CN102796229A - Super-nylon 66 alloy prepared by in-situ reactive compatibilization method and preparation method thereof - Google Patents
Super-nylon 66 alloy prepared by in-situ reactive compatibilization method and preparation method thereof Download PDFInfo
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Abstract
The invention discloses super-nylon 66 alloy prepared by an in-situ reactive compatibilization method and a preparation method thereof, and the preparation method is used for improving the compatibility of nylon 66 and POE (poly ortho ester), and preparing the super-nylon 66 alloy with high toughness, low temperature resistance and low water absorption rate. The super-nylon 66 alloy comprises the following compounds in parts by weight: 55 to 95 parts of nylon 66, 5 to 45 parts of POE, 0.01 to 1 part of initiating agent, and 0.1 to 4 parts of maleic anhydride, wherein the initiating agent is organic peroxide. The super-nylon 66 alloy provided by the invention has excellent comprehensive performance, in particular high notch impact strength, excellent low temperature impact resistance and low water absorption rate; and the product can be used in producing various automobile parts, mechanical parts, electronic appliances, package materials and the like with high toughness, abrasion resistance and excellent self-lubrication performance.
Description
Technical field
The invention belongs to field of materials, be specifically related to a kind of method of utilizing the reaction in increase-volume prepare have H.T., nylon 66 alloys of lower temperature resistance and low water absorption.
Background technology
Polymeric amide is claimed nylon (PA) again, is that purposes is the widest in the five big general engineering plastic, kind is maximum, output is maximum, the base resin of high comprehensive performance.PA66 is translucent or opaque oyster white crystalline polymer, and it has advantages such as intensity height, wear-resisting, anti-solvent and use temperature scope are wide, is widely used in fields such as automobile making, mechanical means, electronic apparatus, medicine equipment and precision instrument.But PA66 is because strong polar characteristics, and shortcoming such as have that water absorbability is strong, the notched Izod impact strength under poor dimensional stability and low temperature and the dry state is low is restricted its application.
Super-toughened nylon is as a big kind of modification of nylon, and is main through adding toughner such as rubber elastomer, thermoplastic elastomer, metallocene-polyolefin, makes through the twin screw extruder blend.Simultaneously, toughner generally all is amino or carboxyl reaction and the consistency between Reinforced Nylon resin and the toughner through grafting polar group and nylon tip.The adding of toughner can increase substantially the notched Izod impact strength and the lower temperature resistance of nylon, has also reduced the water-absorbent of nylon simultaneously.
POE is the multipolymer of ethene and octene; Have excellent stability to aging, ultraviolet resistance, good mechanical performance and processing rheological property, low-temperature flexibility is good, the cost performance advantage of higher; Thereby in the system of polyolefin elastomer tenacity increased nylon, POE uses many a kind of elastomericss.But POE is nonpolar elastomerics, and the mechanical property of the blend that POE and PA66 simple blend obtain is also bad, therefore need carry out graft modification to POE.Patent CN03116291.6 discloses through nylon, maleic anhydride graft polyolefin elastomer and superoxide dynamic vulcanization and has prepared super-toughened nylon; Patent CN200710047048.8 discloses a kind of nylon 66 ultra-tough thermoplastic engineering plastics; CN200910233106.5 discloses cold-resistant super-toughened nylon 66 and manufacture craft thereof, and patent 201010139598.4 discloses with nylon and methylene-succinic acid grafting POE and prepared super-tough nylon alloy.
The reaction in increase-volume is meant puts into the vinyl monomer of two kinds of superpolymer, polar functionalities and initiator in the parallel double-screw extruder in the lump; In extrusion, produce earlier the superpolymer of polar functionalities on the spot, this superpolymer and another superpolymer form the superpolymer that has compatibilization then.
The present invention adopts the method for original position increase-volume; In parallel double-screw extruder; POE molecule Malaysia anhydride group in the grafting under action of evocating makes it have stronger polarity, utilizes the amino reaction of end of anhydride group and the nylon 66 of POE-g-MAH to improve the consistency of PA66/POE system; Thereby obtain the super-toughened nylon 66 alloy of excellent performance, use this method to belong to contriver's initiative at present at home and abroad.
