CN109749334A - A kind of halogen-free flame-retardant thermoplastic elastomer and its preparation method and application of the anti-UV of xenon lamp - Google Patents
A kind of halogen-free flame-retardant thermoplastic elastomer and its preparation method and application of the anti-UV of xenon lamp Download PDFInfo
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Abstract
The invention discloses the halogen-free flame-retardant thermoplastic elastomers and preparation method thereof of the anti-UV of xenon lamp a kind of.A kind of halogen-free flame-retardant thermoplastic elastomer of the anti-UV of xenon lamp, is made of raw material below: styrene analog thermoplastic elastomer, filling oil, polyphenylene oxide resin, polyolefin resin, phosphorus-nitrogen containing flame retardant, anti-UV auxiliary agent, processing aid.The preparation method of the halogen-free flame-retardant thermoplastic elastomer of the anti-UV of this xenon lamp is also disclosed simultaneously, also discloses the application of the halogen-free flame-retardant thermoplastic elastomer of the anti-UV of this xenon lamp.The halogen-free flame-retardant thermoplastic elastomer of the anti-UV of xenon lamp of the present invention can satisfy the requirement of E≤2.0 xenon lamp anti-UV Continuous irradiation 300h, △, have excellent flame retardant property.Halogen-free flame-retardant thermoplastic elastomer excellent combination property provided by the invention, preparation process is simple, is worthy of popularization.
Description
Technical field
The present invention relates to the halogen-free flame-retardant thermoplastic elastomers and its preparation method and application of the anti-UV of xenon lamp a kind of.
Background technique
Styrene analog thermoplastic elastomer is a kind of elastomeric material for having plastics and rubber property.And poly- (styrene-
Ethylene-butylene-styrene) copolymer (SEBS) be SBS through hydrogenated processing after product, have superior ageing-resistant performance,
And good mechanical property.Thus become outer one of the main material by sizing material of consumer electronics product, data transmission
Line, earphone cable are its typical use.
Material as consumer electronics product, it is desirable that have Halogen, fire-retardant, not brominated antimony, without using red phosphorus, and meet
The standard requirements such as ROHS, REACH.With this condition, existing typical products formula can add polyphenylene oxide resin and the resistance of phosphorus nitrogen system
Combustion agent makes product have good flame retardant property.Polyphenylene oxide resin is in the product in addition to that can significantly improve the mechanical property of product
Outside, it is also used as a kind of carbon forming agent, fine and close carbon-coating is formed when encountering open fire burning, has completely cut off oxygen, played fire retardation.
And phosphorus-nitrogen containing flame retardant is selected, there is phosphorus nitrogen system synergistic effect, cooperate with polyphenylene oxide resin, play excellent flame retardant property.
Without adding polyphenylene oxide resin, merely using phosphorus-nitrogen containing flame retardant as flame-retardant system, it may appear that fire-retardant unstable situation.And because
The increase of phosphorus-nitrogen containing flame retardant additive amount causes the extreme difficulties of product processing.Polyphenylene oxide resin is not added simultaneously, will lead to
The mechanical property of product is relatively low, and product is easy to appear the unfavorable condition of damaged cracking in use.
In consumer electronics product industry, the appearance of product sizing material is paid much attention to, it is desirable that product is being placed for a long time
Under there can be no metachromatisms, that is to say, that must have good UV resistance.And the polyphenylene oxide tree added in existing formula
Rouge, because the reason of ehter bond, being easy to appear xanthochromia in its structure.It is difficult to meet UV resistance in production white and whens light-coloured prods and want
It asks.This forms great technical problem for dealer.
Accordingly, the anti-UV standard of industry mainstream is ultraviolet lamp (QUV) test, and length of testing speech is full within 96h
The sufficient range of △ E≤3.0.Be added to the styrene analog thermoplastic elastomer of polyphenylene oxide resin, can only excessive addition anti-UV agent come
It meets the requirements, is easy to appear the problem of anti-UV agent is precipitated.With the development of the social economy, competition is more fierce, in order to more meet
Actual applicable cases, more clients propose the testing standard of the anti-UV of xenon lamp.Xenon lamp test is different from ultraviolet lamp test, more
It is irradiated close to actual sunlight, therefore more harsh.It also increases in the duration of xenon lamp test, part of standards requires product
Length of testing speech 300h meets the range of △ E≤2.0.It is more difficult that the anti-UV test of xenon lamp allows styrenic elastomer material to be faced with
Challenge.
