CN101781455A - Super-tough nylon alloy and preparation method thereof - Google Patents
Super-tough nylon alloy and preparation method thereof Download PDFInfo
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- CN101781455A CN101781455A CN201010139598A CN201010139598A CN101781455A CN 101781455 A CN101781455 A CN 101781455A CN 201010139598 A CN201010139598 A CN 201010139598A CN 201010139598 A CN201010139598 A CN 201010139598A CN 101781455 A CN101781455 A CN 101781455A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
- B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/04—Particle-shaped
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/9258—Velocity
- B29C2948/9259—Angular velocity
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
- B29C2948/92885—Screw or gear
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
- B29C2948/92895—Barrel or housing
Abstract
The invention discloses a super-tough nylon alloy, which is characterized by comprising raw material by weight percent: 65-90% of nylon, 10-35% of itaconic acid grafting ethylene-alpha-octylene copolymer (POE-g-ITA), 0.1-1% of antioxygen, 0.2-1% of lubricating agent, TAF. A method for preparing the super-tough nylon alloy is characterized by comprising the following steps: placing all raw material into a high mixer and mixing the raw materials for 5-10min; then placing the mixed raw materials into a double screw extrusion machine for extrusion and pelleting; carrying out traction, cooling and grain-sized dicing, finally drying the grain material; wherein main engine speed is 200-400r/min, temperature is 250-280 DEG C. The invention aims to prepare a novel super-tough nylon material which can be widely applied to the fields such as automobiles, electric products, office appliances and constructional engineering.
Description
Technical field
The present invention relates to a kind of super-tough nylon alloy and preparation method thereof, particularly a kind of method of methylene-succinic acid graft polyolefin elastomer production super-toughened nylon, can be applicable to fields such as automobile, electronic apparatus, office accommodations, construction work, belong to the engineering plastic modification technical field.
Background technology
Polymeric amide (being commonly referred to nylon) be output maximum in the five big general engineering plastic, kind at most, one of the engineering materials of the widest, the high comprehensive performance of purposes, can be widely used in all respects such as automobile, electronic apparatus, office accommodations, construction work.Nylon is very outstanding in the performance of aspects such as flexural strength, wear-resisting, anti-creep, electrical property, but the shock-resistance of most of nylon kind is relatively poor, and especially resistance to low temperature is relatively poor, and water-intake rate is bigger, therefore, has therefore limited its application in many aspects.
Super-toughened nylon mainly is by adding rubber elastomer, thermoplastic elastomer, metallocene-polyolefin etc., making through the twin screw extruder blend as a big kind of modification of nylon.Simultaneously, toughner generally all is by the grafting polar group, the compatilizer of amino by polar group and nylon tip or acid-base reaction and Reinforced Nylon resin and toughner.The adding of toughner can significantly improve the shock strength and the lower temperature resistance of nylon, has also reduced the water-absorbent of nylon simultaneously.
Domestic patent CN90106778, CN91101624, CN97100554, CN97108021, CN99109924, and foreign patent DE19502819, EP0377511, EP0400964, EP0455507, EP0469693, US6303691, US6444754, modern material processed and applied 1,998 10 (3): 8, modern material processed and applied 2,001 13 (4): 8, China's plastics 1,999 13 (9): 30, China's plastics 200115 (12): 21 grades are all being added solubilizing agent with polyolefine material tenacity increased nylon or direct report aspect functionalised polyolefin material tenacity increased nylon, and its solubilizing agent that adopts is maleic anhydride (MAH) grafted polyethylene, polypropylene, ABS, SBS, SEBS, EPDM, EPR, polyolefine materials such as POE.The toughner that the present invention adopts is ethylene-alpha-octylene copolymers (POE), but the difference of the present invention and these reports is to adopt polar monomer methylene-succinic acid (ITA) graft modification POE, with its increase-volume nylon.
