CN111808405B - Polyester material with high glowing filament ignition temperature resistance and preparation method thereof - Google Patents
Polyester material with high glowing filament ignition temperature resistance and preparation method thereof Download PDFInfo
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- CN111808405B CN111808405B CN202010585622.0A CN202010585622A CN111808405B CN 111808405 B CN111808405 B CN 111808405B CN 202010585622 A CN202010585622 A CN 202010585622A CN 111808405 B CN111808405 B CN 111808405B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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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
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention discloses a polyester material with high glowing filament ignition temperature resistance, which comprises the following components in parts by weight: 25-40 parts of polyester resin, 25-40 parts of alkali-free glass fiber, 18-30 parts of brominated flame retardant, 3-8 parts of nitrogen-containing smoke suppressant and 2-10 parts of phosphate flame retardant synergist; the alkali-free glass fiber is treated by a coupling agent. The halogen flame retardant and the nitrogen-phosphorus compound synergist are effectively combined, and the glass fiber reinforced flame-retardant polyester material is obtained without containing antimony compounds, has excellent mechanical properties, various colors and wall thickness of 1.0-2.0mm, and has GWIT of 875 ℃ or more. Meanwhile, the invention also discloses a preparation method of the polyester material.
Description
Technical Field
The invention relates to the field of modification of high polymer materials, in particular to a polyester material with high glowing filament ignition temperature resistance and a preparation method thereof.
Background
Polybutylene terephthalate (PBT) and polyethylene terephthalate (PET) are two thermoplastic polyester materials commonly used as functional structural members in the electronic and electrical industry, and have excellent electrical property, mechanical strength and processability due to crystallization and linear saturation, and the modified polyester is widely applied to the fields of electronics and electricity, household appliances, automobiles and the like. The safety requirements of materials are more and more strict, besides the requirement of meeting the flame retardant grade of UL94, the requirement of Glow Wire Ignition Temperature (GWIT) in IEC60695 standard is also enforced, the GWIT of plastic parts used by electric appliances which are unsupervised for a long time is provided to meet the requirement of being more than or equal to 775 ℃, and the GWIT requirements of specific parts such as connectors, relay housings, breaker housings and the like reach 850 ℃ or more along with the realization of more and more functions of electronic appliances.
In the actual GWIT test process, the flame-retardant glass fiber reinforced polyester material can obtain higher GWIT at both a thinner thickness level (e.g. 0.75mm or less) and a higher thickness level (e.g. 3.0mm or more), but has lower GWIT at an intermediate thickness (e.g. 1.0-2.0 mm), such as: the GWIT of the same type of flame retardant material is 700 ℃ or 725 ℃ at a thickness of 1.5mm, but can reach 750 ℃ or 775 ℃ at a thickness of 3.0mm or 0.75 mm.
In the prior art, most of halogen flame-retardant polyester materials with high glowing filament ignition temperature use antimony compound for synergism, and antimony compounds, particularly antimony white, are listed as 2B class carcinogens in 2017 by the world health organization international cancer research institution, and skin may have anaphylactic reaction, generate inflammation and influence production when the antimony compounds are in direct contact; and GWIT of the materials rarely reports that the thickness is more than 850 ℃ at 1.0-2.0mm, and even if the thickness is 875 ℃ at 2.0mm, the mechanical property is low, and the strength is difficult to meet the functional test requirement of the plastic product in the electronic and electrical industry as a connecting or supporting function.
Disclosure of Invention
Based on this, the object of the present invention is to overcome the above-mentioned disadvantages of the prior art and to provide a polyester material having a high glow-wire ignition temperature resistance. The halogen flame retardant and the nitrogen-phosphorus compound synergist are effectively combined, and the glass fiber reinforced flame-retardant polyester material is obtained without containing antimony compounds, has excellent mechanical properties, multiple colors and GWIT (glow wire ignition temperature) of 875 ℃ or more with the wall thickness of 1.0-2.0 mm.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a polyester material with high glowing filament ignition temperature resistance comprises the following components in parts by weight: 25-40 parts of polyester resin, 25-40 parts of alkali-free glass fiber, 18-30 parts of brominated flame retardant, 3-8 parts of nitrogen-containing smoke suppressant and 2-10 parts of phosphate flame retardant synergist; the alkali-free glass fiber is treated by a coupling agent.
