CN109486136A - PBT/PET alloy material and preparation method thereof - Google Patents
PBT/PET alloy material and preparation method thereof Download PDFInfo
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- CN109486136A CN109486136A CN201811517244.1A CN201811517244A CN109486136A CN 109486136 A CN109486136 A CN 109486136A CN 201811517244 A CN201811517244 A CN 201811517244A CN 109486136 A CN109486136 A CN 109486136A
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- 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
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- C08K2003/328—Phosphates of heavy metals
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- 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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- C08L2205/00—Polymer mixtures characterised by other features
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Abstract
The present invention relates to a kind of PBT/PET alloy materials and preparation method thereof.The PBT/PET alloy material includes the raw material of following parts by weight: 30~70 parts of PBT resin；10~30 parts of PET resin；20~40 parts of glass fibre；1~3 part of toughener；0.5~1 part of nucleating agent；Compound 0.5~2 part of anti-glass emergence on the surface agent；1-3 parts of basic zirconium phosphate；0.2~0.6 part of antioxidant；Wherein, the compound anti-glass emergence on the surface agent is by fatty acid amide series lubricant agent, organosiloxane series lubricant agent and chloroflo series lubricant agent (2~5) in mass ratio: (2~5): 1 mixes；The PBT resin is low viscosity resin, 0.65~0.95dL/g of inherent viscosity；The PET resin is low viscosity resin, 0.50~0.80dL/g of inherent viscosity.The alloy material content of glass fiber is high, has superior mechanical property, the characteristic of excellent heat resistance and good appearance.
Description
Technical field
The present invention relates to technical field of polymer materials, more particularly to PBT/PET alloy material and preparation method thereof.
Background technique
Polybutylene terephthalate (PBT) (PBT) is one of five big general engineering plastics, is that a kind of crystalline thermoplastic is poly-
Ester has the characteristics that excellent heat resistance, electrical insulating property, processability, low water imbibition and chemically-resistant solvent, in electronics electricity
The fields such as work, automobile, family's electric parts are widely applied.With PBT material purposes further extensively, every profession and trade is to material
The requirement of various performances is also higher and higher, without glass fibre reinforced modified PBT material since mechanical property is poor, molding is received
The defects such as shrinkage is big, heat distortion temperature is low are unable to satisfy many product requirements.Therefore, glass fibre is carried out to PBT material
Enhancing modification has great importance, and modified PBT material mechanical strength and heat distortion temperature have all obtained greatly mentioning
It rises, and the content of composite material glass fibre is higher, the mechanical strength for enhancing modified material is higher.
By glass fibre reinforced modified PBT material, although mechanical property and heat distortion temperature have obtained larger promotion,
But due to compatibility and viscosity differences of glass fibre and PBT resin matrix etc., in injection molding process, glass
Fiber is easily floating to be exposed at article surface, so that article surface is coarse, and influences glass fibre institute accounting in appearance, especially material
After example is more than 30%, this floating fine phenomenon is further obvious, seriously limits the use of product.Therefore, the mechanics of materials is not being reduced
With improvement glass emergence on the surface problem in the case where thermal property, a kind of PBT material with the high glass fiber content of excellent appearance is developed
It is imperative.
In view of the above-mentioned problems, fine problem floating to improvement fiber glass reinforced PBT has done some researchs in currently available technology, such as
Chinese patent CN106987102A discloses a kind of low floating short fiber enhanced PBT/ABS of fibre of the heat-resisting impact resistance that can be used for electric appliance casing
Alloy material and preparation method thereof only improves floating fibre by short glass fiber；Chinese patent CN106366584A discloses low floating fine high
Gloss glass fiber reinforced polyethylene terephthalate improves material gloss using transparent resin and improves floating fibre；Chinese patent
The numerous patents such as CN 106084685A, Chinese patent CN103709680A and Chinese patent CN103665792A report one
The low floating fine flame-retardant enhanced PBT material of kind is all floating fine by the way that anti-glass emergence on the surface agent improvement is added；Chinese patent CN105199338A
Disclose low floating fine flame-retardant reinforced PBT composition of a kind of high-performance and preparation method thereof, the glass improver that leaks outside is PET, this is specially
The not authenticated glass fiber content of benefit is greater than floating fine improvement when 30%.
Summary of the invention
Based on this, it is necessary to provide a kind of PBT/PET alloy material, the alloy material content of glass fiber is high, has excellent
More mechanical property, the characteristic of excellent heat resistance and good appearance, can be applied to the fields such as electron and electrician, automobile, household electrical appliances.
In order to achieve the above objectives, the present invention uses following scheme:
A kind of PBT/PET alloy material, includes the raw material of following parts by weight:
Wherein, the compound anti-glass emergence on the surface agent is by fatty acid amide series lubricant agent, organosiloxane series lubricant agent and hydrocarbon
Wax class lubricant (2~5) in mass ratio: (2~5): 1 mixes；
The PBT is low viscosity resin, 0.65~0.95dL/g of inherent viscosity；
The PET is low viscosity resin, 0.50~0.80dL/g of inherent viscosity.
The PBT/PET alloy material in one of the embodiments, includes the raw material of following parts by weight:
Weight accounting of the glass fibre in the raw material is greater than 30% in one of the embodiments,.
0.8~0.9dL/g of inherent viscosity of the PBT resin in one of the embodiments,；The spy of the PET resin
0.6~0.7dL/g of property viscosity.
The fatty acid amide series lubricant agent is modified ethylene bis-fatty acid amides in one of the embodiments,；It is described
Organosiloxane series lubricant agent is dimethyl silicone polymer；The chloroflo series lubricant agent is polyethylene wax.
The compound anti-glass emergence on the surface agent is by fatty acid amide series lubricant agent, organosilicon oxygen in one of the embodiments,
Alkanes lubricant and chloroflo series lubricant agent (2~3) in mass ratio: (2~3): 1 mixes.
The basic zirconium phosphate is organically-modified alpha zirconium phosphate in one of the embodiments,.
