CN112574535A - Damping halogen-free flame-retardant reinforced PBT (polybutylene terephthalate) material and preparation method thereof - Google Patents
Damping halogen-free flame-retardant reinforced PBT (polybutylene terephthalate) material and preparation method thereof Download PDFInfo
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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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
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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
- C08L2201/02—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
- C08L2201/22—Halogen free composition
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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
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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
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
Abstract
The invention relates to a damping halogen-free flame-retardant reinforced PBT (polybutylene terephthalate) material, which comprises the following components in parts by weight: 30-45 parts of PBT resin, 8-15 parts of flaky filler, 6-12 parts of damping polymer, 2-5 parts of compatilizer, 20-30 parts of glass fiber, 10-20 parts of phosphorus flame retardant, 5-10 parts of nitrogen-containing flame retardant synergist and 0.1-2 parts of processing aid. The invention discloses and reports that polyester containing a glass fiber halogen-free flame retardant system in engineering plastics has a damping effect for the first time; the inventionThe obtained damping halogen-free flame-retardant reinforced polyester material has the tensile strength of more than 70MPa and the notch impact strength of 6.2kJ/m2Above (ISO standard).
Description
Technical Field
The invention relates to a damping halogen-free flame-retardant reinforced PBT (polybutylene terephthalate) material and a preparation method thereof, in particular to a damping halogen-free flame-retardant reinforced PBT material used in the fields of cooling fan frames, motor shells, sound box shells and the like in the electronic and electrical industry and a preparation method thereof, belonging to the technical field of engineering plastics.
Background
Polybutylene terephthalate (PBT) has 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 and the like. The flame-retardant glass fiber reinforced PBT material is commonly used as a cooling fan frame, a motor shell and other parts, and is accepted in the industry in a large quantity, but the requirements on the material are more rigorous along with the improvement of functional requirements, such as higher and higher rotating speed, smaller and smaller flame-retardant thickness and the like. The traditional material needs to be endowed with new functions, such as shock absorption and damping, and the like, so that the energy produced by the workpiece in the high-speed operation process can be effectively absorbed or alleviated, and the shock absorption is carried out to reduce the noise and improve the stability of the function of the workpiece.
A plurality of methods for realizing shock absorption and damping by using the reported polymers are disclosed, and CN01814142 and CN02830074 disclose that a thermoplastic elastomer of a multi-block copolymer obtained by a cross-linkable polymer through a dynamic cross-linking reaction has excellent shock absorption effect and is used as a sole material of footwear; CN03809473 is molded to make polypropylene into a foaming material with a buffering and damping effect; CN200980107747 discloses flame retardant composite foam prepared by mixing flame retardant, foaming agent and the like into thermoplastic elastomer, wherein the flame retardant composite foam is used for insulation, shock absorption and protection and is used in the form of plates, plane materials, pipes, sectional materials, gaskets and the like singly or compositely; CN200710100042 obtains polyurethane-vinyl polymer IPN (blending, copolymerization and interpenetrating polymer network) bi-component damping material by mixing and copolymerizing isocyanate and vinyl-containing monomer; CN201110025089 discloses that a high damping composition obtained by adding calcium carbonate or carbon black to epoxidized natural rubber and mixing calcium stearate is used for moderating or absorbing vibration energy transmission, i.e., for vibration isolation, vibration reduction, vibration isolation, etc., in order to use a high damping member containing rubber or the like as a base resin. CN201511004497 is used as an automotive interior material, and a crosslinked polymer containing a polystyrene hard segment and an ethylene branched polydiene soft segment is added into ABS resin to synergistically play a role in sound insulation and shock absorption with hollow glass beads; CN202010068682 discloses a method for preparing packaging material, building material, shock-absorbing material, automobile buffer, sports protection product, and protection member of body-building equipment by using polymer foam particles with skin structure and polymer composite material containing at least one dynamic covalent bond on polymer chain, which are prepared by direct foaming or 3D printing.
