CN104479308B - Flame-retardant reinforced PBT plastic that a kind of 850 degree of glowing filaments are nonflammable and preparation method thereof - Google Patents
Flame-retardant reinforced PBT plastic that a kind of 850 degree of glowing filaments are nonflammable and preparation method thereof Download PDFInfo
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- CN104479308B CN104479308B CN201410852365.7A CN201410852365A CN104479308B CN 104479308 B CN104479308 B CN 104479308B CN 201410852365 A CN201410852365 A CN 201410852365A CN 104479308 B CN104479308 B CN 104479308B
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 40
- 239000004033 plastic Substances 0.000 title claims abstract description 30
- 229920003023 plastic Polymers 0.000 title claims abstract description 30
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims description 15
- 239000003822 epoxy resin Substances 0.000 claims abstract description 13
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 13
- 239000000314 lubricant Substances 0.000 claims abstract description 11
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 10
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 10
- AYEKOFBPNLCAJY-UHFFFAOYSA-O thiamine pyrophosphate Chemical compound CC1=C(CCOP(O)(=O)OP(O)(O)=O)SC=[N+]1CC1=CN=C(C)N=C1N AYEKOFBPNLCAJY-UHFFFAOYSA-O 0.000 claims abstract description 9
- 239000003365 glass fiber Substances 0.000 claims abstract description 8
- NSBGJRFJIJFMGW-UHFFFAOYSA-N trisodium;stiborate Chemical compound [Na+].[Na+].[Na+].[O-][Sb]([O-])([O-])=O NSBGJRFJIJFMGW-UHFFFAOYSA-N 0.000 claims abstract description 8
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 4
- 239000004927 clay Substances 0.000 claims description 4
- 229910000077 silane Inorganic materials 0.000 claims description 4
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical group CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 3
- 229920001296 polysiloxane Polymers 0.000 claims description 3
- 239000007977 PBT buffer Substances 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 abstract description 5
- 230000000979 retarding effect Effects 0.000 abstract description 4
- 229920001707 polybutylene terephthalate Polymers 0.000 description 53
- 238000012360 testing method Methods 0.000 description 6
- -1 Polybutylene terephthalate Polymers 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000010348 incorporation Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- ZQKXQUJXLSSJCH-UHFFFAOYSA-N melamine cyanurate Chemical compound NC1=NC(N)=NC(N)=N1.O=C1NC(=O)NC(=O)N1 ZQKXQUJXLSSJCH-UHFFFAOYSA-N 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 150000003918 triazines Chemical class 0.000 description 2
- 229920013683 Celanese Polymers 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910000410 antimony oxide Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229920006225 ethylene-methyl acrylate Polymers 0.000 description 1
- 239000012757 flame retardant agent Substances 0.000 description 1
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000007786 learning performance Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention discloses the flame-retardant reinforced PBT plastic that a kind of 850 degree of glowing filaments are nonflammable, its percentage includes following components: PBT 25～35%, PET 5～10%, MCA 5～10%, TDE 5～8%, brominated epoxy resin 5～8%, sodium antimonate 3～5%, TPP 3～5%, EMA g GMA 1～3%, Firebrake ZB 1～3%, antioxidant 0.5～1%, lubricant 0.4～1%, glass fibre 25～30%.The PBT plastic of the present invention is to use polynary fire retardant to compound, the consumption of fire retardant can be reduced while improving flame retarding efficiency, take into account fire resistance and mechanical property, the requirement of the nonflammable temperature of glowing filament 850 DEG C can not only be reached, mechanical property also meets use requirement, is suitable for reality application.
Description
Technical field
The present invention relates to technical field of polymer materials, be specifically related to the flame-retardant reinforced PBT that a kind of 850 degree of glowing filaments are nonflammable
Plastics and preparation method thereof.
Background technology
Polybutylene terephthalate (PBT), English name polybutylene terephthalate (is called for short PBT), is thermoplasticity
Polyester, is to be developed by Celanese company of the U.S. the last century initial stage seventies.PBT has extraordinary and hot, resistance to
Hou Xing, chemical-resistant, and there is the advantages such as excellent electric properties, water absorption is little, surface is good, it is widely used in
The industries such as electric, automobile, machinery, household electrical appliance, the most electric industry.
Normally, electric industry mostly has flame-retardancy requirements to material, typically requires that the omnidistance nonflammable temperature of glowing filament reaches
750℃.PBT material in early days is modified by adding substantial amounts of fire retardant, and the omnidistance nonflammable temperature of glowing filament can reach 750 DEG C.