The glass fibre is alkali-free chopped glass of the surface using the processing of silane type size in one of the embodiments,
Glass fiber, diameter are 7~17 μm, and length is 1~10mm.
The toughener is ethylene-methacrylic acid copolymer, ethylene-methyl acrylate-in one of the embodiments,
Glycidyl methacrylate copolymer, ethylene-methyl methacrylate butyl ester-glycidyl acrylate copolymer, ethylene-the third
At least one of e pioic acid methyl ester copolymer, polyethylene octene-glycidyl acrylate copolymer.
Nucleating agent is talcum powder, calcium carbonate, mica, at least one in long-chain carboxylic acid's sodium salt in one of the embodiments,
Kind.
Long-chain carboxylic acid's sodium salt is the sodium salt of the monoacid containing 12~37 carbon atoms in one of the embodiments,.
The antioxidant is Hinered phenols antioxidant, suffocated amine antioxidant, phosphoric acid ester in one of the embodiments,
At least one of antioxidant, thioester antioxidant.
The antioxidant is [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] season penta in one of the embodiments,
The mixture of tetrol (antioxidant 1010) and three [2,4- di-tert-butyl-phenyl] phosphite esters (irgasfos 168).Preferred weight ratio
For 1:0.5~1.5.
The present invention also provides a kind of preparation methods of PBT/PET alloy material, comprising the following steps:
Step 1: drying 4~6h for the PBT resin and PET resin at a temperature of 120~140 DEG C, after the completion of dry,
It is cooled to room temperature；
Step 2: by the PBT resin after cooling and PET resin, with the toughener, nucleating agent, compound anti-glass
Outer distillate medicinal water, antioxidant are put the mixture into a stirrer, and are stirred 5~10min at normal temperature；
Step 3: the mixed material of step 2 is added in the hopper of parallel double-screw extruder, by the glass
Fiber is added into the glass bucket in the parallel double-screw extruder middle section, through melting extrusion, cooling, air-dries, pelletizing.
In one of the embodiments, in step 3, the technological parameter of the melting extrusion are as follows: area's temperature be 160~
180 DEG C, two area's temperature are 240~260 DEG C, and three area's temperature are 240~260 DEG C, and four area's temperature are 240~260 DEG C, five Qu Wendu
It is 240~260 DEG C, six area's temperature are 220~240 DEG C, and seven area's temperature are 240~240 DEG C, and eight area's temperature are 220~240 DEG C,
Die head temperature is 240~260 DEG C, and screw speed is 300~500rpm.
The principle of the present invention is as follows:
In order to solve the problems, such as the common floating fibre of current fiber glass reinforced PBT material, the present invention uses the alloy material side PBT/PET
PET resin is added in alloy material compared to common fiber glass reinforced PBT material in case, can reduce the crystalline rate of intermingling material
It with crystallinity, prevents from leading to glass emergence on the surface because of rapid crystallization, improves material appearance；Meanwhile using the PBT of certain intrinsic viscosity with
PET resin improves the mobility of material, improves dispersion of the glass in resin matrix；Moreover, the compound anti-glass used
Outer distillate medicinal water has interior lubrication, outer lubrication and the comprehensive function for improving compatibility between resin and glass fibre simultaneously, and certain ratio is added
The compound anti-glass emergence on the surface agent of example can reduce intermolecular friction during material flowing, can reduce material in injection moulding process
With the frictional force of die surface, prevent causes glass fibre to be deposited in article surface because of rubbing action there is floating fibre, meanwhile, it is multiple
Boundary strength between resin and glass fibre can be increased by closing anti-glass emergence on the surface agent, promote resin to the cladding energy of glass fibre
Power prevents glass fibre from separating the floating fibre of appearance with resin matrix；Basic zirconium phosphate is novel and multifunctional mesoporous material, is had higher
Thermal stability, mechanical strength and large specific surface area, the interface that can largely increase between resin and glass fibre is strong
Degree, prevents glass from accumulating, and basic zirconium phosphate has lubricating action, can improve point of the glass fibre in resin in process
It dissipates, meanwhile, basic zirconium phosphate also can increase the mechanical strength, impact resistance and heat resistance of composite material.
Compared with prior art, the beneficial effects of the present invention are:
PBT/PET alloy material of the invention has superior mechanical property, the characteristic of excellent heat resistance and good appearance.Specifically
It is as follows:
1, PBT/PET alloy material of the present invention, glass fibre occupation ratio is high in material, since glass fibre has
There is the features such as tensile strength is big, rigidity is good, can largely absorb impact energy, is heat-resist, therefore by glass fibre reinforced modified
Material afterwards has excellent mechanical property and heat resistance.
2, PBT/PET alloy material of the present invention joined PET resin compared to common fiber glass reinforced PBT material
The crystalline rate and crystallinity that can reduce intermingling material prevent from leading to glass emergence on the surface because of rapid crystallization, improve material appearance, and
Using low viscous PBT resin and low viscous PET resin, mobility is high, keeps glass fibre fully dispersed in resin；What cooperation used answers
It closes anti-glass emergence on the surface agent while there is interior lubrication, outer lubrication and the comprehensive function for improving compatibility between resin and glass fibre, add
Intermolecular friction during material flowing can be reduced by entering a certain proportion of compound anti-glass emergence on the surface agent, can be reduced and be molded
The frictional force of material and die surface in journey, prevents that glass fibre is caused to be deposited in article surface because of rubbing action, floats
Fibre, meanwhile, compound anti-glass emergence on the surface agent can increase the boundary strength between resin and glass fibre, promote resin to glass fibers
The cladding ability of dimension prevents glass fibre from separating the floating fibre of appearance with resin matrix；In addition, basic zirconium phosphate can largely increase
Add the boundary strength between resin and glass fibre, prevent glass from accumulating, and basic zirconium phosphate has lubricating action, can improve processing
Dispersion of the glass fibre in resin in the process, at the same basic zirconium phosphate also can increase the mechanical strength of composite material, impact resistance with it is resistance to
Hot property.Thus obtained PBT/PET alloy material has excellent mechanical property, excellent heat resistance and good appearance.
