CN104610739B - A kind of reflecting plate daiamid composition - Google Patents
A kind of reflecting plate daiamid composition Download PDFInfo
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- CN104610739B CN104610739B CN201510029804.9A CN201510029804A CN104610739B CN 104610739 B CN104610739 B CN 104610739B CN 201510029804 A CN201510029804 A CN 201510029804A CN 104610739 B CN104610739 B CN 104610739B
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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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Abstract
The invention discloses a kind of reflecting plate daiamid composition,（A）100 parts of semiaromatic polyamide composition PA/Z；Wherein, based on whole monomeric units, PA/Z includes at least 20mol% repeat unit based on terephthalic acid (TPA)；0.01 ~ 5mol% compound the Z containing secondary amine group is also included in molar content based on diamines, PA/Z；（B）9 300 parts of Chinese white（B1）And/or reinforcer（B2）；Based on whole component weight, the phosphorus content of the daiamid composition is 30 3000ppm；The present invention is using compound of the certain content containing secondary amine group and the daiamid composition of the phosphorus content of certain content, it can solve the problem that the silica gel that LED component is easy to occur in encapsulation process solidifies the technical problem that not exclusively or even can not solidify completely, realize later stage silica gel completion of cure.
Description
Technical field
The present invention relates to modifying polyamide polymers compositions field, more particularly to a kind of reflecting plate polyamide compositions
Thing.
Background technology
LED is because it exceedes many advantages of conventional light source and is increasingly being used as light source.LED generally with white heat
Light source is compared with other light sources, is consumed less power, is required lower operating voltage and has to mechanical shock good
Resistance.Therefore, LED/light source is positive in many purposes substitutes incandescent source and other light sources and has been used to the neck that differs
In domain, such as traffic signals, inside and outside illumination, mobile phone display screen, automobile display screen and flash lamp.
LED component, such as shell and reflection support require that material has excellent colour stability and high temperature resistance discolouration.,
Ceramics can meet requirements above, but not only price is high but also needs higher working process technology for ceramics, and processing efficiency is low.Thermoplastic
Property polymer because it may be used as injection molding, it is succinct, flexibly, efficiently, therefore polymer composition has been carried out widely
Research and develop to substitute ceramics as the material of lower cost.The requirement of LED reflection stent applications has good light tight
Property and outstanding reflection characteristic.But generally thermoplastic polymer is easy to jaundice when in light and high temperature.For example sealed in LED
During dress, LED parts are heated at about 180 DEG C so as to cured epoxy resin or silicon encapsulant.Carrying out reflow soldering
During operation, at a temperature of LED parts are also exposed to higher than 260 DEG C.In addition, in use, LED light source block such as automobile is big
Lamp, temperature in use is higher than 80 DEG C of temperature.This exposure in high temperature causes the polymer group for forming LED parts
The jaundice of compound.
Therefore the thermoplastic polymer composition applied to LED reflection support, it should meet and a variety of require to include high light
Reflectivity（The reflectivity of visible ray）, high whiteness, good machinability（Such as good moldability）, high size
Stability（Low linear expansion coefficient）, high mechanical strength and high heat resistance（It is low when exposed to high temperature to fade and low
Reflection loss）.
As it was previously stated, in LED encapsulation process, LED component is heated to certain temperature so that silica gel solidifies.This is LED
The essential link of encapsulation, and be vital link.Research is found, is easy to produce silica gel solid in this process
Change the problem of not solidifying completely even not exclusively, causing the production process in later stage can not be carried out, and product can not be used.For how
LED reflection support is solved the problem of whiteness and reflectivity decline when in light and heat, has more patent and document to enter
Row description；But rarely have and refer to the problem of silica gel solidifies in LED encapsulation process, more do not refer to LED reflection support to silica gel solid
The influence of change.
The content of the invention
The silica gel solidification occurred in order to solve LED component to be easy in encapsulation process can not exclusively or even completely consolidate
The technical problem of change, can realize that later stage silica gel solidifies complete reflecting plate polyamide it is an object of the invention to provide one kind
Composition.
A kind of reflecting plate daiamid composition, by weight, includes following component：
（A）100 parts of semiaromatic polyamide composition PA/Z；Wherein, based on whole monomeric units, PA/Z includes at least 20mol%
The repeat unit based on terephthalic acid (TPA)；Contain secondary amine also comprising 0.01 ~ 5mol% in molar content based on diamines, PA/Z
The compound Z of group；
（B）9-300 parts of Chinese white（B1）And/or reinforcer（B2）；
Based on whole component weight, the phosphorus content of the daiamid composition is 30-3000ppm.