Summary of the invention
The objective of the invention is to adopt the method for reaction in increase-volume; After nylon 66, ethene and octene copolymer (POE), initiator and MALEIC ANHYDRIDE blend; In parallel double-screw extruder; Original position generates grafted superpolymer POE-g-MAH; And condensation reaction can take place and forms and have the superpolymer POE-g-MAH-g-PA66 of compatibilization in the anhydride group of POE-g-MAH with the end of nylon 66 is amino, thereby improves the consistency between nylon 66 and the POE, prepare have H.T., the super-toughened nylon 66 alloy of lower temperature resistance and low water absorption.
In order to realize the object of the invention, technical scheme of the present invention is: being equipped with the super-toughened nylon 66 alloy with reaction in increase-volume legal system provides one group of compsn, and said composition comprises the compound of following weight part:
66 55～95 parts of nylon,
5～45 parts of POE,
0.01～1 part of initiator,
0.1～4 part of MALEIC ANHYDRIDE,
Therein among some embodiment; Said initiator is an organic type of superoxide; Comprise hydroperoxide type, dialkyl class, peroxo-two acyl classes, peroxyesters, peroxy dicarbonates; Select a kind of initiator arbitrarily, their adding is played and is caused the effect that produces grafting superpolymer POE-g-MAH.
Among some embodiment, said organic type of superoxide is the Di Cumyl Peroxide 99,2 in the dialkyl class, 5-dimethyl--2,5-di-t-butyl hexane peroxide therein.
Another object of the present invention provides the method for using reaction in increase-volume legal system to be equipped with the super-toughened nylon 66 alloy, and concrete technical scheme may further comprise the steps:
⑴, the initiator and the MALEIC ANHYDRIDE of above-mentioned weight part is dissolved in the thinner, places subsequent use;
⑵, place vacuum drying oven to dry processing the nylon 66 of above-mentioned weight part; The control oven temperature is at 80～100 ℃; Dry 4～12 hours, place vacuum drying oven to dry processing the POE of above-mentioned weight part, the control oven temperature is at 60～80 ℃; Dry 4～12 hours, then nylon 66 is cooled to room temperature with POE;
⑶, the nylon 66 that will dry processing mix with POE, initiator and MALEIC ANHYDRIDE mixing solutions are poured in the blend of nylon 66 and POE, and blend is positioned in the air, and thinner is volatilized away, obtains premix;
⑷, place parallel double-screw extruder to melt extrude the premix that mixes, granulation, both;
Working process parameter is following:
Said parallel double-screw extruder has seven temperature controlled region, wherein, and 150～260 ℃ of district's temperature; 170～280 ℃ of two district's temperature, 250～285 ℃ of three district's temperature, 250～285 ℃ of four district's temperature; 250～285 ℃ of five district's temperature, 250～285 ℃ of six district's temperature, 250～285 ℃ of seven district's temperature; 250～285 ℃ of die head temperatures, screw speed are 25～200r/min.
Among embodiment, preparing method's preferred version may further comprise the steps therein:
⑴, the initiator and the MALEIC ANHYDRIDE of above-mentioned weight part is dissolved in the thinner acetone, places subsequent use;
⑵, place vacuum drying oven to dry processing the nylon 66 of above-mentioned weight part; The control oven temperature is at 90 ℃; Dry 4～6 hours, place vacuum drying oven to dry processing the POE of above-mentioned weight part, the control oven temperature is at 70 ℃; Dry 4～6 hours, then nylon 66 is cooled to room temperature with POE;
⑶, initiator and MALEIC ANHYDRIDE mixing solutions are poured in the blend of nylon 66 and POE, blend is positioned in the air, and thinner acetone is volatilized away;
⑷, place parallel double-screw extruder to melt extrude the premix that mixes, granulation;
Complete processing is following: the parallel double-screw extruder screw speed is 25～100r/min, 150～200 ℃ of district's temperature, 170～210 ℃ of two district's temperature; 250～270 ℃ of three district's temperature; 260～270 ℃ of four district's temperature, 260～270 ℃ of five district's temperature, 260～270 ℃ of six district's temperature; 260～270 ℃ of seven district's temperature, 260～270 ℃ of die head temperatures.