Along with the development of society, electronic product increasingly trends towards high-end development, and the standard of PBT material journey is carried again by Europe electronic product
A high step, temperature nonflammable to glowing filament is risen to 850 DEG C by original 750 DEG C.But, according to traditional improvement
Method, continues to add fire retardant, although can make the glowing filament of PBT material on the PBT material that the nonflammable temperature of glowing filament reaches 750 DEG C
Nonflammable temperature reaches 850 DEG C, but the mechanical property of material can completely lose, and does not has actual application value.Such as, existing use
Brominated triazine, antimony oxide, MCA fire retardant (Chinese name: melamine cyanurate) are compound, improve the resistance of PBT material
Combustion performance, but the PBT material mechanical property obtained is excessively poor.Being additionally, since fire retardant addition big, powder is without place
Reason is directly added into, and causes processing technique to be difficult to control to.It addition, fire retardant duplicate kind is few, flame retarding efficiency, glowing filament efficiency
The lowest, therefore addition is big, and the cost intensive of brominated triazine, cause relatively costly, be not suitable for actual application.
Summary of the invention
This defect aiming to overcome that above-mentioned prior art being, it is provided that the fire-retardant increasing that a kind of 850 degree of glowing filaments are nonflammable
Strong PBT plastic and preparation method thereof.The PBT plastic of the present invention is to use polynary fire retardant to compound, and is improving flame retarding efficiency
The consumption of fire retardant can be reduced simultaneously, take into account fire resistance and mechanical property, the nonflammable temperature of glowing filament can not only be reached
The requirement of 850 DEG C, mechanical property also meets use requirement, is suitable for reality application.
Technical scheme is as follows:
The flame-retardant reinforced PBT plastic that a kind of 850 degree of glowing filaments are nonflammable, its percentage includes following components:
Preferably, the flame-retardant reinforced PBT plastic that 850 degree of glowing filaments of the present invention are nonflammable, its percentage includes
Following components:
Preferably, described PBT is mixed by granular PBT and powder PBT.
Preferably, in order to improve flame retarding efficiency and the stability of product, described brominated epoxy resin selection weight average molecular weight is
The brominated epoxy resin of 30000-40000.
Preferably, MCA uses silane coupler to carry out surface preparation so that the compatibility of MCA with PBT is good, thus is carrying
Product stable mechanical property can be made while the anti-flammability of high product.
Preferably, described antioxidant is antioxidant 1010, and described lubricant is silicone powder.
The preparation method of the flame-retardant reinforced PBT plastic that 850 degree of glowing filaments of the present invention are nonflammable comprises the following steps:
(1) take part PBT material to clay into power, be subsequently adding fire retardant MCA, TDE, brominated epoxy resin,
Sodium antimonate, TPP, EMA-g-GMA, Firebrake ZB mix homogeneously；
(2) remaining PBT and antioxidant, lubricant, glass fibre mixing are added；
(3) pelletize is melt extruded.
Preferably, step (1) take 50～60% PBT material clay into power.
Preferably, the time that step (1) PBT powder and fire retardant are mixed is 5～10min.
Compared with prior art, the invention has the beneficial effects as follows:
1, the fire retardant that the PBT material of the present invention is added is that polynary fire retardant compounds and forms, it is possible to significantly improve PBT line effect
Rate, while improving the glow wire temperature of PBT, it is ensured that the mechanical property of PBT plastic disclosure satisfy that use requirement.
2, the present invention selects fire retardant with low cost to compound, and is improving PBT glow wire temperature and is ensureing PBT plastic power
While learning performance, reduce raw-material cost.
3, mixing with fire retardant after the PBT material pulverizing of the present invention, between powder and powder, contact area is big, overcomes powder again
With granule segregative defect in mixed process, it is possible to make PBT and composite flame-retardant agent be sufficiently mixed uniformly.
4, the MCA of the present invention uses silane coupler to carry out surface preparation so that the compatibility of MCA with PBT is good, thus
Product stable mechanical property can be made while improving the anti-flammability of product.
Detailed description of the invention
Below by being embodied as example, the present invention is described in further detail.
Term is explained:
PBT: polybutylene terephthalate (PBT)
PET: polyethylene terephthalate
MCA: melamine cyanurate
TPP: triphenyl phosphate
EMA-g-GMA: ethylene-methyl acrylate copolymer graft glycidyl methacrylate
In following embodiment, brominated epoxy resin selects weight average molecular weight to be the brominated epoxy resin of 30000-40000.
In following anti-embodiment, oxygen agent is antioxidant 1010, and described lubricant is silicone powder.
Following MCA uses silane coupler to carry out surface preparation, and preprocess method is: at a temperature of 80-100 DEG C,
Mixed processing under the speed conditions of 1200-1300rpm.