3, raw material needed for PBT/PET alloy material of the present invention have market sale, are easier to obtain.
4, the preparation method of PBT/PET alloy material of the present invention is simple to operation, does not cause environmental pollution, work easy to accomplish
Industry continuous production.
Detailed description of the invention
Fig. 1 is the preparation technology flow chart of PBT/PET alloy material described in one embodiment of the invention.
Specific embodiment
PBT/PET alloy material and preparation method thereof of the invention is made below in conjunction with specific embodiment further details of
Explanation.
Raw material used in the embodiment of the present invention is as follows:
Polybutylene terephthalate (PBT) (PBT) is selected from blue star Nantong stars synthetic material PBT 1084, inherent viscosity
For 0.84 ± 0.02dL/g；
Polyethylene terephthalate (PET) is selected from Yizheng Chemical Fiber Co., Ltd., SINOPEC PET SD500,
Its inherent viscosity is 0.67 ± 0.02dL/g；
Toughener such as ethylene-methyl acrylate-glyceryl methacrylate copolymer is selected from DuPont Corporation；
Glass fiber diameter is 13 μm, length 4.5mm, is selected from Taishan glass fiber Ltd T436H；
Nucleating agent long-chain carboxylic acid's sodium salt is selected from Clariant Chemical Co., Ltd., for the monoacid containing 12~37 carbon atoms
Sodium salt；
Compound anti-glass emergence on the surface agent self-control；
Alpha zirconium phosphate is selected from Mianzhu Yao Long Chemical Co., Ltd.；
Antioxidant such as four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythrite (antioxidant 1010), three [2,
4- di-tert-butyl-phenyl] phosphite ester (irgasfos 168) is selected from Yixing City angel and synthesizes Chemical Co., Ltd., use in embodiment
The mixture of the two, ratio are weight ratio.
Embodiment 1:
A kind of PBT/PET alloy material of the present embodiment, is prepared by the raw material of following parts by weight:
Compound anti-glass emergence on the surface agent is by being modified ethylene bis-fatty acid amides, dimethyl silicone polymer and polyethylene wax by quality
It is mixed than 2:2:1, additional amount is respectively modified 0.2 part of ethylene bis-fatty acid amides, 0.2 part of dimethyl silicone polymer and gathers
0.1 part of ethylene waxes.
The preparation method of above-mentioned PBT/PET alloy material the following steps are included:
Step 1: the raw material of each parts by weight is weighed respectively, and by weighed PBT resin, PET resin at 120 DEG C
At a temperature of dry 6h be cooled to room temperature after the completion of dry；
Step 2: PBT resin, PET resin and the toughener (ethylene-methyl acrylate-metering system of room temperature be will be cooled to
Acid glycidyl ester copolymer), nucleating agent (long-chain carboxylic acid's sodium salt), compound anti-glass emergence on the surface agent, basic zirconium phosphate, antioxidant (1010:
It 168=1:1) is put into high-speed mixer and is mixed, stir 5min at normal temperature；
Step 3: the mixed material of step 2 is added in the hopper of parallel double-screw extruder, by glass fibre
It is added in the glass bucket in parallel double-screw extruder middle section, through melting extrusion, cooling, air-dries, pelletizing；Technological parameter is as follows: one
Area's temperature is 160 DEG C, and two area's temperature are 240 DEG C, and three area's temperature are 240 DEG C, and four area's temperature are 240 DEG C, and five area's temperature are 240
DEG C, six area's temperature are 220 DEG C, and seven area's temperature are 220 DEG C, and eight area's temperature are 220 DEG C, and die head temperature is 240 DEG C, and screw speed is
300rpm.The alloy property is shown in Table 2.
Embodiment 2:
A kind of PBT/PET alloy material of the present embodiment, is prepared by the raw material of following parts by weight:
Compound anti-glass emergence on the surface agent is by being modified ethylene bis-fatty acid amides, dimethyl silicone polymer and polyethylene wax by quality
It is mixed than 2:2:1, additional amount is respectively modified 0.2 part of ethylene bis-fatty acid amides, 0.2 part of dimethyl silicone polymer and gathers
0.1 part of ethylene waxes.
The preparation method of above-mentioned PBT/PET alloy material the following steps are included:
Step 1: the raw material of each parts by weight is weighed respectively, and by weighed PBT resin and PET resin at 120 DEG C
At a temperature of dry 6h be cooled to room temperature after the completion of dry；
Step 2: PBT resin, PET resin and the toughener (ethylene-methyl acrylate-metering system of room temperature be will be cooled to
Acid glycidyl ester copolymer), nucleating agent (long-chain carboxylic acid's sodium salt), compound anti-glass emergence on the surface agent, basic zirconium phosphate, antioxidant (1010:
It 168=1:1) is put into high-speed mixer and is mixed, stir 5min at normal temperature；
Step 3: the mixed material of step 2 is added in the hopper of parallel double-screw extruder, by glass fibre
It is added in the glass bucket in parallel double-screw extruder middle section, through melting extrusion, cooling, air-dries, pelletizing；Technological parameter is as follows: one
Area's temperature is 160 DEG C, and two area's temperature are 240 DEG C, and three area's temperature are 240 DEG C, and four area's temperature are 240 DEG C, and five area's temperature are 240
DEG C, six area's temperature are 220 DEG C, and seven area's temperature are 220 DEG C, and eight area's temperature are 220 DEG C, and die head temperature is 240 DEG C, and screw speed is
400rpm.The alloy property is shown in Table 2.
Embodiment 3:
A kind of PBT/PET alloy material of the present embodiment, is prepared by the raw material of following parts by weight:
Compound anti-glass emergence on the surface agent is by being modified ethylene bis-fatty acid amides, dimethyl silicone polymer and polyethylene wax by quality
It is mixed than 2:2:1, additional amount is respectively modified 0.2 part of ethylene bis-fatty acid amides, 0.2 part of dimethyl silicone polymer and gathers
0.1 part of ethylene waxes.