Whole component weight are preferably based on, the phosphorus content of the daiamid composition is 50 ~ 1000ppm.
Wherein, the content of the partially aromatic polyamide PA/Z is 20 ~ 95wt% based on the daiamid composition gross weight,
Preferably 30 ~ 70wt%.
The compound Z containing secondary amine group is selected from NH (C2H4NH2)2、H2N[C2H4NH]2C2H4NH2、H2N[C2H4NH]3C2H4NH2、NH[(CH2)4NH2)2、NH[(CH2)5NH2)2、NH[(CH2)6NH2)2、NH[(CH2)7NH2)2、NH[(CH2)8NH2)2、
NH[(CH2)9NH2)2、NH[(CH2)10NH2)2、NH[(CH2)11NH2)2、NH[(CH2)12NH2)2、NH[(CH2)13NH2)2、NH
[(CH2)14NH2)2、NH[(CH2)15NH2)2、NH[(CH2)16NH2)2、NH[(CH2)17NH2)2、NH[(CH2)18NH2)2、H2N
(H2C)10NH(CH2)5NH2、H2N(H2C)10NH(CH2)6NH2、H2N(H2C)10NH(CH2)7NH2、H2N(H2C)10NH(CH2)8NH2、
H2N(H2C)10NH(CH2)9NH2、H2N(H2C)10NH(CH2)11NH2、H2N(H2C)10NH(CH2)12NH2、H2N(H2C)9NH(CH2)6CH(CH3)CH2NH2、H2N(H2C)9NHCH2CH(CH3)(CH2)6NH2、NH[(CH2)6CH(CH3)CH2NH2]2、NH[CH2CH(CH3)
(CH2)6NH2]2In one or more.
Preferably, the molar content of the compound X containing secondary amine group is 0.05 ~ 2mol%.
The Chinese white（B1）As fundamental so that the change of xanthochromia minimizes and assigns good reflection, select
It is self-contained but be not limited only to titanium dioxide, zinc oxide, zinc sulphide, white lead, zinc sulfate, barium sulfate, calcium carbonate, aluminum oxide.These
The shape of particle is not particularly limited；They can be notably round, laminar, flat etc..
The Chinese white is preferably titanium dioxide（TiO2）；The form of titanium dioxide is not particularly limited and can used
Diversified crystal form, such as anatase form, rutile form and monoclinic crystal type.However, rutile form is excellent
Choosing, because its refractive index is higher and its photostability is superior.The preparation method of titanium dioxide can also be it is diversified,
Such as sulfuric acid process, chloridising.However, chloridising is preferred.
In the surface treatment of titanium dioxide, independent inorganic surface treatment can be used, independent organic table can also be used
Face inorganic agent, inorganic and organic mixed processing can also be used.It is even more preferably independent inorganic surface treatment and inorganic
Organic mixed processing.
Inorganic surface treatment agent includes but is not limited to Al2O3、SiO2、ZrO2, sodium metasilicate, sodium aluminate, sodium aluminium silicate
(sodium silicate aluminium), zinc oxide, mica etc..Surface conditioning agent can be used alone or be made with its combination
With.
Organic surface treatment includes but is not limited to dimethyl silicone polymer, trimethyl propane (TMP), pentaerythrite etc..
Surface conditioning agent can be used alone or is applied in combination with it.
Based on the titanium dioxide of 100 parts by weight, about 0.3 parts by weight or less titanium dioxide can be coated with it is inorganic or
Organic surface treatment.Based on the titanium dioxide of 100 parts by weight, preferably pass through the Al less than 5 parts by weight2O3It is used as inorganic table
The titanium dioxide of face inorganic agent coating.
The average grain diameter of titanium dioxide it is excessive or it is too small there is a situation where light reflectivity reduction, therefore preferably 0.1~
0.5 μm, more preferably at 0.15~0.4 μm, particularly preferably in the range of 0.2~0.3 μm.Herein, can also will be block or flat
The equal big titanium dioxide of particle diameter is suitably crushed, and is classified as needed with sieve etc., so as to be used after reaching above-mentioned average grain diameter.