In the above-mentioned steps, the thinner of choosing is acetone, butanone, and thinner is preferably: acetone; The initiator of choosing is preferably: 2, and 5-dimethyl--2,5-di-t-butyl hexane peroxide;
Wherein the screw rod of parallel double-screw extruder is shaped as single thread; The ratio (L/D) of spiro rod length (L) and diameter (D) is 20～60, preferred 35～60; Screw rod must have more than one gear block district, preferred 2 gear block districts, and the gear block district helps material in forcing machine, to mix more evenly; Screw rod must have more than one left-hand thread district, preferred 2 left-hand thread districts, and the left-hand thread district helps material in forcing machine, to mix more evenly, and can prolong the time that material stops in forcing machine, makes that original position increase-volume reaction is more abundant.
The preparation method that reaction in increase-volume legal system provided by the present invention is equipped with the super-toughened nylon 66 alloy has the following advantages:
1, adopt method of the present invention to prepare the super-toughened nylon 66 alloy, excellent combination property, especially notched Izod impact strength is higher, low-temperature impact property is good and water-intake rate is low.
2, adopt method of the present invention to prepare the super-toughened nylon 66 alloy, its technology is simple, is easy to control, and not high to equipment requirements, employed equipment is general polymer processing equipment, invests not high.
3, adopt method of the present invention to prepare the super-toughened nylon 66 alloy, shortened technical process, save the energy, improved production efficiency, be easy to apply.
4, product of the present invention can be used for production H.T., wear-resisting, various trolley parts that self lubricity is good, mechanical part, electronic apparatus, wrapping material etc.; Can be used for making corrosion resistant container and equipment at chemical field; Electrical apparatus industry can be used for producing shell, component of insulating material and instrument etc.
Description of drawings
Shown in Figure 1 is the dispersing morphology of POE in PA66 in the comparative example 2;
Shown in Figure 2 is the dispersing morphology of POE in PA66 among the embodiment 1;
Shown in Figure 3 is the dispersing morphology of POE in PA66 among the embodiment 3;
Shown in Figure 4 is the schematic flow sheet of embodiment;
Shown in Figure 5 is the reaction mechanism synoptic diagram of embodiment.
Embodiment
For further understanding characteristic of the present invention, technique means and the specific purposes that reached, function, resolve advantage of the present invention and spirit, through embodiment the present invention is done further elaboration by following.
The reaction mechanism that reaction in increase-volume legal system of the present invention is equipped with the super-toughened nylon 66 alloy is (the reaction process synoptic diagram is asked for an interview Fig. 4, and the reaction mechanism synoptic diagram is asked for an interview Fig. 5) as follows: (molecular structure signal)
Wherein RO-OR is an initiator.
The employed raw material of the embodiment of the invention is following:
Nylon 66 (PA66) is available from toray, trade mark CM3001-N;
Ethene and octene copolymer (POE) are available from DOW Chemical (DOW), the trade mark 8150;
2,5-dimethyl--2,5-di-t-butyl hexane peroxide (L-101) is available from U.S. Sigma-Aldrich company;
MALEIC ANHYDRIDE (MAH) is available from Chemical Reagent Co., Ltd., Sinopharm Group.
Embodiment 1:
Reaction in increase-volume legal system is equipped with the super-toughened nylon 66 alloy and is cooperated by the raw material of following weight part and form: 90 parts of polyamide 66s (PA66); 10 parts of ethene and octene copolymers (POE), 2,5-dimethyl--2; 0.1 part of 5-di-t-butyl hexane peroxide (L-101), 0.5 part of MALEIC ANHYDRIDE (MAH).
