CN103788589A - Glass fiber-reinforced polyethylene terephthalate composite material and preparation method thereof - Google Patents
Glass fiber-reinforced polyethylene terephthalate composite material and preparation method thereof Download PDFInfo
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- CN103788589A CN103788589A CN201210429867.XA CN201210429867A CN103788589A CN 103788589 A CN103788589 A CN 103788589A CN 201210429867 A CN201210429867 A CN 201210429867A CN 103788589 A CN103788589 A CN 103788589A
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Abstract
The invention relates to a glass fiber-reinforced polyethylene terephthalate composite material and a preparation method thereof. The composite material is prepared from the following components by weight: 100 parts of polyethylene terephthalate, 0.2-3.0 parts of nucleating agents, 0-1.0 part of coupling agents, 1.0-9.0 parts of crystallization promoters, 0.1-0.5 part of anti-oxidants, 0.2-0.6 part of liquid paraffin, and 10-40 parts of glass fibers. The glass fibers are treated by the coupling agent, and then the above raw materials are subjected to extrusion granulation in a screw extruder, and standard strip preparation in an injection molding machine to obtain the product. According to the invention, with the nucleating agent, the crystallization efficiency of polyethylene terephthalate is effectively increased, and the crystal grain size is enabled to be fine; with the glass fiber used as a reinforcing body and the addition of the coupling agent, the tensile strength, bending strength and impact strength of polyethylene terephthalate are improved greatly.
Description
Technical field
The invention belongs to technical field of polymer composite materials, especially relate to a kind of glass fiber reinforced polyethylene terephthalate matrix material and preparation method thereof.
Background technology
Along with the rapid growth of global economy, more and more higher to engineering plastics mechanical property requirements, in order to meet the demand of electronic apparatus and automobile market, conventionally take glass fibre as reinforcement, improve the mechanical property of engineering plastics.
Polyethylene terephthalate (PET) is one of five large general engineering plastic, there is excellent mechanical property, thermotolerance, electrical insulating property, chemical reagent resistance, and more cheap than other engineering plastics, application market is extensive, and development prospect is good.Therefore, PET engineering plastics price has competitive power compared with other general-purpose plastics.And the mechanical property of glass fibre REINFORCED PET engineering plastics is very outstanding, after adding glass fibre, the growth maximum of PET mechanical property.But for a long time, because PET self molecular chain structure rigidity is larger, second-order transition temperature high (70～90 ℃), fusing point is 260 ℃ of left and right, crystallization range is quite large, crystallization at normal temperatures when injection, because freeze at 70 ℃ of left and right PET segments, cause in actual production process crystallization rate too slow, degree of crystallinity is very low, die temperature up to 90～130 ℃ between, shaping cycle is long etc., and problem has proposed very high request to actual processing condition and equipment, serious has influence on its development in engineering plastics field.The root problem of accelerating PET through engineering approaches progress is how to improve PET crystallization rate, and most popular method is also that basic solution is to add nucleator in PET resin matrix at present.
In addition, in matrix material, to be combined with the interface of corpus fibrosum be the important factor that affects material property to matrix, and the use of coupling agent can obviously strengthen matrix is combined with the interface of corpus fibrosum, can improve well the impact property of matrix material.
Summary of the invention
Object of the present invention is exactly to provide a kind of fiberglass reinforced polyethyleneterephthalate matrix material and preparation method thereof in order to overcome the defect that above-mentioned prior art exists.
The present invention by adding nucleator and crystallization promoter in matrix material, improve the crystallization velocity of polyethylene terephthalate and impel fine grain size, select glass fibre as reinforcement, add coupling agent simultaneously, can improve significantly tensile strength, flexural strength and the shock strength of polyethylene terephthalate.
Object of the present invention can be achieved through the following technical solutions:
Glass fiber reinforced polyethylene terephthalate matrix material, made by the component that comprises following weight part:
The limiting viscosity of described polyethylene terephthalate is 0.8～1.0dl/g.
Described nucleator is selected from one or more in talcum powder, Magnesium Stearate, Sodium Benzoate or Surlyn8920.
Described coupling agent is selected from the one in 3-aminopropyl triethoxysilane, 3-glycidyl ether oxygen propyl trimethoxy silicane or 3-(iso-butylene acyl-oxygen) propyl trimethoxy silicane.
Described crystallization promoter is selected from one or more in polycaprolactone, polyoxyethylene glycol or polypropylene glycol.
