CN109749371A - A kind of polyester molding compounds and the preparation method and application thereof - Google Patents
A kind of polyester molding compounds and the preparation method and application thereof Download PDFInfo
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- CN109749371A CN109749371A CN201811642070.1A CN201811642070A CN109749371A CN 109749371 A CN109749371 A CN 109749371A CN 201811642070 A CN201811642070 A CN 201811642070A CN 109749371 A CN109749371 A CN 109749371A
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- molding compounds
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Abstract
The present invention discloses a kind of polyester molding compounds, including following components: 50-80 parts of PCT resin；10-30 parts of white pigment；Reinforcing material and/or 10-30 parts of filler；It further include the sulfur-containing compound for meeting following below formula, wherein R1For alkyl or contain the functional group of ester group, R2For alkyl, X 0-20；Total weight based on polyester molding compounds, the sulfur content in the polyester molding compounds are 50-2000ppm.Preparation method is mixture and reinforcing material and/or filler to be added in double screw extruder, melt blending, extruding pelletization obtains polyester molding compounds according to the proportion by polyester resin, white pigment, sulfur-containing compound in high-speed mixer and mixing.Polyester molding compounds of the present invention and metal material belt binding force are strong, have good air-tightness, reflectivity and fast light and heat aging performance.
Description
Technical field
The present invention relates to a kind of polyester and resin composition, in particular to a kind of polyester molding that can be used for LED reflector plate
Composition.
Background technique
Industry LED novel as one, application surface is boundless, mainly includes that LED shows and illuminates, such as room lighting
Lamp, street lamp, traffic signals, cell phone keyboard, digital camera, large-size liquid crystal television, note-book computer display screen and other displays
Screen etc..
SMD type LED reflection bracket is by punching molding, and the metal material belt being electroplated is put into injection mould, then by LED
Reflection timbering material is injected on metal material belt by injection molding machine, makes LED reflection timbering material and metal material belt that band reflection be made
Chamber can SMT welding LED function part.After die bond, bonding wire, encapsulation, the light that LED chip is issued is anti-by certain angle
It shoots out, reduces light loss, then through encapsulating materials such as epoxy resin or silica gel, form the light source of LED illumination or display.It can
To say, LED reflection timbering material is a kind of core material of LED illumination, is directly related to brightness and the service life of LED light source.
In order to improve SMD type LED reflection bracket reflectivity, the metal material belt surface used is needed by vacuum sputtering skill
Art, ion plating technique, plating or electroless plating technology, deposited metal silver.After being packaged into lamp bead, if being used for LED reflection bracket
Expect that, oxygen in external environment poor with plating metal material strip binding force, sulfur-bearing contain chlorine, brominated class gas and moisture easily enter
It encapsulates inside LED lamp bead, causes silvering easily to cure, bromination, oxidation etc., cause LED light or LED display to work and lose
Effect.
The material that LED reflection bracket uses at present is PPA and high temperature resistance polyester.PPA material has preferable original intensity, from
There is good mouldability from the point of view of in its chemical structure, it is common LED reflection timbering material, still that processing, which is easier to realize,
The light-heat aging decaying of PPA material is very fast, and PPA material is only used for small-power product at present.With the release of high-voltage LED, gather
Ester is since its low hygroscopicity and ester bond are lower to hot oxygen sensitivity, using with more on middle great power LED reflecting plate
Big advantage.
But in the application of great power LED reflecting plate, while having under light and heat action condition, polyester material is with respect to PPA material
Material is poor with metal material belt binding force, causes lamp bead air-tightness poor, influences LED light service life.
Publication No. is that the patent document of 106084672 A of CN 104672821 A and CN is referred to by adding phosphate
To realize excellent reflectivity and light efficiency while stable at high temperature.
Notification number be CN 104650547B patent document refer to by feature viscosity resin and specific phosphorus content come so that
Polymer has silica gel solidification effect when good reflexive, anti-yellowing property and encapsulation.
Publication No., which refers to for the patent document of 103849126 A of CN through addition metal oxide, improves polyester group
Close the light and heat ageing properties of object.
