CN103044913B - Super-toughened nylon 66 nano composite material prepared by in situ compatibilization and preparation method thereof - Google Patents
Super-toughened nylon 66 nano composite material prepared by in situ compatibilization and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a super-toughened nylon 66 nano composite material prepared by in situ compatibilization and a preparation method thereof. The super-toughened nylon 66 nano composite material comprises the following raw materials in part by weight: 55 to 95 parts of nylon 66, 5 to 45 parts of ethylene propylene diene monomer, 0.01 to 1 part of initiator, 0.1 to 4 parts of maleic anhydride and 1 to 5 parts of organic montmorillonite; and the initiator is organic peroxide and comprises hydroperoxides, dialkyl peroxides, dibenzoyl peroxides, lipoperoxides and peroxydicarbonates. The super-toughened nylon 66 nano composite material provided by the invention has excellent comprehensive performance, particularly has high notched impact strength, excellent low temperature impact resistance and low water adsorption, shortens the process flow, improves production efficiency and is easy to popularize and apply.
Description
Technical field
The invention belongs to Material Field, be specifically related to a kind of super-toughened nylon 66 nano composite material that uses the method preparation of in situ reactive compatibilization to there is high tenacity, lower temperature resistance and low water absorption.
Background technology
Polymeric amide, claims again nylon (PA), is that in five large general engineering plastic, purposes is the widest, 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 high, wear-resisting, the resistance to solvent of intensity and the advantage such as use temperature scope is wide, is widely used in the fields such as automobile making, mechanical means, electronic apparatus, medicine equipment and precision instrument.But PA66 is due to strong polarity, the shortcoming such as have that water absorbability is strong, notched Izod impact strength under poor dimensional stability and low temperature and dry state is low, is restricted its application.
Super-toughened nylon is as a large kind of modification of nylon, main by adding the toughner such as rubber elastomer, thermoplastic elastomer, metallocene-polyolefin, makes through twin screw extruder blend.Toughner is all generally the consistency by the amino of grafting polar group and nylon tip or carboxyl reaction and between Reinforced Nylon resin and toughner, toughner add the notched Izod impact strength and the lower temperature resistance that have improved significantly PA66, also reduced its water-absorbent.Therefore, modified Pa 66 has been expanded the scope of its use, by client is liked.Patent 03116291.6 discloses by the polyolefin elastomer of nylon, maleic anhydride graft and peroxide cross-linking agent are joined in twin screw extruder, makes super-toughened nylon by the technology of dynamic vulcanization; Patent 200910039160.6 discloses by nylon 6, ultra-fine barium sulfate, POE-g-MAH, oxidation inhibitor and mix lubricant are joined after evenly and in twin screw extruder, has prepared super-toughened nylon; Patent 201010139598.4 discloses nylon, POE-g-ITA, oxidation inhibitor, lubricant is joined and in twin screw extruder, prepare super-toughened nylon.
Ethylene-propylene rubber(EPR) mainly comprises ethylene propylene rubber (EPM) and terpolymer EP rubber (EPDM), the multipolymer that wherein terpolymer EP rubber (EPDM) is made up of ethene, propylene and non-conjugated diene hydrocarbon, because the ethene on its molecular backbone chain and propylene monomer are random arrangement, lose the regularity of polyethylene or polypropylene structure, thereby become elastomerics, and the diolefine of terpolymer EP rubber is positioned on side chain, therefore the structure of terpolymer EP rubber is conducive to the carrying out of situ-formed graft reaction, and it has also kept the various characteristics of ethylene propylene rubber simultaneously.
Polynite (MMT) is a kind of clay being made up of the silicate lamella of nano thickness, and sheet interlayer spacing is 0.96～2.1nm.Polynite is filled in polyamide 6 matrix by the compound method of intercalation, realizes compound on nanoscale of polynite and matrix resin.Due to the bonding interface that nanometer small-size effect is become reconciled, this matrix material has excellent mechanical property and thermotolerance, and its flame retardant resistance, barrier and weathering resistance all increase.
In situ reactive compatibilization refers to be put into the vinyl monomer of two kinds of superpolymer, polar functionalities and initiator in parallel double-screw extruder in the lump, in extrusion, produce the superpolymer of polar functionalities, then this superpolymer and another superpolymer form the superpolymer with compatibilization.
