CN102757556A - Nanodiamond powder-filled nylon composite material and preparation method thereof - Google Patents
Nanodiamond powder-filled nylon composite material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technological field of nylon composite materials and discloses a nanodiamond powder-filled nylon composite material and a preparation method thereof. The nanodiamond powder-filled nylon composite material comprises the following components in part by weight: 73-99.7 parts of nylon monomer, 0.1-5 parts of pretreated nanodiamond powder, 0-20 parts of deionized water, 0-0.5 parts of catalyst, 0.2-0.5 parts of antioxidant and 0-1 part of molecular weight regulating agent. The invention further discloses the preparation method of the nanodiamond powder-filled nylon composite material. Under the condition that the adding amount of the diamond powder is very small, the hardness and the strength of the nanodiamond powder-filled nylon composite material can be significantly improved and the wear resistance is greatly improved; and the nanodiamond powder-filled nylon composite material has the characteristics of good heat resistance, toughness and dimensional stability, low water absorption and the like, Therefore, the application range of the nanodiamond powder-filled nylon composite material is greatly widened.
Description
Technical field
The invention belongs to the nylon composite materials technical field, be specifically related to a kind of nano-diamond powder filling nylon composite material and preparation method thereof.
Background technology
Since mid-term in 20th century, the development of novel material is a dark horse, and makes rapid progress.Matrix material is because the designability of its excellent comprehensive performance and performance is widely used in aerospace and people's daily production, various fields in life.Nano material makes material self have small size effect, surface and interface effect etc., thereby makes it have many physics different with traditional material, chemical property owing to the material particular structural.
Nano diamond is that median size is the diadust of nanometer scale, and it has possessed the dual nature of nanoparticle and superhard material, huge specific surface area (300-400m
2/ g), a large amount of textural defect and surface oxygen functional group etc. make to have bigger potentiality aspect its novel material that has property in exploitation.At present, nano-diamond powder has application very widely in fields such as compound coating, oil dope, abrasive substance and metal-based nano diamond composites.In matrix material, adding the superhard material powder, to improve performance of composites be an important channel, but use method that the nano-scale bortz powder prepares matrix material also seldom.
Nylon formal name used at school polymeric amide, since developing by institute of du pont company central authorities and realize industriallization the thirties in 20th century, existing more than 60 year history.Because nylon has excellent mechanical property and electrical property preferably, have advantages such as wear-resisting, oil resistant, anti-solvent, self-lubricity, self-extinguishing, erosion resistance and good processing properties again, be widely used.Nylon is as engineering plastics, and its maximum shortcoming is that water-absorbent is bigger, thereby causes product size and changes of properties.In some Application Areas, performances such as the intensity of pure nylon resin, wear resistance, hardness often do not reach the performance requriements of material yet.
But, contain amido and carboxyl, under certain conditions, have the certain reaction activity at nylon macromolecular main chain end.Therefore, can carry out chemistry and physically modified, can overcome because water-absorbent can increase substantially other performance when bringing the shortcoming of product size and performance change more greatly through methods such as block, grafting, blend.Therefore, the output of nylon in engineering plastics ranks the first always, has become industrial indispensable structured materials such as automobile, electronic apparatus, machinery, electric, space flight and aviation.
Also do not increase the report of the over-all properties of resin at present through the method for in nylon resin, adding nano-diamond powder.
Summary of the invention
The objective of the invention is to propose a kind of nano-diamond powder filling nylon composite material, the intensity of this material, hardness, wear resistance and impact property can be enhanced simultaneously.
Another object of the present invention provides a kind of preparation method of above-mentioned nano-diamond powder filling nylon composite material.
Technical scheme of the present invention is following:
The invention provides a kind of nano-diamond powder filling nylon composite material, this nylon composite materials comprises following component and parts by weight:
Described nylon monomer select oneself lactan, nylon salt, nylon 612 salt, nylon 1010 salt, nylon 1212 salt, amido undeeanoic acid or amido laurostearic acid.
