CN115651375A - Halogen flame-retardant PBT (polybutylene terephthalate) material as well as preparation method and application thereof - Google Patents
Halogen flame-retardant PBT (polybutylene terephthalate) material as well as preparation method and application thereof Download PDFInfo
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- CN115651375A CN115651375A CN202211319149.7A CN202211319149A CN115651375A CN 115651375 A CN115651375 A CN 115651375A CN 202211319149 A CN202211319149 A CN 202211319149A CN 115651375 A CN115651375 A CN 115651375A
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- pbt material
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- 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 54
- 239000003063 flame retardant Substances 0.000 title claims abstract description 46
- 239000000463 material Substances 0.000 title claims abstract description 45
- 229910052736 halogen Inorganic materials 0.000 title claims abstract description 24
- 150000002367 halogens Chemical class 0.000 title claims abstract description 24
- -1 polybutylene terephthalate Polymers 0.000 title claims description 6
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 229920001707 polybutylene terephthalate Polymers 0.000 title description 29
- 239000003365 glass fiber Substances 0.000 claims abstract description 11
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 3
- 239000011324 bead Substances 0.000 claims description 23
- 239000011521 glass Substances 0.000 claims description 22
- 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 description 21
- 239000002245 particle Substances 0.000 claims description 14
- 238000002844 melting Methods 0.000 claims description 11
- 230000008018 melting Effects 0.000 claims description 11
- 239000003963 antioxidant agent Substances 0.000 claims description 6
- 230000003078 antioxidant effect Effects 0.000 claims description 6
- 239000000314 lubricant Substances 0.000 claims description 6
- 239000004593 Epoxy Substances 0.000 claims description 4
- 239000004793 Polystyrene Substances 0.000 claims description 4
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 claims description 4
- 239000000835 fiber Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 239000004033 plastic Substances 0.000 claims description 4
- 229920003023 plastic Polymers 0.000 claims description 4
- 229920002223 polystyrene Polymers 0.000 claims description 4
- 238000001125 extrusion Methods 0.000 claims description 3
- 238000005469 granulation Methods 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 3
- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 2
- 229920000388 Polyphosphate Polymers 0.000 claims description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 2
- VSVVZZQIUJXYQA-UHFFFAOYSA-N [3-(3-dodecylsulfanylpropanoyloxy)-2,2-bis(3-dodecylsulfanylpropanoyloxymethyl)propyl] 3-dodecylsulfanylpropanoate Chemical compound CCCCCCCCCCCCSCCC(=O)OCC(COC(=O)CCSCCCCCCCCCCCC)(COC(=O)CCSCCCCCCCCCCCC)COC(=O)CCSCCCCCCCCCCCC VSVVZZQIUJXYQA-UHFFFAOYSA-N 0.000 claims description 2
- OCKWAZCWKSMKNC-UHFFFAOYSA-N [3-octadecanoyloxy-2,2-bis(octadecanoyloxymethyl)propyl] octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(COC(=O)CCCCCCCCCCCCCCCCC)(COC(=O)CCCCCCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCCCCCC OCKWAZCWKSMKNC-UHFFFAOYSA-N 0.000 claims description 2
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 2
- 239000008116 calcium stearate Substances 0.000 claims description 2
- 235000013539 calcium stearate Nutrition 0.000 claims description 2
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 claims description 2
- 239000001205 polyphosphate Substances 0.000 claims description 2
- 235000011176 polyphosphates Nutrition 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 abstract description 22
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 2
- 239000011707 mineral Substances 0.000 abstract description 2
- 239000011347 resin Substances 0.000 abstract description 2
- 229920005989 resin Polymers 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 6
- 238000011056 performance test Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000009472 formulation Methods 0.000 description 3
- 238000002955 isolation Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- 239000013065 commercial product Substances 0.000 description 2
- 229920006351 engineering plastic Polymers 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229920001169 thermoplastic Polymers 0.000 description 2
- 239000004416 thermosoftening plastic Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000011325 microbead Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000006060 molten glass Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229930184616 taxin Natural products 0.000 description 1
- KOTXAHKUCAQPQA-AAUVPWARSA-N taxine Chemical compound C1([C@@H]([C@@H](O)C(=O)O[C@@H]2C=3/C[C@@](C([C@H](O)C4=C(C)[C@@H](OC(C)=O)CC(C4(C)C)[C@@H](OC(C)=O)\C=3)=O)(C)[C@@H](O)C2)N(C)C)=CC=CC=C1 KOTXAHKUCAQPQA-AAUVPWARSA-N 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a halogen flame-retardant PBT material and a preparation method and application thereof, wherein the halogen flame-retardant PBT material comprises the following components in parts by weight: 36-78 parts of PBT resin; 10-30 parts of glass fiber; 1-15 parts of a flame retardant; 2-5 parts of a flame retardant; 1-3 parts of a flame retardant; 5-10 parts of minerals; 0.5-1 part of an auxiliary agent. The halogen flame-retardant PBT material provided by the invention has excellent flame retardance and CTI (comparative tracking index) performance, so that the PBT material can be applied to the field with higher requirements on the electrical performance of the material.