The preparation method of above-mentioned PBT/PET alloy material the following steps are included:
Step 1: the raw material of each parts by weight is weighed respectively, and by weighed PBT resin and PET resin at 140 DEG C
At a temperature of dry 4h be cooled to room temperature after the completion of dry；
Step 2: PBT resin, PET resin and the toughener (ethylene-methyl acrylate-metering system of room temperature be will be cooled to
Acid glycidyl ester copolymer), nucleating agent (long-chain carboxylic acid's sodium salt), compound anti-glass emergence on the surface agent, basic zirconium phosphate, antioxidant (1010:
It 168=1:1) is put into high-speed mixer and is mixed, stir 5min at normal temperature；
Step 3: the mixed material of step 2 is added in the hopper of parallel double-screw extruder, by glass fibre
It is added in the glass bucket in parallel double-screw extruder middle section, through melting extrusion, cooling, air-dries, pelletizing；Technological parameter is as follows: one
Area's temperature is 160 DEG C, and two area's temperature are 240 DEG C, and three area's temperature are 240 DEG C, and four area's temperature are 240 DEG C, and five area's temperature are 240
DEG C, six area's temperature are 220 DEG C, and seven area's temperature are 220 DEG C, and eight area's temperature are 220 DEG C, and die head temperature is 240 DEG C, and screw speed is
500rpm.The alloy property is shown in Table 2.
Embodiment 4:
A kind of PBT/PET alloy material of the present embodiment, is prepared by the raw material of following parts by weight:
Compound anti-glass emergence on the surface agent is by being modified ethylene bis-fatty acid amides, dimethyl silicone polymer and polyethylene wax by quality
It is mixed than 2:2:1, additional amount is respectively modified 0.2 part of ethylene bis-fatty acid amides, 0.2 part of dimethyl silicone polymer and gathers
0.1 part of ethylene waxes.
The preparation method of above-mentioned PBT/PET alloy material includes the following steps that flow chart is shown in Fig. 1:
Step 1: the raw material of each parts by weight is weighed respectively, and by weighed PBT resin and PET resin at 140 DEG C
At a temperature of dry 4h be cooled to room temperature after the completion of dry；
Step 2: PBT resin, PET resin and the toughener (ethylene-methyl acrylate-metering system of room temperature be will be cooled to
Acid glycidyl ester copolymer), nucleating agent (long-chain carboxylic acid's sodium salt), compound anti-glass emergence on the surface agent, basic zirconium phosphate, antioxidant (1010:
It 168=1:1) is put into high-speed mixer and is mixed, stir 8min at normal temperature；
Step 3: the mixed material of step 2 is added in the hopper of parallel double-screw extruder, by glass fibre
It is added in the glass bucket in parallel double-screw extruder middle section, through melting extrusion, cooling, air-dries, pelletizing；Technological parameter is as follows: one
Area's temperature is 170 DEG C, and two area's temperature are 250 DEG C, and three area's temperature are 250 DEG C, and four area's temperature are 250 DEG C, and five area's temperature are 250
DEG C, six area's temperature are 230 DEG C, and seven area's temperature are 230 DEG C, and eight area's temperature are 230 DEG C, and die head temperature is 250 DEG C, and screw speed is
500rpm.The alloy property is shown in Table 2.
Embodiment 5:
A kind of PBT/PET alloy material of the present embodiment, is prepared by the raw material of following parts by weight:
Compound anti-glass emergence on the surface agent is by being modified ethylene bis-fatty acid amides, dimethyl silicone polymer and polyethylene wax by quality
It is mixed than 2:2:1, additional amount is respectively modified 0.8 part of ethylene bis-fatty acid amides, 0.8 part of dimethyl silicone polymer and gathers
0.4 part of ethylene waxes.
The preparation method of above-mentioned PBT/PET alloy material the following steps are included:
Step 1: the raw material of each parts by weight is weighed respectively, and by weighed PBT resin and PET resin at 140 DEG C
At a temperature of dry 4h be cooled to room temperature after the completion of dry；
Step 2: PBT resin, PET resin and the toughener (ethylene-methyl acrylate-metering system of room temperature be will be cooled to
Acid glycidyl ester copolymer), nucleating agent (long-chain carboxylic acid's sodium salt), compound anti-glass emergence on the surface agent, basic zirconium phosphate, antioxidant (1010:
It 168=1:1) is put into high-speed mixer and is mixed, stir 10min at normal temperature；
Step 3: the mixed material of step 2 is added in the hopper of parallel double-screw extruder, by glass fibre
It is added in the glass bucket in parallel double-screw extruder middle section, through melting extrusion, cooling, air-dries, pelletizing；Technological parameter is as follows: one
Area's temperature is 180 DEG C, and two area's temperature are 260 DEG C, and three area's temperature are 260 DEG C, and four area's temperature are 260 DEG C, and five area's temperature are 260
DEG C, six area's temperature are 240 DEG C, and seven area's temperature are 240 DEG C, and eight area's temperature are 240 DEG C, and die head temperature is 260 DEG C, and screw speed is
500rpm.The alloy property is shown in Table 2.
Embodiment 6:
A kind of PBT/PET alloy material of the present embodiment, is prepared by the raw material of following parts by weight:
Compound anti-glass emergence on the surface agent is by being modified ethylene bis-fatty acid amides, dimethyl silicone polymer and polyethylene wax by quality
It is mixed than 2:2:1, additional amount is respectively modified 0.8 part of ethylene bis-fatty acid amides, 0.8 part of dimethyl silicone polymer and gathers
0.4 part of ethylene waxes.