Summary of the invention
The present invention is with new type of toughening agent methylene-succinic acid grafted ethylene-alpha-octylene copolymers (POE-g-ITA) modification of nylon, and purpose is to provide a kind of super-tough nylon alloy and preparation method thereof.Its notched Izod impact strength of nylon after the modification strengthens greatly, and low-temperature performance improves, and water-absorbent also is reduced, and it can be widely used in automobile, electronic apparatus, office accommodations, building engineering field.For realizing above purpose, technical scheme of the present invention provides a kind of super-tough nylon alloy, it is characterized in that, it is made by following raw materials by weight percent:
Nylon 65-90%
Methylene-succinic acid grafted ethylene-alpha-octylene copolymers 10-35%
Oxidation inhibitor 0.1-1%
Lubricant TAF 0.2-1%
Described nylon is any fatty polyamide.This fatty polyamide can for density at 1.1-1.16g/cm
-1, fusing point is at 250-260 ℃, and the limiting viscosity index is at the nylon 66 of 2.3-2.9; Also can for density at 1.1-1.15g/cm
-1, fusing point is at 220-230 ℃, and the limiting viscosity index is at the nylon 6 of 2.3-2.9.Nylon easily absorbs water, and is following dry 8～12 hours at 80～90 ℃ before use.
Described methylene-succinic acid grafted ethylene-alpha-octylene copolymers (POE-g-ITA) is a kind of polymkeric substance with following repeated structural unit, and its percentage of grafting is 0.5%～1.5%, and melt flow rate (MFR) is 1～4g/10min:
Wherein: n=5000～30000, m=100～3000;
R1, R2, R3, R4, R5 at least one be:
All the other are H;
Wherein: n '=0～10, m '=0～10.
Described oxidation inhibitor is the compound system of a kind of Hinered phenols antioxidant and phosphite ester kind antioxidant, be 1010/168 composite, 1010 is [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, 168 is (2, the 4-di-tert-butyl-phenyl) tris phosphite.Oxidation inhibitor can improve polymkeric substance in the resistance of oxidation of the course of processing and the ageing resistance in the use.
Described lubricant is the ethylene bis-fatty acid amides TAF of modified with polar, improves the processing fluidity of matrix material, improves the surface smoothness of matrix material.
A kind of super-tough nylon alloy and preparation method thereof, it is characterized in that, method is as follows: nylon is following dry 8～12 hours at 80～90 ℃, even in high-speed mixer and mixing according to proportioning batching, material dropped into carry out granulation in the twin screw extruder, extrusion temperature is 250～280 ℃, and engine speed is 200r/min～400r/min, through traction, cooling, pelletizing, pellet is in 80～90 ℃ of down dry 8～12h.
Specific embodiments
By the following examples the present invention is further described, but the present invention is not confined to these embodiment.
Embodiment 1
With mass percent is nylon 6665%, methylene-succinic acid grafted ethylene-alpha-octylene copolymers 35%, antioxidant 1010 0.25%, oxidation inhibitor 168 0.25%, lubricant TAF0.5%, in high mixer after mixing under the room temperature state, material is thrown in the twin screw extruder, extrusion temperature is 260-280 ℃, engine speed is 300r/min, through traction, cooling, pelletizing, pellet was in 80 ℃ of following vacuum-dryings 8 hours.
Embodiment 2
With mass percent is nylon 66 70%, methylene-succinic acid grafted ethylene-alpha-octylene copolymers 30%, antioxidant 1010 0.25%, oxidation inhibitor 168 0.25%, lubricant TAF0.5%, in high mixer after mixing under the room temperature state, material is thrown in the twin screw extruder, extrusion temperature is 260-280 ℃, engine speed is 300r/min, through traction, cooling, pelletizing, pellet was in 80 ℃ of following vacuum-dryings 8 hours.
Embodiment 3
With mass percent is nylon 66 75%, methylene-succinic acid grafted ethylene-alpha-octylene copolymers 25%, antioxidant 1010 0.25%, oxidation inhibitor 168 0.25%, lubricant TAF0.5%, in high mixer after mixing under the room temperature state, material is thrown in the twin screw extruder, extrusion temperature is 260-280 ℃, engine speed is 300r/min, through traction, cooling, pelletizing, pellet was in 80 ℃ of following vacuum-dryings 8 hours.
Embodiment 4
With mass percent is nylon 66 80%, methylene-succinic acid grafted ethylene-alpha-octylene copolymers 20%, antioxidant 1010 0.25%, oxidation inhibitor 168 0.25%, lubricant TAF0.5%, in high mixer after mixing under the room temperature state, material is thrown in the twin screw extruder, extrusion temperature is 260-280 ℃, engine speed is 300r/min, through traction, cooling, pelletizing, pellet was in 80 ℃ of following vacuum-dryings 8 hours.
Comparative Examples 1
With mass percent is nylon 66 80%, POE 20%, antioxidant 1010 0.25%, oxidation inhibitor 1680.25%, lubricant TAF0.5%, in high mixer after mixing under the room temperature state, material is thrown in the twin screw extruder, extrusion temperature is 260-280 ℃, engine speed is 300r/min, through traction, cooling, pelletizing, pellet was in 80 ℃ of following vacuum-dryings 8 hours.