Summary of the invention
The present inventor is based on prior art problem by in-depth study, and discovery is keeping polyphenylene oxide resin additive amount constant
In the case where, it can be by the discoloration of the addition control polyphenylene oxide resin of anti-UV adjuvant system, in excellent fireproof performance and mechanics
In the case where property retention, meet the requirement of E≤2.0 xenon lamp anti-UV length of testing speech 300h, △.Therefore, the purpose of the present invention it
One is to provide the halogen-free flame-retardant thermoplastic elastomer of anti-UV of xenon lamp a kind of, and the second object of the present invention is to provide this xenon lamp
The preparation method of the halogen-free flame-retardant thermoplastic elastomer of anti-UV, the third object of the present invention are to provide the anti-UV's of this xenon lamp
The application of halogen-free flame-retardant thermoplastic elastomer.This halogen-free flame-retardant thermoplastic elastomer has xenon lamp UV resistance, excellent resistance
Performance is fired, and mechanical property is maintained.
The technical solution used in the present invention is:
A kind of halogen-free flame-retardant thermoplastic elastomer of the anti-UV of xenon lamp, is made of the raw material of following mass percent:
Preferably, the halogen-free flame-retardant thermoplastic elastomer of the anti-UV of a kind of xenon lamp is the raw material group by following mass percent
At:
Preferably, in the halogen-free flame-retardant thermoplastic elastomer of the anti-UV of this xenon lamp, styrene analog thermoplastic elastomer is
Styrene mass content in SEBS, SEBS is 25%~35%.SEBS refers to poly- (styrene-ethylene-butylene-styrene)
Triblock copolymer.
Preferably, in the halogen-free flame-retardant thermoplastic elastomer of the anti-UV of this xenon lamp, filling oil is paraffinic base white oil, naphthenic base
At least one of white oil.
Preferably, in the halogen-free flame-retardant thermoplastic elastomer of the anti-UV of this xenon lamp, polyphenylene oxide resin (poly- 2,6- dimethyl-
Isosorbide-5-Nitrae-phenylate, also referred to as PPE or PPO) inherent viscosity be 30cm3/ g~50cm3/g。
Preferably, in the halogen-free flame-retardant thermoplastic elastomer of the anti-UV of this xenon lamp, polyolefin resin is polypropylene, poly- second
At least one of alkene, the copolymer of ethylene and propylene, ethylene and hexene copolymer, ethylene and octene copolymer；It is further excellent
Choosing, polyolefin resin is at least one of polypropylene, polyethylene.
Preferably, in the halogen-free flame-retardant thermoplastic elastomer of the anti-UV of this xenon lamp, phosphorus-nitrogen containing flame retardant is phosphorus flame retardant
With the compound flame retardant of nitrogenated flame retardant composition, one of phosphorus-nitrogen composite combustion inhibitor or a variety of；Phosphorus flame retardant is diethyl
Hypo-aluminum orthophosphate, dibutyl hypo-aluminum orthophosphate, diphenyl hypo-aluminum orthophosphate, hypo-aluminum orthophosphate, zinc hypophosphite, ammonium polyphosphate, phosphorous triphenyl phosphate
At least one of ester, isooctyl diphenyl phosphite；Nitrogenated flame retardant is melamine, melamine cyanurate (MCA), trimerization
At least one of cyanamide diamides, ammelide, boric acid melamine, oxalic acid melamine；Phosphorus-nitrogen composite flame-proof
Agent is at least one of melamine pyrophosphate, melamine phosphate, ammonium polyphosphate；It is further preferred that phosphorus nitrogen system hinders
It fires in agent, phosphorus flame retardant is at least one of diethyl hypo-aluminum orthophosphate, hypo-aluminum orthophosphate, zinc hypophosphite；Nitrogenated flame retardant is
At least one of melamine, melamine cyanurate；Phosphorus-nitrogen composite combustion inhibitor is melamine pyrophosphate, melamine
At least one of phosphate.In some preferred embodiments of the present invention, phosphorus-nitrogen containing flame retardant is phosphorus flame retardant
With nitrogenated flame retardant with mass ratio 1:(1~2) compound flame retardant that forms.