The preparation method of above-mentioned PBT/PET alloy material the following steps are included:
Step 1: the raw material of each parts by weight is weighed respectively, and by weighed PBT resin and PET resin at 140 DEG C
At a temperature of dry 4h be cooled to room temperature after the completion of dry；
Step 2: PBT resin, PET resin and the toughener (ethylene-methyl acrylate-metering system of room temperature be will be cooled to
Acid glycidyl ester copolymer), nucleating agent (long-chain carboxylic acid's sodium salt), compound anti-glass emergence on the surface agent, basic zirconium phosphate, antioxidant (1010:
It 168=1:1) is put into high-speed mixer and is mixed, stir 10min at normal temperature；
Step 3: the mixed material of step 2 is added in the hopper of parallel double-screw extruder, by glass fibre
It is added in the glass bucket in parallel double-screw extruder middle section, through melting extrusion, cooling, air-dries, pelletizing；Technological parameter is as follows: one
Area's temperature is 180 DEG C, and two area's temperature are 260 DEG C, and three area's temperature are 260 DEG C, and four area's temperature are 260 DEG C, and five area's temperature are 260
DEG C, six area's temperature are 240 DEG C, and seven area's temperature are 240 DEG C, and eight area's temperature are 240 DEG C, and die head temperature is 260 DEG C, and screw speed is
500rpm.The alloy property is shown in Table 2.
Comparative example 1:
PBT resin used in this comparative example is middle viscosity resin, and inherent viscosity is 1.05 ± 0.02dL/g, PET resin
For middle viscosity resin, inherent viscosity is 0.86 ± 0.02dL/g；Remaining raw material and identical as embodiment.
A kind of high good appearance PBT/PET alloy material of glass fiber content of this comparative example, by the raw material preparation of following parts by weight
At:
Compound anti-glass emergence on the surface agent is by being modified ethylene bis-fatty acid amides, dimethyl silicone polymer and polyethylene wax by quality
It is mixed than 2:2:1, additional amount is respectively modified 0.8 part of ethylene bis-fatty acid amides, 0.8 part of dimethyl silicone polymer and gathers
0.4 part of ethylene waxes.
The preparation method of above-mentioned PBT/PET alloy material the following steps are included:
Step 1: the raw material of each parts by weight is weighed respectively, and by weighed PBT resin and PET resin at 140 DEG C
At a temperature of dry 4h be cooled to room temperature after the completion of dry；
Step 2: PBT resin, PET resin and the toughener (ethylene-methyl acrylate-metering system of room temperature be will be cooled to
Acid glycidyl ester copolymer), nucleating agent (long-chain carboxylic acid's sodium salt), compound anti-glass emergence on the surface agent, basic zirconium phosphate, antioxidant (1010:
It 168=1:1) is put into high-speed mixer and is mixed, stir 10min at normal temperature；
Step 3: the mixed material of step 2 is added in the hopper of parallel double-screw extruder, by glass fibre
It is added in the glass bucket in parallel double-screw extruder middle section, through melting extrusion, cooling, air-dries, pelletizing；Technological parameter is as follows: one
Area's temperature is 180 DEG C, and two area's temperature are 260 DEG C, and three area's temperature are 260 DEG C, and four area's temperature are 260 DEG C, and five area's temperature are 260
DEG C, six area's temperature are 240 DEG C, and seven area's temperature are 240 DEG C, and eight area's temperature are 240 DEG C, and die head temperature is 260 DEG C, and screw speed is
500rpm.The alloy property is shown in Table 2.
Comparative example 2:
Raw material used in this comparative example is identical as embodiment.
A kind of PBT/PET alloy material of this comparative example, is prepared by the raw material of following parts by weight:
Compound anti-glass emergence on the surface agent is by being modified ethylene bis-fatty acid amides, dimethyl silicone polymer and polyethylene wax by quality
It is mixed than 2:2:1, additional amount is respectively modified 0.8 part of ethylene bis-fatty acid amides, 0.8 part of dimethyl silicone polymer and gathers
0.4 part of ethylene waxes.
The preparation method of above-mentioned PBT/PET alloy material the following steps are included:
Step 1: the raw material of each parts by weight is weighed respectively, and will be dry at a temperature of 120 DEG C of weighed PBT resin
4h is cooled to room temperature after the completion of dry；
Step 2: will be cooled to the PBT resin of room temperature, (ethylene-methyl acrylate-Glycidyl methacrylate is sweet with toughener
Grease copolymer), nucleating agent (long-chain carboxylic acid's sodium salt), compound anti-glass emergence on the surface agent, basic zirconium phosphate, antioxidant (1010:168=1:
1) it is put into high-speed mixer and is mixed, stir 5min at normal temperature；
Step 3: the mixed material of step 2 is added in the hopper of parallel double-screw extruder, by glass fibre
It is added in the glass bucket in parallel double-screw extruder middle section, through melting extrusion, cooling, air-dries, pelletizing；Technological parameter is as follows: one
Area's temperature is 160 DEG C, and two area's temperature are 240 DEG C, and three area's temperature are 240 DEG C, and four area's temperature are 240 DEG C, and five area's temperature are 240
DEG C, six area's temperature are 220 DEG C, and seven area's temperature are 220 DEG C, and eight area's temperature are 220 DEG C, and die head temperature is 240 DEG C, and screw speed is
500rpm.The alloy property is shown in Table 2.
Comparative example 3:
Raw material used in this comparative example is identical as embodiment.
A kind of PBT/PET alloy material of this comparative example, is prepared by the raw material of following parts by weight:
The preparation method of above-mentioned PBT/PET alloy material the following steps are included:
Step 1: the raw material of each parts by weight is weighed respectively, and by weighed PBT resin and PET resin at 140 DEG C
At a temperature of dry 4h be cooled to room temperature after the completion of dry；
Step 2: PBT resin, PET resin and the toughener (ethylene-methyl acrylate-metering system of room temperature be will be cooled to
Acid glycidyl ester copolymer), nucleating agent (long-chain carboxylic acid's sodium salt), compound anti-glass emergence on the surface agent, basic zirconium phosphate, antioxidant (1010:
It 168=1:1) is put into high-speed mixer and is mixed, stir 10min at normal temperature；
Step 3: the mixed material of step 2 is added in the hopper of parallel double-screw extruder, by glass fibre
It is added in the glass bucket in parallel double-screw extruder middle section, through melting extrusion, cooling, air-dries, pelletizing；Technological parameter is as follows: one
Area's temperature is 180 DEG C, and two area's temperature are 260 DEG C, and three area's temperature are 260 DEG C, and four area's temperature are 260 DEG C, and five area's temperature are 260
DEG C, six area's temperature are 240 DEG C, and seven area's temperature are 240 DEG C, and eight area's temperature are 240 DEG C, and die head temperature is 260 DEG C, and screw speed is
500rpm.The alloy property is shown in Table 2.