The present invention adopts the method for In Situ Compatibilization, in parallel double-screw extruder, EPDM molecule Malaysia anhydride group in grafting under the effect of initiator, make it have stronger polarity, utilize the amino consistency of reacting to improve PA66/EPDM system of the anhydride group of EPDM-g-MAH and the end of nylon 66, thereby obtain the super-toughened nylon 66 nano composite material of excellent performance.
Summary of the invention
The object of the invention is to adopt the method for In Situ Compatibilization, by nylon 66, terpolymer EP rubber (EPDM), initiator, after MALEIC ANHYDRIDE and organo montmorillonite (OMMT) blend, in parallel double-screw extruder, original position generates the superpolymer EPDM-g-MAH of grafting, and the anhydride group of EPDM-g-MAH can form the superpolymer EPDM-g-MAH-g-PA66 with compatibilization with the amino generation of the end of nylon 66 condensation reaction, thereby improve the consistency between nylon 66 and EPDM, prepare and there is high tenacity, the super-toughened nylon 66 nano composite material of lower temperature resistance and low water absorption.
In order to realize object of the present invention, technical scheme of the present invention is: In Situ Compatibilization is prepared super-toughened nylon 66 nano composite material, and one group of composition is provided, and said composition comprises the compound of following weight part:
Nylon 66(PA66) 55～95 parts;
5～45 parts of terpolymer EP rubbers (EPDM);
Nylon 66(PA66) with the weight part summation of terpolymer EP rubber (EPDM) be 100 parts;
0.01～1 part of initiator;
0.1～4 part of MALEIC ANHYDRIDE (MAH);
1～5 part of organo montmorillonite (OMMT).
Therein in some embodiment, described initiator is organic superoxide, comprise hydroperoxide type, dialkyl class, peroxidation two acyl classes, peroxyesters, peroxy dicarbonates, select arbitrarily a kind of initiator, they add to play and cause the effect that produces graft polymer EPDM-g-MAH.
In some embodiment, described organic superoxide is the dicumyl peroxide, 2 in dialkyl class, 5-dimethyl-2,5-di-t-butyl hexane peroxide therein.
Another object of the present invention is to provide the preparation method of above-mentioned super-toughened nylon 66 nano composite material, and concrete technical scheme is as follows:
(1), described weight part initiator and MALEIC ANHYDRIDE are dissolved in thinner, obtain mixing solutions, place for subsequent use;
(2), described weight part nylon 66 is placed in to vacuum drying oven and carries out drying and processing, control oven temperature at 80～100 DEG C, dry 4～12 hours, described weight part terpolymer EP rubber is placed in vacuum drying oven and carries out drying and processing, control oven temperature at 60～80 DEG C, dry 4～12 hours, then nylon 66 and terpolymer EP rubber are cooled to room temperature, the nylon 66 carrying out after drying and processing is mixed in proportion with terpolymer EP rubber, obtain blend;
(3), the mixing solutions in step (1) is poured in the blend of nylon 66 and terpolymer EP rubber, obtain premix, premix is positioned in air, and thinner is volatilized away;
(4), the premix mixing is placed in to parallel double-screw extruder, and add after organo montmorillonite in the side direction Si district of parallel double-screw extruder, melt extrude, granulation, to obtain final product;
Complete processing is as follows: parallel double-screw extruder screw speed is 25～200r/min, one 150～260 DEG C of district's temperature, two 170～280 DEG C of district's temperature, three 250～285 DEG C of district's temperature, four 250～285 DEG C of district's temperature, five 250～285 DEG C of district's temperature, six 250～285 DEG C of district's temperature, seven 250～285 DEG C of district's temperature, 250～285 DEG C of die head temperatures.
In an embodiment, the initiator of choosing in above-mentioned steps can be therein: the dicumyl peroxide, 2 in dialkyl class, 5-dimethyl-2,5-di-t-butyl hexane peroxide; Thinner can be: acetone, butanone.