Preferably, in the halogen-free flame-retardant thermoplastic elastomer of the anti-UV of this xenon lamp, anti-UV auxiliary agent is that benzophenone light is steady
Determine agent, benzotriazole light stabilizer, at least two compositions in hindered amine light stabilizer mixtures；Further preferably
, anti-UV auxiliary agent is 2-hydroxy-4-n-octoxybenzophenone (UV531), 2- (2- hydroxy-5-methyl base phenyl) benzotriazole
(UV-P), 2- (2'- hydroxyl -5'- t-octyl phenyl) benzotriazole (UV5411), poly-succinic (4- hydroxyl -2,2,6,6- four
Methyl-1-piperidine ethanol) mixture that is formed with arbitrary proportion of ester (UV622)；Still further preferably, anti-UV auxiliary agent is 2- hydroxyl
Base -4- oxy-octyl benzophenone, 2- (2- hydroxy-5-methyl base phenyl) benzotriazole, 2- (2'- hydroxyl -5'- t-octyl phenyl)
Benzotriazole, poly-succinic (4- hydroxyl -2,2,6,6- tetramethyl -1- piperidine ethanol) ester are with mass ratio (2~4): (3~5): (1
~3): the mixture of 1 composition.
Preferably, in the halogen-free flame-retardant thermoplastic elastomer of the anti-UV of this xenon lamp, processing aid be lubricant, antioxidant,
At least one of colorant.
Preferably, in the processing aid of the halogen-free flame-retardant thermoplastic elastomer of the anti-UV of this xenon lamp, lubricant is that silicone is female
Grain, dimethyl silicone polymer, fatty acid amide, erucyl amide, ethylene bis stearic acid amide, pentaerythritol stearate, poly- second
At least one of alkene wax, paraffin.Lubricant play promote formula each component double screw extruder peptizaiton, reduce with
The friction of machinery equipment, and the surface feel of product can be improved.
Preferably, in the processing aid of the halogen-free flame-retardant thermoplastic elastomer of the anti-UV of this xenon lamp, antioxidant is hindered phenol
At least one of kind antioxidant, phosphite ester antioxidant；It is further preferred that in antioxidant, Hinered phenols antioxidant is
Antioxidant 245,264,300,702,703,1010,1024,1076,1098,1135,2246,3114, B215, B225, B900,
At least one of B911, DLTDP, DSTDP；Phosphite ester antioxidant be irgasfos 168,626,627, in P-EPQ extremely
Few one kind；It is further preferred that antioxidant is the compound of Hinered phenols antioxidant and phosphite ester antioxidant mixing composition,
It such as can be selected from antioxidant B215.Antioxidant can prevent formula each component from generating decomposition when processing in double screw extruder, mention
The service life of high product.
Preferably, in the processing aid of the halogen-free flame-retardant thermoplastic elastomer of the anti-UV of this xenon lamp, colorant be titanium dioxide,
At least one of carbon black, toner.
A kind of preparation method of the halogen-free flame-retardant thermoplastic elastomer of the anti-UV of xenon lamp, comprising the following steps:
A) raw material is weighed according to composition above-mentioned；
B) by styrene analog thermoplastic elastomer and filling oil mixing, obtain it is oil-filled after styrene analog thermoplastic elasticity
Body；
C) styrene analog thermoplastic elastomer after will be oil-filled is mixed with other raw materials, obtains mixture；
D) mixture is squeezed out by double screw extruder, is granulated, obtains the halogen-free combustion-proof thermoplastic of the anti-UV of xenon lamp
Elastomer.