Embodiment 1
The flame-retardant reinforced PBT plastic that a kind of 850 degree of glowing filaments are nonflammable, its percentage includes following components:
The preparation method of the flame-retardant reinforced PBT plastic that above-mentioned 850 degree of glowing filaments are nonflammable is:
(1) take powder PBT material, add fire retardant MCA, TDE, brominated epoxy resin, sodium antimonate,
TPP, EMA-g-GMA, Firebrake ZB mix homogeneously, incorporation time is 5min；
(2) granular PBT and antioxidant, lubricant, glass fibre mixing are added；
(3) pelletize is melt extruded.
Take above-mentioned prepared PBT plastic and carry out Mechanics Performance Testing, Mechanics Performance Testing environment: 23 degree, dry state, the results are shown in Table
1。
Table 1PBT plastics mechanical experimental results
Embodiment 2
The flame-retardant reinforced PBT plastic that a kind of 850 degree of glowing filaments are nonflammable, its percentage includes following components:
The preparation method of the flame-retardant reinforced PBT plastic that above-mentioned 850 degree of glowing filaments are nonflammable is:
(1) take powder PBT material, add fire retardant MCA, TDE, brominated epoxy resin, sodium antimonate,
TPP, EMA-g-GMA, Firebrake ZB mix homogeneously, incorporation time is 10min；
(2) granular PBT and antioxidant, lubricant, glass fibre mixing are added；
(3) pelletize is melt extruded.
Take above-mentioned prepared PBT plastic and carry out Mechanics Performance Testing, Mechanics Performance Testing environment: 23 degree, dry state, the results are shown in Table
2。
Table 2PBT plastics mechanical experimental results
Embodiment 3
The flame-retardant reinforced PBT plastic that a kind of 850 degree of glowing filaments are nonflammable, its percentage includes following components:
The preparation method of the flame-retardant reinforced PBT plastic that above-mentioned 850 degree of glowing filaments are nonflammable is:
(1) take powder PBT material, add fire retardant MCA, TDE, brominated epoxy resin, sodium antimonate,
TPP, EMA-g-GMA, Firebrake ZB mix homogeneously, incorporation time is 10min；
(2) granular PBT and antioxidant, lubricant, glass fibre mixing are added；
(3) pelletize is melt extruded.
Take above-mentioned prepared PBT plastic and carry out Mechanics Performance Testing, Mechanics Performance Testing environment: 23 degree, dry state, the results are shown in Table
3。
Table 3PBT plastics mechanical experimental results
The announcement of book and teaching according to the above description, above-mentioned embodiment can also be entered by those skilled in the art in the invention
Row change and amendment.Therefore, the invention is not limited in detailed description of the invention disclosed and described above, to the present invention
A little modifications and changes should also be as falling in the scope of the claims of the present invention.Although additionally, this specification employing
Some specific terms, but these terms are merely for convenience of description, and the present invention does not constitute any restriction.
Claims (6)
1. the flame-retardant reinforced PBT plastic that 850 degree of glowing filaments are nonflammable, it is characterised in that percentage include with
Lower component:
PBT 25～35%
PET 5～10%
MCA 5～10%
TDE 5～8%
Brominated epoxy resin 5～8%
Sodium antimonate 3～5%
TPP 3～5%
EMA-g-GMA 1～3%
Firebrake ZB 1～3%
Antioxidant 0.5～1%
Lubricant 0.4～1%
Glass fibre 25～30%；
Described PBT is mixed by granular PBT and powder PBT；
The weight average molecular weight of described brominated epoxy resin is 30000-40000；
Described MCA uses silane coupler to carry out surface preparation.
The flame-retardant reinforced PBT plastic that 850 degree of glowing filaments the most as claimed in claim 1 are nonflammable, it is characterised in that by weight
Percent meter includes following components:
PBT 31%
PET 8%
MCA 10%
TDE 5%
Brominated epoxy resin 5%
Sodium antimonate 3%
TPP 3%
EMA-g-GMA 1%
Firebrake ZB 1%
Antioxidant 0.6%
Lubricant 0.4%
Glass fibre 30%.
The flame-retardant reinforced PBT plastic that 850 degree of glowing filaments the most as claimed in claim 1 or 2 are nonflammable, it is characterised in that:
Described antioxidant is antioxidant 1010, and described lubricant is silicone powder.