The above patents generally adopt polymer elastomer as matrix, or add elastomer into general plastic, and through foaming method; or compounding a polymer containing covalent bonds to realize the damping effect, and the flame-retardant damping engineering material added with glass fiber and the realization method thereof are not reported in the air.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides the damping halogen-free flame-retardant reinforced PBT material and the preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that: the damping and damping halogen-free flame-retardant reinforced PBT material comprises the following components in parts by weight: 30-45 parts of PBT resin, 8-15 parts of flaky filler, 6-12 parts of damping polymer, 2-5 parts of compatilizer, 20-30 parts of glass fiber, 10-20 parts of phosphorus flame retardant, 5-10 parts of nitrogen-containing flame retardant synergist and 0.1-2 parts of processing aid.
According to the invention, the PBT material is added with the flaky filler, the elastomer with multi-block copolymerization is used as a damping polymer, the acrylate compatilizer, the phosphorus-containing halogen-free flame retardant and the nitrogen-containing flame retardant synergist are compounded for flame retardance, and the PBT material with high mechanical property and damping effect is obtained through glass fiber reinforcement.
In the halogen-free flame-retardant system, the damping polymer and the flaky filler are compounded for use, and the damping polymer and the flaky filler can not be used in amounts of 6 parts and 8 parts respectively, so that the damping effect can be achieved.
As a preferable embodiment of the PBT material, the PBT resin is used in 32-40 parts, the compatilizer is used in 2-3 parts, the phosphorus flame retardant is used in 10-15 parts, the nitrogen-containing flame retardant synergist is used in 5-6 parts, the processing aid is used in 1-1.5 parts, the damping polymer is used in 7-10 parts, and the flaky filler is used in 9-12 parts.
In a preferred embodiment of the PBT material, the intrinsic viscosity of the PBT resin is 0.7-1.0 dl/g, and the flaky filler is mica powder with 40-400 meshes.
As a preferred embodiment of the PBT material, the damping polymer is a hydrogenated styrene-butadiene block copolymer, the purity of the hydrogenated styrene-butadiene block copolymer is more than 98%, the cyclohexane content in impurities is less than 0.5%, and the Shore hardness is 65-90; the compatilizer is acrylate compatilizer, and the acrylate compatilizer is at least one of ethylene-acrylate and ethylene-acrylate-glycidyl methacrylate terpolymer.
As a preferred embodiment of the PBT material, the glass fiber is alkali-free glass fiber, the diameter of the glass fiber is 10-13 μm, and the length of the glass fiber is 3-5 mm; the phosphorus flame retardant is aluminum diethylphosphinate. If a damping material with higher strength performance is to be obtained, high-modulus glass fiber can be adopted.
As a preferable embodiment of the PBT material, the nitrogen-containing flame-retardant synergist is melamine cyanurate or melamine polyphosphate, and the processing aid is at least one of a lubricant, an ester exchange inhibitor, an antioxidant and a pigment.
As a preferable embodiment of the PBT material, the lubricant is at least one of an aliphatic carboxylic acid ester wax lubricant and a polyolefin wax lubricant; the antioxidant is at least one of hindered phenol antioxidant, phosphite antioxidant and organic sulfur antioxidant.
In a second aspect, the invention provides a preparation method of the PBT material, which comprises the following steps:
(1) pre-drying the PBT resin, adding the pre-dried PBT resin, the phosphorus flame retardant, the nitrogen-containing flame retardant synergist, the flaky filler, the damping polymer, the compatilizer, the glass fiber and the processing aid into a high-speed stirring mixer in proportion, and uniformly mixing or independently feeding the mixture into a premixer through a metering feeder to obtain a mixed material;
(2) and (2) feeding the mixed material obtained in the step (1) into a double-screw extruder, fully melting and plasticizing, kneading and mixing, extruding through a machine head, bracing, cooling, granulating, drying and finally packaging under the conveying and shearing action of the double-screw extruder to obtain the damping, halogen-free and flame-retardant reinforced PBT material.
As a preferred embodiment of the preparation method, in the step (1), the pre-drying temperature is 120-140 ℃, and the pre-drying time is 4-6 hours.