Preferably, in the step d) of preparation method, the draw ratio of double screw extruder is 60:1, and double screw extruder is most
Elevated operating temperature is not higher than 230 DEG C.
The halogen-free flame-retardant thermoplastic elastomer of this anti-UV of xenon lamp is preparing the application in electronic product coated material.
Preferably, in, electronic product coated material is consumer electronics product coated material；It is further preferred that electronics
Product coated material can be data line coated material or earphone cord tegument material.
The beneficial effects of the present invention are:
The halogen-free flame-retardant thermoplastic elastomer of the anti-UV of xenon lamp of the present invention can satisfy anti-UV Continuous irradiation 300h, the △ E of xenon lamp
≤ 2.0 requirement has excellent flame retardant property.Halogen-free flame-retardant thermoplastic elastomer excellent combination property provided by the invention,
Preparation process is simple, is worthy of popularization.
Specifically:
Present invention seek to address that halogen-free flame-retardant thermoplastic elastomer, before keeping good flame retardant property and mechanical property
It puts, solves the requirement that product meets E≤2.0 xenon lamp anti-UV length of testing speech 300h, △.
By the compound system of anti-UV agent, the discoloration effect of polyphenylene oxide resin is effectively inhibited.Anti- UV agent system adds
Dosage is few, not will cause the reduction of properties of product.And by experiment test, precipitation will not be generated using anti-UV system of the invention
Problem adversely affects product appearance.
In the present invention, polyphenylene oxide resin and phosphorus-nitrogen containing flame retardant are used cooperatively.Phosphorus-nitrogen containing flame retardant is hindered with gas phase
Based on combustion effect, and there is solidifying phase fire retardation.And polystyrene resin is capable of forming fine and close carbon-coating, thus starvation,
The generation for preventing drip phenomenon makes material have excellent flame retardant property.
Specific embodiment
The contents of the present invention are described in further detail below by way of specific embodiment.Original used in embodiment
Material unless otherwise specified, can be obtained from routine business approach.
Raw material used in embodiment and comparative example are as shown in table 1.
The raw material information of 1 embodiment and comparative example of table
The recipe ingredient of Examples 1 to 4 and comparative example 1~3 is as shown in table 2 below.
The recipe ingredient of table 2 Examples 1 to 4 and comparative example 1~3
Embodiment 1-4 and comparative example 1-3's the preparation method is as follows:
A) each raw material are weighed by 2 recipe ingredient of table:
B) by styrene analog thermoplastic elastomer with filling oil carry out high-speed stirred mix, obtain it is oil-filled after phenylethylene
Thermoplastic elastomer (TPE)；
C) styrene analog thermoplastic elastomer after will be oil-filled carries out high-speed stirred with other ingredients and mixes, after obtaining mixing
Material；
D) mixed material is poured into and carries out extruding pelletization in double screw extruder.The draw ratio of double screw extruder is
60:1.Each warm area set temperature of double screw extruder are as follows: 180 DEG C, 210 DEG C, 230 DEG C, 230 DEG C, 230 DEG C, 230 DEG C, 225
DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 220 DEG C, 220 DEG C, 220 DEG C, 220 DEG C, 215 DEG C.Engine speed 400r/min.
Embodiment 1
According to the halogen-free flame-retardant thermoplastic elastomer of the ingredient percent composition anti-UV of xenon lamp of embodiment 1 in table 2.Its
Middle styrenic elastomer is poly- (styrene-ethylene-butylene-styrene) triblock copolymer (SEBS), and styrene-content is
31%.Filling oil is paraffinic base white oil.Polyphenylene oxide resin is poly- 2,6- dimethyl-Isosorbide-5-Nitrae-phenylate (PPE), inherent viscosity
35cm3/g.Polyolefin resin is being used cooperatively for polypropylene and polyethylene.Phosphorus-nitrogen containing flame retardant is melamine cyanurate and two
Ethyl hypo-aluminum orthophosphate is used cooperatively.Anti- UV agent system is ratio of the UV531:UV-P:UV5411:UV622 according to mass ratio 3:4:2:1
Example mixing, additive amount 2%.Lubricant is silicone master batch.Colorant is titanium dioxide.Antioxidant is B215, is resisted by Hinered phenols
Oxygen agent and phosphite ester antioxidant compound.