Comparative example 4:
Raw material used in this comparative example is identical as embodiment.
A kind of PBT/PET alloy material of this comparative example, is prepared by the raw material of following parts by weight:
Compound anti-glass emergence on the surface agent is by being modified ethylene bis-fatty acid amides, dimethyl silicone polymer and polyethylene wax by quality
It is mixed than 1:1:3, additional amount is respectively modified 0.4 part of ethylene bis-fatty acid amides, 0.4 part of dimethyl silicone polymer and gathers
1.2 parts of ethylene waxes.
The preparation method of above-mentioned PBT/PET alloy material the following steps are included:
Step 1: the raw material of each parts by weight is weighed respectively, and by weighed PBT resin and PET resin at 140 DEG C
At a temperature of dry 4h be cooled to room temperature after the completion of dry；
Step 2: PBT resin, PET resin and the toughener (ethylene-methyl acrylate-metering system of room temperature be will be cooled to
Acid glycidyl ester copolymer), nucleating agent (long-chain carboxylic acid's sodium salt), compound anti-glass emergence on the surface agent, basic zirconium phosphate, antioxidant is put into
It is mixed in high-speed mixer, stirs 10min at normal temperature；
Step 3: the mixed material of step 2 is added in the hopper of parallel double-screw extruder, by glass fibre
It is added in the glass bucket in parallel double-screw extruder middle section, through melting extrusion, cooling, air-dries, pelletizing；Technological parameter is as follows: one
Area's temperature is 180 DEG C, and two area's temperature are 260 DEG C, and three area's temperature are 260 DEG C, and four area's temperature are 260 DEG C, and five area's temperature are 260
DEG C, six area's temperature are 240 DEG C, and seven area's temperature are 240 DEG C, and eight area's temperature are 240 DEG C, and die head temperature is 260 DEG C, and screw speed is
500rpm.The alloy property is shown in Table 2.
Comparative example 5:
Raw material used in this comparative example is identical as embodiment.
A kind of high good appearance PBT/PET alloy material of glass fiber content of this comparative example, by the raw material preparation of following parts by weight
At:
Compound anti-glass emergence on the surface agent is by being modified ethylene bis-fatty acid amides, dimethyl silicone polymer and polyethylene wax by quality
It is mixed than 2:2:0, additional amount is respectively modified 1.0 parts of ethylene bis-fatty acid amides, 1.0 parts of dimethyl silicone polymer.
The preparation method of above-mentioned PBT/PET alloy material the following steps are included:
Step 1: the raw material of each parts by weight is weighed respectively, and by weighed PBT resin and PET resin at 140 DEG C
At a temperature of dry 4h be cooled to room temperature after the completion of dry；
Step 2: PBT resin, PET resin and the toughener (ethylene-methyl acrylate-metering system of room temperature be will be cooled to
Acid glycidyl ester copolymer), nucleating agent (long-chain carboxylic acid's sodium salt), compound anti-glass emergence on the surface agent, basic zirconium phosphate, antioxidant (1010:
It 168=1:1) is put into high-speed mixer and is mixed, stir 10min at normal temperature；
Step 3: the mixed material of step 2 is added in the hopper of parallel double-screw extruder, by glass fibre
It is added in the glass bucket in parallel double-screw extruder middle section, through melting extrusion, cooling, air-dries, pelletizing；Technological parameter is as follows: one
Area's temperature is 180 DEG C, and two area's temperature are 260 DEG C, and three area's temperature are 260 DEG C, and four area's temperature are 260 DEG C, and five area's temperature are 260
DEG C, six area's temperature are 240 DEG C, and seven area's temperature are 240 DEG C, and eight area's temperature are 240 DEG C, and die head temperature is 260 DEG C, and screw speed is
500rpm.The alloy property is shown in Table 2.
Comparative example 6:
Raw material used in this comparative example is identical as embodiment.
A kind of high good appearance PBT/PET alloy material of glass fiber content of this comparative example, by the raw material preparation of following parts by weight
At:
Compound anti-glass emergence on the surface agent is by being modified ethylene bis-fatty acid amides, dimethyl silicone polymer and polyethylene wax by quality
It is mixed than 2:2:1, additional amount is respectively modified 0.8 part of ethylene bis-fatty acid amides, 0.8 part of dimethyl silicone polymer and gathers
0.4 part of ethylene waxes.
The preparation method of above-mentioned PBT/PET alloy material the following steps are included:
Step 1: the raw material of each parts by weight is weighed respectively, and by weighed PBT resin and PET resin at 140 DEG C
At a temperature of dry 6h be cooled to room temperature after the completion of dry；
Step 2: PBT resin, PET resin and the toughener (ethylene-methyl acrylate-metering system of room temperature be will be cooled to
Acid glycidyl ester copolymer), nucleating agent (long-chain carboxylic acid's sodium salt), compound anti-glass emergence on the surface agent, antioxidant (1010:168=1:
1) it is put into high-speed mixer and is mixed, stir 10min at normal temperature；
Step 3: the mixed material of step 2 is added in the hopper of parallel double-screw extruder, by glass fibre
It is added in the glass bucket in parallel double-screw extruder middle section, through melting extrusion, cooling, air-dries, pelletizing；Technological parameter is as follows: one
Area's temperature is 180 DEG C, and two area's temperature are 260 DEG C, and three area's temperature are 260 DEG C, and four area's temperature are 260 DEG C, and five area's temperature are 260
DEG C, six area's temperature are 240 DEG C, and seven area's temperature are 240 DEG C, and eight area's temperature are 240 DEG C, and die head temperature is 260 DEG C, and screw speed is
500rpm.The alloy property is shown in Table 2.
