CN103214830A - Preparation method of high-strength and high-toughness polyamide/polyester alloy - Google Patents
Preparation method of high-strength and high-toughness polyamide/polyester alloy Download PDFInfo
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- CN103214830A CN103214830A CN2013101534641A CN201310153464A CN103214830A CN 103214830 A CN103214830 A CN 103214830A CN 2013101534641 A CN2013101534641 A CN 2013101534641A CN 201310153464 A CN201310153464 A CN 201310153464A CN 103214830 A CN103214830 A CN 103214830A
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Abstract
The invention discloses a preparation method of a high-strength and high-toughness polyamide/polyester alloy. The preparation method comprises the following steps of: processing PET (polyethylene Terephthalate) through sodium benzoate to obtain a high terminal carboxyl group PET; processing polyamide through polyolefin grafted maleic anhydride to obtain carboxyl-terminated polyamide; reacting a bifunctional epoxide with the terminal carboxyl group PET and the carboxyl-terminated polyamide to obtain a copolymer of the PET and the polyamide; and carrying out capacity increasing and chain extension on the PET and the polyamide, thus obtaining the high-strength and high-toughness polyamide/polyester alloy. According to the preparation method of the high-strength and high-toughness polyamide/polyester alloy, the polyolefin grafted maleic anhydride is adopted, an anhydride group and the terminal amino group are reacted and grafted at a molten state, and the resulting product which is the terminal carboxyl group has high output, and the toughness of the product is greatly improved due to an introduced graft; the bifunctional epoxide is adopted, thus the copolymer material gains high toughness of modified polyamide, and also gains the mechanical strength which is increased along with the raise of molecular weight; and the preparation method has the advantages that the adopted raw components are wide in resource and low in price, and the industrialization is easily realized accordingly.
Description
Technical field
The present invention relates to a kind of preparation method of high-intensity high-tenacity polyamide/polyester alloy, belong to technical field of polymer materials.
Background technology
Polymeric amide PA6 and polyester PET have tangible relative merits separately as the important engineering plastics.PA6 is because height regularity, high crystalline and the good comprehensive mechanical property of its structure, and is widely used in machinery, automobile and other industries.But shortcoming such as there is poor dimensional stability, high-hydroscopicity, cost an arm and a leg.PET structure height symmetry, weathering resistance, dimensional stability better have good film-forming properties and cheap.But engineering plastics are higher because of its second-order transition temperature the most, and crystallization velocity is slow under common processing mould temperature, and shaping cycle is long, surface irregularity, easy deformation, the injection moulding plastic is fragility, be difficult to be applied to large-scale shortcomings such as mechanical part, limited its widespread use.
The report of probing into the PA6/PET matrix material in recent years is many, what wherein inquire into mostly is the film properties that is spun to of compound system, as document " preparation of PA6/PET hollow tangerine lobe type bicomponent spunbond ultra-fine fibre ", author Zhao Yixia etc. utilizes the tubular type drawing-off to prepare 16 lobe PA6/PET(40/60) hollow tangerine lobe type two-pack ultra-fine fibre goods, by to water content, DSC, drying process and melt-spinning technology analysis, the cross section structure that has shown PA6/PET tangerine lobe type two-pack ultra-fine fibre goods is subjected to the influence of melt pressure and spinning temperature.
Patent CN1749314A has reported a kind of preparation method of PA/PET high molecule alloy material, after PET, PA and SEBS vacuum-drying, mix in high-speed mixer, adding MDI chainextender, oxidation inhibitor (DPN/DLTP) continuation mixing drop into the twin screw extruder reaction and extrude after 10 minutes.Patent CN102850781A has reported that PET, nylon, oxidation inhibitor, fire retardant, lubricant are done mixed back the mixing with glass fibre in twin screw extruder in super mixer extrude the preparation matrix material.The impact property of patent CN1749314A interalloy has reached 60kJ/m2, and tensile strength is 56MPa, and flexural strength is 63 MPa, though improved impact property preferably, but tensile strength and flexural strength deficiency have limited its Application Areas, such as the engine case lid.The impact property of matrix material is 10kJ/m among the patent CN102850781A
2, flexural strength is 102MPa, tensile strength is 99 MPa, but impact property is lower, and owing to added glass, causes the material surface for preparing coarse and water absorbability is big, can not finely be applied to the precision optical machinery parts.This patent product material smooth surface and strength high toughness are big.