Embodiment 2
Embodiment 2 and the difference of embodiment 1 are poly- (styrene-ethylene-butylene-styrene) triblock copolymer (SEBS)
It is 40%.Polyolefin resin is polypropylene, additive amount 5%.Phosphorus-nitrogen containing flame retardant is 30%.Other ingredient percents
It is shown in Table 2.
Embodiment 3
Embodiment 3 and the difference of embodiment 1 are poly- (styrene-ethylene-butylene-styrene) triblock copolymer (SEBS)
It is 24.5%.Polyphenylene oxide resin (PPE) is 15%.Phosphorus-nitrogen containing flame retardant is 32%.Anti- UV agent system is 2.5%.It can compare
The △ E value of different polyphenylene oxide resin additive amounts changes.Other ingredient percents are shown in Table 2.
Embodiment 4
Embodiment 4 and the difference of embodiment 1 are poly- (styrene-ethylene-butylene-styrene) triblock copolymer (SEBS)
It is 21%.Polyphenylene oxide resin (PPE) is 20%.Phosphorus-nitrogen containing flame retardant is 30%.Anti- UV agent system is 3%.It can compare in difference
The △ E value of polyphenylene oxide resin additive amount changes.Other ingredient percents are shown in Table 2.
Comparative example 1
Comparative example 1 and the difference of embodiment 1 are not add anti-UV agent.Other ingredient percents are shown in Table 2.
Comparative example 2
Comparative example 2 and embodiment 1, which are distinguished, to be only to add anti-UV agent UV5411, the anti-UV body in additive amount and embodiment 1
System is consistent.Other ingredient percents are shown in Table 2.
Comparative example 3
Comparative example 3 and the difference of embodiment 1 are not add PPE resin.Phosphorus-nitrogen containing flame retardant is 47%.It can compare and not add
In the case where adding PPE ingredient, the performance change of material.Other ingredient percents are shown in Table 2.
Embodiment 1-4 and comparative example 1-3 prepares the performance test results such as 3 institute of table of the hot elastomer of resulting halogen-free flameproof
Show.
The performance test results of table 3 embodiment 1-4 and comparative example 1-3
Xenon lamp irradiation test condition in table 3 is specific as follows:
Xenon lamp aging instrument: Xe-3, raw manufacturer Q-lab；
Irradiation intensity is 0.55w/m2, fluorescent tube wavelength is 340nm, optical filter DAYLIGHT-Q；
Humidity 30%, 55 DEG C of blackboard temperature；
Length of testing speech: 300h Continuous irradiation；
Determine to require: E≤2.0 △ are qualification.
By the result of embodiment 1-4 in table 3 it is found that in halogen-free flame-retardant thermoplastic elastomer in the embodiment of the present invention,
In the case where the anti-addition of UV agent system 2-3%, polyphenylene oxide resin (PPE) additive amount 10-20%, it can satisfy the anti-UV of xenon lamp and survey
Try 300h continuous illumination, the requirement of E≤2.0 △.
By the result of comparative example 1 and comparative example 2 in table 3 it is found that single in the anti-UV agent system of no addition or addition
In the case where anti-UV agent, material is unable to satisfy the requirement of the anti-UV test of xenon lamp.
By the result of the comparative example 3 in table 3 it is found that in the case where no addition polyphenylene oxide resin, increase phosphorus nitrogen system
Fire retardant is 47%, and the tensile strength of material is decreased obviously, be unable to satisfy in UL1581 standard about tensile strength >=
The requirement of 8.3MPa, and the flame-retardancy requirements of UL1581VW-1 can not be passed through.
Halogen-free flame-retardant thermoplastic elastomer UV test anti-to xenon lamp in the present invention proposes feasible solution, can be wide
It is general to be used for consumer electronics product field (such as data line coated material, earphone cord tegument material), and can expand to plastic bag
The fields such as glue, toy, automobile interior decoration.