In the step (2), the feeding speed of the twin-screw extruder is 450 to 800 kg/h, and the temperatures of the twin-screw extruder from the feeding port to the head are 220 to 230 ℃ in the feeding section, 230 to 240 ℃ in the conveying section, 203 to 240 ℃ in the melt mixing section I, 240 to 250 ℃ in the melt mixing section II, 250 to 260 ℃ in the natural exhaust section, 240 to 250 ℃ in the mixing section I, 240 to 250 ℃ in the mixing section II, 230 to 240 ℃ in the vacuum exhaust section, 230 to 240 ℃ in the extrusion metering section and 250 to 400rpm in the screw rotating speed.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention discloses and reports that polyester containing a glass fiber halogen-free flame retardant system in engineering plastics has a damping effect for the first time;
(2) the damping halogen-free flame-retardant reinforced polyester material obtained by the invention has the tensile strength of more than 70MPa and the notch impact strength of 6.2kJ/m2The above (ISO standard);
(3) the damping halogen-free flame-retardant reinforced polyester material obtained by the invention can obtain structural functional components through molding processes such as injection molding, extrusion, mould pressing and the like, and can be widely applied to the fields of cooling fans, motor shells, sound components, automobile buffering parts and the like in the electronic and electrical industry.
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 PBT material in the embodiment and the comparative example comprises the following steps:
(1) drying the PBT resin at 130 ℃ for more than 4 hours, and controlling the water content to be less than 0.03%;
(2) preparing various raw materials according to a ratio;
(3) adding the dried PBT resin, the phosphorus flame retardant, the nitrogen-containing flame-retardant synergist, the flaky filler, the shock-absorbing polymer, the compatilizer, the glass fiber and the processing aid into a high-speed stirring mixer in proportion, and uniformly mixing or independently feeding the mixture into a premixer through a metering feeder to obtain a mixed material;
(4) feeding the mixed material into a double-screw extruder, adjusting the feeding amount to be 450-800 kg/h, feeding the mixed material 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 ℃ in a feeding section, 240 ℃ in a conveying section, 240 ℃ in a melting and mixing I section, 250 ℃ in a melting and mixing II section, 260 ℃ in a natural exhaust section, 250 ℃ in a mixing I section, 240 ℃ in a mixing II section, 230 ℃ in a vacuum exhaust section, 230 ℃ in an extrusion metering section and the rotation speed of the screws is 400rpm, fully melting and plasticizing, kneading and mixing the mixed material, extruding the mixed material through the machine head, bracing, cooling, granulating, drying and finally packaging to obtain the damping halogen-free flame-retardant reinforced PBT material.
The test methods of the examples and comparative examples of the present invention are as follows:
(1) drying a product obtained by extruding and granulating 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 527-2012 standard, the notched Izod impact strength is tested according to ISO180-2000 standard, the flame retardant property is tested according to UL 94-2013 standard, and the loss tangent is as follows: the damping performance was tested by a dynamic viscoelasticity tester at different temperatures with a sweep frequency.
The information on the raw materials used in the examples of the present invention and the comparative examples is as follows:
PBT resin, A1: taiwan Changchun 1200-211M, intrinsic viscosity of 0.8 dl/g; a2: taiwan Changchun 1100-211M, intrinsic viscosity of 1.0 dl/g;
B. glass fiber, B1: ECS11-4.5-534A (glass fiber diameter 11 μm, length 4.5mm, boulder group); b2: HMG436S-10-4.0 (glass fiber diameter 10 μm, length 4.0mm, Taishan glass fiber Co., Ltd.);
C. mica powder, selecting C1: AY-03N (Tahita mica materials Co., Ltd., 40 mesh); c2: mica powder 400 mesh (Dachao chemical Co., Ltd.);
D. phosphorus flame retardant, selected from Craine EXOLIT OP 1230;
E. nitrogen-containing flame retardant synergist: e1 is selected: MCA (sichuan fine chemical); e2: MPP (shou guang wei dong chemical industry);
F. damping polymer: SEBS, namely S.O.E.S1605, wherein the purity of the product is more than 98%, the cyclohexane content in impurities is less than 0.5%, and the Shore hardness is 65-90;
G. the compatilizer is G1: ethylene-acrylate-glycidyl methacrylate terpolymer, designation PTW (dupont); g2: ethylene-methyl acrylate dipolymer, designation ELVALOY AC1125 (dupont);
H. the processing aid is prepared from antioxidant (1010, 168, 412S, linaron), pigment (zinc sulfide, Hensman; black master PE2718, cabot), and lubricant (PED 521, Craine; PETS, hair base).