The brominated flame retardant, the nitrogen-containing smoke suppressant and the phosphorus-containing flame retardant synergist can play a good synergistic effect in the content range, so that the polyester material has a good flame retardant effect, high mechanical strength and high glow wire ignition temperature resistance.
Coating the precursor of the glass fiber with an impregnating compound containing a silane coupling agent in the drawing process, and then drying and dicing to obtain alkali-free glass fiber treated by the coupling agent; the glass fiber treated by the coupling agent is tightly combined with the polyester resin interface, and the mechanical strength of the composite material is greatly improved.
Preferably, the diameter of the alkali-free glass fiber is 10-13 μm.
Preferably, the polyester resin is at least one of polybutylene terephthalate and polyethylene terephthalate.
Preferably, the brominated flame retardant is brominated triazine. The bromine content of the brominated triazine is higher than that of other common bromine flame retardants, and the brominated triazine contains nitrogen, and the flame retardant mechanism is of a heat absorption decomposition removal type, so that the flame retardant efficiency is higher.
Preferably, the nitrogen-containing smoke suppressant is at least one of melamine cyanurate and melamine polyphosphate. The melamine nitrogen-containing smoke suppressant and the phosphorus flame retardant have good coordinated flame retardant effect, and have the characteristics of small using amount, good flame retardant effect, small smoke generation amount and the like.
Preferably, the phosphate flame-retardant synergist is diphenyl phosphate.
Preferably, the polyester material with high glow wire ignition temperature resistance further comprises the following components in parts by weight: 0-8 parts of toughening agent and 0-5 parts of processing aid.
More preferably, the toughening agent is at least one of ethylene-acrylate-glycidyl methacrylate terpolymer, ethylene-methyl acrylate binary copolymer and ethylene-butyl acrylate binary copolymer; the processing aid comprises a composite antioxidant system, a lubricant and a pigment, wherein the composite antioxidant system is formed by compounding a hindered phenol antioxidant, a phosphite antioxidant and an organic sulfur antioxidant, and the lubricant is at least one of an aliphatic carboxylic ester lubricant and a polyolefin lubricant.
Meanwhile, the invention also provides a preparation method of the polyester material with high glowing filament ignition temperature resistance, which comprises the following steps:
the preparation method comprises the steps of pre-drying polyester resin at 120-140 ℃ for 4-6 hours, mixing the dried polyester resin with other components except for alkali-free glass fibers, uniformly mixing, feeding the mixed material into a double-screw extruder, adding the alkali-free glass fibers into a side feed port of the double-screw extruder, extruding, bracing, cooling, granulating, drying and packaging to obtain the polyester material with high glowing filament ignition temperature resistance.
Preferably, the feeding material of the double-screw extruder is 450-800 kg/hour; the temperature of each section of the screw of the twin-screw extruder from the charging port to the head is respectively 220-.