Described oxidation inhibitor is selected from four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, three [2,4-di-tert-butyl-phenyl] one or more in phosphorous acid ester or the positive octadecanol ester of β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid.
The diameter of described glass fibre is 5～25 μ m.
The preparation method of glass fiber reinforced polyethylene terephthalate matrix material, comprises the following steps:
(1) content mixes the polyethylene terephthalate of 100 parts of dryings, 0.2～3.0 portion of nucleator, 1.0～9.0 parts of crystallization promoters, 0.1～0.5 part of oxidation inhibitor, 0.2～0.6 part of whiteruss in mixing machine by weight;
(2) coupling agent is dissolved in dehydrated alcohol, is mixed with coupling agent-ethanolic soln, utilize spray method by spray solution on glass fibre, and the glass fibre that is sprayed with coupling agent solution is dry in baking oven;
(3) by compound in step (1) through upstream spout, send into twin screw extruder, simultaneously by 10～40 parts of glass fibre in step (2) through downstream spout, send into that twin screw extruder melt extrudes, granulation;
(4) by above-mentioned pellet process injection moulding machine preparation standard batten, obtain product.
The drying conditions of the polyethylene terephthalate described in step (1) is: dry 8～16h in 100～120 ℃ of baking ovens; The mixing machine adopting is high-speed mixer, and mixing time is 3～7min.
The concentration of the coupling agent-ethanolic soln described in step (2) is 0.5～2.0wt%, and the glass fibre drying conditions that is sprayed with coupling agent solution is: dry 30～90min in the baking oven of 80～120 ℃.
In twin screw extruder described in step (3), melt extruding temperature is 245～270 ℃.
The temperature of described step (4) injection moulding machine preparation standard batten is 250～270 ℃.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) in matrix material, add nucleator and crystallization promoter simultaneously, add nucleator or promotor than single, improve better crystallization velocity, crystalline size and the crystallization time of polyethylene terephthalate, thereby improve the mechanical property of polyethylene terephthalate.
(2), preparing in polyethylene terephthalate matrix material, by the use of arranging in pairs or groups of different nucleators, can greatly improve the crystal property of polyethylene terephthalate.
(3) in the present invention, also use glass fibre as reinforcement, tensile strength, the flexural strength of polyethylene terephthalate improve a lot, and shock strength also has certain increase.
(4) in the present invention, selected coupling agent to fiberglass surfacing processing, the use of coupling agent can obviously strengthen matrix is combined with the interface of corpus fibrosum, can improve well the impact property of matrix material.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
In following examples, the tensile property of products obtained therefrom is according to standard A STM-D638 test, and bending property is according to standard A STM-D790 test, and notch shock performance is tested according to standard A STM-D256.
Surlyn8920 in following examples is purchased from du pont company.
In following examples, whiteruss is commercially available.
Embodiment 1
(1) first PET (limiting viscosity is 0.9dl/g) dry 16h in the baking oven of 100 ℃, get 100 parts of dry PET, the nucleator talcum powder of 0.2 part, the crystallization promoter polycaprolactone of 1.0 parts, 0.1 part of antioxidant 1010, the whiteruss of 0.2 part, in high-speed mixer, mix 3min;
(2) the coupling agent 3-aminopropyl triethoxysilane (KH550) of 0.05 part is dissolved in dehydrated alcohol, be mixed with concentration and be coupling agent-ethanolic soln of 0.5%, utilize spray method by spray solution on glass fibre, and will be sprayed with glass fibre dry 30min in 120 ℃ of baking ovens of coupling agent solution;
(3) by compound in above-mentioned (1) through upstream spout, send into twin screw extruder, by 10 parts of glass fibre in above-mentioned (2), (diameter is that 15 μ are m) through downstream spout simultaneously, send into that twin screw extruder melt extrudes, granulation, each section of temperature of forcing machine is: 245 ℃, a district, two 255 ℃, districts, three 260 ℃, districts, four 265 ℃, districts, five 270 ℃, districts, head temperature is 260 ℃;
(4) by above-mentioned pellet process injection moulding machine preparation standard batten, survey its performance, refer to table 1, wherein each section of temperature of injection moulding machine is: 270 ℃ of first paragraphs, 265 ℃, the 3rd section 250 ℃ of second segments.