Examples 1 to 7
The components and the amounts of the PBT materials of examples 1 to 7 are shown in Table 1. The processing aids in examples 1, 6 and 7 and comparative example 1 comprise 101025 wt% of antioxidant, 16825 wt% of antioxidant and 50 wt% of lubricant PETS; in examples 2 and 3 and comparative example 2, the processing aids comprise 101020 wt% of antioxidant, 16820 wt% of antioxidant, 20 wt% of zinc sulfide and 40 wt% of lubricant PETS; in examples 4 and 5 and comparative example 3, the processing aids comprise 101020 wt% of antioxidant, 412S 20 wt% of antioxidant, 271810 wt% of black master batch PE, and 52150 wt% of lubricant PED; the performance test results of the PBT materials of the examples 1-7 are shown in Table 2.
Comparative examples 1 to 3
The components and the use amount of the PBT material of comparative examples 1 to 3 are shown in Table 1. The performance test results of the PBT materials of comparative examples 1-3 are shown in Table 2.
TABLE 1
TABLE 2
As can be seen from Table 2, the loss tangent of the PBT material with good damping effect is higher than that of the PBT material without damping effect, and the loss tangent is obviously increased along with the increase of the frequency, while the loss tangent of the PBT material without damping effect is slightly reduced along with the increase of the frequency. The PBT material prepared by the invention has the damping effect while maintaining good mechanical property. Comparative example 1 does not contain a vibration-damping polymer, and its vibration-damping is inferior to that of the present invention; comparative example 2 does not contain a plate-like filler, and its damping is inferior to that of the present invention; the comparative example 3 in which the vibration-damping polymer and the plate-like filler were used in amounts other than the ranges of the present invention was inferior in vibration-damping performance to the present invention.
Effect example 1
In order to investigate the influence of the use amounts of the damping polymer and the flaky filler on the damping effect of the PBT material, test groups 1-5 and comparison groups 1-4 are arranged. In the test groups 1-5 and the control groups 1-4, only the amounts of the damping polymer and the flaky filler are different, as shown in Table 3; the specific selected substances of all the components are the same, and the use amounts of the other components are the same. Meanwhile, the PBT materials of the test groups 1-5 and the comparison groups 1-4 are subjected to performance tests, and the test results are shown in Table 3.
TABLE 3
As can be seen from Table 3, when the amounts of the vibration-damping polymer and the flake filler are within the range of the present invention, the PBT material has a good vibration-damping effect. In the control groups 3-4, the use amounts of the damping polymer and the flaky filler are not all in the range of the invention, and the damping effect is not as good as that of the test group 1; the control group 1 did not contain a vibration-damping polymer, and the control group 2 did not contain a plate-like filler, and the vibration-damping effect was far inferior to that of the test group 1. The damping polymer and the flaky filler are compounded, so that the synergistic effect is achieved, and the damping performance can be greatly improved.
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 (10)
1. The damping and damping halogen-free flame-retardant reinforced PBT material is characterized by comprising the following components in parts by weight: 30-45 parts of PBT resin, 8-15 parts of flaky filler, 6-12 parts of damping polymer, 2-5 parts of compatilizer, 20-30 parts of glass fiber, 10-20 parts of phosphorus flame retardant, 5-10 parts of nitrogen-containing flame retardant synergist and 0.1-2 parts of processing aid.
2. The PBT material of claim 1, wherein the PBT resin is used in an amount of 32 to 40 parts, the compatibilizer is used in an amount of 2 to 3 parts, the phosphorus flame retardant is used in an amount of 10 to 15 parts, the nitrogen-containing flame retardant synergist is used in an amount of 5 to 6 parts, the processing aid is used in an amount of 1 to 1.5 parts, the vibration damping polymer is used in an amount of 7 to 10 parts, and the flake filler is used in an amount of 9 to 12 parts.
3. The PBT material according to claim 1 or 2, wherein the PBT resin has an intrinsic viscosity of 0.8 to 1.0dl/g, and the flake filler is mica powder of 40 to 400 mesh.