In an embodiment, its preferred version comprises the following steps therein:
(1), described weight part initiator and MALEIC ANHYDRIDE are dissolved in thinner acetone, obtain mixing solutions, place for subsequent use;
(2), described weight part nylon 66 is placed in to vacuum drying oven and carries out drying and processing, control oven temperature at 80～100 DEG C, dry 4～8 hours, described weight part terpolymer EP rubber is placed in vacuum drying oven and carries out drying and processing, control oven temperature at 60～80 DEG C, dry 4～8 hours, then nylon 66 and terpolymer EP rubber are cooled to room temperature, the nylon 66 carrying out after drying and processing is mixed in proportion with terpolymer EP rubber, obtain blend;
(3), the mixing solutions in step (1) is poured in the blend of nylon 66 and terpolymer EP rubber, obtain premix, premix is positioned in air, and thinner acetone is volatilized away;
(4), the premix mixing is placed in to parallel double-screw extruder, and add after organo montmorillonite in the side direction Si district of parallel double-screw extruder, melt extrude, granulation, to obtain final product;
Complete processing is as follows: parallel double-screw extruder screw speed is 25～100r/min, one 150～200 DEG C of district's temperature, two 170～210 DEG C of district's temperature, three 250～270 DEG C of district's temperature, four 260～270 DEG C of district's temperature, five 260～270 DEG C of district's temperature, six 260～270 DEG C of district's temperature, seven 260～270 DEG C of district's temperature, 260～270 DEG C of die head temperatures.
In an embodiment, described screw rod is shaped as single thread therein; The ratio (L/D) of spiro rod length (L) and diameter (D) is 20～60, preferably 35～60; Screw rod must have more than one gear block district, preferably 2 gear block districts, and it is more even that gear block district contributes to material to be mixed to get in forcing machine; Screw rod must have more than one left-hand thread district, preferably 2 left-hand thread districts, and it is more even that left-hand thread district contributes to material to be mixed to get in forcing machine, and can extend the time that material stops in forcing machine, makes In Situ Compatibilization reaction more abundant.
In above-mentioned steps, the initiator of choosing is preferably: 2,5-dimethyl-2,5-di-t-butyl hexane peroxide; Thinner is preferably: acetone.
The method that In Situ Compatibilization provided by the present invention is prepared super-toughened nylon 66 nano composite material has the following advantages:
1, adopt method of the present invention to prepare super-toughened nylon 66 nano composite material, 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 super-toughened nylon 66 nano composite material, its technique is simple, is easy to control, and not high to equipment requirements, the equipment using is general polymer processing equipment, invests not high;
3, adopt method of the present invention to prepare super-toughened nylon 66 nano composite material, shortened technical process, save the energy, improved production efficiency, be easy to apply.
Brief description of the drawings
Figure 1 shows that embodiment schematic flow sheet;
Figure 2 shows that embodiment reaction mechanism schematic diagram;
Figure 3 shows that embodiment 3 scanning electron microscope (SEM) photographs.
Embodiment
For further understanding feature of the present invention, technique means and the specific purposes that reach, function, resolve the advantages and spirit of the present invention, by the present invention is further elaborated by the following examples.
In Situ Compatibilization of the present invention is prepared the reaction mechanism following (reaction process schematic diagram is asked for an interview Fig. 1, and reaction mechanism schematic diagram is asked for an interview Fig. 2) of super-toughened nylon 66 nano composite material: (molecular structure signal)
Wherein RO-OR is initiator.
Initiator is first all cleaved into elementary free radical, sees formula (1); Then this elementary free radical is grabbed the hydrogen atom on terpolymer EP rubber (EPDM) main chain, forms macromolecular radical EPDM, sees formula (2); A hydrogen atom on the two keys of macromolecular radical EPDM and MALEIC ANHYDRIDE (MAH) forms EPDM-g-MAH, sees formula (3); The amino condensation reaction of end of the anhydride group of EPDM-g-MAH and nylon 66 forms EPDM-g-MAH-g-PA66, sees formula (4) and formula (5).
The raw material that the embodiment of the present invention is used is as follows:
Nylon 66(PA66) purchased from toray, trade mark CM3001-N;
Terpolymer EP rubber (EPDM) is purchased from Dupont Tao Shi product (DuPont-Dow), trade mark Nordel IP3745P;
2,5-dimethyl-2,5-di-t-butyl hexane peroxide (L-101) is purchased from Sigma-Aldrich company of the U.S.;
Dicumyl peroxide (DCP) is purchased from Chemical Reagent Co., Ltd., Sinopharm Group;
MALEIC ANHYDRIDE (MAH) is purchased from Chemical Reagent Co., Ltd., Sinopharm Group;
Organo montmorillonite (OMMT) is purchased from Zhejiang Fenghong New Material Co., Ltd., trade mark DK5.