Publication No., which refers to for the patent document of CN 106461824A through addition specific structure chemical combination object, improves polyester
The light and heat ageing properties of composition.
Although above-mentioned patent document can improve the light and heat ageing properties of polyester material and have it is good reflexive and
Packaging effect, but do not refer in LED reflection bracket the binding force of timbering material and metal material belt and its for lamp bead air-tightness and
The influence of LED light service life.
Summary of the invention
The object of the present invention is to provide a kind of polyester molding groups for meeting encapsulation lamp bead air-tightness requirement with metallic cohesion
Close object.
The present invention is achieved by the following scheme:
A kind of polyester molding compounds, which is characterized in that calculate by weight, including following components:
50-80 parts of PCT resin；
10-30 parts of white pigment；
Reinforcing material and/or 10-30 parts of filler；
The polyester molding compounds further include a kind of sulfur-containing compound for meeting following below formula,,
Wherein R1For alkyl or contain the functional group of ester group, R2For alkyl, X 0-20；
Total weight based on polyester molding compounds, the sulfur content of the polyester molding compounds are 50ppm-2000ppm.
The R1For the alkyl containing 1-25 carbon atom or contain-(CH2)XCOO-R2The functional group of ester group, wherein X be
0-20,；R2For the alkyl containing 1-25 carbon atom.
Preferably, the sulfur content in the polyester molding compounds is 200ppm-1500ppm.
The structural formula of PCT resin is, PCT tree of the invention
Rouge can be passed through under the effect of the catalyst by 1,4 cyclohexane dimethanol and dimethyl terephthalate (DMT) or terephthalic acid (TPA)
Transesterification or direct esterification reaction carry out polycondensation again and are made.
Metal material belt can form hydroxyl organic protection layer on surface after plating, and use is of the present invention
After polyester molding compounds and metal material belt injection molding are combined together, possessed ester group can on the sulfur-containing compound in composition
To form hydrogen bond with the hydroxyl organic protection layer in metal material belt surface, to increase the binding force between metal, meet envelope
Fill the air-tightness requirement of lamp bead.Sulfur content in polymer blend is too low, is unfavorable for forming hydrogen bond, and sulfur content is too high, and meeting
It is precipitated when with metal material belt injection molding, leads to the air-tightness requirement for being unsatisfactory for encapsulation lamp bead.
The sulfur-containing compound is selected from S- [CH2CH2COOC24H49]2、S-[CH2CH2COOC20H41]2、S-
[CH2CH2COOC18H37]2、S-[CH2CH2COOC14H29]2、S-[CH2CH2COOC13H27]2、S-[CH2CH2COOC12H25]2、C-
[CH2COOCH2CH2SC12H25]4、C-[CH2COOCH2CH2SC18H37]4、C-[CH2COOCH2CH2SC14H29]4、C-
[CH2COOCH2CH2SC13H27]4One of or combinations thereof.
The fusing point of the sulfur-containing compound is 30-90 DEG C, relative molecular weight 500-1500.
The fusing point and molecular weight of the sulfur-containing compound are too low, are being easy to volatilize in process, and fusing point and molecule
Measure too high and easy precipitation.This is all unfavorable for the generation of hydrogen bond.
The PCT resin has through thermomechanical analysis (TMA), 75 to 105 measured with the heating rate of 5 DEG C/min
DEG C glass transition temperature.
The PCT resin has through differential scanning calorimetry (DSC), 245 measured with the rate of temperature fall of 20 DEG C/min
To 285 DEG C of crystallization temperature.
If glass transition temperature and crystallization temperature are too low, it can be recrystallized in processing, make itself and metal material belt
Between generate gap, cause air-tightness to be deteriorated；If glass transition temperature and crystallization temperature are too high, and will affect molding, from
And air-tightness is made to be deteriorated.
The white pigment is titanium dioxide, and average grain diameter is 0.2-0.4 μm.
The reinforcing material and/or filler be selected from one of glass fibre, wollastonite, potassium titanate crystal whisker or more than one
Mixture.