Embodiment 2
(1), first by PET (limiting viscosity is 0.9dl/g) dry 12h in the baking oven of 110 ℃, get 100 parts of dry PET, the nucleator Magnesium Stearate of 0.6 part, the crystallization promoter polyoxyethylene glycol of 3.0 parts, the irgasfos 168 of 0.2 part, the whiteruss of 0.3 part and in high-speed mixer, mix 4min;
(2) the coupling agent 3-glycidyl ether oxygen propyl trimethoxy silicane (KH560) of 0.1 part is dissolved in dehydrated alcohol, be mixed with concentration and be coupling agent-ethanolic soln of 1.0%, utilize spray method by spray solution on glass fibre, and will be sprayed with glass fibre dry 45min in 110 ℃ of baking ovens of coupling agent solution;
(3) by compound in above-mentioned (1) through upstream spout, send into twin screw extruder, by 20 parts of glass fibre in above-mentioned (2), (diameter is that 15 μ are m) through downstream spout simultaneously, send into that twin screw extruder melt extrudes, granulation, each section of temperature of forcing machine is: 245 ℃, a district, two 255 ℃, districts, three 260 ℃, districts, four 265 ℃, districts, five 270 ℃, districts, head temperature is 260 ℃
(4) by above-mentioned pellet process injection moulding machine preparation standard batten, survey its performance, refer to table 1, wherein each section of temperature of injection moulding machine is: 270 ℃ of first paragraphs, 265 ℃, the 3rd section 250 ℃ of second segments.
Embodiment 3
(1) first by PET (limiting viscosity is 0.9dl/g) dry 8h in the baking oven of 120 ℃, get 100 parts of dry PET, the nucleator of 1.0 parts, wherein Sodium Benzoate and Surlyn 8920 weight part ratios are 1: 1, the crystallization promoter polypropylene glycol of 4.2 parts, the oxidation inhibitor of 0.3 part, the whiteruss that wherein antioxidant 1010 is 1: 1,0.4 part with irgasfos 168 weight part ratio mixes 5min in high-speed mixer;
(2) the coupling agent 3-of 0.125 part (iso-butylene acyl-oxygen) propyl trimethoxy silicane (KH570) is dissolved in dehydrated alcohol, be mixed with concentration and be coupling agent-ethanolic soln of 1.25%, utilize spray method by spray solution on glass fibre, and will be sprayed with glass fibre dry 60min in 100 ℃ of baking ovens of coupling agent solution;
(3) by compound in above-mentioned (1) through upstream spout, send into twin screw extruder, by 25 parts of glass fibre in above-mentioned (2), (diameter is that 15 μ m) send into through downstream spout that twin screw extruder melt extrudes, granulation simultaneously, each section of temperature of forcing machine is: 245 ℃, a district, two 255 ℃, districts, three 260 ℃, districts, four 265 ℃, districts, five 270 ℃, districts, head temperature is 260 ℃
(4) by above-mentioned pellet process injection moulding machine preparation standard batten, survey its performance, refer to table 1, wherein each section of temperature of injection moulding machine is: 270 ℃ of first paragraphs, 265 ℃, the 3rd section 250 ℃ of second segments.
Embodiment 4
(1) first by PET (limiting viscosity is 0.9dl/g) dry 8h in the baking oven of 120 ℃, get 100 parts of dry PET, the nucleator of 1.4 parts, wherein Magnesium Stearate and Sodium Benzoate weight part ratio are the crystallization promoter of 1: 1,5.0 parts, it is that polypropylene glycol and polyoxyethylene glycol weight part ratio are the oxidation inhibitor of 1: 1,0.4 part, and the whiteruss that wherein antioxidant 1010 is 1: 1,0.4 part with irgasfos 168 weight part ratio mixes 6min in high-speed mixer;
(2) the coupling agent 3-glycidyl ether oxygen propyl trimethoxy silicane (KH560) of 0.15 part is dissolved in dehydrated alcohol, be mixed with concentration and be coupling agent-ethanolic soln of 1.75%, utilize spray method by spray solution on glass fibre, and will be sprayed with glass fibre dry 75min in 90 ℃ of baking ovens of coupling agent solution;
(3) by compound in above-mentioned (1) through upstream spout, send into twin screw extruder, by 30 parts of glass fibre in above-mentioned (2), (diameter is that 15 μ are m) through downstream spout simultaneously, send into that twin screw extruder melt extrudes, granulation, each section of temperature of forcing machine is: 245 ℃, a district, two 255 ℃, districts, three 260 ℃, districts, four 265 ℃, districts, five 270 ℃, districts, head temperature is 260 ℃
(4) by above-mentioned pellet process injection moulding machine preparation standard batten, survey its performance, refer to table 1, wherein each section of temperature of injection moulding machine is: 270 ℃ of first paragraphs, 265 ℃, the 3rd section 250 ℃ of second segments.