4. a preparation method for the flame-retardant reinforced PBT plastic that 850 degree of glowing filaments described in claim 1 are nonflammable, it is special
Levy and be to comprise the following steps:
(1) take part PBT material to clay into power, be subsequently adding fire retardant MCA, TDE, brominated epoxy resin,
Sodium antimonate, TPP, EMA-g-GMA, Firebrake ZB mix homogeneously；
(2) remaining PBT and antioxidant, lubricant, glass fibre mixing are added；
(3) pelletize is melt extruded.
The preparation method of the flame-retardant reinforced PBT plastic that 850 degree of glowing filaments the most as claimed in claim 4 are nonflammable, its feature
Be: step (1) take 50～60% PBT material clay into power.
The preparation method of the flame-retardant reinforced PBT plastic that 850 degree of glowing filaments the most as claimed in claim 4 are nonflammable, its feature
It is: the time that step (1) PBT powder and fire retardant are mixed is 5～10min.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410852365.7A CN104479308B (en) | 2014-12-30 | 2014-12-30 | Flame-retardant reinforced PBT plastic that a kind of 850 degree of glowing filaments are nonflammable and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410852365.7A CN104479308B (en) | 2014-12-30 | 2014-12-30 | Flame-retardant reinforced PBT plastic that a kind of 850 degree of glowing filaments are nonflammable and preparation method thereof |
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| Publication Number | Publication Date |
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| CN104845299A (en) * | 2015-05-27 | 2015-08-19 | 佛山市顺德区美的洗涤电器制造有限公司 | Glass fiber reinforced flame-retardant PBT material for washing pump and washing pump |
| CN105647134A (en) * | 2016-03-06 | 2016-06-08 | 贝克兰(厦门)新材料有限公司 | Flame-retardant glass fiber reinforced PBT (polybutylene terephthalate) with high glow wires and high CTI (comparative tracking index) value and method for preparing flame-retardant glass fiber reinforced PBT |
| CN106380796A (en) * | 2016-08-31 | 2017-02-08 | 广东顺德顺炎新材料股份有限公司 | Low-cost PBT making glowing filaments incombustible at temperature of 870 DEG C in whole process and preparation method thereof |
| CN107841093A (en) * | 2016-09-19 | 2018-03-27 | 黑龙江鑫达企业集团有限公司 | A kind of PBT plastic of heat conductive insulating fire resistance enhancing and preparation method thereof |
| CN106280323A (en) * | 2016-09-26 | 2017-01-04 | 广东思汗新材料有限公司 | A kind of 850 DEG C of glowing filaments of enhancement mode are nonflammable, PBT/ASA composite and preparation method thereof |
| CN110003624A (en) * | 2019-03-25 | 2019-07-12 | 广东顺德顺炎新材料股份有限公司 | A kind of HI high impact, high-glowing-filament-temperature flame-retardancy enhancing PBT plastic and preparation method thereof |
| CN110028765A (en) * | 2019-03-25 | 2019-07-19 | 广东顺德顺炎新材料股份有限公司 | A kind of high-glowing-filament-temperature flame-retardancy enhancing laser print wrongly written or mispronounced character PBT plastic and preparation method thereof |
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| CN102115579A (en) * | 2010-01-04 | 2011-07-06 | 佛山市顺德区威林工程塑料有限公司 | High-toughness high-glowing-filament-ignition-temperature flame-retardant reinforced PBT (polybutylene terephthalate) material and preparation method thereof |
| CN102070885B (en) * | 2010-12-15 | 2012-10-03 | 深圳市富恒塑胶新材料有限公司 | Halogen-free flame-retardant glass fiber reinforced polyester terephthalate (PET)/poly butylenes terephthalate (PBT) alloy and preparation method thereof |
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Denomination of invention: A flame retardant reinforced PBT plastic with 850 degree glow wire and its preparation method Effective date of registration: 20201222 Granted publication date: 20161130 Pledgee: Shunde Guangdong rural commercial bank Limited by Share Ltd. Daliang branch Pledgor: GUANGDONG SHUNDE SHUNYAN NEW MATERIAL Co.,Ltd. Registration number: Y2020980009785 |
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| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20211215 Granted publication date: 20161130 Pledgee: Shunde Guangdong rural commercial bank Limited by Share Ltd. Daliang branch Pledgor: GUANGDONG SHUNDE SHUNYAN NEW MATERIAL Co.,Ltd. Registration number: Y2020980009785 |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: The invention relates to a flame retardant reinforced PBT plastic without ignition of 850 degree hot wire and a preparation method thereof Effective date of registration: 20211217 Granted publication date: 20161130 Pledgee: Guangdong Shunde Rural Commercial Bank Co.,Ltd. science and technology innovation sub branch Pledgor: GUANGDONG SHUNDE SHUNYAN NEW MATERIAL Co.,Ltd. Registration number: Y2021980015381 |