Description
Technical Field
The invention belongs to the technical field of engineering plastics, and particularly relates to a halogen flame-retardant PBT material as well as a preparation method and an application thereof.
Background
Polybutylene terephthalate (PBT), a polyester produced by polycondensation of terephthalic acid and 1, 4-butanediol, is also one of the most important thermoplastic polyesters, five major engineering plastics. PBT is a milky translucent to opaque semi-crystalline thermoplastic polyester, and has the characteristics of high heat resistance (capable of working for a long time at 140 ℃), toughness, fatigue resistance, self-lubrication, low friction coefficient, organic solvent resistance and the like. Due to these excellent properties, PBT is widely used in the fields of automobiles, mechanical equipment, precision instrument parts, electronic and electrical appliances, textiles, and the like. Compared with halogen-free flame-retardant materials, the halogen-containing flame-retardant PBT material has better mechanical properties. However, the existing halogen flame-retardant PBT material has a lower CTI value, so that the halogen flame-retardant PBT material cannot be used on parts with certain high-pressure requirements.
Therefore, how to improve the CTI value of the halogen flame-retardant PBT material and widen the application range of the PBT material is a problem to be solved urgently.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a halogen flame-retardant PBT material, and a preparation method and application thereof. The halogen flame-retardant PBT material provided by the invention has excellent flame-retardant performance and CTI value.
The method is realized by the following technical scheme:
the halogen flame-retardant PBT material comprises the following components in parts by weight:
the flame retardant 1 is brominated polystyrene and/or brominated epoxy flame retardant;
the flame retardant 2 is antimony white or crystalline polyphosphate;
the flame retardant 3 is zinc borate.
The melting point of the glass beads is 330-400 ℃, and the glass beads and zinc borate are compounded, so that when the material is combusted, the glass beads can be rapidly melted and a compact glass layer is formed on the surface of the material due to the low melting point of the glass beads, and the flame retardant property and CTI of the material are obviously improved. The zinc borate can also improve CTI, but the zinc borate can be used alone, the addition amount is very high to achieve a certain effect, but the addition amount is too high to cause poor mechanical strength of the material, and the zinc borate and the low-melting-point microbeads are compounded, and can be used for assisting in melting in a synergistic manner, so that an isolation layer is more easily formed on the surface.
Further, the particle size of the zinc borate is 2-4 μm. The zinc borate has small particle size and is easy to disperse in the material, which is beneficial to better forming an insulating layer.
Further, the particle size of the glass beads is 5-25 μm. The particle size is small, the dispersion is easy, an isolation layer formed in melting is more compact, and the better the CTI value improving effect is.
Further, the weight ratio of the glass beads to the zinc borate is (2-3): 1. The glass beads and the zinc borate have certain difference in particle size, and the zinc borate with low particle size can make up for pores generated after the protective layer is formed by the beads with larger relative particle size. The smaller the bead size, the lower the zinc borate ratio. The two complement each other, and the formed isolation layer is better, thereby better improving the CTI value.
Further, the glass fiber is chopped fiber with the length of 3-5 mm.
Further, the auxiliary agent is an antioxidant and/or a lubricant. Specifically, the antioxidant may be one or more of tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] pentaerythritol ester, pentaerythritol tetrakis (3-laurylthiopropionate) and tris [2, 4-di-tert-butylphenyl ] phosphite; the lubricant is one or more of Ethylene Bis Stearamide (EBS), E wax, calcium stearate and pentaerythritol tetrastearate.
The invention also provides a preparation method of the halogen flame-retardant PBT material, which comprises the following steps:
s1: weighing the components according to the proportion, premixing the components except the glass fiber, and then adding the components into an extruder;
s2: and (3) adding glass fibers into the extruder from the side feeding, and performing melt extrusion and granulation to obtain the halogen flame-retardant PBT material.