If it is present gross weight of the amount based on said composition that the Chinese white is present is preferably at least 1wt%, preferably
At least 6wt%, more preferably at least 10wt% and most preferably at least 15wt%.In addition, when it is present, the Chinese white is present
Amount based on being also preferably most 50wt%, more preferably up to 40wt% according to the gross weight of composition of the present invention.
If the consumption of Chinese white is too low, reflectivity and yellowing resistance can be deteriorated.If the consumption of Chinese white is excessive
When, the toughness and mouldability of material can be deteriorated.
The reinforcer（B2）Selected from threadiness, tabular, needle-like, cross-like strengthening material；It is described fibee reinforced
Material is selected from glass fibre, carbon fiber, aramid fibre, liquid crystal polymer（LCP）Fiber, one kind of metallic fiber or its
Combination；The tabular strengthening material is selected from mica, one kind of talcum or its combination；The needle-like strengthening material is selected from potassium titanate
Whisker, aluminium borate whisker, calcium carbonate crystal whisker, magnesium sulfate crystal whisker, wollastonite, sepiolite, eakleite, one kind of ZnOw
Or its combination；The cross-like strengthening material silica, aluminum oxide, barium carbonate, magnesium carbonate, aluminium nitride, boron nitride, metatitanic acid
Potassium, alumina silicate（Kaolin, clay, pyrophillite, bentonite）, calcium silicates, magnesium silicate（Attapulgite）, aluminium borate, calcium sulfate, sulphur
Sour barium, magnesium sulfate, asbestos, bead, graphite, CNT, carborundum, sericite, hydrotalcite, molybdenum disulfide, phenolic resin,
Cross-linked styrene system resin, one kind of cross-linked acrylic acid system resin or its combination.
In order to improve the dispersiveness or raising and the cohesive of polyamide in polyamide, the table of these strengthening materials
Face can by the macromolecules such as silane coupler, titanate coupling agent, acrylic resin, polyurethane resin, epoxy resin or its
Its low molecular compound is surface-treated.
In above-mentioned reinforcer, from low cost, it can obtain the high products formed of mechanical strength and consider, preferably threadiness enhancing
Filler and/or needle-like reinforcer.From the viewpoint of high intensity, low cost, the reinforcer preferably uses glass fibre,
From the viewpoint of it can obtain the high products formed of surface smoothness, needle-like strengthening material is preferably used.Particularly from holding whiteness
From the viewpoint of, preferably using in glass fibre, wollastonite, potassium titanate crystal whisker, calcium carbonate crystal whisker and aluminium borate whisker
At least one, more preferably using glass fibre and/or wollastonite.
The amount that described reinforcer is present is the 0wt% based on the daiamid composition gross weight to 40wt%.It is preferred that
10wt%-30wt%。
Daiamid composition of the present invention, can optionally further comprise phosphorus-containing compound, such as selected from potassium phosphate,
One kind or its group in sodium phosphate, potassium dihydrogen phosphate, sodium dihydrogen phosphate, phosphate, phosphite ester, Sodium Acid Pyrophosphate etc.
Close.
Daiamid composition of the present invention, can optionally further comprise magnesia and/or magnesium hydroxide, it contains
Measure as 0.5~10wt% based on the daiamid composition gross weight, preferably 1~5wt%.Thus, even if carry out especially long
Between heating when, can also suppress the reduction of xanthochromia and whiteness.When the content is less than 0.5wt%, suppress after heating
Color changeable effect it is small, and during more than 10wt%, the mouldability reduction of material.
Average grain diameter to magnesia and/or magnesium hydroxide is not particularly limited, from the viewpoint of various physical property are improved,
Preferably 0.05~10 μm, more preferably 0.1~5 μm.In addition, in order to improve its adaptation and dispersiveness with polyamide,
Surface treated magnesia and/or magnesium hydroxide can be used.It is used as surface conditioning agent, including amino silane, epoxy silicon
The silane couplers such as alkane；The organo-silicon compound such as organosilicon；The organic titanic compounds such as titanium coupling agent；Organic acid, polyalcohol etc. have
Machine thing etc..
The daiamid composition can also include calcium carbonate, and/or polytetrafluoroethylene (PTFE), and/or the benzene with syndiotactic structure
Vinyl thermoplastic resin.