The glass fibre is calculated by weight percentage, including following components: silica 58-70wt%；Aluminium oxide 30-
42wt%。
The polyester molding compounds further include the antioxidant of 0.1-2 parts by weight, light stabilizer, stabilizer, fire retardant, take off
One of mould agent, fluorescent whitening agent, plasticizer, lubricant, thickener, nucleating agent or more than one mixture.
The present invention also provides a kind of preparation methods of polyester molding compounds, comprising the following steps: according to the proportion by PCT tree
Mixture and reinforcing material and/or filler are added to twin-screw in high-speed mixer and mixing by rouge, white pigment, sulfur-containing compound
In extruder, melt blending, extruding pelletization obtains polyester molding compounds.
Wherein the heating temperature of extruder is as follows: 1 250~290 DEG C of area, 260~300 DEG C of 2nd~4 area, 5~7 areas 270~
310 DEG C, 260~300 DEG C of 8th~9 area and 250~290 DEG C of head.
Preferably, the reinforcing material and/or filler claim to control charging in 4~9 sections of side feed material of extruder with weightless.
The present invention also provides a kind of mechanographs prepared by above-mentioned polyester molding compounds.
The mechanograph have measured at 460nm, the wavelength of 550nm using colorimeter it is 90% or bigger initial anti-
Penetrate rate.
The present invention also provides a kind of reflecting plates, are obtained using above-mentioned polyester molding compounds in in-mould injection molding.
The application that it is another object of the present invention to polyester molding compounds in light-emitting diode.
Sulfur-containing compound is improving the application in polyester molding compounds and metal material belt binding force, the sulfur-containing compound
Meet following molecular formula:
,
Wherein R1For alkyl or contain the functional group of ester group, R2For alkyl, X 0-20.
Based on the total weight of the polyester molding compounds, the sulfur content in the polyester molding compounds is 50ppm-
2000ppm。
Beneficial effects of the present invention are as follows: it has been investigated that, using with particular glass transition temperature, specific crystallization temperature
Its combination between metal material belt can be improved in polyester molding compounds prepared by the PCT resin and sulfur-containing compound of degree
Power meets encapsulation lamp bead air-tightness requirement, and can be realized high reflectance and fast light and heat aging performance is good.
Specific embodiment
The present invention further illustrates the present invention by following embodiment, but the present invention is not limited by the following examples.
The raw materials used in the present invention source is as follows, but is not limited by following raw material.
PCT Resin A 1: glass transition temperature Tg: 80 DEG C, Tc:250 DEG C of crystallization temperature；
PCT Resin A 2: glass transition temperature Tg: 90 DEG C, Tc:260 DEG C of crystallization temperature；
PCT Resin A 3: glass transition temperature Tg: 100 DEG C, Tc:280 DEG C of crystallization temperature；
PET resin A4: glass transition temperature Tg: 90 DEG C, Tc:260 DEG C of crystallization temperature；
White pigment B: the titanium dioxide (TiO for being subjected to the surface treatment using poly- silicon oxide compound is used2) (R105, Du Pont have
Limit company (DuPont Co., Ltd.) (U.S.)), average grain diameter: 0.31 μm；
Reinforcing material C:F7x28: NITTO BOSEKI, Japan by long 3mm, main cross section (28 μm of axis, secondary cross section axis
7 μm, axis ratio 4(non-circular cross sections) E- glass constitute short glass fiber CSG3PA-820, silica 60-67wt%,
Aluminium oxide 33-40%；
Sulfur-containing compound D1:S- [CH2CH2COOC12H25]2, fusing point: 42.5 DEG C, molecular weight 515；
Sulfur-containing compound D2:C- [CH2COOCH2CH2SC12H25]4, fusing point: 52 DEG C, molecular weight: 1162.
Test method or standard:
Sulfur content test
Polymer blend sulphur content determination is measured according to USEPA method 3052:1996 using ICP-OES method.
Initial reflectance: Color Eye 7000A type colorimeter measurement is used.The length prepared using injection molding
For 60mm, width 60mm, with a thickness of the test film of 1mm.Find out the reflectivity of wavelength region 360nm to 740nm.
Initial stage reflectivity is evaluated using the reflectivity of 460nm and 550nm as typical value.