Summary of the invention
The object of the present invention is to provide a kind of preparation method with polyamide/polyester alloy of high tenacity high mechanical strength.
The preparation method of high-intensity high-tenacity polyamide/polyester alloy of the present invention comprises the steps:
1) PET and Sodium Benzoate are pressed mass ratio 100:1-3 input high-speed mixer, mix the back and extrude, must hold the PET of carboxyl by twin screw extruder;
2) polymeric amide and polyolefine grafted maleic anhydride are pressed mass ratio 100:5-20 input high-speed mixer, mix the back and extrude, must hold the polymeric amide of carboxyl by twin screw extruder;
3) will hold the PET of carboxyl, polymeric amide, bifunctional epoxy compound and the additive of end carboxyl to drop into the high-speed mixer mixing after twin screw extruder is extruded, get the high-intensity high-tenacity polyamide/polyester alloy by mass ratio 25-40:60-75:0.5-1:5-10.
The described PET limiting viscosity of step 1) is preferably 0.6 ~ 1.0dl/g.
The described extruder temperature of step 1) is 190 ℃ ~ 270 ℃, screw speed 200 ~ 400r/min.
Step 2) described polymeric amide is preferably PA6 or PA66 or PA1010.
Step 2) described polyolefine grafted maleic anhydride is preferably PP-g-MAH or PE-g-MAH or POE-g-MAH.
Step 2) described extruder temperature is 160 ℃ ~ 240 ℃, and screw speed is 200 ~ 400r/min.
The described bifunctional epoxy compound of step 3) is 1,4-butanediol diglycidyl ether or 1,6-hexanediol diglycidyl ether.
The described additive of step 3) is talcum powder or graphite or molybdenumdisulphide.
The described extruder temperature of step 3) is 160 ℃ ~ 270 ℃, and screw speed is 200 ~ 400r/min.
The present invention's innovative point and improvement effect compared with prior art is as follows: (1) the present invention uses Sodium Benzoate can improve the PET content of carboxyl end group, and can be used as the PET crystallization nucleating agent; (2) the present invention uses the polyolefine grafted maleic anhydride, under molten state, anhydride group improves both consistencies with the amino reactive grafting of end, the introducing of strong polar group, products therefrom content of carboxyl end group height, the grafts of introducing also improve the toughness of product greatly.(3) the present invention uses the bifunctional epoxy compound, polymeric amide and the polyester original position formation PET of end carboxyl and the multipolymer of polymeric amide with high tenacity end carboxyl, PET and polymeric amide are carried out increase-volume, and PET, polymeric amide carried out chain extension, molecular weight increases, form random long-chain copolymerization structure, make this copolymer material have the high toughness of modified polyamide simultaneously and follow molecular weight to increase and the physical strength that increases, simultaneously, used each the feed composition wide material sources low price of the present invention, be easy to industrialization.
Embodiment
Below in conjunction with specific embodiment flesh and blood of the present invention is further illustrated.If no special instructions, described umber is mass parts.