Suitable calcium carbonate mineral is the Natural Types of grinding and the type of precipitation（PCC）, it preferably has at least 97 weights
Measure % calcium carbonate content and most 0.2 weight % Fe2O3Content.Chalk, grinding are divided into according to naturally occurring form
Calcite, ground marble and grinding lime stone.It is preferred that crystal structure be aragonite and calcite, preferably needle-like, cigar shape and
Cube crystalline form.Especially preferably cigar shape crystalline form, such as by the product Socal P2 from Solvay Chemicals or
What P3 had.The example of the natural whiting of grinding is：Hydrocarb, Setacarb- from Pl ü ss-Staufer AG
OG（It is ultra-fine）、Calcigloss-GU（Extra-fine grinding marble）.
Natural whiting filler can be obtained with a variety of classified grinding fineness.It is this to be classified as from d50m values being about 1 micro-
Rice and maximum particle diameter for 6 to 10 microns superfine product to have narrow particle diameter distribution the form of chips in the range of millimeter.
Specific surface area is 1 to 10 m2/ g, but 10 m are only can be only achieved when being ground to most thin2/ g.In the situation of PCC types
Under, the fine type has 6 to 10 m2/ g specific surface area, ultra-fine type specific surface area is 20-35 m2/ g。
It is scattered in thermoplastic in order to improve calcium carbonate, appropriate surface treatment can be passed through（Coating）To assign
Calcium carbonate lipophilicity.Suitable surface treatment agent is such as calcium stearate and stearic acid, and for the organic table of titanium dioxide
The carboxylic acid that face processing is already mentioned above.
If it does, the content of the calcium carbonate is up to 50%, it is preferably up to 30%.
The daiamid composition can further include the styrene analog thermoplastic resin with syndiotactic structure.It is wherein described
Styrene analog thermoplastic resin has the weight average molecular weight in the range of 10,000 to 5,000,000 grams/mol.It is wherein described
Styrene analog thermoplastic resin has the fusing point in the range of 200 to 320 DEG C.
A kind of anti-impact modifier can optionally be further comprised.It is preferred that anti-impact modifier include be typically used for
Those of polyamide, include the TPO of carboxyl substitution, these TPOs are that have to be attached to thereon, or are attached at certainly
The TPO of carboxylic acid group in the polyolefin backbone or side chain of body.These carboxylic acid groups mean hydroxy-acid group, such as a kind of or many
Plant omega-dicarboxylic acids, two esters, diacyloxy monoesters class, anhydrides, and monocarboxylic acid class and esters.
The anti-impact modifier can be based preferably on ethylene/alpha-olefin polyolefin.Double vinyl monomers such as 1,4- butadiene；
1,4- hexadienes；Or dicyclopentadiene can optionally for the polyolefin preparation.Preferably TPO is included by 1,4-
Ethylene-propylendiene prepared by hexadiene and/or dicyclopentadiene（EPDM）Polymer and styrene-ethylene=butadiene-benzene
Ethene（SEBS）Polymer.The impact modifier can have or can be without the multiple carboxyl portions being attached to thereon living
Point.
The carboxy moiety can during the preparation of the polyolefin by with many undersaturated carboxyl group-containing monomer copolymerization and
Introduce.The preferably copolymer of ethene and maleic anhydride monoethylester.The carboxy moiety can also be by using a kind of portion containing carboxyl
The unsaturated compound divided such as acid, ester, diacid, diester, acid esters or acid anhydrides are grafted the polyolefin and introduced.A kind of preferred grafting
Agent is maleic anhydride.A kind of preferred anti-impact modifier is a kind of EPDM polymer or the POE polymerizations for being grafted with maleic anhydride
Thing.
Another additive that may reside in polymer composition is polytetrafluoroethylene polymer.Include polytetrafluoroethyl-ne
Alkene polymer can improve the reflectivity and whitness index of the product manufactured by polymer composition.Can be with less than about 50
Micron, the form of the fine powder of for example, less than about 10 microns of particle mean size adds polytetrafluoroethylene polymer to composition.Example
Such as, in one embodiment, polytetrafluorethylepowder powder can have about 1 micron-about 8 microns of particle mean size.Polytetrafluoro
Ethene polymers can be present in composition with about 0.05wt%- about 10wt%, e.g., from about 0.1wt%- about 6wt% amount.
Daiamid composition of the present invention, can optionally further comprise inorganic nucleator, the inorganic nucleation
Agent is selected from silica, talcum, clay, aluminum oxide, mica, zirconium oxide, titanium dioxide, tin oxide, tin indium oxide, the oxidation of antimony tin
Thing, calcium carbonate, one kind of zeolite or its combination, excellent result is obtained when using talcum；The inorganic nucleator contains
Measure as 0.5 ~ 5wt% based on the daiamid composition gross weight, preferably 2 ~ 4wt%.