Comparative example 1:
Nylon 66 is placed in to vacuum drying oven and carries out drying and processing, control oven temperature at 90 DEG C, dry 4 hours, then nylon 66 is cooled to room temperature.Finally the nylon of drying and processing 66 is placed in to parallel double-screw extruder and melt extrudes, granulation.Complete processing is as follows: parallel double-screw extruder screw speed is 75r/min, 170 DEG C of district's temperature, two 200 DEG C of district's temperature, three 255 DEG C of district's temperature, four 265 DEG C of district's temperature, five 265 DEG C of district's temperature, six 265 DEG C of district's temperature, seven 265 DEG C of district's temperature, 260 DEG C of die head temperatures.
Comparative example 2:
Nylon 66 is placed in to vacuum drying oven and carries out drying and processing, control oven temperature at 90 DEG C, dry 4 hours, EPDM was placed in vacuum drying oven and carries out drying and processing, controlled oven temperature at 70 DEG C, dry 4 hours, then nylon 66 and EPDM was cooled to room temperature.After finally nylon 66 and EPDM being mixed by 70 weight parts, 30 weight parts respectively, be placed in parallel double-screw extruder, and add after the OMMT of 5 weight parts in the side direction Si district of parallel double-screw extruder (Gong Ba district), melt extrude granulation.Complete processing is as follows: parallel double-screw extruder screw speed is 75r/min, 170 DEG C of district's temperature, two 200 DEG C of district's temperature, three 255 DEG C of district's temperature, four 265 DEG C of district's temperature, five 265 DEG C of district's temperature, six 265 DEG C of district's temperature, seven 265 DEG C of district's temperature, 260 DEG C of die head temperatures.
Embodiment 1:
In Situ Compatibilization is prepared super-toughened nylon 66 nano composite material and is coordinated and formed by the raw material of following weight part: nylon 66(PA66) 90 parts, 10 parts of terpolymer EP rubbers (EPDM), 0.1 part of dicumyl peroxide (DCP), 1 part of MALEIC ANHYDRIDE (MAH), 5 parts of organo montmorillonites (OMMT).
In Situ Compatibilization is prepared the method for super-toughened nylon 66 nano composite material, comprises the following steps:
(1), initiator dicumyl peroxide (DCP) and MALEIC ANHYDRIDE (MAH) are dissolved in butanone, obtain mixing solutions, place for subsequent use;
(2), nylon 66 is placed in to vacuum drying oven and carries out drying and processing, control oven temperature at 90 DEG C, dry 4 hours, EPDM is placed in vacuum drying oven and carries out drying and processing, control oven temperature at 70 DEG C, dry 4 hours, then nylon 66 and EPDM are cooled to room temperature, the nylon 66 carrying out after drying and processing is mixed according to the above ratio with EPDM, obtain blend;
(3), the mixing solutions in step (1) is poured in the blend of nylon 66 and EPDM, obtain premix, premix is positioned in air, and thinner butanone is volatilized away;
(4), the premix mixing is placed in to parallel double-screw extruder, and add after OMMT in the side direction Si district of parallel double-screw extruder (Gong Ba district), melt extrude granulation.Complete processing is as follows: parallel double-screw extruder screw speed is 200r/min, 170 DEG C of district's temperature, two 200 DEG C of district's temperature, three 255 DEG C of district's temperature, four 265 DEG C of district's temperature, five 265 DEG C of district's temperature, six 265 DEG C of district's temperature, seven 265 DEG C of district's temperature, 260 DEG C of die head temperatures.
Embodiment 2:
In Situ Compatibilization is prepared super-toughened nylon 66 nano composite material and is coordinated and formed by the raw material of following weight part: nylon 66(PA66) 80 parts, 20 parts of terpolymer EP rubbers (EPDM), 2,5-dimethyl-2,0.1 part of 5-di-t-butyl hexane peroxide (L-101), 1 part of MALEIC ANHYDRIDE (MAH), 5 parts of organo montmorillonites (OMMT).
