CN104962048A - Glass fiber reinforced flame-retardant PBT (polybutylene terephthalate) material and preparation method thereof - Google Patents
Glass fiber reinforced flame-retardant PBT (polybutylene terephthalate) material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a glass fiber reinforced flame-retardant PBT (polybutylene terephthalate) material and a preparation method thereof. The glass fiber reinforced flame-retardant PBT material comprises the following components in percentage by weight: 40-70% of PBT, 18-30% of flame-retardant master batches, 10-30% of glass fibers, 0.1-0.5% of glycidyl amine type epoxy resin, 0.1-0.5% of hydrotalcite and 0.5-1.0% of other processing aids. The reinforced flame-retardant PBT material with a high CTI value, high breakdown voltage and excellent mechanical properties is prepared by adopting a two-step method, and the method comprises the following steps: 1, preparing the flame-retardant master batches by using a double-screw extruder; and 2, preparing the reinforced flame-retardant PBT material. The PBT material can be applied to plastic products for electronic and electric appliances.
Description
Technical field
The present invention relates to polymeric material field, in particular a kind of fiberglass reinforced fire retardant PBT material.
Background technology
Strengthen flame-retardant PBT material and be widely used in electronic apparatus goods, electronic apparatus goods require that material not only has excellent mechanical property, require the electrical property possessed simultaneously, particularly this two indices of creepage trace exponential sum voltage breakdown of material requires very high, and the fire retardant that PBT flame-retardant system uses mostly is halogenated flame retardant, but they are easily separated out from material surface, corrosion mould, and a large amount of conductive ion and carbon granule settling can be produced, impel leakage of current, greatly reduce the creepage trace index (hereinafter referred to as CTI) of material, the voltage breakdown of material is not high yet simultaneously, be usually less than 225V.For obtaining the fiberglass reinforced fire retardant PBT material of high CTI value and high-breakdown-voltage, usual employing phosphorus system or nitrogen system carry out alternative halogenated flame retardant, or take composite means, the consumption reducing halogenated flame retardant reaches the object carrying high CTI value, but the flame retarding efficiency of halogenated flame retardant is optimum for PBT material, required addition is also relatively low, this provides possibility for obtaining high mechanical property, therefore, adopt halogenated flame retardant flame-retardant PBT, require that the higher CTI value of acquisition and high breakdown voltage are the technical problems being badly in need of solving simultaneously.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of fiberglass reinforced fire retardant PBT material and preparation method thereof.
A kind of fiberglass reinforced fire retardant PBT material, comprises following component (weight percent):
PBT：40％～70％
Fire-retardant master granule: 18 ~ 30%
Glass fibre: 10 ~ 30%
Glycidyl amine epoxy resin: 0.1 ~ 0.5%
Hydrotalcite: 0.1 ~ 0.5%
Other processing aids: 0.5 ~ 1.0%
Described PBT limiting viscosity 0.7 ~ 1.3;
Described fire retardant master batch comprises main flame retardant, fire retarding synergist and vector resin.Main flame retardant is at least one in TDE, brominated epoxy resin, brominated Polystyrene, brominated polycarbonate, fire retarding synergist is antimonous oxide, main flame retardant and fire retarding synergist weight ratio are 3: 1 or 2: 1 or 4: 1, vector resin is Nylon 66 or Nylon 6, in fire retardant master batch, vector resin weight percent is 30%, and in fire retardant master batch, the weight ratio of main flame retardant and fire retarding synergist sum is 70%;
Described glass fibre is the alkali-free glass fiber of filament diameter 10 ~ 15 μm;
Described glycidyl amine epoxy resin is at least one in triglycidyl group p-aminophenol, the two aminomethyl cyclohexane of four Racemic glycidols-1,3-, N, N-diglycidyl-4-Racemic glycidol oxo aniline, diisopropyl fork penylene type four glycidyl amine; The effect of glycidyl amine epoxy resin is the CTI value improving material;
Specific surface area≤the 15m2/g of described hydrotalcite, high CTI value is carried in the effect of hydrotalcite, improves the voltage breakdown of material simultaneously;
Other processing aids described comprise oxidation inhibitor and lubricant, as conventional antioxidant 1010, and irgasfos 168, Lubricate EBS;
A preparation method for fiberglass reinforced fire retardant PBT material, comprises two steps, and first step is the preparation of fire-retardant master granule, and second step is the blending extrusion of matrix material, described in specific as follows:
PA66 resin, main flame retardant, fire retarding synergist proportionally weigh by the first step, stir 3 ~ 5 minutes in high-speed stirring pot, then join twin screw extruder and extrude, extrusion temperature is 250 ~ 270 degree, vacuum tightness is 0.04 ~ 0.08MPa, through the obtained fire-retardant master granule of water-cooled pelletizing packaging.Be placed on by fire-retardant master granule in blowing-type drying machine dry rear for subsequent use, drying temperature is 120 degree, 4 ~ 6 hours time of drying.