Term " inorganic nucleator " is intended to indicate that with least 1 μm of weight average size（Equivalent diameter）Mineral grain.It is excellent
Selection of land, the weight average size of these particles is at least 2 μm.In addition, it is preferably most 10 μm.
In the present invention, also following additive can be added according to purposes in the range of invention effect is not damaged, that is, resisted
Oxidant, heat-resisting stabilizing agent, light stabilizer, other polymers, impact modifier, fire retardant, fluorescent whitening agent, lubricant, increasing
Mould agent, thickener, antistatic additive, releasing agent, one kind of pigment or its combination；The antioxidant is selected from phenols, amine, sulphur class
One kind or its combination；The heat-resisting stabilizing agent is selected from lactone compound, vitamin E class, hydroquinones, copper halide, iodine compound
One kind or its combination；The light stabilizer is selected from benzotriazole, triazines, benzophenone, benzoates, hindered amine
Class, oxanilide（Oxanilide）One kind of class or its combination；The other polymers are selected from TPO, ethene-the third
Alkene copolymer, ethene -1- butylene copolymer olefin copolymers, the olefin copolymer, polyphenyl second such as propylene -1- butylene copolymers
Alkene, polyamide, makrolon, polyacetals, polysulfones, polyphenylene oxide, fluororesin, silicone resin, LCP one kind or its combination；It is described
Fire retardant is selected from bromine system, chlorine system, phosphorus system, antimony system, one kind of inorganic system or its combination.Added in the daiamid composition of the present invention
During these compositions, its content is preferably below 5wt%.
The present invention is using compound of the certain content containing secondary amine group and the polyamide compositions of the phosphorus content of certain content
Thing, can solve the problem that the silica gel that LED component is easy to occur in encapsulation process solidifies the technology that not exclusively or even can not solidify completely
Problem, realizes later stage silica gel completion of cure.
Brief description of the drawings
Fig. 1 is molded into the schematic diagram of sample for the reflecting plate of the present invention with daiamid composition particle；
Fig. 2 is molded into another schematic diagram of sample for the reflecting plate of the present invention with daiamid composition particle.
Embodiment
The present invention is further illustrated below by embodiment, following examples are the present invention preferably embodiment party
Formula, but embodiments of the present invention are not limited by following embodiments.
Glass fibre：As OCV995 from OWENS CORNING composite company（OCVTM Reinforcements）Can
Commercially available E- glass fibres.
Titanium dioxide：From Ishihara Sangyo Kaisha, Ltd.（Ishihara Sangyo Kaisha）It is commercially available.
The rutile TiO that PC-3- is manufactured by chloride process2, with silica and alumina treatment mistake.
Phosphorus containg substances 1：Sodium tripolyphosphate, commercially available from the Tian Peng Fine Chemical Co., Ltd of Yixing.
Phosphorus containg substances 2：HostanoxP-EPQ, commercially available from Clariant Corporation (Clariant).
Phosphorus containg substances 3：Potassium metaphosphate, commercially available from the Rui Feng Chemical Co., Ltd.s of Jiangsu.
Inorganic nucleator：As HTP4 from Yi meter Fa ratios (IMl FabiTM) commercially available talcum.
Lubricant：From AmeriLubes, the commercially available PED191 of L.L.C, a kind of polyethylene of the oxidation of HMW
Wax.
LED packaging silicon rubbers：From the commercially available LED packaging silicon rubbers of Beijing Kang Meite Science and Technology Ltd.s, MO-006 AB glue.
The measuring method of each performance indications
The method of testing of the relative viscosity of polyamide：With reference to GB12006.1-89, polyamide viscosity number assay method；It is specific to survey
Method for testing is：25 ± 0.01oRelative viscosity of the concentration for 0.25g/dl polyamide is measured in C 98% concentrated sulfuric acidη r；
The method of testing of the fusing point of polyamide：With reference to ASTM D3418-2003, Standard Test Method for
Transition Temperatures of Polymers By Differential Scanning Calorimetry；Specifically
Method of testing is：Using the fusing point of Perkin Elmer Diamond dsc analysis instrument test samples；Nitrogen atmosphere, flow velocity is
40mL/min；First with 10 during testoC/min is warming up to 340oC, 340oC keeps 2min, then with 10oC/min is cooled to
50oC, then with 10oC/min is warming up to 340oC, fusing point is set to by endotherm peak temperature nowT m；
The phosphorus detection of daiamid composition：According to USEPA methods 3052:1996 determine, and are divided using ICP-OES
Analysis.