SMT aging reflectivity: using air SMT welder, carries out reflow process:
(1) temperature warm-up phase: is increased to 150 DEG C from room temperature within 60-120 seconds time；
(2) temperature the heating period: is increased to 190 DEG C from 150 DEG C within 60-90 seconds time；
(3) refluxing stage: 217 DEG C are raised the temperature to 2.5 DEG C of heating rate per second, then within 40-80 seconds time
Temperature is increased to 260 DEG C from 217 DEG C and is down to 217 DEG C again；
(4) room temperature temperature-fall period: is cooled the temperature to 2 DEG C per second or more of rate of temperature fall.
It is 60mm by length, width 60mm, with a thickness of the test film of 1mm crosses furnace three times, uses Color Eye 7000A
Type colorimeter measurement crosses the test piece after furnace.Find out the reflectivity of wavelength region 360nm to 740nm.With 460nm and
The reflectivity of 550nm is as SMT aging reflectivity.
Air tightness test: characterization bracket air-tightness is tested by red ink, by LED support material and plating metal material strip through mould
The LED reflection cup of interior injection molding is soaked into red ink, and red ink is made to submerge pin, places 10min, has seen whether red ink
It penetrates into inside reflector, if there is red ink to penetrate into reflector, it was demonstrated that plastic cement and metal material belt binding force are poor, will lead to lamp bead
Poor air-tightness.Conversely, red ink does not enter in reflector, then prove that plastic cement and metal material belt binding force are strong, the lamp bead being packaged into
Air-tightness is excellent.
Bending strength: ISO 178-2010
Embodiment and comparative example:
Various PCT resins, white pigment, reinforcing material, sulfur-containing compound D1, sulfur-bearing are weighed respectively according to the parts by weight in table 1
Compound D2, respectively by various PCT resins, white pigment, sulfur-containing compound D1, sulfur-containing compound D2 in high-speed mixer and mixing,
It adding mixture in double screw extruder, reinforcing material claims control charging with weightless in 4~9 sections of side feed material of extruder,
It is respectively 270 DEG C of 1st area, 280 DEG C of 2nd~4 area, 290 DEG C of 5th~7 area, 280 DEG C of 8th~9 area, 270 DEG C of head in each area's temperature of extruder
In the state of melt blending, extruding pelletization obtains polyester molding compounds.
The concrete composition and its test performance result (parts by weight) respectively formed in table 1. embodiment 1-8 and comparative example 1-5
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 | Embodiment 8 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | |
| PCT Resin A 1 | 50 | - | - | - | - | - | - | - | - | - | - | - | - |
| PCT Resin A 2 | - | 60 | - | 60 | 60 | 80 | 60 | 60 | - | 60 | 60 | 60 | 60 |
| PCT Resin A 3 | - | - | 70 | - | - | - | - | - | - | - | - | - | - |
| PET resin A4 | - | - | - | - | - | - | - | - | 60 | - | - | - | - |
| White pigment B | 20 | 20 | 20 | 20 | 20 | 20 | 30 | 10 | 20 | 20 | 20 | 40 | - |
| Reinforcing filler C | 20 | 20 | 20 | 20 | 20 | 20 | 10 | 30 | 20 | 20 | 20 | - | 40 |
| Sulfur-containing compound D1 | 0.5 | 0.5 | 0.5 | 0.05 | 3 | - | - | - | 0.5 | 0 | 5 | - | - |
| Sulfur-containing compound D2 | - | - | - | - | - | 0.5 | 0.5 | 0.5 | - | - | - | 0.5 | 0.5 |
| Initial reflectance (R-460nm) % | 95 | 94 | 93 | 93.6 | 94.1 | 93.8 | 95.2 | 91.2 | 92.2 | 91 | 93.2 | 95.4 | 82 |
| SMT aging reflectivity (R-460nm) % three times | 91 | 92 | 92.5 | 91.5 | 92.5 | 91.9 | 92.9 | 89.1 | 79 | 89 | 91.9 | 94.2 | 74 |
| The test of reflector red ink | ok | ok | ok | ok | ok | ok | ok | ok | ok | NG | ok | OK | NG |
| Reflector three times test by SMT aging red ink | ok | ok | ok | ok | ok | ok | ok | ok | NG | NG | ok | NG | NG |
| Bending strength (MPa) | 98 | 97 | 99 | 92 | 91 | 97 | 89 | 110 | 96 | 99 | 76 | 72 | 132 |
| Sulfur content, ppm | 294 | 306 | 310 | 31 | 1860 | 551 | 523 | 536 | 301 | 0 | 3100 | 544 | 559 |
Note: OK=red ink does not enter reflector；
NG=there is red ink to enter reflector.