Compared with the prior art, the invention has the beneficial effects that:
(1) the antimony-free brominated flame-retardant reinforced polyester composite material with high glowing filament ignition temperature resistance, which is obtained by the invention, has the flame retardance of UL-94 standard V-0 grade, and the GWIT in the thickness of 1.0-2.0mm can reach 875 ℃ or above;
(2) the antimony-free brominated flame-retardant reinforced polyester composite material with high glowing filament ignition temperature resistance, which is obtained by the invention, has the tensile strength of more than 100MPa and the notch impact strength of 7.5kJ/m2The above (ISO standard);
(3) the antimony-free brominated flame-retardant reinforced polyester composite material with high glowing filament ignition temperature resistance, which is obtained by the invention, does not contain antimony and compounds thereof, and avoids the problems of heavy metal exceeding and the like possibly caused by antimony compounds and the risks of occupational diseases and the like possibly caused by using antimony compounds in the aspect of environmental substance management and control.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
The preparation method of the polyester material in the examples and the comparative examples comprises the following steps:
(1) drying the polyester resin at 130 ℃ for 4-6 hours, and controlling the water content to be less than 0.03%;
(2) preparing various raw materials according to a mixture ratio;
(3) uniformly mixing the dried polyester resin and other components except the alkali-free glass fiber in a high-speed stirring mixer in proportion or independently feeding the polyester resin and the components into a premixer through a metering feeder to obtain a premix;
(4) feeding the mixed material into a double-screw extruder, adjusting the feeding amount to be 450-800 kg/h, adding alkali-free glass fiber into a side feeding port in the double-screw extruder, wherein the temperatures of screws in all sections of the double-screw extruder from a feeding port to a machine head are respectively 230 ℃, 240 ℃, 250 ℃, 260 ℃, 250 ℃, 240 ℃, 230 ℃ and 230 ℃, and the screw rotating speed is 400rpm, and fully melting and plasticizing, kneading and mixing, extruding through the machine head, drawing strips, cooling, granulating, drying and finally packaging are carried out under the conveying and shearing actions of the double-screw extruder.
The specific performance test method of the obtained product is as follows:
(1) drying the product obtained by extrusion and granulation at the temperature of 120-130 ℃ for 3-4 hours;
(2) preparing a test sample wafer according to corresponding standard injection molding;
(3) the tensile strength is tested according to ISO 527 standard, the notched Izod impact strength is tested according to ISO 180 standard, the flame retardant property is tested according to UL94 standard, and the GWIT is tested according to IEC60695 standard.
The main representative materials used in the examples and comparative examples are as follows:
a polyester resin
A1: PBT resin, Taiwan Changchun 1100-;
a2: PET resin, inscription fiber FG 600;
b bromine series flame retardant
B1: brominated epoxy F-2100, Israel ICL;
b2: bromo-triazine FR-245, israel ICL;
b3: decabromodiphenylethane 8010, yabao;
c, antimony white: selecting S-05N, Chenzhou antimony industry;
d nitrogen-containing smoke suppressant
D1: MCA (melamine cyanurate), sichuan fine chemical industry;
d2: MPP (melamine polyphosphate), chemical engineering in the light of life and defense;
d3: APP (ammonium polyphosphate), siersi chemical;
e phosphate ester synergist:
e1: diphenyl phosphate; WSFR-PX220 (hydroquinone bis (diphenyl phosphate)), prosperous;
e2: phenyl phosphate; WSFR-RDP (resorcinol (diphenyl phosphate)), panacea;
f flexibilizer
F1: ethylene-acrylate-glycidyl methacrylate terpolymer, designation PTW (dupont);
f2: ethylene-methyl acrylate dipolymer, designation ELVALOY AC 1125 (dupont);
f3: ethylene-butyl acrylate copolymer, trade name ELVALOY AC 34035 (dupont);
g alkali-free glass fiber
G1: ECS13-4.5-534A (glass fiber diameter 13 μm, coupling agent treatment, boulder group);
g2: ECS10-4.5-T436H (glass fiber diameter 10 μm, coupling agent treatment, Mount Taishan glass fiber Co., Ltd.);
g3: EMG200 (glass fiber diameter 13 μm, no coupling agent treatment, Taishan fiberglass Co., Ltd.);
h: processing aids, examples 6 of which respectively select antioxidants (hindered phenol antioxidant 1010, phosphite antioxidant 168, organic sulfur antioxidant 412S, linaron), pigments (zinc sulfide, Hensman; Black masterbatch PE2718, cabot), lubricants (polyolefin lubricant PED 521, Kelaien; aliphatic carboxylic acid ester lubricant PETS, hair base), ester exchange inhibitors (sodium dihydrogen phosphate, Wuhan Huachuang), and the weight ratio of the components in the processing aids is 2:1:1:10:10:5:5: 3; the processing aids of the other examples and comparative examples were the same as those of example 6 except that they did not contain the transesterification inhibitor.