Embodiment 5
(1) first by PET (limiting viscosity is 0.9dl/g) dry 8h in the baking oven of 120 ℃, get 100 parts of dry PET, the nucleator of 2.0 parts, wherein Magnesium Stearate and Surlyn 8920 weight part ratios are the crystallization promoter of 1: 1,7.0 parts, wherein polypropylene glycol and polyoxyethylene glycol weight part ratio are the oxidation inhibitor of 1: 1,0.4 part, and the whiteruss that wherein antioxidant 1010 is 1: 1,0.5 part with irgasfos 168 weight part ratio mixes 7min in high-speed mixer;
(2) the coupling agent 3-aminopropyl triethoxysilane (KH550) of 0.175 part is dissolved in dehydrated alcohol, be mixed with concentration and be coupling agent-ethanolic soln of 2.0%, utilize spray method by spray solution on glass fibre, and will be sprayed with glass fibre dry 90min in 80 ℃ of baking ovens of coupling agent solution;
(3) by compound in above-mentioned (1) through upstream spout, send into twin screw extruder, by 35 parts of glass fibre in above-mentioned (2), (diameter is that 15 μ m) send into through downstream spout that twin screw extruder melt extrudes, granulation simultaneously, each section of temperature of forcing machine is: 245 ℃, a district, two 255 ℃, districts, three 260 ℃, districts, four 265 ℃, districts, five 270 ℃, districts, head temperature is 260 ℃
(4) by above-mentioned pellet process injection moulding machine preparation standard batten, survey its performance, refer to table 1, wherein each section of temperature of injection moulding machine is: 270 ℃ of first paragraphs, 265 ℃, the 3rd section 250 ℃ of second segments.
Embodiment 6
(1) first by PET (limiting viscosity is 0.9dl/g) dry 8h in the baking oven of 120 ℃, get 100 parts of dry PET, the crystallization promoter of 8920,9.0 parts of nucleator Surlyn of 3.0 parts, wherein polypropylene glycol and polyoxyethylene glycol weight part ratio are that 1: 1,0.5 part antioxidant 1076, the whiteruss of 0.6 part mix 7min in high-speed mixer;
(2) the coupling agent 3-of 0.2 part (iso-butylene acyl-oxygen) propyl trimethoxy silicane (KH570) is dissolved in dehydrated alcohol, be mixed with concentration and be coupling agent-ethanolic soln of 2.0%, utilize spray method by spray solution on glass fibre, and will be sprayed with glass fibre dry 90min in 80 ℃ of baking ovens of coupling agent solution;
(3) by compound in above-mentioned (1) through upstream spout, send into twin screw extruder, by 40 parts of glass fibre in above-mentioned (2), (diameter is that 15 μ are m) through downstream spout simultaneously, send into that twin screw extruder melt extrudes, granulation, each section of temperature of forcing machine is: 245 ℃, a district, two 255 ℃, districts, three 260 ℃, districts, four 265 ℃, districts, five 270 ℃, districts, head temperature is 260 ℃;
(4) by above-mentioned pellet process injection moulding machine preparation standard batten, survey its performance, refer to table 1, wherein each section of temperature of injection moulding machine is: 270 ℃ of first paragraphs, 265 ℃, the 3rd section 250 ℃ of second segments.
Embodiment 7
(1) first by PET (limiting viscosity is 0.9dl/g) dry 8h in the baking oven of 120 ℃, get 100 parts of dry PET, the nucleator of 2.0 parts, wherein Magnesium Stearate and Surlyn 8920 weight part ratios are the crystallization promoter of 1: 1,7.0 parts, wherein polypropylene glycol and polyoxyethylene glycol weight part ratio are the oxidation inhibitor of 1: 1,0.4 part, and the whiteruss that wherein antioxidant 1010 is 1: 1,0.5 part with irgasfos 168 weight part ratio mixes 7min in high-speed mixer;
(2) without coupling agent, directly by above-mentioned compound through upstream spout, send into twin screw extruder, by the glass fibre of 35 parts, (diameter is that 15 μ m) send into through downstream spout that twin screw extruder melt extrudes, granulation, and each section of temperature of forcing machine is: 245 ℃, a district, two 255 ℃, districts simultaneously, three 260 ℃, districts, four 265 ℃, districts, five 270 ℃, districts, head temperature is 260 ℃;
(3) by above-mentioned pellet process injection moulding machine preparation standard batten, survey its performance, refer to table 1, wherein each section of temperature of injection moulding machine is: 270 ℃ of first paragraphs, 265 ℃, the 3rd section 250 ℃ of second segments.