The description of book according to the above description, those skilled in the art in the invention can also carry out above embodiment
Change and modification.Therefore, the invention is not limited to above-mentioned specific embodiments, also answer some modifications and changes of invention
This belongs within claims of the invention.
Claims (10)
1. a kind of halogen-free flame-retardant thermoplastic elastomer of the anti-UV of xenon lamp, it is characterised in that: be by the raw material of following mass percent
Composition:
2. the halogen-free flame-retardant thermoplastic elastomer of the anti-UV of xenon lamp according to claim 1 a kind of, it is characterised in that: styrene
Analog thermoplastic elastomer is SEBS, and the styrene mass content in SEBS is 25%~35%.
3. the halogen-free flame-retardant thermoplastic elastomer of the anti-UV of xenon lamp according to claim 1 a kind of, it is characterised in that: filling oil
For at least one of paraffinic base white oil, naphthenic base white oil.
4. the halogen-free flame-retardant thermoplastic elastomer of the anti-UV of xenon lamp according to claim 1 a kind of, it is characterised in that: polyphenylene oxide
Inherent viscosity be 30cm3/ g~50cm3/g。
5. the halogen-free flame-retardant thermoplastic elastomer of the anti-UV of xenon lamp according to claim 1 a kind of, it is characterised in that: polyolefin
Resin is in copolymer, ethylene and the hexene copolymer, ethylene and octene copolymer of polypropylene, polyethylene, ethylene and propylene
It is at least one.
6. the halogen-free flame-retardant thermoplastic elastomer of the anti-UV of xenon lamp according to claim 1 a kind of, it is characterised in that: phosphorus nitrogen system
Fire retardant is one of the compound flame retardant of phosphorus flame retardant and nitrogenated flame retardant composition, phosphorus-nitrogen composite combustion inhibitor or a variety of；
Phosphorus flame retardant is diethyl hypo-aluminum orthophosphate, dibutyl hypo-aluminum orthophosphate, diphenyl hypo-aluminum orthophosphate, hypo-aluminum orthophosphate, zinc hypophosphite, gathers
At least one of ammonium phosphate, triphenyl phosphite, isooctyl diphenyl phosphite；Nitrogenated flame retardant is melamine, cyanuric acid
At least one of melamine, ammeline, ammelide, boric acid melamine, oxalic acid melamine；
Phosphorus-nitrogen composite combustion inhibitor is at least one of melamine pyrophosphate, melamine phosphate, ammonium polyphosphate.
7. the halogen-free flame-retardant thermoplastic elastomer of the anti-UV of xenon lamp according to claim 1 a kind of, it is characterised in that: anti-UV is helped
Agent is benzophenone light stabilizer, benzotriazole light stabilizer, at least two compositions in hindered amine light stabilizer
Mixture.
8. the halogen-free flame-retardant thermoplastic elastomer of the anti-UV of xenon lamp according to claim 1 a kind of, it is characterised in that: processing helps
Agent is at least one of lubricant, antioxidant, colorant.
9. a kind of preparation method of the halogen-free flame-retardant thermoplastic elastomer of the anti-UV of xenon lamp, it is characterised in that: the following steps are included:
A) composition according to any one of claims 1 to 8 weighs raw material；
B) by styrene analog thermoplastic elastomer and filling oil mixing, obtain it is oil-filled after styrene analog thermoplastic elastomer；
C) styrene analog thermoplastic elastomer after will be oil-filled is mixed with other raw materials, obtains mixture；
D) mixture is squeezed out by double screw extruder, is granulated, obtain the halogen-free combustion-proof thermoplastic elasticity of the anti-UV of xenon lamp
Body.
10. a kind of any one of claim 1~8 halogen-free flame-retardant thermoplastic elastomer of the anti-UV of xenon lamp is preparing electronic product
Application in coated material.
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| CN113603960A (en) * | 2021-09-14 | 2021-11-05 | 广东聚石化学股份有限公司 | Halogen-free flame-retardant material and preparation method and application thereof |
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Application publication date: 20190514 |