The present application sets forth examples 1-10 and comparative examples 1-4, and the ingredients, content selections, and performance data for the specific examples 1-10 and comparative examples 1-4 are shown in table 1, in parts by weight:
TABLE 1 ingredients, selection of contents, and Performance data for examples 1-10 and comparative examples 1-4
As can be seen from table 2, compared to example 1, comparative example 1 contains only a brominated flame retardant and antimony white, comparative example 2 contains only a brominated flame retardant and a nitrogen-containing smoke suppressant, and comparative example 3 contains only a brominated flame retardant and a flame retardant synergist; the high glow wire ignition temperature resistance of the comparative examples 1-3 is significantly lower than that of the example 1. Comparing comparative example 4 with example 1, it can be seen that the alkali-free glass fiber in example 1 is treated with the coupling agent, and the alkali-free glass fiber in comparative example 4 is not treated with the coupling agent; as can be seen from the comparison of the performance data, the high glow wire ignition temperature resistance in comparative example 4 is lower than that in example 1, and the tensile strength and the notched Izod impact strength are also significantly inferior to those in example 1.
Examples 7 and 8 are the same as example 1 except that the brominated flame retardant is selected differently; comparison of the performance data shows that the high glow wire ignition temperature resistance in examples 7 and 8 is lower than that in example 1, and the tensile strength and izod notched impact strength are slightly inferior to those in example 1. Example 9 the procedure was as in example 1 except that the nitrogen-containing smoke suppressant was selected differently; from the comparison of the performance data, it is found that the glow wire ignition temperature resistance in example 9 is lower than that in example 1, and the tensile strength and the izod notched impact strength are slightly inferior to those in example 1. The selection of the phosphate ester synergist in example 10 is different, and the rest is the same as that in example 1; from the comparison of the performance data, it is seen that the glow wire ignition temperature resistance in example 10 is lower than that in example 1, and the tensile strength and the izod notched impact strength are also inferior to those in example 1.
In conclusion, the data show that the nitrogenous brominated flame retardant, the nitrogenous smoke suppressant and the phosphorous flame retardant synergist are assisted by the alkali-free glass fiber treated by the coupling agent through the combined action of a proper proportion, so that the polyester composite material which has high GWIT and high mechanical strength and meets the strength requirement of electronic and electrical structural parts can be obtained.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (6)
1. The polyester material with high glowing filament ignition temperature resistance is characterized by comprising the following components in parts by weight: 25-40 parts of polyester resin, 25-40 parts of alkali-free glass fiber, 18-30 parts of brominated flame retardant, 3-8 parts of nitrogen-containing smoke suppressant and 2-10 parts of phosphate flame retardant synergist; the polyester material does not contain other flame-retardant auxiliaries; the alkali-free glass fiber is treated by a coupling agent;
wherein the brominated flame retardant is brominated triazine; the nitrogen-containing smoke suppressant is at least one of melamine cyanurate and melamine polyphosphate; the phosphate flame-retardant synergist is diphenyl phosphate.
2. The high glow wire ignition temperature resistant polyester material of claim 1, wherein said polyester resin is at least one of polybutylene terephthalate and polyethylene terephthalate.
3. The polyester material with high glowing filament ignition temperature resistance of claim 1 or 2, further comprising the following components in parts by weight: 0-8 parts of toughening agent and 0-5 parts of processing aid.
4. The high glow wire ignition temperature resistant polyester material of claim 3, wherein said toughening agent is at least one of ethylene-acrylate-glycidyl methacrylate terpolymer, ethylene-methyl acrylate copolymer, ethylene-butyl acrylate copolymer; the processing aid comprises a composite antioxidant system, a lubricant and a pigment, wherein the composite antioxidant system is formed by compounding a hindered phenol antioxidant, a phosphite antioxidant and an organic sulfur antioxidant, and the lubricant is at least one of an aliphatic carboxylic ester lubricant and a polyolefin lubricant.