Embodiment 8
(1) first by PET (limiting viscosity is 0.9dl/g) dry 8h in the baking oven of 120 ℃, get 100 parts of dry PET, the nucleator of 2.0 parts, wherein Magnesium Stearate and Surlyn 8920 weight part ratios are the crystallization promoter of 1: 1,7.0 parts, wherein polypropylene glycol and polyoxyethylene glycol weight part ratio are the oxidation inhibitor of 1: 1,0.4 part, and the whiteruss that wherein antioxidant 1010 is 1: 1,0.5 part with irgasfos 168 weight part ratio mixes 7min in high-speed mixer;
(2) the coupling agent 3-aminopropyl triethoxysilane (KH550) of 0.035 part is dissolved in dehydrated alcohol, be mixed with concentration and be coupling agent-ethanolic soln of 0.5%, utilize spray method by spray solution on glass fibre, and will be sprayed with glass fibre dry 30min in 120 ℃ of baking ovens of coupling agent solution;
(3) by compound in above-mentioned (1) through upstream spout, send into twin screw extruder, by 35 parts of glass fibre in above-mentioned (2), (diameter is that 15 μ m) send into through downstream spout that twin screw extruder melt extrudes, granulation simultaneously, each section of temperature of forcing machine is: 245 ℃, a district, two 255 ℃, districts, three 260 ℃, districts, four 265 ℃, districts, five 270 ℃, districts, head temperature is 260 ℃;
(4) by above-mentioned pellet process injection moulding machine preparation standard batten, survey its performance, refer to table 1, wherein each section of temperature of injection moulding machine is: 270 ℃ of first paragraphs, 265 ℃, the 3rd section 250 ℃ of second segments.
Embodiment 9
(1) first by PET (limiting viscosity is 0.9dl/g) dry 8h in the baking oven of 120 ℃, get 100 parts of dry PET, the nucleator of 2.0 parts, wherein Magnesium Stearate and Surlyn 8920 weight part ratios are the crystallization promoter of 1: 1,7.0 parts, wherein polypropylene glycol and polyoxyethylene glycol weight part ratio are the oxidation inhibitor of 1: 1,0.4 part, and the whiteruss that wherein antioxidant 1010 is 1: 1,0.5 part with irgasfos 168 weight part ratio mixes 7min in high-speed mixer;
(2) the coupling agent 3-aminopropyl triethoxysilane (KH550) of 0.35 part is dissolved in dehydrated alcohol, be mixed with concentration and be coupling agent-ethanolic soln of 2.0%, utilize spray method by spray solution on glass fibre, and will be sprayed with glass fibre dry 45min in 110 ℃ of baking ovens of coupling agent solution;
(3) by compound in above-mentioned (1) through upstream spout, send into twin screw extruder, by 35 parts of glass fibre in above-mentioned (2), (diameter is that 15 μ m) send into through downstream spout that twin screw extruder melt extrudes, granulation simultaneously, each section of temperature of forcing machine is: 245 ℃, a district, two 255 ℃, districts, three 260 ℃, districts, four 265 ℃, districts, five 270 ℃, districts, head temperature is 260 ℃
(4) by above-mentioned pellet process injection moulding machine preparation standard batten, survey its performance, refer to table 1, wherein each section of temperature of injection moulding machine is: 270 ℃ of first paragraphs, 265 ℃, the 3rd section 250 ℃ of second segments.