PBT resin is placed in blowing-type drying machine dry by second step, and drying temperature is 120 degree, 4 ~ 6 hours time of drying.Weigh PBT resin in proportion, fire-retardant master granule pour in high-speed stirring pot stir 1 ~ 2 minute, pour the glycidyl amine epoxy resin of corresponding proportion into, stir 1 ~ 2 minute, finally pour hydrotalcite and other processing aids of corresponding proportion into, stir 1 ~ 2 minute, add from the main spout of twin screw and extrude, glass adds from the side spout of twin screw.Extrusion temperature is 230 ~ 250 degree, and vacuum tightness is 0.04 ~ 0.08MPa, through the obtained fiberglass reinforced fire retardant PBT material of water-cooled pelletizing packaging.
Embodiment
The formula of comparative example 1 ~ 5 is as following table 1:
Table 1: contrast 1 ~ 5 formula
The formula of embodiment 1 ~ 5 is as following table 2:
Table 2: embodiment 1 ~ 5 is filled a prescription
TDE in the fire-retardant master granule of embodiment 1: antimonous oxide: nylon66 fiber ratio is 9: 3: 5; Brominated epoxy resin in the fire-retardant master granule of embodiment 2: antimonous oxide: nylon66 fiber ratio is 9: 3: 5, glycidyl amine epoxy resin is triglycidyl group p-aminophenol;
Brominated Polystyrene in the fire-retardant master granule of embodiment 3: antimonous oxide: nylon66 fiber ratio is 9: 3: 5, glycidyl amine epoxy resin is the two aminomethyl cyclohexane of four Racemic glycidols-1,3-;
Brominated epoxy resin in the fire-retardant master granule of embodiment 4: antimonous oxide: nylon66 fiber ratio is 9: 3: 5, glycidyl amine epoxy resin is N, N-diglycidyl-4-Racemic glycidol oxo aniline epoxy resin; Brominated polycarbonate in the fire-retardant master granule of embodiment 5: antimonous oxide: nylon66 fiber ratio is 9: 3: 5, glycidyl amine epoxy resin is diisopropyl fork penylene type four glycidyl amine;
Comparative example and embodiment detected result are as following table 3:
Table 3: comparative example 1 ~ 5 and embodiment 1 ~ 5 detect data
Can find from the result detected: fire-retardant master granule, glycidyl amine epoxy resin and hydrotalcite can carry high CTI value, especially hydrotalcite, not only can carry high CTI value, also improve material breakdown voltage.
The conclusion that other embodiments and corresponding comparative example draw is all with above-mentioned similar.PBT viscosity 0.7 ~ 1.2, between glass fiber content 10 ~ 30%, in fire-retardant master granule, main flame retardant is several composite or vector resin is nylon 6, all shows the rule that table 3 draws.
Claims (8)
1. a fiberglass reinforced fire retardant PBT material, comprises following component (weight percent):
PBT：40％～70％
Fire-retardant master granule: 18 ~ 30%
Glass fibre: 10 ~ 30%
Glycidyl amine epoxy resin: 0.1 ~ 0.5%
Hydrotalcite: 0.1 ~ 0.5%
Other processing aids: 0.5 ~ 1.0%.
2. PBT limiting viscosity 0.7 ~ 1.3 according to claim 1.
3. fire retardant master batch comprises main flame retardant, fire retarding synergist and vector resin according to claim 1.Main flame retardant is at least one in TDE, brominated epoxy resin, brominated Polystyrene, brominated polycarbonate, fire retarding synergist is antimonous oxide, main flame retardant and fire retarding synergist weight ratio are 3: 1 or 2: 1 or 4: 1, vector resin is Nylon 66 or Nylon 6, in fire retardant master batch, vector resin weight percent is 30%, and in fire retardant master batch, the weight ratio of main flame retardant and fire retarding synergist sum is 70%.
4. glass fibre is the alkali-free glass fiber of filament diameter 10 ~ 15 μm according to claim 1.
5. glycidyl amine epoxy resin is triglycidyl group p-aminophenol, four Racemic glycidols-1 according to claim 1, at least one in the two aminomethyl cyclohexane of 3-, N, N-diglycidyl-4-Racemic glycidol oxo aniline, diisopropyl fork penylene type four glycidyl amine.
6. specific surface area≤the 15m2/g of hydrotalcite according to claim 1.
7. other processing aids comprise oxidation inhibitor and lubricant according to claim 1.