The invention also provides application of the halogen flame-retardant PBT material in preparing electronic and electric plastic parts, and is particularly suitable for preparing plastic parts with higher requirements on electric properties, such as automotive copper bars, household appliance circuit breakers, automotive current sensors and the like.
Has the advantages that:
according to the invention, the mineral and zinc borate are added into the PBT resin, so that a molten glass layer is formed in the material in the combustion process, the CTI value of the halogenated flame-retardant PBT material is improved, and the problem that the halogenated flame-retardant PBT material cannot be applied to the field with higher requirements on electrical properties because the CTI value is low is solved. The flame retardant grade of the halogen flame retardant PBT material provided by the invention can reach V-0, and the CTI value is 300V-375V.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
< preparation of examples and comparative examples >
The raw materials used in the examples and comparative examples of the present invention are derived from self-made or commercially available sources, but are not limited to these materials:
PBT: designation GX112, purchased from instrumented chemical fibers;
glass fiber: chopped fibers 3.0mm in length and made of ECS11-3.0-534A, purchased from China boulder;
brominated polystyrene: trade designation Saytex 621, available from yabao, usa;
brominated epoxy flame retardants: trade designation F-2100, from Israel dead sea;
antimony white: trade designation S-12N, available from Guangzhou Sipun antimony;
zinc borate A: particle size 2-4 μm, trade designation FIREBREKE 500, available from Rio Tinto, USA;
the zinc borate B has the grain diameter of 5-8 mu m and the mark HT-207, and is purchased from Taxin fine chemical engineering;
glass bead A: melting point is 330 ℃, particle size is 5-15 μm, and the mark is FD46, purchased from micro-nano of Anhui province;
and (3) glass bead B: melting point 400 deg.C, particle size 10-25 μm, and trade mark D240 from Anhui micro-nano;
and (3) glass beads C: melting point 600 deg.C, particle size 15-20 μm, designation 050-20-215, available from Sofitie Deg;
and (3) glass beads D: melting point 380 deg.C, particle size 30-40 μm, brand HS38, available from Zhengzhou Shenglaite;
antioxidant: commercially available, the same commercial product was used in parallel experiments;
lubricant: commercially available, the same commercial product was used in parallel experiments.
The preparation methods of the examples of the present invention and the comparative examples are as follows:
s1: weighing the components according to the proportion, premixing the components except the glass fiber, and then adding the components into an extruder;
s2: and (3) feeding glass fibers into the extruder from the side, and performing melt extrusion and granulation to obtain the halogen flame-retardant PBT material.
In the present specification, "part(s)" means "part(s) by weight" unless otherwise specified.
< methods for Performance test >
The performance test method of each example and comparative example of the present invention is as follows:
the flame retardant property is as follows: UL94,1.6mm;
CTI performance: IEC 60112-2020. Conventionally, the CTI value is 225-250V, and the CTI effect can be improved when the CTI value exceeds the range.
TABLE 1 EXAMPLES 1-6 formulations
| Components | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 |
| PBT (parts) | 50 | 50 | 36 | 78 | 50 | 50 |
| Glass fiber (share) | 20 | 20 | 30 | 10 | 20 | 20 |
| Brominated polystyrene (parts) | 10 | 10 | 15 | 10 | 10 | |
| Brominated epoxy flame retardant (part) | 5 | |||||
| Antimony white (share) | 3 | 3 | 5 | 1 | 3 | 3 |
| Zinc borate A (parts) | 2 | 2 | 1 | 3 | 2 | 2 |
| Glass bead A (share) | 7 | 5 | 10 | 6 | 9 | |
| Glass bead B (share) | 7 | |||||
| Antioxidant (share) | 0.5 | 0.5 | 1 | 0 | 0.5 | 0.5 |
| Lubricant (parts) | 0.5 | 0.5 | 0 | 1 | 0.5 | 0.5 |
TABLE 2 EXAMPLES 7-12 formulations
TABLE 3 results of the Performance test of examples 1 to 6
| Test item | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 |
| Flame retardant rating | V-0 | V-0 | V-0 | V-0 | V-0 | V-0 |
| CTI(V) | 350 | 350 | 300 | 320 | 325 | 375 |
TABLE 4 Performance test results for examples 7-12
| Test items | Example 7 | Example 8 | Example 9 | Example 10 | Example 11 | Example 12 |
| Flame retardant rating | V-0 | V-0 | V-0 | V-0 | V-0 | V-0 |
| CTI(V) | 325 | 325 | 375 | 375 | 325 | 300 |
TABLE 5 comparative examples 1-7 formulations
TABLE 6 Performance test results of comparative examples 1 to 7
| Test items | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 | Comparative example 7 |
| Flame retardant rating | V-0 | V-0 | V-0 | V-0 | V-0 | V-0 | V-0 |
| CTI | 250V | 225V | 250V | 250V | 225V | 275V | 225V |
According to the test results of the examples 1 to 12, the flame retardant grades of the examples 1 to 12 can reach V-0, and the CTI value is within the range of 300 to 375V, so that the CTI value of the halogen flame-retardant PBT material provided by the invention is effectively improved, and the halogen flame-retardant PBT material can be suitable for electronic and electrical plastic parts with higher requirements on the CTI value.