Reaction in increase-volume legal system is equipped with the method for super-toughened nylon 66 alloy, may further comprise the steps:
(1), with initiator 2,5-dimethyl--2,5-di-t-butyl hexane peroxide and MALEIC ANHYDRIDE are dissolved in the acetone, place subsequent use;
(2), place vacuum drying oven to dry processing nylon 66, the control oven temperature is at 90 ℃, and dry 4 hours, POE placed vacuum drying oven to dry processing, and the control oven temperature dry 4 hours, is cooled to room temperature with nylon 66 with POE then at 70 ℃;
(3), with initiator 2,5-dimethyl--2,5-di-t-butyl hexane peroxide and MALEIC ANHYDRIDE mixing solutions are poured in the blend of nylon 66 and POE, blend is positioned in the air, and solvent acetone is volatilized away, obtains premix;
(4), place parallel double-screw extruder to melt extrude the premix that mixes, granulation.Complete processing is following: the parallel double-screw extruder screw speed is 75r/min, 170 ℃ of district's temperature, 200 ℃ of two district's temperature; 255 ℃ of three district's temperature, 265 ℃ of four district's temperature, 265 ℃ of five district's temperature; 265 ℃ of six district's temperature, 265 ℃ of seven district's temperature, 260 ℃ of die head temperatures.
Embodiment 2:
Reaction in increase-volume legal system is equipped with the super-toughened nylon 66 alloy and is cooperated by the raw material of following weight part and form: 80 parts of polyamide 66s (PA66); 20 parts of ethene and octene copolymers (POE), 2,5-dimethyl--2; 0.5 part of 5-di-t-butyl hexane peroxide (L-101), 2.5 parts of MALEIC ANHYDRIDEs (MAH).
Reaction in increase-volume legal system is equipped with the method for super-toughened nylon 66 alloy, and its step is with embodiment 1.
Embodiment 3:
Reaction in increase-volume legal system is equipped with the super-toughened nylon 66 alloy and is cooperated by the raw material of following weight part and form: 70 parts of polyamide 66s (PA66); 30 parts of ethene and octene copolymers (POE), 2,5-dimethyl--2; 0.1 part of 5-di-t-butyl hexane peroxide (L-101), 1 part of MALEIC ANHYDRIDE (MAH).
Reaction in increase-volume legal system is equipped with the method for super-toughened nylon 66 alloy, and its step is with embodiment 1.
Embodiment 4:
Reaction in increase-volume legal system is equipped with the super-toughened nylon 66 alloy and is cooperated by the raw material of following weight part and form: 60 parts of polyamide 66s (PA66); 40 parts of ethene and octene copolymers (POE), 2,5-dimethyl--2; 0.8 part of 5-di-t-butyl hexane peroxide (L-101), 3.5 parts of MALEIC ANHYDRIDEs (MAH).
Reaction in increase-volume legal system is equipped with the method for super-toughened nylon 66 alloy, and its step is with embodiment 1.
Embodiment 5:
Reaction in increase-volume legal system is equipped with the super-toughened nylon 66 alloy and is cooperated by the raw material of following weight part and form: 70 parts of polyamide 66s (PA66); 30 parts of ethene and octene copolymers (POE), 2,5-dimethyl--2; 0.1 part of 5-di-t-butyl hexane peroxide (L-101), 0.5 part of MALEIC ANHYDRIDE (MAH).
Reaction in increase-volume legal system is equipped with the method for super-toughened nylon 66 alloy, and its step is with embodiment 1.
Embodiment 6:
Reaction in increase-volume legal system is equipped with the super-toughened nylon 66 alloy and is cooperated by the raw material of following weight part and form: 70 parts of polyamide 66s (PA66); 30 parts of ethene and octene copolymers (POE), 2,5-dimethyl--2; 0.1 part of 5-di-t-butyl hexane peroxide (L-101), 1.5 parts of MALEIC ANHYDRIDEs (MAH).
Reaction in increase-volume legal system is equipped with the method for super-toughened nylon 66 alloy, and its step is with embodiment 1.