Described nano-diamond powder is through pre-treatment, and treatment step is following: in the autoclave, add the nano-diamond powder of 1~2kg and the concentrated nitric acid of 5-10L, and 150-180 ℃, stirred 5-8 hour, filter, extremely neutral with deionized water wash; Be the concentration of removing nano-diamond powder and 5-10L behind the trace impurity in 10% the sodium hydroxide solution adding autoclave; 100-150 ℃; Stirred 5-8 hour, and filtered, extremely neutral with deionized water wash; The concentration that dry back adds 5-10L is in 0.5% the silane coupling agent KH550 ethanolic soln, to soak into the 30-60min filtering drying; The nano-diamond powder sealing of handling well is preserved.
Described nano-diamond powder purity>=95%, median size are 3.2nm, specific surface area 246.02m
2/ g.
Described catalyzer is a tetrabutyl titanate.
Described oxidation inhibitor is selected from one or both the mixture in oxidation inhibitor 1098 or the oxidation inhibitor 168.
Described molecular weight regulator select oneself diacid, sebacic acid, undecane diacid or dodecanedioic acid.
The present invention also provides a kind of preparation method of above-mentioned nano-diamond powder filling nylon composite material, and this method may further comprise the steps:
(1) in reaction kettle, adds 73~99.6 parts nylon monomer, 0.1~5 part of pretreated nano-diamond powder, 0~20 part deionized water, 0~0.5 part catalyzer, 0.2~0.5 part oxidation inhibitor and 0~1 part molecular weight regulator, sealed reactor; Substitute vacuum towards nitrogen 3 times, start whipping appts, temperature transfers to 180-230 ℃, reaction 1-3 hour;
(2) temperature of reaction is risen to 240-285 ℃, pressure remains on 1.5-2.5MPa, reacts 2-4 hour, opens the venting valve; Slowly venting behind the recovery normal pressure, was reacted 1-2 hour; The open vacuum pump vacuumizes, and gauge pressure is-0.1MPA; Stop after 1-2 hour to stir, close vacuum pump, discharging obtains the nano-diamond powder filling nylon composite material.The present invention compares with prior art, has following advantage and beneficial effect:
The nylon composite materials of the present invention's preparation is under bortz powder addition few cases; Hardness, intensity just can have tangible lifting; Wear resisting property is greatly improved, and is higher than the effect that general weighting material such as carbon black, molybdenumdisulphide, silit etc. are filled, and to have thermotolerance, toughness, dimensional stability good for the nylon composite materials of invention preparation in addition; Characteristics such as water-intake rate is low have been widened the range of application of nylon material greatly.
Embodiment
Below in conjunction with embodiment the present invention is further described.
Nano-diamond powder purity>=95% of using among the following embodiment, median size 3.2nm, specific surface area 246.02m
2/ g.
The test of tensile property: GB1040/T-1992, plastic tensile method for testing performance, 1992. draw speed 5mm/min.
The test of bending property: GB/T 9341-2000, the bending property test of plastics.Trial speed 5mm/min.
The test of impact property: the socle girder notched Izod impact strength is according to GB/T1843-1996, plastics izodtest method, 1996.
The test of wear resisting property: adopt friction wear testing machine, mating plate is No. 45 steel loops of 40mm*10mm, and the whole back HRC that requires to quench is 40-45, and the outer round surface roughness is 0.4m, and specimen size is 16mm*15mm*7mm.Test conditions is under the room temperature DRY SLIDING, and rotating speed is 0.42m/s, and to time consuming 2h, loading is 196N.With the quality after the electronic balance weighing wearing and tearing.