Embodiment 5
With mass percent is nylon 66 85%, methylene-succinic acid grafted ethylene-alpha-octylene copolymers 15%, antioxidant 1010 0.25%, oxidation inhibitor 168 0.25%, lubricant TAF0.5%, in high mixer after mixing under the room temperature state, material is thrown in the twin screw extruder, extrusion temperature is 260-280 ℃, engine speed is 300r/min, through traction, cooling, pelletizing, pellet was in 80 ℃ of following vacuum-dryings 8 hours.
Embodiment 6
With mass percent is nylon 66 90%, methylene-succinic acid grafted ethylene-alpha-octylene copolymers 10%, antioxidant 1010 0.25%, oxidation inhibitor 168 0.25%, lubricant TAF0.5%, in high mixer after mixing under the room temperature state, material is thrown in the twin screw extruder, extrusion temperature is 260-280 ℃, engine speed is 300r/min, through traction, cooling, pelletizing, pellet was in 80 ℃ of following vacuum-dryings 8 hours.
Embodiment 7
With mass percent is nylon 66 95%, methylene-succinic acid grafted ethylene-alpha-octylene copolymers 5%, antioxidant 1010 0.25%, oxidation inhibitor 168 0.25%, lubricant TAF0.5%, in high mixer after mixing under the room temperature state, material is thrown in the twin screw extruder, extrusion temperature is 260-280 ℃, engine speed is 300r/min, through traction, cooling, pelletizing, pellet was in 80 ℃ of following vacuum-dryings 8 hours.
Comparative Examples 2
With mass percent is nylon 66 100%, antioxidant 1010 0.25%, oxidation inhibitor 168 0.25%, lubricant TAF0.5%, in high mixer after mixing under the room temperature state, material is thrown in the twin screw extruder, extrusion temperature is 260-280 ℃, engine speed is 300r/min, through traction, cooling, pelletizing, pellet was in 80 ℃ of following vacuum-dryings 8 hours.
The prescription of embodiment 1-7 and Comparative Examples 1 and 2 and every The performance test results see the following form:
Table 1
| Material name | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative Examples 1 | Embodiment 5 | Embodiment 6 | Embodiment 7 | Comparative Examples 2 |
| Nylon 66/% | ??65 | ??70 | ??75 | ??80 | ??80 | ??85 | ??90 | ??95 | ??100 |
| ??POE-g-ITA/％ | ??35 | ??30 | ??25 | ??20 | ??- | ??15 | ??10 | ??5 | ??- |
| ??POE/％ | ??- | ??- | ??- | ??- | ??20 | ??- | ?- | ??- | ??- |
| Antioxidant 1010/168/% | ??0.5 | ??0.5 | ??0.5 | ??0.5 | ??0.5 | ??0.5 | ??0.5 | ??0.5 | ??0.5 |
| Lubricant TAF/% | ??0.5 | ??0.5 | ??0.5 | ??0.5 | ??0.5 | ??0.5 | ??0.5 | ??0.5 | ??0.5 |
| Socle girder impact/KJm -2 | ??102.5 | ??91.6 | ??84.7 | ??74.8 | ??9.0 | ??14.2 | ??7.7 | ??4.2 | ??3.6 |
| Tensile strength/MPa | ??40.6 | ??41.6 | ??44.9 | ??51.1 | ??62 | ??55.8 | ??65.9 | ??76.8 | ??88.7 |
| Flexural strength/MPa | ??38.6 | ??44.7 | ??50.8 | ??61.6 | ??65.1 | ??66.8 | ??78.8 | ??86.7 | ??103.4 |
| Modulus in flexure/GPa | ??1.3 | ??1.5 | ??1.7 | ??2.1 | ??2.1 | ??2.2 | ??2.6 | ??2.8 | ??3.3 |
| Elongation at break/% | ??180.2 | ??129.9 | ??91.7 | ??55.1 | ??22.6 | ??45.3 | ??30.1 | ??15.8 | ??10.1 |
| Material name | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative Examples 1 | Embodiment 5 | Embodiment 6 | Embodiment 7 | Comparative Examples 2 |
| Melting index/[g (10min -1] | ??2.5 | ??5.9 | ??14.8 | ??25.2 | ??58.8 | ??41.6 | ??68.0 | ??78.9 | ??90 |
The testing method of notched Izod impact strength is GB1043; The testing method of flexural strength, modulus in flexure is GB1042; The testing method of tensile strength, elongation at break is GB1634.