Embodiment 7:
Reaction in increase-volume legal system is equipped with the super-toughened nylon 66 alloy and is cooperated by the raw material of following weight part and form: 70 parts of polyamide 66s (PA66); 30 parts of ethene and octene copolymers (POE), 2,5-dimethyl--2; 0.05 part of 5-di-t-butyl hexane peroxide (L-101), 1 part of MALEIC ANHYDRIDE (MAH).
Reaction in increase-volume legal system is equipped with the method for super-toughened nylon 66 alloy, and its step is with embodiment 1.
Embodiment 8:
Reaction in increase-volume legal system is equipped with the super-toughened nylon 66 alloy and is cooperated by the raw material of following weight part and form: 70 parts of polyamide 66s (PA66); 30 parts of ethene and octene copolymers (POE), 2,5-dimethyl--2; 0.15 part of 5-di-t-butyl hexane peroxide (L-101), 1 part of MALEIC ANHYDRIDE (MAH).
Reaction in increase-volume legal system is equipped with the method for super-toughened nylon 66 alloy, and its step is with embodiment 1.
Below be comparative example and embodiment table look-up:
Table 1 comparative example and embodiment table look-up
| Comparative example and embodiment | PA66 (part) | POE (part) | L-101 (part) | MAH (part) |
| Comparative example 1 | 100 | 0 | 0 | 0 |
| Comparative example 2 | 70 | 30 | 0 | 0 |
| Embodiment 1 | 90 | 10 | 0.1 | 0.5 |
| Embodiment 2 | 80 | 20 | 0.5 | 2.5 |
| Embodiment 3 | 70 | 30 | 0.1 | 1 |
| Embodiment 4 | 60 | 40 | 0.8 | 3.5 |
| Embodiment 5 | 70 | 30 | 0.1 | 0.5 |
| Embodiment 6 | 70 | 30 | 0.1 | 1.5 |
| Embodiment 7 | 70 | 30 | 0.05 | 1 |
| Embodiment 8 | 70 | 30 | 0.15 | 1 |
The made sample of above-mentioned each embodiment is carried out following performance test:
Tensile property: press the GB/T1042-1992 standard testing, rate of extension 50mm/min;
Bending property: press the GB/T9341-2000 standard testing, crooked speed is 2mm/min;
Impact property: press the GB/T1843-1996 standard testing, batten thickness is 3.2mm;
The mensuration of water-intake rate: water-intake rate is tested by GB1034-1998.It is the square (sample is thick in 25mm) of 50 ± 1mm that sample is cut out; Put into the dry 24 ± 1h of 50 ± 2 ℃ of baking ovens then; In moisture eliminator, be cooled to room temperature and be weighed as m1; Again sample is dipped in 23 ± 0.5 ℃ of zero(ppm) water, take out behind soaking time 24 ± 1h and use water that cleaning, exsiccant filter paper wipes specimen surface rapidly once more the weighing sample be m2.The calculation formula of water-intake rate Wm is:
Table 2 comparative example and embodiment performance table look-up
Below be the dispersing morphology of POE in PA66, referring to Fig. 1, Fig. 2, Fig. 3; Schematic flow sheet of the present invention is referring to Fig. 4; Reaction mechanism synoptic diagram of the present invention is referring to Fig. 5.
The above embodiment has only expressed several kinds of embodiments of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to claim of the present invention.Should be pointed out that for the person of ordinary skill of the art under the prerequisite that does not break away from the present invention's design, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with accompanying claims.
Claims (7)
1. a super-toughened nylon 66 alloy is characterized in that, its raw material is formed and weight part is:
66 55～95 parts of nylon,
5～45 parts of POE,
0.01～1 part of initiator,
0.1～4 part of MALEIC ANHYDRIDE,
Described initiator is an organic type of superoxide, comprises hydroperoxide type, dialkyl class, peroxo-two acyl classes, peroxyesters, peroxy dicarbonates.
2. super-toughened nylon 66 alloy according to claim 1 is characterized in that, described organic type of superoxide is the Di Cumyl Peroxide 99,2 in the dialkyl class, 5-dimethyl--2,5-di-t-butyl hexane peroxide.