Embodiment 1
(1) pre-treatment of nano-diamond powder: in the autoclave, add 1kg nano-diamond powder and 5L concentrated nitric acid, 180 ℃, stirred 5 hours, filter, extremely neutral with deionized water wash; After removing the impurity of trace, add nano-diamond powder and 5L sodium hydroxide solution (concentration 10%) in the autoclave once more, 100 ℃, stirred 5 hours, filter, extremely neutral with deionized water wash, drying; The bortz powder of handling is added in the silane coupling agent KH550 ethanolic soln (concentration 0.5%) of 5L, soaked into 30 minutes, filter, oven dry.The bortz powder sealing of handling well is preserved.
(2) in reaction kettle, add hexanolactam, 0.6 part of nano-diamond powder of handling of 79 parts, 20 parts deionized water, the oxidation inhibitor 168 that 0.2 part oxidation inhibitor is 1098,0.2 parts, sealed reactor.Substitute vacuum, towards nitrogen 3 times, start whipping appts, temperature transfers to 200 ℃, reacts pressurize 2 hours.
(3) temperature of reaction is risen to 250 ℃, pressure remains on 2MPa, reacts 4 hours.Open the venting valve, slowly venting behind the recovery normal pressure, was reacted 1 hour, and the open vacuum pump vacuumizes.(gauge pressure-0.1MPA), stop after 2 hours to stir is closed vacuum pump, and discharging obtains the nano-diamond powder filling nylon composite material.Concrete performance is seen table 1.
Embodiment 2
(1) pre-treatment of nano-diamond powder: in the autoclave, add 1kg nano-diamond powder and 8L concentrated nitric acid, 180 ℃, stirred 5 hours, filter, extremely neutral with deionized water wash; After removing the impurity of trace, add nano-diamond powder and 8L sodium hydroxide solution (concentration 10%) in the autoclave once more, 100 ℃, stirred 5 hours, filter, extremely neutral with deionized water wash, drying; The bortz powder of handling is added in the silane coupling agent KH550 ethanolic soln (concentration 0.5%) of 5L, soaked into 30 minutes, filter, oven dry.The bortz powder sealing of handling well is preserved.
(2) in reaction kettle, add nylon salt, 5 parts of nano-diamond powders of handling of 94.4 parts, 0.1 part hexanodioic acid, the oxidation inhibitor 168 that 0.2 part oxidation inhibitor is 1098,0.3 parts, sealed reactor.Substitute vacuum, towards nitrogen 3 times, start whipping appts, temperature transfers to 230 ℃, reacts pressurize 2 hours.
(3) temperature of reaction is risen to 285 ℃, pressure remains on 2MPa, reacts 4 hours.Open the venting valve, slowly venting behind the recovery normal pressure, was reacted 1 hour, and the open vacuum pump vacuumizes.(gauge pressure-0.1MPA), stop after 2 hours to stir is closed vacuum pump, and discharging obtains the nano-diamond powder filling nylon composite material.Concrete performance is seen table 1.
Embodiment 3
(1) pre-treatment of nano-diamond powder: in the autoclave, add 2kg nano-diamond powder and 10L concentrated nitric acid, 180 ℃, stirred 5 hours, filter, extremely neutral with deionized water wash; After removing the impurity of trace, add nano-diamond powder and 10L sodium hydroxide solution (concentration 10%) in the autoclave once more, 100 ℃, stirred 5 hours, filter, extremely neutral with deionized water wash, drying; Pretreated bortz powder is added in the silane coupling agent KH550 ethanolic soln (concentration 0.5%) of 10L, soaked into 30 minutes, filter, oven dry.The bortz powder sealing of handling well is preserved.
(2) in reaction kettle, add 98.2 parts amido undeeanoic acid, 0.5 part tetrabutyl titanate, 0.1 part of nano-diamond powder of handling, the undecane diacid that the oxidation inhibitor that 0.1 part oxidation inhibitor is 1098,0.1 parts is 168,1 parts, sealed reactor.Substitute vacuum, towards nitrogen 3 times, start whipping appts, temperature transfers to 180 ℃, reacts pressurize 1 hour.