Comparative example 7:
Raw material used in this comparative example is identical as embodiment.
A kind of high good appearance PBT/PET alloy material of glass fiber content of this comparative example, by the raw material preparation of following parts by weight
At:
Compound anti-glass emergence on the surface agent is by being modified ethylene bis-fatty acid amides, dimethyl silicone polymer and polyethylene wax by quality
It is mixed than 2:2:1, additional amount is respectively modified 0.8 part of ethylene bis-fatty acid amides, 0.8 part of dimethyl silicone polymer and gathers
0.4 part of ethylene waxes.
The preparation method of above-mentioned PBT/PET alloy material the following steps are included:
Step 1: the raw material of each parts by weight is weighed respectively, and by weighed PBT resin and PET resin at 140 DEG C
At a temperature of dry 6h be cooled to room temperature after the completion of dry；
Step 2: PBT resin, PET resin and the toughener (ethylene-methyl acrylate-metering system of room temperature be will be cooled to
Acid glycidyl ester copolymer), nucleating agent (long-chain carboxylic acid's sodium salt), compound anti-glass emergence on the surface agent, basic zirconium phosphate, antioxidant (1010:
It 168=1:1) is put into high-speed mixer and is mixed, stir 10min at normal temperature；
Step 3: the mixed material of step 2 is added in the hopper of parallel double-screw extruder, by glass fibre
It is added in the glass bucket in parallel double-screw extruder middle section, through melting extrusion, cooling, air-dries, pelletizing；Technological parameter is as follows: one
Area's temperature is 180 DEG C, and two area's temperature are 260 DEG C, and three area's temperature are 260 DEG C, and four area's temperature are 260 DEG C, and five area's temperature are 260
DEG C, six area's temperature are 240 DEG C, and seven area's temperature are 240 DEG C, and eight area's temperature are 240 DEG C, and die head temperature is 260 DEG C, and screw speed is
500rpm.The alloy property is shown in Table 2.
The following are embodiments and comparative example list (table 1):
1 embodiment of table and comparative example raw material form parts by weight list
The various embodiments described above and the made plastic part sample of comparative example are subjected to following performance test (the results are shown in Table 2):
Tensile property: GB/T 1040.1-2006 standard testing, rate of extension 50mm/min are pressed；
Bending property: pressing GB/T 9341-2008 standard testing, is bent rate 2mm/min；
Impact property: GB/T 1843-2008 standard testing is pressed；
Heat distortion temperature: GB/T 1634.2-2004 standard testing, load bend stress 0.45MPa are pressed；
Appearance: being evaluated by visual comparison, and five observers observe by visual observation in identical environment, provides scoring (0.0-
12.0 points), take five to divide for each person, appearance rating to poor, is followed successively by bright (10.0-12.0 points), very well (8.0- by good
9.9 points), excellent (6.0-7.9 point), good (4.0-5.9 points), general (2.0-3.9 points), poor (0-1.9 points).
2 embodiment of table and comparative example performance list
As can be seen that the additive amount of glass fibre is more from Examples 1 to 6, the intensity of PBT/PET alloy material is got over
Height, heat resistance also rise with it, but floating fine also increasingly severe, and appearance is poorer；The additional amount of PET resin increases, alloy material
The appearance of material is better, and mechanical property slightly rises with heat resistance；Compound anti-glass emergence on the surface agent additional amount is more, can effectively mention
The appearance of material is risen, basic zirconium phosphate additional amount increases, and material appearance is obviously improved, and mechanical property also rises with it with heat resistance.
In summary the comprehensive performance of factor, embodiment 6 is best.
Compared with Example 6 compared with PBT resin that comparative example 1 uses and PET resin raw material are to glue to set during viscosity is higher
Rouge, mobility is poor, influences dispersion of the glass in resin matrix, and alloy material appearance is caused to be deteriorated；Comparative example 2 is not added with
PET resin quickly due to PBT resin crystallization rate causes glass to expose on the surface of the material, and material is floating fine serious, and appearance is obvious
It is deteriorated, and intensity and heat resistance also relative reduction；To comparative example 3 compared with Example 6 compared with compound anti-glass emergence on the surface is not added
Agent, resin and glass fibre compatibility are insufficient, and due to lack of lubrication during machine-shaping, due to resin when melt flows
Viscosity differences between glass fibre cause the two in flow process that discrete state is presented, and floating fibre occur；Comparative example 4 and reality
It applies example 6 to compare, the ratio of compound anti-glass emergence on the surface agent is different, and the additional amount of polyethylene wax is relatively more, has primarily served table
The effect of face lubrication, but modified ethylene bis-fatty acid amides and the additional amount of dimethyl silicone polymer are relatively fewer, and material is flowing
Interior lack of lubrication in dynamic forming process, intermolecular friction power is big, and glass is easy accumulation, occurs floating fine and material appearance is caused to become
Difference；Comparative example 5 is not compared with Example 6 compared with polyethylene wax being added in compound anti-glass emergence on the surface agent, material is in flowing forming process
China and foreign countries' lack of lubrication, due to melt and die surface frictional force effect it is larger cause glass hold expose on the surface of the material so that material
Expect that appearance is deteriorated；Comparative example 6 compared with Example 6 compared with, be not added basic zirconium phosphate, resin and glass fibre boundary strength are insufficient,
When the effects of being sheared, being rubbed in process, glass fibre easily separates between resin matrix and causes to accumulate, and occurs
Floating fibre；Comparative example 7 is compared with Example 6 compared with the additional amount of basic zirconium phosphate is more, but has no significant effect to appearance, and composite material
Mechanical strength and heat resistance without being obviously improved, and basic zirconium phosphate is added and excessively will lead to stress concentration, so that impact property reduces.