In Situ Compatibilization is prepared the method for super-toughened nylon 66 nano composite material, comprises the following steps:
(1), by initiator 2,5-dimethyl-2,5-di-t-butyl hexane peroxide (L-101) and MALEIC ANHYDRIDE (MAH) are dissolved in acetone, obtain mixing solutions, place for subsequent use;
(2), nylon 66 is placed in to vacuum drying oven and carries out drying and processing, control oven temperature at 90 DEG C, dry 4 hours, EPDM is placed in vacuum drying oven and carries out drying and processing, control oven temperature at 70 DEG C, dry 4 hours, then nylon 66 and EPDM are cooled to room temperature, the nylon 66 carrying out after drying and processing is mixed according to the above ratio with EPDM, obtain blend;
(3), the mixing solutions in step (1) is poured in the blend of nylon 66 and EPDM, obtain premix, premix is positioned in air, and thinner acetone is volatilized away;
(4), the premix mixing is placed in to parallel double-screw extruder, and add after OMMT in the side direction Si district of parallel double-screw extruder (Gong Ba district), melt extrude granulation.Complete processing is as follows: parallel double-screw extruder screw speed is 100r/min, 170 DEG C of district's temperature, two 200 DEG C of district's temperature, three 255 DEG C of district's temperature, four 265 DEG C of district's temperature, five 265 DEG C of district's temperature, six 265 DEG C of district's temperature, seven 265 DEG C of district's temperature, 260 DEG C of die head temperatures.
Embodiment 3:
In Situ Compatibilization is prepared super-toughened nylon 66 nano composite material and is coordinated and formed by the raw material of following weight part: nylon 66(PA66) 70 parts, 30 parts of terpolymer EP rubbers (EPDM), 2,5-dimethyl-2,0.1 part of 5-di-t-butyl hexane peroxide (L-101), 1 part of MALEIC ANHYDRIDE (MAH), 5 parts of organo montmorillonites (OMMT).
In Situ Compatibilization is prepared the method for super-toughened nylon 66 nano composite material, comprises the following steps:
(1), by initiator 2,5-dimethyl-2,5-di-t-butyl hexane peroxide (L-101) and MALEIC ANHYDRIDE (MAH) are dissolved in acetone, obtain mixing solutions, place for subsequent use;
(2), nylon 66 is placed in to vacuum drying oven and carries out drying and processing, control oven temperature at 90 DEG C, dry 4 hours, EPDM is placed in vacuum drying oven and carries out drying and processing, control oven temperature at 70 DEG C, dry 4 hours, then nylon 66 and EPDM are cooled to room temperature, the nylon 66 carrying out after drying and processing is mixed according to the above ratio with EPDM, obtain blend;
(3), the mixing solutions in step (1) is poured in the blend of nylon 66 and EPDM, obtain premix, premix is positioned in air, and thinner acetone is volatilized away;
(4), the premix mixing is placed in to parallel double-screw extruder, and add after OMMT in the side direction Si district of parallel double-screw extruder (Gong Ba district), melt extrude granulation.Complete processing is as follows: parallel double-screw extruder screw speed is 75r/min, 170 DEG C of district's temperature, two 200 DEG C of district's temperature, three 255 DEG C of district's temperature, four 265 DEG C of district's temperature, five 265 DEG C of district's temperature, six 265 DEG C of district's temperature, seven 265 DEG C of district's temperature, 260 DEG C of die head temperatures.
The scanning electron microscope (SEM) photograph (2000 times) of the super-toughened nylon 66 nano composite material of the present embodiment gained as shown in Figure 3, has shown EPDM and the OMMT dispersing morphology in PA66 in figure.As can be seen from Figure 3, section has obvious crazing-shear zone to produce, and phase interface becomes very fuzzy, and EPDM particle and OMMT particle are scattered in the matrix of nylon 66 well, show as ductile rupture.
Embodiment 4:
In Situ Compatibilization is prepared super-toughened nylon 66 nano composite material and is coordinated and formed by the raw material of following weight part: nylon 66(PA66) 70 parts, 30 parts of terpolymer EP rubbers (EPDM), 2,5-dimethyl-2,1 part of 5-di-t-butyl hexane peroxide (L-101), 4 parts of MALEIC ANHYDRIDE (MAH), 5 parts of organo montmorillonites (OMMT).
In Situ Compatibilization is prepared the method for super-toughened nylon 66 nano composite material, and its step is with embodiment 3.
Embodiment 5:
In Situ Compatibilization is prepared super-toughened nylon 66 nano composite material and is coordinated and formed by the raw material of following weight part: nylon 66(PA66) 70 parts, 30 parts of terpolymer EP rubbers (EPDM), 2,5-dimethyl-2,0.01 part of 5-di-t-butyl hexane peroxide (L-101), 0.1 part of MALEIC ANHYDRIDE (MAH), 5 parts of organo montmorillonites (OMMT).
In Situ Compatibilization is prepared the method for super-toughened nylon 66 nano composite material, and its step is with embodiment 3.