(3) temperature of reaction is risen to 250 ℃, pressure remains on 2MPa, reacts 4 hours.Open the venting valve, slowly venting behind the recovery normal pressure, was reacted 1 hour, and the open vacuum pump vacuumizes.(gauge pressure-0.1MPA), stop after 1 hour to stir is closed vacuum pump, and discharging obtains the nano-diamond powder filling nylon composite material.Concrete performance is seen table 1.
Embodiment 4
(1) pre-treatment of nano-diamond powder: in the autoclave, add 1.5kg nano-diamond powder and 8L concentrated nitric acid, 180 ℃, stirred 5 hours, filter, extremely neutral with deionized water wash; After removing the impurity of trace, add nano-diamond powder and 10L sodium hydroxide solution (concentration 10%) in the autoclave once more, 100 ℃, stirred 5 hours, filter, extremely neutral with deionized water wash, drying; Pretreated bortz powder is added in the silane coupling agent KH550 ethanolic soln (concentration 0.5%) of 5L, soaked into 30 minutes, filter, oven dry.The bortz powder sealing of handling well is preserved.
(2) in reaction kettle, add 98.1 parts nylon 1010 salt, 1 part of nano-diamond powder of handling, the sebacic acid that the oxidation inhibitor that 0.2 part oxidation inhibitor is 1098,0.2 parts is 168,0.5 parts, sealed reactor.Substitute vacuum, towards nitrogen 3 times, start whipping appts, temperature transfers to 220 ℃, reacts pressurize 3 hours.
(3) temperature of reaction is risen to 270 ℃, pressure remains on 2MPa, reacts 3 hours.Open the venting valve, slowly venting behind the recovery normal pressure, was reacted 2 hours, and the open vacuum pump vacuumizes.(gauge pressure-0.1MPA), stop after 1 hour to stir is closed vacuum pump, and discharging obtains the nano-diamond powder filling nylon composite material.Concrete performance is seen table 1.
Embodiment 5
(1) pre-treatment of nano-diamond powder: in the autoclave, add 1.8kg nano-diamond powder and 5L concentrated nitric acid, 180 ℃, stirred 5 hours, filter, extremely neutral with deionized water wash; After removing the impurity of trace, add nano-diamond powder and 5L sodium hydroxide solution (concentration 10%) in the autoclave once more, 100 ℃, stirred 5 hours, filter, extremely neutral with deionized water wash, drying; Pretreated bortz powder is added in the silane coupling agent KH550 ethanolic soln (concentration 0.5%) of 10L, soaked into 30 minutes, filter, oven dry.The bortz powder sealing of handling well is preserved.
(2) in reaction kettle, add nylon 1212 salt, 3 parts of nano-diamond powders that part was handled of 96.4 parts, the dodecanedioic acid that the oxidation inhibitor that 0.2 part oxidation inhibitor is 1098,0.2 parts is 168,0.2 parts, sealed reactor.Substitute vacuum, towards nitrogen 3 times, start whipping appts, temperature transfers to 180 ℃, reacts pressurize 1 hour.
(3) temperature of reaction is risen to 240 ℃, pressure remains on 1.5MPa, reacts 4 hours.Open the venting valve, slowly venting behind the recovery normal pressure, was reacted 2 hours, and the open vacuum pump vacuumizes.(gauge pressure-0.1MPA), stop after 1 hour to stir is closed vacuum pump, and discharging obtains the nano-diamond powder filling nylon composite material.Concrete performance is seen table 1.
Embodiment 6
(1) pre-treatment of nano-diamond powder: in the autoclave, add 1.2kg nano-diamond powder and 7L concentrated nitric acid, 180 ℃, stirred 5 hours, filter, extremely neutral with deionized water wash; After removing the impurity of trace, add nano-diamond powder and 6L sodium hydroxide solution (concentration 10%) in the autoclave once more, 100 ℃, stirred 5 hours, filter, extremely neutral with deionized water wash, drying; Pretreated bortz powder is added in the silane coupling agent KH550 ethanolic soln (concentration 0.5%) of 8L, soaked into 30 minutes, filter, oven dry.The bortz powder sealing of handling well is preserved.