Embodiment 1
100 parts of PET and 1 part of Sodium Benzoate are put into 75 ℃ of high-speed mixers mix and drop into twin screw extruder behind the 5min and extrude, must hold the PET of carboxyl, extruder temperature is 190 ℃ ~ 270 ℃, screw speed 200 ~ 400r/min.100 parts of PA6,10 parts of PP-g-MAH are added high-speed mixers mix, mixture is dropped into the PA6 of the high tenacity end carboxyl that twin screw extruder extrudes, extruder temperature is 160 ℃ ~ 240 ℃, screw speed 200 ~ 400r/min.Get the PET, 0.5 part 1 of the PA6 of above-mentioned 60 parts of high tenacity end carboxyls and 40 parts of end carboxyls, 4-butanediol diglycidyl ether and 5 parts of graphite add the high 10min of mixing of 75 ℃ of heating of high-speed mixer, mixture is dropped into the twin screw extruder extruding pelletization, extruder temperature is 160 ℃ ~ 270 ℃, and screw speed is 200 ~ 400r/min.Tensile strength 81 MPa of gained polyamide/polyester alloy, flexural strength 101 MPa, simply supported beam notched Izod impact strength 25 kJ/m
2
Embodiment 2
100 parts of PET and 1 part of Sodium Benzoate are put into 75 ℃ of high-speed mixers mix and drop into twin screw extruder behind the 5min and extrude, must hold the PET of carboxyl, extruder temperature is 240 ~ 270 ℃, screw speed 200 ~ 400r/min.100 parts of PA6,5 parts of PP-g-MAH are added high-speed mixers mix, mixture is dropped into the PA6 of the high tenacity end carboxyl that twin screw extruder extrudes, extruder temperature is 160 ℃ ~ 240 ℃, and screw speed is 200 ~ 400r/min.Get the PET, 0.5 part 1 of the PA6 of above-mentioned 60 parts of high tenacity end carboxyls and 40 parts of end carboxyls, 6-hexanediol diglycidyl ether and 5 parts of talcum powder add the high 10min of mixing of 75 ℃ of heating of high-speed mixer, mixture is dropped into the twin screw extruder extruding pelletization, extruder temperature is 160 ℃ ~ 270 ℃, and screw speed is 200 ~ 400r/min.Tensile strength 85 MPa of gained polyamide/polyester alloy, flexural strength 108 MPa, simply supported beam notched Izod impact strength 31 kJ/m
2
Embodiment 3
100 parts of PET and 3 parts of Sodium Benzoates are put into 75 ℃ of high-speed mixers mix and drop into twin screw extruder behind the 5min and extrude, must hold the PET of carboxyl, extruder temperature is 240 ~ 270 ℃, screw speed 200 ~ 400r/min.100 parts of PA66,10 parts of PE-g-MAH are added high-speed mixers mix, with mixture drop into twin screw extruder extrude the PA66 of high tenacity end carboxyl, extruder temperature is 160 ℃ ~ 240 ℃, screw speed is 200 ~ 400r/min.Get the PET, 0.5 part 1 of above-mentioned 70 parts of modified Pa 6s 6 and 30 parts end carboxyls, 4-butanediol diglycidyl ether and 7.5 parts of talcum powder add the high 10min of mixing of 75 ℃ of heating of high-speed mixer, mixture is dropped into the twin screw extruder extruding pelletization, extruder temperature is 160 ℃ ~ 270 ℃, and screw speed is 200 ~ 400r/min.The tensile strength 80MPa of gained polyamide/polyester alloy, flexural strength 97 MPa, simply supported beam notched Izod impact strength 24 kJ/m
2
Embodiment 4
100 parts of PET and 1 part of Sodium Benzoate are put into 75 ℃ of high-speed mixers mix and drop into twin screw extruder behind the 5min and extrude, must hold the PET of carboxyl, extruder temperature is 240 ~ 270 ℃, screw speed 200 ~ 400r/min.100 parts of PA66,5 parts of PE-g-MAH are added high-speed mixers mix, mixture is dropped into the PA66 of the high tenacity end carboxyl that twin screw extruder extrudes, extruder temperature is 160 ℃ ~ 240 ℃, and screw speed is 200 ~ 400r/min.Get the PET, 0.5 part 1 of the PA66 of above-mentioned 60 parts of high tenacity end carboxyls and 40 parts of end carboxyls, 6-hexanediol diglycidyl ether and 5 parts of talcum powder add the high 10min of mixing of 75 ℃ of heating of high-speed mixer, mixture is dropped into the twin screw extruder extruding pelletization, extruder temperature is 160 ℃ ~ 270 ℃, and screw speed is 200 ~ 400r/min.Tensile strength 87 MPa of gained polyamide/polyester alloy, flexural strength 112 MPa, simply supported beam notched Izod impact strength 34 kJ/m