Comparative example 1-7 and Comparative Examples 2 results show, when the notched Izod impact strength of POE-g-ITA content nylon 66 alloys 20% time increases by 20 times, reached super malleableize purpose, further increasing notched Izod impact strength with POE-g-ITA content significantly increases, but stretches and also decline thereupon of flexural strength.Comparative example 4 and Comparative Examples 1 result show that compare no grafted POE with POE-g-ITA not remarkable to nylon 66 toughening effects.
Claims (5)
1. a super-tough nylon alloy is characterized in that, it is made by following materials of weight proportions:
Nylon 65-90%
Methylene-succinic acid grafted ethylene-alpha-octylene copolymers 10-35%
Oxidation inhibitor 0.1-1%
Lubricant TAF 0.2-1%
2. the method for claim 1 is characterized in that, described nylon is any fatty polyamide.This fatty polyamide can for density at 1.1-1.16g/cm
-1, fusing point is at 250-260 ℃, and the limiting viscosity index is at the nylon 66 of 2.3-2.9; Also can for density at 1.1-1.15g/cm
-1, fusing point is at 220-230 ℃, and the limiting viscosity index is at the nylon 6 of 2.3-2.9.
3. the method for claim 1 is characterized in that, described methylene-succinic acid grafted ethylene-alpha-octylene copolymers (POE-g-ITA) is a kind of polymkeric substance with following repeated structural unit, and its percentage of grafting is 0.5%～1.5%:
Wherein: n=5000～30000, m=100～3000;
R1, R2, R3, R4, R5 at least one be:
All the other are H;
Wherein: n '=0～10, m '=0～10.
4. the method for claim 1, it is characterized in that, described oxidation inhibitor is the compound system of a kind of Hinered phenols antioxidant and phosphite ester kind antioxidant, be 1010/168 composite, 1010 is [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, 168 is (2, the 4-di-tert-butyl-phenyl) tris phosphite.
5. the method for claim 1 is characterized in that, described lubricant is the ethylene bis-fatty acid amides TAF of modified with polar.The method of claim 1, it is characterized in that, nylon is following dry 8～12 hours at 80～90 ℃, even in high-speed mixer and mixing according to proportioning batching, material dropped into carry out granulation in the twin screw extruder, extrusion temperature is 250～280 ℃, and engine speed is 200r/min～400r/min, through traction, cooling, pelletizing, pellet is in 80～90 ℃ of down dry 8～12h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010101395984A CN101781455B (en) | 2010-03-22 | 2010-03-22 | Super-tough nylon alloy |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010101395984A CN101781455B (en) | 2010-03-22 | 2010-03-22 | Super-tough nylon alloy |
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| CN101781455B CN101781455B (en) | 2012-05-23 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102417727A (en) * | 2011-11-24 | 2012-04-18 | 上海日之升新技术发展有限公司 | High and low temperature-resistant cycling glass fiber reinforcement polyamide 66 (PA66) composite material and production method thereof |
| CN108587142A (en) * | 2018-03-28 | 2018-09-28 | 上海金发科技发展有限公司 | Tenacity increased nylon and preparation method thereof |
| CN111849154A (en) * | 2020-07-23 | 2020-10-30 | 江苏恒峰线缆有限公司 | Preparation method of novel nylon |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4114455A1 (en) * | 1991-05-03 | 1992-11-05 | Basf Ag | Thermoplastic moulding materials contg. poly:aryl ether and polyamide |
-
2010
- 2010-03-22 CN CN2010101395984A patent/CN101781455B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4114455A1 (en) * | 1991-05-03 | 1992-11-05 | Basf Ag | Thermoplastic moulding materials contg. poly:aryl ether and polyamide |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102417727A (en) * | 2011-11-24 | 2012-04-18 | 上海日之升新技术发展有限公司 | High and low temperature-resistant cycling glass fiber reinforcement polyamide 66 (PA66) composite material and production method thereof |
| CN108587142A (en) * | 2018-03-28 | 2018-09-28 | 上海金发科技发展有限公司 | Tenacity increased nylon and preparation method thereof |
| CN111849154A (en) * | 2020-07-23 | 2020-10-30 | 江苏恒峰线缆有限公司 | Preparation method of novel nylon |
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| CN101781455B (en) | 2012-05-23 |
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