Silica gel solidifies performance test：By the daiamid composition particle injection of gained as test specimens as illustrated in fig. 1 and 2
Part；
MO-006 A glue is with MO-006 B glue with mass ratio 1：4 it is well mixed after take 0.02g to drop to the recessed of exemplar upper surface
In hole, layer of silica gel is laid in hole bottom, then exemplar is put into baking oven, precuring 1h, is then warming up under the conditions of 80 DEG C
150 DEG C are continued to solidify end after 4h.Flat board is taken out, with the naked eye the silica gel solidification situation directly in observation pit.Table is fully cured
" ⊙ " is shown as, does not solidify and is expressed as " ↓ ".
Embodiment A ~ E and comparative example F ~ G polyamide are synthesized by the following method：
Being stirred equipped with magnetic coupling, in the autoclave pressure of condenser pipe, gas phase mouth, charge door, pressure explosion-proof mouthful by form
Ratio add reaction raw materials；Add sodium hypophosphite, benzoic acid and deionized water.Sodium hypophosphite weight is in addition to deionized water
The 0.1% of other charged material weights, the amount of benzoic acid species is the 4% of the amount of diacid total material, and deionized water weight is the weight that always feeds intake
The 30% of amount.Vacuumize and be filled with high pure nitrogen as protection gas, start reaction.Reactant mixture is warming up to 220 DEG C of stirrings 1 small
When, the temperature of reactant is increased to 230 DEG C under agitation；Reaction under 230 DEG C of constant temperature and 2.2MPa constant pressure after
Continue progress 2 hours, the formed water by removing and keep pressure constant, valve discharging is opened after the completion of reaction, pre-polymerization is obtained
Thing.Prepolymer carries out solid-phase tack producing 10 hours after being dried in vacuo 24 hours at 80 DEG C, obtains polyamide.Polyamide resin
The performance indications such as the fusing point of fat are listed in Table 1 below.
Table 1
The preparation of daiamid composition：
It is its parts by weight that each component content is listed in table 2 ~ 4, and polyamide is entered via a weight-loss type feed appliance
Material is into first machine barrel of the ZSK-26 double screw extruders comprising 12 areas.The set point temperatures of the machine barrel are 150
In the range of DEG C -330 DEG C and will be resin melting before the 5th area.Other solid constituents are passed through into a mistake in the 5th area
Weight formula feed appliance is fed via a lateral sizer.The screw speed is in the range of 150rpm to 220rpm.Make extrusion
Thing is cooled down and granulated with conventional equipment.
Table 2
Table 3
Table 4
From the embodiment 1 ~ 16 and comparative example 1 ~ 9 in table 2 ~ 4 as can be seen that the daiamid composition that embodiment is prepared
The problem of solidifying not exclusively or can not solidify completely without generation silica gel during the silica gel solidification in later stage.
Comparative example 1 and 2 meets the phosphorus content requirement of daiamid composition, but is unsatisfactory in polyamide containing secondary amine
There is the defect that silica gel does not solidify in the requirement of the compounds content of group, gained daiamid composition.Although comparative example 3 ~ 9 is met
The requirement of terephthalic acid (TPA) and the compounds content containing secondary amine group in polyamide, but the phosphorus of daiamid composition contains
Amount is not in the particular range of the present invention, and gained daiamid composition equally exists the defect that silica gel does not solidify.
Claims (12)
1. a kind of reflecting plate daiamid composition, by weight, includes following component：
（A）100 parts of semiaromatic polyamide composition PA/Z；Wherein, based on whole monomeric units, PA/Z includes at least 20mol% base
In the repeat unit of terephthalic acid (TPA)；Contain secondary amine group also comprising 0.01 ~ 5mol% in molar content based on diamines, PA/Z
Compound Z；
（B）9-300 parts of Chinese white（B1）And/or reinforcer（B2）；
Characterized in that, based on whole component weight, the phosphorus content of the daiamid composition is 30-3000ppm；
The molar content of the compound Z containing secondary amine group is 0.05 ~ 2mol%.
2. reflecting plate daiamid composition according to claim 1, it is characterised in that based on whole component weight, should
The phosphorus content of daiamid composition is 50 ~ 1000ppm.