Embodiment 10
(1) first by PET (limiting viscosity is 0.9dl/g) dry 8h in the baking oven of 120 ℃, get 100 parts of dry PET, the nucleator of 2.0 parts, wherein Magnesium Stearate and Surlyn 8920 weight part ratios are the crystallization promoter of 1: 1,7.0 parts, wherein polypropylene glycol and polyoxyethylene glycol weight part ratio are the oxidation inhibitor of 1: 1,0.4 part, and the whiteruss that wherein antioxidant 1010 is 1: 1,0.5 part with irgasfos 168 weight part ratio mixes 7min in high-speed mixer;
(2) the coupling agent 3-aminopropyl triethoxysilane (KH550) of 0.5 part is dissolved in dehydrated alcohol, be mixed with concentration and be coupling agent-ethanolic soln of 2.0%, utilize spray method by spray solution on glass fibre, and will be sprayed with glass fibre dry 60min in 100 ℃ of baking ovens of coupling agent solution;
(3) by compound in above-mentioned (1) through upstream spout, send into twin screw extruder, by 35 parts of glass fibre in above-mentioned (2), (diameter is that 15 μ m) send into through downstream spout that twin screw extruder melt extrudes, granulation simultaneously, each section of temperature of forcing machine is: 245 ℃, a district, two 255 ℃, districts, three 260 ℃, districts, four 265 ℃, districts, five 270 ℃, districts, head temperature is 260 ℃;
(4) by above-mentioned pellet process injection moulding machine preparation standard batten, survey its performance, refer to table 1, wherein each section of temperature of injection moulding machine is: 270 ℃ of first paragraphs, 265 ℃, the 3rd section 250 ℃ of second segments.
Embodiment 11
(1) first by PET (limiting viscosity is 0.9dl/g) dry 8h in the baking oven of 120 ℃, get 100 parts of dry PET, the nucleator of 2.0 parts, wherein Magnesium Stearate and Surlyn 8920 weight part ratios are the crystallization promoter of 1: 1,7.0 parts, wherein polypropylene glycol and polyoxyethylene glycol weight part ratio are the oxidation inhibitor of 1: 1,0.4 part, and the whiteruss that wherein antioxidant 1010 is 1: 1,0.5 part with irgasfos 168 weight part ratio mixes 7min in high-speed mixer;
(2) the coupling agent 3-aminopropyl triethoxysilane (KH550) of 0.8 part is dissolved in dehydrated alcohol, be mixed with concentration and be coupling agent-ethanolic soln of 2.0%, utilize spray method by spray solution on glass fibre, and will be sprayed with glass fibre dry 60min in 100 ℃ of baking ovens of coupling agent solution;
(3) by compound in above-mentioned (1) through upstream spout, send into twin screw extruder, by 35 parts of glass fibre in above-mentioned (2), (diameter is that 15 μ m) send into through downstream spout that twin screw extruder melt extrudes, granulation simultaneously, each section of temperature of forcing machine is: 245 ℃, a district, two 255 ℃, districts, three 260 ℃, districts, four 265 ℃, districts, five 270 ℃, districts, head temperature is 260 ℃;
(4) by above-mentioned pellet process injection moulding machine preparation standard batten, survey its performance, refer to table 1, wherein each section of temperature of injection moulding machine is: 270 ℃ of first paragraphs, 265 ℃, the 3rd section 250 ℃ of second segments.
Embodiment 12
(1) first by PET (limiting viscosity is 0.9dl/g) dry 8h in the baking oven of 120 ℃, get 100 parts of dry PET, the nucleator of 2.0 parts, wherein Magnesium Stearate and Surlyn 8920 weight part ratios are the crystallization promoter of 1: 1,7.0 parts, wherein polypropylene glycol and polyoxyethylene glycol weight part ratio are the oxidation inhibitor of 1: 1,0.4 part, and the whiteruss that wherein antioxidant 1010 is 1: 1,0.5 part with irgasfos 168 weight part ratio mixes 7min in high-speed mixer;
(2) the coupling agent 3-aminopropyl triethoxysilane (KH550) of 1.0 parts is dissolved in dehydrated alcohol, be mixed with concentration and be coupling agent-ethanolic soln of 2.0%, utilize spray method by spray solution on glass fibre, and will be sprayed with glass fibre dry 60min in 100 ℃ of baking ovens of coupling agent solution;
(3) by compound in above-mentioned (1) through upstream spout, send into twin screw extruder, by 35 parts of glass fibre in above-mentioned (2), (diameter is that 15 μ m) send into through downstream spout that twin screw extruder melt extrudes, granulation simultaneously, each section of temperature of forcing machine is: 245 ℃, a district, two 255 ℃, districts, three 260 ℃, districts, four 265 ℃, districts, five 270 ℃, districts, head temperature is 260 ℃
(4) by above-mentioned pellet process injection moulding machine preparation standard batten, survey its performance, refer to table 1, wherein each section of temperature of injection moulding machine is: 270 ℃ of first paragraphs, 265 ℃, the 3rd section 250 ℃ of second segments.