3. a reaction in increase-volume legal system is equipped with the method for each said super-toughened nylon 66 alloy of claim 1～2, it is characterized in that, may further comprise the steps:
⑴, the initiator and the MALEIC ANHYDRIDE of said weight part is dissolved in the thinner, places subsequent use;
⑵, place vacuum drying oven to dry processing the nylon 66 of said weight part; The control oven temperature is at 80～100 ℃; Dry 4～12 hours, place vacuum drying oven to dry processing the POE of said weight part, the control oven temperature is at 60～80 ℃; Dry 4～12 hours, then nylon 66 is cooled to room temperature with POE;
⑶, the nylon 66 that will dry processing mix with POE, initiator and MALEIC ANHYDRIDE mixing solutions are poured in the blend of nylon 66 and POE, and blend is positioned in the air, and thinner is volatilized away, obtains premix;
⑷, place parallel double-screw extruder to melt extrude the premix that mixes, granulation promptly gets;
Working process parameter is following:
Said parallel double-screw extruder has seven temperature controlled region, wherein, and 150～260 ℃ of district's temperature; 170～280 ℃ of two district's temperature, 250～285 ℃ of three district's temperature, 250～285 ℃ of four district's temperature; 250～285 ℃ of five district's temperature, 250～285 ℃ of six district's temperature, 250～285 ℃ of seven district's temperature; 250～285 ℃ of die head temperatures, screw speed are 25～200r/min.
4. preparation method according to claim 3 is characterized in that, may further comprise the steps:
⑴, the initiator and the MALEIC ANHYDRIDE of said weight part is dissolved in the thinner acetone, places subsequent use;
⑵, place vacuum drying oven to dry processing the nylon 66 of said weight part; The control oven temperature is at 90 ℃; Dry 4～6 hours, place vacuum drying oven to dry processing the POE of said weight part, the control oven temperature is at 70 ℃; Dry 4～6 hours, then nylon 66 is cooled to room temperature with POE;
⑶, initiator and MALEIC ANHYDRIDE mixing solutions are poured in the blend of nylon 66 and POE, blend is positioned in the air, and thinner acetone is volatilized away;
⑷, place parallel double-screw extruder to melt extrude the premix that mixes, granulation;
Complete processing is following: the parallel double-screw extruder screw speed is 25～100r/min, 150～200 ℃ of district's temperature, 170～210 ℃ of two district's temperature; 250～270 ℃ of three district's temperature; 260～270 ℃ of four district's temperature, 260～270 ℃ of five district's temperature, 260～270 ℃ of six district's temperature; 260～270 ℃ of seven district's temperature, 260～270 ℃ of die head temperatures.
5. preparation method according to claim 3 is characterized in that, said thinner is acetone, butanone.
6. preparation method according to claim 3 is characterized in that said screw rod is shaped as single thread; The ratio L/D of spiro rod length L and diameter D is 20～60.
7. preparation method according to claim 3 is characterized in that, said screw rod must have more than one gear block district, and said screw rod must have more than one left-hand thread district.
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| CN103044913A (en) * | 2012-12-14 | 2013-04-17 | 东莞市信诺橡塑工业有限公司 | Super-toughened nylon 66 nano composite material prepared by in situ compatibilization and preparation method thereof |
| CN112210047A (en) * | 2020-09-24 | 2021-01-12 | 杭州津源新材料有限公司 | Plastic-dipped powder and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103044913A (en) * | 2012-12-14 | 2013-04-17 | 东莞市信诺橡塑工业有限公司 | Super-toughened nylon 66 nano composite material prepared by in situ compatibilization and preparation method thereof |
| CN103044913B (en) * | 2012-12-14 | 2014-09-03 | 东莞市信诺橡塑工业有限公司 | Super-toughened nylon 66 nano composite material prepared by in situ compatibilization and preparation method thereof |
| CN112210047A (en) * | 2020-09-24 | 2021-01-12 | 杭州津源新材料有限公司 | Plastic-dipped powder and preparation method thereof |
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Application publication date: 20121128 |