3. reflecting plate daiamid composition according to claim 1 or 2, it is characterised in that described to contain secondary amine group
Compound Z be selected from NH (C2H4NH2)2、H2N[C2H4NH]2C2H4NH2、H2N[C2H4NH]3C2H4NH2、NH[(CH2)4NH2]2、NH
[(CH2)5NH2]2、NH[(CH2)6NH2]2、NH[(CH2)7NH2]2、NH[(CH2)8NH2]2、NH[(CH2)9NH2]2、NH[(CH2)10NH2]2、NH[(CH2)11NH2]2、NH[(CH2)12NH2]2、NH[(CH2)13NH2]2、NH[(CH2)14NH2]2、NH[(CH2)15NH2
]2、NH[(CH2)16NH2]2、NH[(CH2)17NH2]2、NH[(CH2)18NH2]2、H2N(H2C)10NH(CH2)5NH2、H2N(H2C)10NH
(CH2)6NH2、H2N(H2C)10NH(CH2)7NH2、H2N(H2C)10NH(CH2)8NH2、H2N(H2C)10NH(CH2)9NH2、H2N(H2C)10NH(CH2)11NH2、H2N(H2C)10NH(CH2)12NH2、H2N(H2C)9NH(CH2)6CH(CH3)CH2NH2、H2N(H2C)9NHCH2CH
(CH3)(CH2)6NH2、NH[(CH2)6CH(CH3)CH2NH2]2、NH[CH2CH(CH3)(CH2)6NH2]2In one or more.
4. reflecting plate daiamid composition according to claim 1, it is characterised in that the Chinese white（B1）It is selected from
Comprising but be not limited only to titanium dioxide, zinc oxide, zinc sulphide, white lead, zinc sulfate, barium sulfate, calcium carbonate, aluminum oxide.
5. reflecting plate daiamid composition according to claim 4, it is characterised in that the reinforcer（B2）It is selected from
Threadiness, tabular, needle-like, cross-like strengthening material；The fibee reinforced material is selected from glass fibre, carbon fiber, aromatics
Fypro, liquid crystal polymer（LCP）Fiber, one kind of metallic fiber or its combination；The tabular strengthening material is selected from
Mica, one kind of talcum or its combination；The needle-like strengthening material be selected from potassium titanate crystal whisker, aluminium borate whisker, calcium carbonate crystal whisker,
Magnesium sulfate crystal whisker, wollastonite, sepiolite, eakleite, one kind of ZnOw or its combination；The cross-like strengthening material
Selected from silica, aluminum oxide, barium carbonate, magnesium carbonate, aluminium nitride, boron nitride, potassium titanate, alumina silicate, calcium silicates, magnesium silicate,
Aluminium borate, calcium sulfate, barium sulfate, magnesium sulfate, asbestos, bead, graphite, CNT, carborundum, sericite, hydrotalcite, two
Molybdenum sulfide, phenolic resin, cross-linked styrene system resin, one kind of cross-linked acrylic acid system resin or its combination.
6. reflecting plate daiamid composition according to claim 5, it is characterised in that the alumina silicate is selected from clay.
7. reflecting plate daiamid composition according to claim 6, it is characterised in that the clay be selected from kaolin,
Pyrophillite, bentonitic a kind of or its combination.
8. reflecting plate daiamid composition according to claim 5, it is characterised in that the magnesium silicate is selected from green slope thread
Stone.
9. reflecting plate daiamid composition according to claim 1, it is characterised in that also including inorganic nucleator, institute
State inorganic nucleator be selected from silica, talcum, clay, aluminum oxide, mica, zirconium oxide, titanium dioxide, tin oxide, tin indium oxide,
Antimony tin oxide, calcium carbonate, one kind of zeolite or its combination, its content for based on the daiamid composition gross weight 0.5 ~
5wt%。
10. reflecting plate daiamid composition according to claim 9, it is characterised in that the inorganic nucleator contains
Measure as 2 ~ 4wt% based on the daiamid composition gross weight.