4. The PBT material of claim 1 or 2, wherein the vibration absorbing polymer is a hydrogenated styrene-butadiene block copolymer having a purity of greater than 98% and a Shore hardness of 65 to 90; the compatilizer is acrylate compatilizer, and the acrylate compatilizer is at least one of ethylene-acrylate and ethylene-acrylate-glycidyl methacrylate terpolymer.
5. The PBT material according to claim 1 or 2, wherein the glass fibers are alkali-free glass fibers, and have a diameter of 10 to 13 μm and a length of 3 to 5 mm; the phosphorus flame retardant is aluminum diethylphosphinate.
6. The PBT material of claim 1 or 2, wherein the nitrogen-containing flame retardant synergist is melamine cyanurate or melamine polyphosphate, and the processing aid is at least one of a lubricant, a transesterification inhibitor, an antioxidant, and a pigment.
7. The PBT material of claim 6, wherein the lubricant is at least one of an aliphatic carboxylic acid ester wax lubricant, a polyolefin-based wax lubricant; the antioxidant is at least one of hindered phenol antioxidant, phosphite antioxidant and organic sulfur antioxidant.
8. The preparation method of the PBT material according to any one of claims 1 to 7, comprising the steps of:
(1) pre-drying the PBT resin, adding the pre-dried PBT resin, the phosphorus flame retardant, the nitrogen-containing flame retardant synergist, the flaky filler, the damping polymer, the compatilizer, the glass fiber and the processing aid into a high-speed stirring mixer in proportion, and uniformly mixing or independently feeding the mixture into a premixer through a metering feeder to obtain a mixed material;
(2) and (2) feeding the mixed material obtained in the step (1) into a double-screw extruder, fully melting and plasticizing, kneading and mixing, extruding through a machine head, bracing, cooling, granulating, drying and finally packaging under the conveying and shearing action of the double-screw extruder to obtain the damping, halogen-free and flame-retardant reinforced PBT material.
9. The method according to claim 8, wherein in the step (1), the pre-drying temperature is 120 to 140 ℃ and the pre-drying time is 4 to 6 hours.
10. The preparation method according to claim 8, wherein in the step (2), the feeding speed of the twin-screw extruder is 450 to 800 kg/h, and the temperatures of the twin-screw extruder from the feeding port to the head are 220 to 230 ℃ in the feeding section, 230 to 240 ℃ in the conveying section, 203 to 240 ℃ in the melt-mixing section I, 240 to 250 ℃ in the melt-mixing section II, 250 to 260 ℃ in the natural gas-discharging section, 240 to 250 ℃ in the mixing section I, 240 to 250 ℃ in the mixing section II, 230 to 240 ℃ in the vacuum gas-discharging section, 230 to 240 ℃ in the extrusion metering section, and the screw rotation speed is 250 to 400 rpm.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011375829.1A CN112574535B (en) | 2020-11-30 | 2020-11-30 | Damping halogen-free flame-retardant reinforced PBT (polybutylene terephthalate) material and preparation method thereof |
| PCT/CN2021/092845 WO2022110672A1 (en) | 2020-11-30 | 2021-05-10 | Shock-absorbing damping halogen-free flame-retardant reinforced pbt material and preparation method therefor |
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| CN202011375829.1A CN112574535B (en) | 2020-11-30 | 2020-11-30 | Damping halogen-free flame-retardant reinforced PBT (polybutylene terephthalate) material and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114230985A (en) * | 2021-12-28 | 2022-03-25 | 上海普利特复合材料股份有限公司 | High-flame-retardancy precipitation-resistant halogen-free flame-retardant reinforced PBT (polybutylene terephthalate) material and preparation method thereof |
| WO2022110672A1 (en) * | 2020-11-30 | 2022-06-02 | 金发科技股份有限公司 | Shock-absorbing damping halogen-free flame-retardant reinforced pbt material and preparation method therefor |
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| CN114230985B (en) * | 2021-12-28 | 2024-04-09 | 上海普利特复合材料股份有限公司 | High-flame-retardance precipitation-resistant halogen-free flame-retardant reinforced PBT material and preparation method thereof |
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| CN112574535B (en) | 2022-04-19 |
| WO2022110672A1 (en) | 2022-06-02 |
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