8. the preparation method of a fiberglass reinforced fire retardant PBT material, comprise two steps, first step is the preparation of fire-retardant master granule, second step is the blending extrusion of matrix material, and PA66 resin, main flame retardant, fire retarding synergist proportionally weigh by the first step, stirs 3 ~ 5 minutes in high-speed stirring pot, then join twin screw extruder to extrude, extrusion temperature is 250 ~ 270 degree, and vacuum tightness is 0.04 ~ 0.08MPa, through the obtained fire-retardant master granule of water-cooled pelletizing packaging.Be placed on by fire-retardant master granule in blowing-type drying machine dry rear for subsequent use, drying temperature is 120 degree, 4 ~ 6 hours time of drying.PBT resin is placed in blowing-type drying machine dry by second step, and drying temperature is 120 degree, 4 ~ 6 hours time of drying.Weigh PBT resin in proportion, fire-retardant master granule pour in high-speed stirring pot stir 1 ~ 2 minute, pour the glycidyl amine epoxy resin of corresponding proportion into, stir 1 ~ 2 minute, finally pour hydrotalcite and other processing aids of corresponding proportion into, stir 1 ~ 2 minute, add from the main spout of twin screw and extrude, glass adds from the side spout of twin screw.Extrusion temperature is 230 ~ 250 degree, and vacuum tightness is 0.04 ~ 0.08MPa, through the obtained fiberglass reinforced fire retardant PBT material of water-cooled pelletizing packaging.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106700435A (en) * | 2015-11-15 | 2017-05-24 | 合肥杰事杰新材料股份有限公司 | PBT (Polybutylene Terephthalate) enhanced material capable of being used as lamp pole of street lamp and preparation method |
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| EP0990013A1 (en) * | 1998-03-13 | 2000-04-05 | Elf Atochem S.A. | A method of producing modified polyester moulded articles, and said moulded articles |
| CN101497738A (en) * | 2008-01-31 | 2009-08-05 | 金发科技股份有限公司 | Halogen-free flame-retardant PBT and preparation thereof |
| CN102241874A (en) * | 2010-09-20 | 2011-11-16 | 深圳市科聚新材料有限公司 | Flame-retardant masterbatch modified polybutylene terephthalate material and preparation method thereof |
| CN103525024A (en) * | 2012-07-02 | 2014-01-22 | 青岛欣展塑胶有限公司 | Glass fiber reinforced halogen-free flame-retardant PBT (polybutylene terephthalate) and preparation method thereof |
| CN103709614A (en) * | 2012-09-29 | 2014-04-09 | 青岛欣展塑胶有限公司 | PBT flame-retardant master batch |
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2015
- 2015-07-12 CN CN201510422376.6A patent/CN104962048B8/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0990013A1 (en) * | 1998-03-13 | 2000-04-05 | Elf Atochem S.A. | A method of producing modified polyester moulded articles, and said moulded articles |
| CN101497738A (en) * | 2008-01-31 | 2009-08-05 | 金发科技股份有限公司 | Halogen-free flame-retardant PBT and preparation thereof |
| CN102241874A (en) * | 2010-09-20 | 2011-11-16 | 深圳市科聚新材料有限公司 | Flame-retardant masterbatch modified polybutylene terephthalate material and preparation method thereof |
| CN103525024A (en) * | 2012-07-02 | 2014-01-22 | 青岛欣展塑胶有限公司 | Glass fiber reinforced halogen-free flame-retardant PBT (polybutylene terephthalate) and preparation method thereof |
| CN103709614A (en) * | 2012-09-29 | 2014-04-09 | 青岛欣展塑胶有限公司 | PBT flame-retardant master batch |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106700435A (en) * | 2015-11-15 | 2017-05-24 | 合肥杰事杰新材料股份有限公司 | PBT (Polybutylene Terephthalate) enhanced material capable of being used as lamp pole of street lamp and preparation method |
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| CN104962048B (en) | 2017-02-01 |
| CN104962048B8 (en) | 2017-04-05 |
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Effective date of registration: 20170117 Address after: 325011 Yueqing Road, Longwan District, Wenzhou champion Street, No. 21, No. Patentee after: WENZHOU YINGCHUANG NEW MATERIAL TECHNOLOGY Co.,Ltd. Address before: 325011 Yueqing Road, Longwan District, Wenzhou champion Street, No. 21, No. Patentee before: Zhu Xuemei |
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Correction item: Patentee Correct: Wenzhou win innovation Material Technology Co., Ltd. False: Zhu Xuemei Number: 05 Volume: 33 |
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Effective date of registration: 20180719 Address after: 516131 Tian Liao Industrial Park, Huzhen Town, Boluo County, Huizhou, Guangdong Patentee after: Huizhou Boluo Huasheng flame retardant material Co.,Ltd. Address before: 325011 No. 21 Yueqing Road, Zhuang Yuan Street, Longwan District, Wenzhou, Zhejiang. Patentee before: WENZHOU YINGCHUANG NEW MATERIAL TECHNOLOGY Co.,Ltd. |
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