5. A method for preparing the polyester material with high glowing filament ignition temperature resistance as claimed in any one of claims 1 to 4, wherein the method comprises the following steps:
the preparation method comprises the steps of pre-drying polyester resin at 120-140 ℃ for 4-6 hours, mixing the dried polyester resin with other components except for alkali-free glass fibers, uniformly mixing, feeding the mixed material into a double-screw extruder, adding the alkali-free glass fibers into a side feed port of the double-screw extruder, extruding, bracing, cooling, granulating, drying and packaging to obtain the polyester material with high glowing filament ignition temperature resistance.
6. The method for preparing the polyester material with high glowing filament ignition temperature resistance as claimed in claim 5, wherein the feeding of the twin-screw extruder is 450-800 kg/h; the temperature of each section of the screw of the twin-screw extruder from the charging port to the head is respectively 220-.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010585622.0A CN111808405B (en) | 2020-06-23 | 2020-06-23 | Polyester material with high glowing filament ignition temperature resistance and preparation method thereof |
| PCT/CN2020/136319 WO2021258674A1 (en) | 2020-06-23 | 2020-12-15 | Polyester material having high glow-wire ignition temperature resistance and preparation method therefor |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010585622.0A CN111808405B (en) | 2020-06-23 | 2020-06-23 | Polyester material with high glowing filament ignition temperature resistance and preparation method thereof |
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| CN111808405A CN111808405A (en) | 2020-10-23 |
| CN111808405B true CN111808405B (en) | 2022-05-10 |
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| CN111808405B (en) * | 2020-06-23 | 2022-05-10 | 金发科技股份有限公司 | Polyester material with high glowing filament ignition temperature resistance and preparation method thereof |
| CN114605787A (en) * | 2022-02-24 | 2022-06-10 | 金发科技股份有限公司 | PBT/PET composite material, and preparation method and application thereof |
| CN114561090B (en) * | 2022-03-07 | 2023-11-21 | 金发科技股份有限公司 | Brominated flame-retardant reinforced polyethylene terephthalate composition easy to mold out and high in glowing filament performance, and preparation method and application thereof |
| CN114736453B (en) * | 2022-03-14 | 2023-09-26 | 金发科技股份有限公司 | Low-halogen flame-retardant PP material and preparation method and application thereof |
| CN114806128B (en) * | 2022-05-10 | 2024-02-09 | 常州杰铭新材料科技有限公司 | Low-temperature-resistant stress-cracking-resistant flame-retardant PC material and preparation method thereof |
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| JP3481453B2 (en) * | 1998-03-25 | 2003-12-22 | 帝人株式会社 | Flame-retardant polyester resin composition, molded article for home appliances comprising the same, and method for producing the same |
| CN102775747A (en) * | 2012-07-30 | 2012-11-14 | 南通星辰合成材料有限公司 | Antimony-free reinforced flame-retardant polybutylece terephthalate (PBT) environmental-friendly material and preparation method thereof |
| CN102952379A (en) * | 2012-12-04 | 2013-03-06 | 上海日之升新技术发展有限公司 | Environment-friendly flame retardant glass fiber reinforced polybutylece terephthalate (PBT) material with high comparative tracking index (CTI) value and high glow wire ignition temperature (GWIT) value and preparation method thereof |
| JP6045909B2 (en) * | 2012-12-26 | 2016-12-14 | 三菱エンジニアリングプラスチックス株式会社 | Polyester resin composition for circuit breakers |
| CN106633682A (en) * | 2015-10-30 | 2017-05-10 | 杜邦公司 | A flame retardant composition including fiber-reinforced poly(ethylene terephthalate) |
| 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 |
| CN109749375A (en) * | 2019-01-22 | 2019-05-14 | 广东顺德同程新材料科技有限公司 | A kind of fire retardant polybutylene terephthalate material and preparation method thereof |
| CN111808405B (en) * | 2020-06-23 | 2022-05-10 | 金发科技股份有限公司 | Polyester material with high glowing filament ignition temperature resistance and preparation method thereof |
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