11. reflecting plate daiamid composition according to claim 1, it is characterised in that also including antioxidant, heat-resisting
Stabilizer, light stabilizer, other polymers, impact modifier, fire retardant, fluorescent whitening agent, lubricant, plasticizer, thickener,
Antistatic additive, releasing agent, one kind of pigment or its combination；The antioxidant is selected from phenols, amine, one kind of sulphur class or its group
Close；The heat-resisting stabilizing agent is selected from lactone compound, vitamin E class, hydroquinones, copper halide, one kind of iodine compound or its group
Close；The light stabilizer is selected from benzotriazole, triazines, benzophenone, benzoates, hindered amines, oxalyl and replaces benzene
Amine（Oxanilide）One kind of class or its combination；The other polymers are selected from TPO, polyamide, makrolon, bunching
Aldehyde, polysulfones, polyphenylene oxide, fluororesin, silicone resin, LCP one kind or its combination；The fire retardant is selected from bromine system, chlorine system, phosphorus
System, antimony system, one kind of inorganic system or its combination.
12. reflecting plate daiamid composition according to claim 11, it is characterised in that the other polymers are selected from
Ethene-propylene copolymer, ethene -1- butylene copolymer olefin copolymers, propylene -1- butylene copolymer olefin copolymers gather
Styrene.
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| CN105602243B (en) * | 2015-11-24 | 2018-08-31 | 金发科技股份有限公司 | A kind of daiamid composition and its application |
| CN105802202A (en) * | 2016-05-16 | 2016-07-27 | 苏州新区华士达工程塑胶有限公司 | Modified polyamide-filled plastic |
| CN105907083A (en) * | 2016-05-30 | 2016-08-31 | 张日龙 | Multi-interface mobile phone charger |
| CN106084753B (en) * | 2016-06-17 | 2018-06-29 | 皖西学院 | A kind of dedicated ultraviolet resistance stretch-proof organic composite material of LED lens and preparation method thereof |
| CN110922749A (en) * | 2019-10-26 | 2020-03-27 | 张家港大塚化学有限公司 | Preparation method of high-weather-resistance and high-reflectivity polyamide composite material for LED |
| CN111500062B (en) * | 2020-05-27 | 2023-02-28 | 杭州本松新材料技术股份有限公司 | Antistatic heat-aging-resistant polyamide composite material and preparation method and application thereof |
| CN112940492A (en) * | 2021-03-30 | 2021-06-11 | 江苏江山红化纤有限责任公司 | Flame-retardant polyamide composite material and preparation method thereof |
| CN115651396B (en) * | 2022-10-13 | 2023-09-26 | 金发科技股份有限公司 | Polyamide resin composite material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1890323A (en) * | 2003-12-09 | 2007-01-03 | 三井化学株式会社 | Resin composition for reflector, and reflector |
| US8426549B2 (en) * | 2005-04-15 | 2013-04-23 | Mitsui Chemicals, Inc. | Resin composition for reflector, and reflector |
| JP2008182172A (en) * | 2006-12-27 | 2008-08-07 | Toyoda Gosei Co Ltd | Resin composition for led reflector |
| WO2012026413A1 (en) * | 2010-08-27 | 2012-03-01 | 東洋紡績株式会社 | Polyamide resin composition used for reflective plate for surface mount led |
| KR101333579B1 (en) * | 2010-12-15 | 2013-11-28 | 제일모직주식회사 | Polyamide Resin Composition Having Good Reflectance, Heat resistance, and Humidity resistance |
| CN103328573B (en) * | 2011-01-28 | 2015-05-20 | 可乐丽股份有限公司 | Polyamide composition for reflective plate, reflective plate, light-emitting device comprising said reflective plate, and illumination device and image display device comprising said light-emitting device |
| US8513376B2 (en) * | 2011-03-15 | 2013-08-20 | Air Products And Chemicals, Inc. | Polyamides and amidoamines from selectively modified amine amines |
| FR2976946B1 (en) * | 2011-06-24 | 2014-01-24 | Arkema France | COMPOSITION COMPRISING A SEMI-AROMATIC POLYAMIDE AND USES THEREOF, IN PARTICULAR FOR AN ELECTROLUMINESCENT DIODE REFLECTOR |
| JP5979846B2 (en) * | 2011-10-26 | 2016-08-31 | 大塚化学株式会社 | RESIN COMPOSITION FOR REFLECTOR AND REFLECTOR |
| JP6042114B2 (en) * | 2012-06-26 | 2016-12-14 | 旭化成株式会社 | Copolymerized polyamide and copolymerized polyamide composition |
| CN103642036A (en) * | 2013-11-12 | 2014-03-19 | 金发科技股份有限公司 | Polyamide resin and polyamide composition composed of same |
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