic polyester: c101, C103, C104, C201; long-chain aromatic polyester structure: c302, C303, C304; heat-resistant aromatic polyester structure: c401 and C403.
White pigment: using titanium dioxide (TiO) subjected to surface treatment with a silicone compound 2 ) (R105, DuPont Co., Ltd (USA)), average particle diameter: 0.31 μm.
Reinforcing materials: f7x 28: NITTO BOSEKI, Japan, short glass fiber CSG3PA-820 consisting of E-glass having a length of 3mm, a main cross-sectional axis of 28 μm, a minor cross-sectional axis of 7 μm and an axial ratio of 4 (non-circular cross-section), silica 60-67 wt%, and alumina 33-40 wt%.
Silica gel: LED packaging silica gel, UH-6950-1(AB gel), commercially available from Shenzhen Yongxinren technologies, Inc.
The reagents, methods and apparatus employed in the present invention are conventional in the art, except as otherwise indicated.
Examples 1 to 15 and comparative examples 1 to 3
The amounts of the raw materials used in the examples of the present invention and the comparative examples are shown in table 1.
The polyester resin compositions of examples 1 to 14 were prepared as follows:
uniformly mixing the PCT resin and the hyperbranched polyester, then carrying out melt blending with the white pigment and the reinforcing material, and carrying out extrusion granulation to obtain the polyester resin composition. Mixing the PCT resin and the hyperbranched polyester by a high-speed stirrer. And carrying out melt blending and extrusion granulation through a double-screw extruder, wherein the temperature of the double-screw extruder is set to be 230-300 ℃.
The polyester resin composition of example 15 was prepared as follows:
uniformly mixing PCT resin and hyperbranched polyester, then melting and blending the mixture with white pigment, extruding and granulating to obtain the polyester resin composition. Mixing the PCT resin and the hyperbranched polyester by a high-speed stirrer. The melt blending and the extrusion granulation are carried out through a double-screw extruder, and the temperature of the double-screw extruder is set to be 230-300 ℃.
Example 16
This example provides a molded article, specifically an LED reflector, injection molded using the polyester resin composition of example 9, having a size of 2835. The light emitting device composed of the LED reflector is shown in fig. 1, where 1 is an LED reflector, 2 is a metal sheet, 3 is a substrate, 4 is LED packaging silica gel, 5 is a wire, and 6 is a blue light emitting diode having a light peak wavelength at 460 nm.
Comparative example 4
This comparative example provides a molded article, specifically an LED reflector plate, made of the polyester resin composition of comparative example 1, size 2835. A light-emitting device having the same structure as in example 16 was constructed using this LED reflection plate; the other components of the light emitting device constructed in this comparative example except for the LED reflection plate were in accordance with example 16.
TABLE 1 raw material usage amounts and performance test results of examples 1 to 15 and comparative examples 1 to 3
TABLE 1
Table 2 luminosity maintenance ratio of light emitting devices made of the LED reflection plates of example 16 and comparative example 4
Test methods or standards
(1) Intrinsic viscosity of PCT resin
A sample of 0.5g was weighed, dissolved in 100mL of 60/40(wt/wt) phenol/tetrachloroethane, and then subjected to intrinsic viscosity measurement using an Ubbelohde viscometer at a constant 25 ℃.
(2) Hyperbranched polyester number average molecular weight
0.01g of hyperbranched polyester is weighed, added into 10g of tetrahydrofuran, shaken for 24 hours for dissolution, and then the solution is subjected to a gel permeation chromatography test, and the number average molecular weight is calculated by a standard curve made of standard polystyrene.
(3) Acid value of hyperbranched polyester
0.2g of hyperbranched polyester was weighed, added to 20.0mL of chloroform, and titrated with 0.1N normality potassium hydroxide ethanol solution using phenolphthalein indicator. The measurement results of the blank containing no sample were subtracted to calculate the acid value (mgKOH/g).
(4) Reflectance test
Preparing a sample: the polyester resin composition sample was injection-molded, and the sample size was 60X 1.0 mm.
The test method comprises the following steps: measured using a Color Eye 7000A type colorimeter. Initial reflectance the reflectance value of the sample at a wavelength of 460nm was directly measured. The samples were aged for 10h at 210 ℃ and the aged reflectance values of the samples at a wavelength of 460nm were measured.
(5) Melt Mass Flow Rate (MFR)
The test is carried out according to the standard GB/T3682.1-2018, the test temperature is 300 ℃, and the load is 2.16 kg.
(6) Breaking force test
Preparing a sample: the polyester resin composition sample was injection-molded, and the sample size was 80X 20X 2.0 mm.
The test method comprises the following steps: uniformly mixing the silica gel A and the silica gel B according to the mass ratio of 1:4, dripping 0.02g of the mixture to one end of the surface of one sample, pressing the silica gel by one end of the other sample, and fixing the silica gel by a clamp. And then putting the sample piece into an oven, pre-curing for 1h at the temperature of 80 ℃, then heating to 150 ℃, and continuing to cure for 4 h. The cured sample specimens were subjected to tensile testing at a tensile rate of 10mm/min and the tensile force was recorded. The present application characterizes the adhesion of molded articles made from the polyester compositions to silicone gels by tensile strength.