As seen from the results in Table 1, made by the PCT resin and sulfur-containing compound of particular glass transition temperature and crystallization temperature
Standby composition has good air-tightness and initial reflectance, while good air-tightness is also able to maintain after light and heat aging
And reflectivity.By embodiment 2, embodiment 4 and embodiment 5 it is found that the composition in sulfur content preferred scope has preferably
Mechanical property.As embodiment 2 and comparative example 1 it is found that using composition prepared by PET polyester resin in experience light and heat aging
Afterwards, reflectivity and air-tightness are all deteriorated.By embodiment 2 and comparative example 2 it is found that being added without the composition air-tightness of sulfur-containing compound
It is bad.And by comparative example 3 it is found that sulfur content can excessively make mechanical properties decrease.
Claims (15)
1. a kind of polyester molding compounds, which is characterized in that calculate by weight, including following components:
50-80 parts of PCT resin；
10-30 parts of white pigment；
Reinforcing material and/or 10-30 parts of filler；
It further include a kind of sulfur-containing compound for meeting following below formula, wherein R1For alkyl or
Functional group containing ester group, R2For alkyl, X 0-20；
Based on the total weight of the polyester molding compounds, the sulfur content in the polyester molding compounds is 50ppm-2000ppm,
Preferably, sulfur content 200ppm-1500ppm.
2. polyester molding compounds according to claim 1, which is characterized in that the R1For 1-25 carbon atom alkyl or
Contain-(CH2)XCOO-R2The functional group of ester group, wherein X is 0-20；R2For the alkyl containing 1-25 carbon atom.
3. polyester molding compounds according to claim 2, which is characterized in that the sulfur-containing compound is selected from S-
[CH2CH2COOC24H49]2、S-[CH2CH2COOC20H41]2、S-[CH2CH2COOC18H37]2、S-[CH2CH2COOC14H29]2、S-
[CH2CH2COOC13H27]2、S-[CH2CH2COOC12H25]2、C-[CH2COOCH2CH2SC12H25]4、C-
[CH2COOCH2CH2SC18H37]4、C-[CH2COOCH2CH2SC14H29]4、C-[CH2COOCH2CH2SC13H27]4One of or its
Combination.
4. polyester molding compounds according to claim 1 to 3, which is characterized in that the fusing point of the sulfur-containing compound
It is 30-90 DEG C, relative molecular weight 500-1500.
5. polyester molding compounds according to claim 1, which is characterized in that the PCT resin has by thermomechanically dividing
Analysis method, 75 to 105 DEG C of the glass transition temperature measured with the heating rate of 5 DEG C/min.
6. polyester molding compounds according to claim 1, which is characterized in that the PCT resin, which has, passes through differential scanning
Calorimetry, 245 to 285 DEG C of the crystallization temperature measured with the rate of temperature fall of 20 DEG C/min.
7. polyester molding compounds according to claim 1, which is characterized in that the white pigment is titanium dioxide, average
Partial size is 0.2-0.4 μm.
8. polyester molding compounds according to claim 1, which is characterized in that the reinforcing material and/or filler are selected from glass
One of glass fiber, wollastonite, potassium titanate crystal whisker or more than one mixture；
Wherein the glass fibre is calculated by weight percentage, including following components: silica 58-70wt%；Aluminium oxide 30-
42wt%。
9. polyester molding compounds according to claim 1, which is characterized in that further include antioxidant, the light of 0.1-2 parts by weight
One of stabilizer, stabilizer, fire retardant, release agent, fluorescent whitening agent, plasticizer, lubricant, thickener, nucleating agent or
More than one mixture.