2
Embodiment 5
100 parts of PET and 1 part of Sodium Benzoate are put into 75 ℃ of high-speed mixers mix and drop into twin screw extruder behind the 5min and extrude, must hold the PET of carboxyl, extruder temperature is 240 ~ 270 ℃, screw speed 200 ~ 400r/min.100 parts of PA1010,10 parts of POE-g-MAH are added high-speed mixer and mix, mixture is dropped into the PA1010 that twin screw extruder gets high tenacity end carboxyl, extruder temperature is 160 ℃ ~ 240 ℃, and screw speed is 200 ~ 400r/min.Get the PET, 0.5 part 1 of the PA1010 of above-mentioned 75 parts of high tenacity end carboxyls and 25 parts of end carboxyls, 4-butanediol diglycidyl ether and 5 parts of molybdenumdisulphide add the high 10min of mixing of 75 ℃ of heating of high-speed mixer, mixture is dropped into the twin screw extruder extruding pelletization, extruder temperature is 160 ℃ ~ 270 ℃, and screw speed is 200 ~ 400r/min.The tensile strength 82MPa of gained polyamide/polyester alloy, flexural strength 93 MPa, simply supported beam notched Izod impact strength 40 kJ/m
2
Embodiment 6
100 parts of PET and 1 part of Sodium Benzoate are put into 75 ℃ of high-speed mixers mix and drop into twin screw extruder behind the 5min and extrude, must hold the PET of carboxyl, extruder temperature is 240 ~ 270 ℃, screw speed 200 ~ 400r/min.100 parts of PA1010,5 parts of POE-g-MAH are added high-speed mixer and mix, mixture is dropped into the PA1010 that twin screw extruder gets high tenacity end carboxyl, extruder temperature is 160 ℃ ~ 240 ℃, and screw speed is 200 ~ 400r/min.Get the PET, 0.5 part 1 of the PA1010 of above-mentioned 60 parts of high tenacity end carboxyls and 40 parts of end carboxyls, 6-hexanediol diglycidyl ether and 5 parts of molybdenumdisulphide add the high 10min of mixing of 75 ℃ of heating of high-speed mixer, mixture is dropped into the twin screw extruder extruding pelletization, extruder temperature is 160 ℃ ~ 270 ℃, and screw speed is 200 ~ 400r/min.Tensile strength 85 MPa of gained polyamide/polyester alloy, flexural strength 104 MPa, simply supported beam notched Izod impact strength 28 kJ/m
2
Embodiment 7
100 parts of PET and 1 part of Sodium Benzoate are put into 75 ℃ of high-speed mixers mix and drop into twin screw extruder behind the 5min and extrude, must hold the PET of carboxyl, extruder temperature is 240 ~ 270 ℃, screw speed 200 ~ 400r/min.100 parts of PA1010,20 parts of PE-g-MAH are added high-speed mixer and mix, mixture is dropped into the PA1010 that twin screw extruder gets high tenacity end carboxyl, extruder temperature is 160 ℃ ~ 240 ℃, and screw speed is 200 ~ 400r/min.Get the PET, 1 part 1 of the PA1010 of above-mentioned 60 parts of high tenacity end carboxyls and 40 parts of end carboxyls, 6-hexanediol diglycidyl ether and 10 parts of molybdenumdisulphide add the high 10min of mixing of 75 ℃ of heating of high-speed mixer, mixture is dropped into the twin screw extruder extruding pelletization, extruder temperature is 160 ℃ ~ 270 ℃, and screw speed is 200 ~ 400r/min.Tensile strength 83 MPa of gained polyamide/polyester alloy, flexural strength 97 MPa, simply supported beam notched Izod impact strength 38 kJ/m
2
Claims (9)
1. the preparation method of a high-intensity high-tenacity polyamide/polyester alloy is characterized in that, comprises the steps:
1) PET and Sodium Benzoate are pressed mass ratio 100:1-3 input high-speed mixer, mix the back and extrude, must hold the PET of carboxyl by twin screw extruder;
2) polymeric amide and polyolefine grafted maleic anhydride are pressed mass ratio 100:5-20 input high-speed mixer, mix the back and extrude, must hold the polymeric amide of carboxyl by twin screw extruder;
3) will hold the PET of carboxyl, polymeric amide, bifunctional epoxy compound and the additive of end carboxyl to drop into the high-speed mixer mixing after twin screw extruder is extruded, get the high-intensity high-tenacity polyamide/polyester alloy by mass ratio 25-40:60-75:0.5-1:5-10.