Embodiment 13
(1) first by PET (limiting viscosity is 0.8dl/g) dry 8h in the baking oven of 120 ℃, get 100 parts of dry PET, the nucleator of 2.0 parts, wherein Magnesium Stearate and Surlyn 8920 weight part ratios are the crystallization promoter of 1: 1,7.0 parts, wherein polypropylene glycol and polyoxyethylene glycol weight part ratio are the oxidation inhibitor of 1: 1,0.4 part, and the whiteruss that wherein antioxidant 1010 is 1: 1,0.5 part with irgasfos 168 weight part ratio mixes 7min in high-speed mixer;
(2) the coupling agent 3-aminopropyl triethoxysilane (KH550) of 0.175 part is dissolved in dehydrated alcohol, be mixed with concentration and be coupling agent-ethanolic soln of 2.0%, utilize spray method by spray solution on glass fibre, and will be sprayed with glass fibre dry 90min in 80 ℃ of baking ovens of coupling agent solution;
(3) by compound in above-mentioned (1) through upstream spout, send into twin screw extruder, by 35 parts of glass fibre in above-mentioned (2), (diameter is that 5 μ m) send into through downstream spout that twin screw extruder melt extrudes, granulation simultaneously, each section of temperature of forcing machine is: 245 ℃, a district, two 255 ℃, districts, three 260 ℃, districts, four 265 ℃, districts, five 270 ℃, districts, head temperature is 260 ℃;
(4) by above-mentioned pellet process injection moulding machine preparation standard batten, survey its performance, refer to table 1, wherein each section of temperature of injection moulding machine is: 270 ℃ of first paragraphs, 265 ℃, the 3rd section 250 ℃ of second segments.
Embodiment 14
(1) first by PET (limiting viscosity is 1.0dl/g) dry 8h in the baking oven of 120 ℃, get 100 parts of dry PET, the nucleator of 2.0 parts, wherein Magnesium Stearate and Surlyn 8920 weight part ratios are the crystallization promoter of 1: 1,7.0 parts, wherein polypropylene glycol and polyoxyethylene glycol weight part ratio are the oxidation inhibitor of 1: 1,0.4 part, and the whiteruss that wherein antioxidant 1010 is 1: 1,0.5 part with irgasfos 168 weight part ratio mixes 7min in high-speed mixer;
(2) the coupling agent 3-aminopropyl triethoxysilane (KH550) of 0.175 part is dissolved in dehydrated alcohol, be mixed with concentration and be coupling agent-ethanolic soln of 2.0%, utilize spray method by spray solution on glass fibre, and will be sprayed with glass fibre dry 90min in 80 ℃ of baking ovens of coupling agent solution;
(3) by compound in above-mentioned (1) through upstream spout, send into twin screw extruder, by 35 parts of glass fibre in above-mentioned (2), (diameter is that 25 μ m) send into through downstream spout that twin screw extruder melt extrudes, granulation simultaneously, each section of temperature of forcing machine is: 245 ℃, a district, two 255 ℃, districts, three 260 ℃, districts, four 265 ℃, districts, five 270 ℃, districts, head temperature is 260 ℃;
(4) by above-mentioned pellet process injection moulding machine preparation standard batten, survey its performance, refer to table 1, wherein each section of temperature of injection moulding machine is: 270 ℃ of first paragraphs, 265 ℃, the 3rd section 250 ℃ of second segments.
Comparative example 1
(1) first by PET (limiting viscosity is 0.9dl/g) dry 8h in the baking oven of 120 ℃, get 100 parts of dry PET, the oxidation inhibitor of 0.3 part, the whiteruss that wherein antioxidant 1010 is 1: 1,0.4 part with irgasfos 168 weight part ratio mixes 5min in high-speed mixer;
(2) by above-mentioned compound through upstream spout, send into twin screw extruder, by the glass fibre of 35 parts, (diameter is that 15 μ are m) through downstream spout simultaneously, send into that twin screw extruder melt extrudes, granulation, each section of temperature of forcing machine is: 245 ℃, a district, two 255 ℃, districts, three 260 ℃, districts, four 265 ℃, districts, five 270 ℃, districts, head temperature is 260 ℃;
(3) by above-mentioned pellet process injection moulding machine preparation standard batten, survey its performance, refer to table 1, wherein each section of temperature of injection moulding machine is: 270 ℃ of first paragraphs, 265 ℃, the 3rd section 250 ℃ of second segments.