It is the PBT/PET alloy material mechanical property that is prepared, resistance to by comparison it can be found that using scheme described in embodiment 6
Hot property is greatly improved with appearance, obtains the PBT/PET alloy material of superior mechanical property, excellent heat resistance and good appearance characteristics
The beneficial effect of material.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. a kind of PBT/PET alloy material, which is characterized in that include the raw material of following parts by weight:
30~70 parts of PBT resin；
10~30 parts of PET resin；
20~40 parts of glass fibre；
The parts by weight summation of PBT resin, PET resin and glass fibre is 100 parts；
The PBT resin is low viscosity resin, 0.65~0.95dL/g of inherent viscosity；
The PET resin is low viscosity resin, 0.5~0.8dL/g of inherent viscosity；
The compound anti-glass emergence on the surface agent is by fatty acid amide series lubricant agent, organosiloxane series lubricant agent and chloroflo series lubricant agent
In mass ratio (2~5): (2~5): 1 mixes.
2. PBT/PET alloy material according to claim 1, which is characterized in that include the raw material of following parts by weight:
30~40 parts of PBT resin；
20~30 parts of PET resin；
35~40 parts of glass fibre；
The parts by weight summation of PBT resin, PET resin and glass fibre is 100 parts；
3. PBT/PET alloy material according to claim 1, which is characterized in that the inherent viscosity 0.8 of the PBT resin
~0.9dL/g；0.6~0.7dL/g of inherent viscosity of the PET resin.
4. PBT/PET alloy material according to claim 1, which is characterized in that the fatty acid amide series lubricant agent is
Modified ethylene bis-fatty acid amides；The organosiloxane series lubricant agent is dimethyl silicone polymer；The chloroflo series lubricant agent
For polyethylene wax.
5. PBT/PET alloy material according to claim 1, which is characterized in that the compound anti-glass emergence on the surface agent is by rouge
Fat acid amide series lubricant agent, organosiloxane series lubricant agent are with chloroflo series lubricant agent (2~3) in mass ratio: (2~3): 1 mixes
It forms.
6. PBT/PET alloy material according to claim 1-5, which is characterized in that the basic zirconium phosphate is α-phosphorus
Sour zirconium.
7. PBT/PET alloy material according to claim 1-5, which is characterized in that the glass fibre is table
Face uses the alkali-free short glass fiber of silane type size processing, and diameter is 7~17 μm, and length is 1~10mm.
8. PBT/PET alloy material according to claim 1-5, which is characterized in that the toughener is ethylene-
Methacrylic acid copolymer, ethylene-methyl acrylate-glyceryl methacrylate copolymer, ethylene-methyl methacrylate fourth
Ester-glycidyl acrylate copolymer, ethylene-methyl acrylate copolymer, polyethylene octene-glycidyl acrylate are total
At least one of polymers, and/or, the nucleating agent is talcum powder, calcium carbonate, mica, at least one in long-chain carboxylic acid's sodium salt
Kind；And/or the antioxidant is Hinered phenols antioxidant, suffocated amine antioxidant, phosphoric acid ester antioxidant, thioesters are anti-
At least one of oxygen agent.
9. a kind of described in any item preparation methods of PBT/PET alloy material of claim 1-8, which is characterized in that including with
Lower step:
Step 1: drying 4~6h for the PBT resin and PET resin at a temperature of 120~140 DEG C, cooling after the completion of dry
To room temperature；
Step 2: by the PBT resin after cooling and PET resin, with the toughener, nucleating agent, compound anti-glass emergence on the surface
Agent, basic zirconium phosphate, antioxidant are put the mixture into a stirrer, and are stirred 5~10min at normal temperature；
Step 3: the mixed material of step 2 is added in the hopper of parallel double-screw extruder, by the glass fibre
It is added into the glass bucket in the parallel double-screw extruder middle section, through melting extrusion, cooling, air-dries, pelletizing.
10. preparation method according to claim 9, which is characterized in that in step 3, the technological parameter of the melting extrusion
Are as follows: area's temperature is 160~180 DEG C, and two area's temperature are 240~260 DEG C, and three area's temperature are 240~260 DEG C, and four area's temperature are
240~260 DEG C, five area's temperature be 240~260 DEG C, six area's temperature be 220~240 DEG C, seven area's temperature be 220~240 DEG C, eight
Area's temperature is 220~240 DEG C, and die head temperature is 240~260 DEG C, and screw speed is 300~500rpm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110551367A (en) * | 2019-07-19 | 2019-12-10 | 深圳市高科塑化有限公司 | Piano black mirror surface gloss spray-free glass fiber reinforced PET (polyethylene terephthalate) polyester material and preparation method thereof |
| CN111534060A (en) * | 2020-05-22 | 2020-08-14 | 浙江钧科新材料有限公司 | Reinforced flame-retardant PBT/PET alloy and preparation method thereof |
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2018
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110551367A (en) * | 2019-07-19 | 2019-12-10 | 深圳市高科塑化有限公司 | Piano black mirror surface gloss spray-free glass fiber reinforced PET (polyethylene terephthalate) polyester material and preparation method thereof |
| CN110551367B (en) * | 2019-07-19 | 2022-02-15 | 深圳市高科塑化有限公司 | Piano black mirror surface gloss spray-free glass fiber reinforced PET (polyethylene terephthalate) polyester material and preparation method thereof |
| CN111534060A (en) * | 2020-05-22 | 2020-08-14 | 浙江钧科新材料有限公司 | Reinforced flame-retardant PBT/PET alloy and preparation method thereof |
| CN115433450A (en) * | 2022-09-30 | 2022-12-06 | 金发科技股份有限公司 | Good-appearance glass mineral composite reinforced PC alloy composition and preparation method and application thereof |
| CN115433450B (en) * | 2022-09-30 | 2024-03-22 | 金发科技股份有限公司 | Glass-ore composite reinforced PC alloy composition with good appearance, and preparation method and application thereof |
| CN116535701A (en) * | 2023-07-03 | 2023-08-04 | 广东永鑫华新型材料有限公司 | Preparation method of glass fiber reinforced ABS composite material |
| CN116535701B (en) * | 2023-07-03 | 2023-09-15 | 广东永鑫华新型材料有限公司 | Preparation method of glass fiber reinforced ABS composite material |
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