Embodiment 6:
In Situ Compatibilization is prepared super-toughened nylon 66 nano composite material and is coordinated and formed by the raw material of following weight part: nylon 66(PA66) 70 parts, 30 parts of terpolymer EP rubbers (EPDM), 2,5-dimethyl-2,0.1 part of 5-di-t-butyl hexane peroxide (L-101), 1 part of MALEIC ANHYDRIDE (MAH), 1 part of organo montmorillonite (OMMT).
In Situ Compatibilization is prepared the method for super-toughened nylon 66 nano composite material, and its step is with embodiment 3.
Embodiment 7:
In Situ Compatibilization is prepared super-toughened nylon 66 nano composite material and is coordinated and formed by the raw material of following weight part: nylon 66(PA66) 70 parts, 30 parts of terpolymer EP rubbers (EPDM), 2,5-dimethyl-2,0.1 part of 5-di-t-butyl hexane peroxide (L-101), 1 part of MALEIC ANHYDRIDE (MAH), 3 parts of organo montmorillonites (OMMT).
In Situ Compatibilization is prepared the method for super-toughened nylon 66 nano composite material, and its step is with embodiment 3.
Be below comparative example and embodiment table look-up:
Table 1 comparative example and embodiment parts by weight of raw materials table look-up
Made the various embodiments described above sample is carried out to following performance test:
Tensile property: press GB/T1042-1992 standard testing, rate of extension 50mm/min;
Impact property: press 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 (the thick 25mm that is less than of sample) of 50 ± 1mm that sample is cut out, then put into the dry 24 ± 1h of 50 ± 2 DEG C of baking ovens, in moisture eliminator, be cooled to room temperature and be weighed as m1, sample is dipped in 23 ± 0.5 DEG C of distilled water, after soaking time 24 ± 1h, taking out and using water clean, that dry filter paper is wiped rapidly specimen surface again to weigh sample is m again
2.Water-intake rate
W
mcalculation formula be:
Table 2 comparative example and embodiment performance table look-up
Comparative example 1 is pure PA66, and comparative example 2 is for to add the ex situ increase-volume of organo montmorillonite (OMMT) to prepare Nylon 66 Nano-composites; Embodiment 1～3 prepares super-toughened nylon 66 nano composite material for In Situ Compatibilization, the weight ratio of fixing initiator and MAH is 1:10, and adjust the weight ratio of PA66 and EPDM, can find out in the time that the addition of EPDM is 30 parts, normal temperature and the low temperature notched shock strength of nano composite material are the highest, and water-intake rate is minimum; Embodiment 4～7 prepares super-toughened nylon 66 nano composite material for In Situ Compatibilization, the weight ratio of fixing PA66 and EPDM is 70:30, and adjust the addition of initiator, MAH and OMMT, can find out that the over-all properties of embodiment 3 nano composite materials will be got well compared to the over-all properties of embodiment 4～7 nano composite materials.
Embodiments of the invention flow process is referring to Fig. 1; Embodiments of the invention reaction mechanism is referring to Fig. 2; Embodiments of the invention 3 scanning electron microscope (SEM) photographs (2000 times) are referring to Fig. 3.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, 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 claims.
Claims (6)
1. a super-toughened nylon 66 nano composite material, is characterized in that, its raw material composition and weight part are:
Described initiator is dicumyl peroxide or 2,5-dimethyl-2,5-di-t-butyl hexane peroxide;
The preparation method of super-toughened nylon 66 nano composite material comprises the steps:
(1), described weight part initiator and MALEIC ANHYDRIDE are dissolved in thinner, obtain mixing solutions, place for subsequent use;
(2), described weight part nylon 66 is placed in to vacuum drying oven and carries out drying and processing, control oven temperature at 80～100 DEG C, dry 4～12 hours, described weight part terpolymer EP rubber is placed in vacuum drying oven and carries out drying and processing, control oven temperature at 60～80 DEG C, dry 4～12 hours, then nylon 66 and terpolymer EP rubber are cooled to room temperature, the nylon 66 carrying out after drying and processing is mixed in proportion with terpolymer EP rubber, obtain blend;
(3), the mixing solutions in step (1) is poured in the blend of nylon 66 and terpolymer EP rubber, obtain premix, premix is positioned in air, and thinner is volatilized away;
(4), the premix mixing is placed in to parallel double-screw extruder, and add after organo montmorillonite in the side direction Si district of parallel double-screw extruder, melt extrude, granulation, to obtain final product;
Complete processing is as follows: parallel double-screw extruder screw speed is 25～200r/min, one 150～260 DEG C of district's temperature, two 170～280 DEG C of district's temperature, three 250～285 DEG C of district's temperature, four 250～285 DEG C of district's temperature, five 250～285 DEG C of district's temperature, six 250～285 DEG C of district's temperature, seven 250～285 DEG C of district's temperature, 250～285 DEG C of die head temperatures.