10. the preparation method of -9 any polyester molding compounds according to claim 1, which is characterized in that including following step
It is rapid: according to the proportion by polyester resin, white pigment, sulfur-containing compound in high-speed mixer and mixing, by mixture and reinforcing material and/
Or filler is added in double screw extruder, melt blending, extruding pelletization obtains polyester molding compounds；
Wherein the heating temperature of extruder is as follows: 1 250~290 DEG C of area, 260~300 DEG C of 2nd~4 area, 270~310 DEG C of 5th~7 area,
8~9 260~300 DEG C of areas and 250~290 DEG C of head；
Preferably, the reinforcing material and/or filler claim to control charging in 4~9 sections of side feed material of extruder with weightless.
11. a kind of mechanograph of the preparation of polyester molding compounds according to claim 1, which is characterized in that the mechanograph
With 90% or the bigger initial reflectance for using colorimeter to measure at 460nm, the wavelength of 550nm.
12. a kind of reflecting plate, which is characterized in that formed using polyester molding compounds described in claim 1 in in-mould injection and
It obtains.
13. a kind of application of polyester molding compounds in light-emitting diode.
14. sulfur-containing compound is improving the application in polyester molding compounds and metal material belt binding force,
The sulfur-containing compound meets following molecular formula:
Wherein R1For alkyl or contain the functional group of ester group, R2For alkyl, X 0-20.
15. application according to claim 14, which is characterized in that the total weight based on the polyester molding compounds, it should
Sulfur content in polyester molding compounds is 50ppm-2000ppm.
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Family
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113861630A (en) * | 2021-09-18 | 2021-12-31 | 珠海万通特种工程塑料有限公司 | Polyester resin composition and preparation method and application thereof |
| CN114685978A (en) * | 2020-12-29 | 2022-07-01 | 珠海万通特种工程塑料有限公司 | PA6T66 molding composition and application thereof |
| CN116462941A (en) * | 2023-03-30 | 2023-07-21 | 金发科技股份有限公司 | Polyester composition and preparation method and application thereof |
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| US5380748A (en) * | 1991-03-07 | 1995-01-10 | Zeria Pharmaceutical Co., Ltd. | Trialkylamine derivative and ameliorant for digestive tract movement containing the same |
| KR20130076027A (en) * | 2011-12-28 | 2013-07-08 | 제일모직주식회사 | Polyester resin composition having good initial reflectance and yellowing resistance in high temperature condition and high temperature/humidity condition |
| CN105143332A (en) * | 2013-01-07 | 2015-12-09 | 沙特基础全球技术有限公司 | Compositions for an LED reflector and articles thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US5380748A (en) * | 1991-03-07 | 1995-01-10 | Zeria Pharmaceutical Co., Ltd. | Trialkylamine derivative and ameliorant for digestive tract movement containing the same |
| KR20130076027A (en) * | 2011-12-28 | 2013-07-08 | 제일모직주식회사 | Polyester resin composition having good initial reflectance and yellowing resistance in high temperature condition and high temperature/humidity condition |
| CN105143332A (en) * | 2013-01-07 | 2015-12-09 | 沙特基础全球技术有限公司 | Compositions for an LED reflector and articles thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114685978A (en) * | 2020-12-29 | 2022-07-01 | 珠海万通特种工程塑料有限公司 | PA6T66 molding composition and application thereof |
| CN114685978B (en) * | 2020-12-29 | 2024-03-01 | 珠海万通特种工程塑料有限公司 | PA6T66 molding composition and application thereof |
| CN113861630A (en) * | 2021-09-18 | 2021-12-31 | 珠海万通特种工程塑料有限公司 | Polyester resin composition and preparation method and application thereof |
| CN113861630B (en) * | 2021-09-18 | 2023-02-21 | 珠海万通特种工程塑料有限公司 | Polyester resin composition and preparation method and application thereof |
| CN116462941A (en) * | 2023-03-30 | 2023-07-21 | 金发科技股份有限公司 | Polyester composition and preparation method and application thereof |
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Application publication date: 20190514 |
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| RJ01 | Rejection of invention patent application after publication |