(7) Luminance maintenance ratio
The light-emitting devices made of the LED reflection plates of example 16 and comparative example 4 were subjected to an energization test at 85 deg.c with a current of 15mA for 1000 hours. The photometric retention was 1000 hours of photometric/0 hour of photometric. For example 16 and comparative example 4, the luminance maintenance ratio was an average value of luminance maintenance ratios obtained by 100 light-emitting devices.
Test results
The results of the test of the reflectance and the breaking force of examples 1 to 15 and comparative examples 1 to 3 are shown in Table 1
As can be seen from Table 1, the molecular weight, acid value, addition amount and white pigment addition amount of the hyperbranched polyester are adjusted in examples 1 to 15 of the present invention, wherein a reinforcing material is further added in examples 1 to 14, the bonding force between the sample prepared from the polyester composition prepared in examples 1 to 15 and silica gel is good, the breaking force is above 312N, and the breaking force between the sample prepared from the polyester composition prepared in comparative examples 1 to 3 and silica gel is poor, and is only 141N at most. Therefore, the molded product prepared from the polyester composition has good binding force with silica gel.
By comparing examples 1 to 9, it can be found that when the molecular weight of the hyperbranched polyester is 1000 to 10000g/mol and the acid value is 200 to 350mg KOH/g, the measured breaking force is further improved to be more than 534N, and the binding force between a sample prepared from the polyester composition and silica gel is further improved.
In addition, by further comparing the binding force, the samples prepared from the polyester compositions of examples 3 and 11 have better binding force with silica gel than those of examples 10 and 12. Therefore, when the weight ratio of the hyperbranched polyester to the polyester resin is (2-5) to 60, the binding force between a sample prepared from the polyester composition and silica gel is better.
As can be seen from the results of the reflectivity and fluidity tests shown in Table 1, the initial reflectivity of the samples obtained from the polyester compositions of examples 1 to 15 of the present invention was 94.5 or more, the aged reflectivity was 84.7 or more, and the MFR values of the polyester compositions were 42g/10min or more. It can be seen that the polyester composition of the present invention has excellent fluidity, and the prepared sample has excellent reflectance.
As can be seen from the results of analyzing the luminance retention rate test of the light emitting devices in table 2, the luminance retention rate of the 1000 hour power-on test of the light emitting device manufactured by using the LED reflector plate injection-molded in example 9 of the present invention reaches 95% in example 16, while the luminance retention rate of the 1000 hour power-on test of the light emitting device manufactured by using the LED reflector plate injection-molded in comparative example 1 in comparative example 4 is only 89%.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (12)
1. A polyester resin composition characterized by comprising a polyester resin and a white pigment;
the polyester resin comprises PCT resin and hyperbranched polyester; the molecular weight of the hyperbranched polyester is 1000-10000 g/mol, and the acid value is 200-350 mg KOH/g; the ratio of the weight of the hyperbranched polyester to the total weight of the polyester resin is (0.5-10): 60.
2. The polyester resin composition according to claim 1, wherein the weight ratio of the hyperbranched polyester to the polyester resin is (2-5): 60.
3. The polyester resin composition according to claim 1, wherein the PCT resin has an intrinsic viscosity of 0.6 to 0.8 dL/g.
4. The polyester resin composition according to claim 1, wherein the white pigment is one or more of titanium dioxide, zinc oxide, zinc sulfide, white lead, zinc sulfate, barium sulfate, calcium carbonate, or aluminum oxide.
5. The polyester resin composition according to claim 1, wherein the weight ratio of the white pigment to the polyester resin is (1-4): 6.
6. The polyester resin composition according to any one of claims 1 to 5, wherein the polyester resin composition further comprises a reinforcing material; the reinforcing material is one or the combination of more than two of glass fiber, wollastonite, potassium titanate whisker, kaolin, talc or mica.
7. The polyester resin composition according to claim 6, wherein the polyester resin is 50 to 60 wt%, the white pigment is 10 to 30 wt%, and the reinforcing material is 10 to 30 wt%.
8. The method for preparing the polyester resin composition according to any one of claims 1 to 5, wherein the PCT resin and the hyperbranched polyester are uniformly mixed, and then are melt-blended with a white pigment and extruded for granulation to obtain the polyester resin composition.
9. The method for preparing the polyester resin composition according to claim 6 or 7, wherein the PCT resin and the hyperbranched polyester are uniformly mixed, and then are melt-blended with a white pigment and a reinforcing material, and are extruded and granulated to obtain the polyester resin composition.
10. Use of the polyester resin composition according to any one of claims 1 to 7 for producing an LED reflector.
11. A molded article obtained from the polyester resin composition according to any one of claims 1 to 7.
12. An LED reflector plate, which is prepared from the polyester resin composition according to any one of claims 1 to 7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010452425.1A CN111732819B (en) | 2020-05-26 | 2020-05-26 | Polyester resin composition and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010452425.1A CN111732819B (en) | 2020-05-26 | 2020-05-26 | Polyester resin composition and preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111732819A CN111732819A (en) | 2020-10-02 |
| CN111732819B true CN111732819B (en) | 2022-08-19 |
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