2. In Situ Compatibilization is prepared a method for super-toughened nylon 66 nano composite material described in claim 1, it is characterized in that, comprises the following steps:
(1), described weight part initiator and MALEIC ANHYDRIDE are dissolved in thinner, obtain mixing solutions, place for subsequent use;
(2), described weight part nylon 66 is placed in to vacuum drying oven and carries out drying and processing, control oven temperature at 80～100 DEG C, dry 4～12 hours, described weight part terpolymer EP rubber is placed in vacuum drying oven and carries out drying and processing, control oven temperature at 60～80 DEG C, dry 4～12 hours, then nylon 66 and terpolymer EP rubber are cooled to room temperature, the nylon 66 carrying out after drying and processing is mixed in proportion with terpolymer EP rubber, obtain blend;
(3), the mixing solutions in step (1) is poured in the blend of nylon 66 and terpolymer EP rubber, obtain premix, premix is positioned in air, and thinner is volatilized away;
(4), the premix mixing is placed in to parallel double-screw extruder, and add after organo montmorillonite in the side direction Si district of parallel double-screw extruder, melt extrude, granulation, to obtain final product;
Complete processing is as follows: parallel double-screw extruder screw speed is 25～200r/min, one 150～260 DEG C of district's temperature, two 170～280 DEG C of district's temperature, three 250～285 DEG C of district's temperature, four 250～285 DEG C of district's temperature, five 250～285 DEG C of district's temperature, six 250～285 DEG C of district's temperature, seven 250～285 DEG C of district's temperature, 250～285 DEG C of die head temperatures.
3. preparation method according to claim 2, is characterized in that, comprises the following steps:
(1), described weight part initiator and MALEIC ANHYDRIDE are dissolved in thinner acetone, obtain mixing solutions, place for subsequent use;
(2), described weight part nylon 66 is placed in to vacuum drying oven and carries out drying and processing, control oven temperature at 80～100 DEG C, dry 4～8 hours, described weight part terpolymer EP rubber is placed in vacuum drying oven and carries out drying and processing, control oven temperature at 60～80 DEG C, dry 4～8 hours, then nylon 66 and terpolymer EP rubber are cooled to room temperature, the nylon 66 carrying out after drying and processing is mixed in proportion with terpolymer EP rubber, obtain blend;
(3), the mixing solutions in step (1) is poured in the blend of nylon 66 and terpolymer EP rubber, obtain premix, premix is positioned in air, and thinner acetone is volatilized away;
(4), the premix mixing is placed in to parallel double-screw extruder, and add after organo montmorillonite in the side direction Si district of parallel double-screw extruder, melt extrude, granulation, to obtain final product;
Complete processing is as follows: parallel double-screw extruder screw speed is 25～100r/min, one 150～200 DEG C of district's temperature, two 170～210 DEG C of district's temperature, three 250～270 DEG C of district's temperature, four 260～270 DEG C of district's temperature, five 260～270 DEG C of district's temperature, six 260～270 DEG C of district's temperature, seven 260～270 DEG C of district's temperature, 260～270 DEG C of die head temperatures.
4. preparation method according to claim 2, is characterized in that, described thinner is acetone, butanone.
5. preparation method according to claim 2, is characterized in that, described screw rod is shaped as single thread; The ratio L/D of spiro rod length L and diameter D is 20～60.
6. preparation method according to claim 2, is characterized in that, described screw rod must have more than one gear block district, and described screw rod must have more than one left-hand thread district.
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| CN102796229A (en) * | 2012-03-12 | 2012-11-28 | 东莞市信诺橡塑工业有限公司 | Super-nylon 66 alloy prepared by in-situ reactive compatibilization method and preparation method thereof |
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| CN102796229A (en) * | 2012-03-12 | 2012-11-28 | 东莞市信诺橡塑工业有限公司 | Super-nylon 66 alloy prepared by in-situ reactive compatibilization method and preparation method thereof |
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