2. according to the preparation method of the described polyamide/polyester alloy of claim 1, it is characterized in that the described PET limiting viscosity of step 1) is 0.6 ~ 1.0dl/g.
3. according to the preparation method of the described polyamide/polyester alloy of claim 1, it is characterized in that the described extruder temperature of step 1) is 190 ℃ ~ 270 ℃, screw speed 200 ~ 400r/min.
4. according to the preparation method of the described polyamide/polyester alloy of claim 1, it is characterized in that step 2) described polymeric amide is PA6 or PA66 or PA1010.
5. according to the preparation method of the described polyamide/polyester alloy of claim 1, it is characterized in that step 2) described polyolefine grafted maleic anhydride is PP-g-MAH or PE-g-MAH or POE-g-MAH.
6. according to the preparation method of the described polyamide/polyester alloy of claim 1, it is characterized in that step 2) described extruder temperature is 160 ℃ ~ 240 ℃, screw speed is 200 ~ 400r/min.
7. according to the preparation method of the described polyamide/polyester alloy of claim 1, it is characterized in that the described bifunctional epoxy compound of step 3) is 1,4-butanediol diglycidyl ether or 1,6-hexanediol diglycidyl ether.
8. according to the preparation method of the described polyamide/polyester alloy of claim 1, it is characterized in that the described additive of step 3) is talcum powder or graphite or molybdenumdisulphide.
9. according to the preparation method of the described polyamide/polyester alloy of claim 1, it is characterized in that the described extruder temperature of step 3) is 160 ℃ ~ 270 ℃, screw speed is 200 ~ 400r/min.
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Cited By (5)
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| CN103740100A (en) * | 2014-01-14 | 2014-04-23 | 苏州三角洲新材料研发有限公司 | Nylon cable sheath material for polyester chain extender and preparation method thereof |
| CN105504801A (en) * | 2015-12-14 | 2016-04-20 | 中广核三角洲（江苏）塑化有限公司 | Nylon material with high strength and low shrinkage for 3D (three-dimensional) printing and preparation method of nylon material |
| CN106751806A (en) * | 2016-12-29 | 2017-05-31 | 上海普利特复合材料股份有限公司 | A kind of reactive compatibilizer prepares the alloy material for reclaiming carpet PA66 resins and recycled PET |
| CN108948688A (en) * | 2018-08-22 | 2018-12-07 | 中广核俊尔（上海）新材料有限公司 | A kind of fiber glass reinforced PBT/PET material |
| CN115181416A (en) * | 2022-07-15 | 2022-10-14 | 华润化学材料科技股份有限公司 | Polyamide engineering plastic and preparation method and application thereof |
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| CN106751806A (en) * | 2016-12-29 | 2017-05-31 | 上海普利特复合材料股份有限公司 | A kind of reactive compatibilizer prepares the alloy material for reclaiming carpet PA66 resins and recycled PET |
| CN108948688A (en) * | 2018-08-22 | 2018-12-07 | 中广核俊尔（上海）新材料有限公司 | A kind of fiber glass reinforced PBT/PET material |
| CN115181416A (en) * | 2022-07-15 | 2022-10-14 | 华润化学材料科技股份有限公司 | Polyamide engineering plastic and preparation method and application thereof |
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