Compared with the example 1, the comparative examples 1 and 2 have no addition of zinc borate, and the comparative example 2 has no addition of glass beads, so that the CTI of the comparative examples 1 and 2 cannot be improved.
Compared with the example 1, the comparative examples 3 and 4 have the advantage that the CTI value is not improved or is not obviously improved when the dosage of the zinc borate is beyond the range. The zinc borate has a high melting point, and plays a certain auxiliary role in fluxing in a CTI test, but cannot melt, so that the CTI value of the material cannot be increased due to an excessively large addition amount.
Compared with the example 1, the comparative examples 5 and 6 have the advantage that the dosage of the glass beads exceeds the range, so that the comparative examples 5 and 6 have poor CTI value improving effect. After reaching a certain continuous phase, the glass beads have no obvious beneficial effect on CTI if the use amount of the glass beads is increased continuously.
In comparative example 7, the melting point of the glass beads exceeded the upper limit compared to example 1, resulting in a severe drop in the CTI value of comparative example 7.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the scope of the present invention, which is intended to cover any modifications, equivalents, improvements, etc. within the spirit and scope of the present invention.
Claims (10)
1. The halogen flame-retardant PBT material is characterized by comprising the following components in parts by weight:
the flame retardant 1 is brominated polystyrene and/or brominated epoxy flame retardant;
the flame retardant 2 is antimony white or crystalline polyphosphate;
the flame retardant 3 is zinc borate;
the melting point of the glass beads is 330-400 ℃.
2. The halogenated flame retardant PBT material of claim 1 wherein said zinc borate has a particle size of 2-4 μm.
3. The halogenated flame retardant PBT material of claim 1 wherein said glass beads have a particle size of 5-25 μm.
4. The halogen flame-retardant PBT material of claim 1, wherein the weight ratio of the glass beads to the zinc borate is (2-3): 1.
5. The halogen flame retardant PBT material of claim 1, wherein said glass fiber is a chopped fiber having a length of 3-5 mm.
6. The halogenated flame-retardant PBT material of claim 1, wherein the auxiliary agent is an antioxidant and/or a lubricant.
7. The halogenated flame retardant PBT material of claim 6 wherein said antioxidant is one or more of pentaerythritol tetrakis [ β - (3, 5-di-t-butyl-4-hydroxyphenyl) propionate ], pentaerythritol tetrakis (3-laurylthiopropionate) and tris [2, 4-di-t-butylphenyl ] phosphite.
8. The halogenated flame retardant PBT material of claim 1 wherein said lubricant is one or more of ethylene bis stearamide, E wax, calcium stearate, and pentaerythritol tetrastearate.
9. A method for preparing a halogenated flame retardant PBT material according to any one of claims 1-8, characterized by comprising the steps of:
s1: weighing the components according to the proportion, premixing the components except the glass fiber, and then adding the components into an extruder;
s2: and (3) feeding glass fibers into the extruder from the side, and performing melt extrusion and granulation to obtain the halogen flame-retardant PBT material.
10. Use of a halogenated flame retardant PBT material according to any one of claims 1-8 for manufacturing plastic articles for electronics and electrical.
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| CN202211319149.7A CN115651375B (en) | 2022-10-26 | 2022-10-26 | Halogen flame-retardant PBT material, and preparation method and application thereof |
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| CN115651375B CN115651375B (en) | 2024-03-12 |
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| 杨家祥;孙菲;吴喜元;陈锐;: "空心玻璃微珠填充无卤玻璃纤维增强阻燃PA66性能研究", 塑料工业, vol. 48, no. 09, pages 127 - 129 * |
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