Comparative example 2
(1) first by PET (limiting viscosity is 0.9dl/g) dry 8h in the baking oven of 120 ℃, get 100 parts of dry PET, the oxidation inhibitor of 0.3 part, the whiteruss that wherein antioxidant 1010 is 1: 1,0.4 part with irgasfos 168 weight part ratio mixes 5min in high-speed mixer;
(2) by above-mentioned compound through upstream spout, send into twin screw extruder, each section of temperature of forcing machine is: 245 ℃, a district, two 255 ℃, districts, three 260 ℃, districts, four 265 ℃, districts, five 270 ℃, districts, head temperature is 260 ℃;
(3) by above-mentioned pellet process injection moulding machine preparation standard batten, survey its performance, refer to table 1, wherein each section of temperature of injection moulding machine is: 270 ℃ of first paragraphs, 265 ℃, the 3rd section 250 ℃ of second segments.
Table 1 glass fiber reinforced polyethylene terephthalate composite property
From table 1, embodiment 1～14 and comparative example 1,2 can be found out, in polyethylene terephthalate matrix material, add glass fibre, nucleator, coupling agent and promotor, can improve to a great extent tensile strength, flexural strength and the shock strength of polyethylene terephthalate.
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.Person skilled in the art obviously can, easily to these embodiment, make various modifications, and General Principle described herein is applied in other embodiment and needn't passes through performing creative labour.Therefore, the invention is not restricted to the embodiment here, those skilled in the art are according to announcement of the present invention, and not departing from the improvement that category of the present invention makes and revise all should be within protection scope of the present invention.
Claims (10)
1. glass fiber reinforced polyethylene terephthalate matrix material, is characterized in that, this matrix material is made up of the component that comprises following weight part:
2. matrix material according to claim 1, is characterized in that, the limiting viscosity of described polyethylene terephthalate is 0.8～1.0dlg.
3. matrix material according to claim 1, is characterized in that, described nucleator is selected from one or more in talcum powder, Magnesium Stearate, Sodium Benzoate or Surlyn8920.
4. matrix material according to claim 1, it is characterized in that, described coupling agent is selected from the one in 3-aminopropyl triethoxysilane, 3-glycidyl ether oxygen propyl trimethoxy silicane or 3-(iso-butylene acyl-oxygen) propyl trimethoxy silicane.
5. matrix material according to claim 1, is characterized in that, described crystallization promoter is selected from one or more in polycaprolactone, polyoxyethylene glycol or polypropylene glycol.
6. matrix material according to claim 1, it is characterized in that, described oxidation inhibitor is selected from four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, three [2,4-di-tert-butyl-phenyl] one or more in phosphorous acid ester or the positive octadecanol ester of β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid.
7. matrix material according to claim 1, is characterized in that, the diameter of described glass fibre is 5～25 μ m.
8. according to the preparation method of the arbitrary described glass fiber reinforced polyethylene terephthalate matrix material of claim 1～7, it is characterized in that, the method comprises the following steps:
(1) content mixes the polyethylene terephthalate of 100 parts of dryings, 0.2～3.0 portion of nucleator, 1.0～9.0 parts of crystallization promoters, 0.1～0.5 part of oxidation inhibitor, 0.2～0.6 part of whiteruss in mixing machine by weight;
(2) coupling agent is dissolved in dehydrated alcohol, is mixed with coupling agent-ethanolic soln, utilize spray method by spray solution on glass fibre, and the glass fibre that is sprayed with coupling agent solution is dry in baking oven;
(3) by compound in step (1) through upstream spout, send into twin screw extruder, simultaneously by 10～40 parts of glass fibre in step (2) through downstream spout, send into that twin screw extruder melt extrudes, granulation;
(4) by above-mentioned pellet process injection moulding machine preparation standard batten, obtain product.
9. the preparation method of matrix material according to claim 8, is characterized in that,
The drying conditions of the polyethylene terephthalate described in step (1) is: dry 8～16h in 100～120 ℃ of baking ovens, and the mixing machine of employing is high-speed mixer, mixing time is 3～7min;
The concentration of the coupling agent-ethanolic soln described in step (2) is 0.5～2.0wt%, and the glass fibre drying conditions that is sprayed with coupling agent solution is: dry 30～90min in the baking oven of 80～120 ℃.
10. the preparation method of matrix material according to claim 8, is characterized in that,
In twin screw extruder described in step (3), melt extruding temperature is 245～270 ℃
In step (4), the temperature of injection moulding machine preparation standard batten is 250～270 ℃.
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