(2) in reaction kettle, add 96.9 parts amido laurostearic acid, 0.5 part tetrabutyl titanate, 2 parts of nano-diamond powders of handling, the dodecanedioic acid that the oxidation inhibitor that 0.2 part oxidation inhibitor is 1098,0.2 parts is 168,0.2 parts, sealed reactor.Substitute vacuum, towards nitrogen 3 times, start whipping appts, temperature transfers to 180 ℃, reacts pressurize 1 hour.
(3) temperature of reaction is risen to 250 ℃, pressure remains on 1.5MPa, reacts 4 hours.Open the venting valve, slowly venting behind the recovery normal pressure, was reacted 2 hours, and the open vacuum pump vacuumizes.(gauge pressure-0.1MPA), stop after 1 hour to stir is closed vacuum pump, and discharging obtains the nano-diamond powder filling nylon composite material.Concrete performance is seen table 1.
The performance table of each embodiment of table 1
The above-mentioned description to embodiment is can understand and use the present invention for ease of the those of ordinary skill of this technical field.The personnel of skilled obviously can easily make various modifications to these embodiment, and needn't pass through performing creative labour being applied in the General Principle of this explanation among other embodiment.Therefore, the invention is not restricted to the embodiment here, those skilled in the art are according to announcement of the present invention, and not breaking away from the improvement that category of the present invention makes and revise all should be within protection scope of the present invention.
Claims (8)
1. nano-diamond powder filling nylon composite material, it is characterized in that: this nylon composite materials comprises following component and parts by weight,
73~99.7 parts of nylon monomers,
0.1~5 part of nano-diamond powder,
0~20 part of deionized water,
0~0.5 part of catalyzer,
0.2~0.5 part in oxidation inhibitor,
0~1 part of molecular weight regulator.
2. nano-diamond powder filling nylon composite material according to claim 1 is characterized in that: described nylon monomer select oneself lactan, nylon salt, nylon 612 salt, nylon 1010 salt, nylon 1212 salt, amido undeeanoic acid or amido laurostearic acid.
3. nano-diamond powder filling nylon composite material according to claim 1; It is characterized in that: described nano-diamond powder is through pre-treatment, and treatment step is following: in the autoclave, add the nano-diamond powder of 1~2kg and the concentrated nitric acid of 5-10L; 150-180 ℃; Stirred 5-8 hour, and filtered, extremely neutral with deionized water wash; Be the concentration of removing nano-diamond powder and 5-10L behind the trace impurity in 10% the sodium hydroxide solution adding autoclave; 100-150 ℃; Stirred 5-8 hour, and filtered, extremely neutral with deionized water wash; The concentration that dry back adds 5-10L is in 0.5% the silane coupling agent KH550 ethanolic soln, to soak into the 30-60min filtering drying; The nano-diamond powder sealing of handling well is preserved.
4. nano-diamond powder filling nylon composite material according to claim 3 is characterized in that: described nano-diamond powder purity>=95%, median size are 3.2nm, specific surface area 246.02m
2/ g.
5. nano-diamond powder filling nylon composite material according to claim 1 is characterized in that: described catalyzer is a tetrabutyl titanate.
6. nano-diamond powder filling nylon composite material according to claim 1 is characterized in that: described oxidation inhibitor is selected from one or both the mixture in oxidation inhibitor 1098 or the oxidation inhibitor 168.
7. nano-diamond powder filling nylon composite material according to claim 1 is characterized in that: described molecular weight regulator select oneself diacid, sebacic acid, undecane diacid or dodecanedioic acid.
8. the preparation method of the arbitrary described nano-diamond powder filling nylon composite material of claim 1 to 7, it is characterized in that: this method may further comprise the steps,
(1) in reaction kettle, adds 73~99.7 parts nylon monomer, 0.1~5 part of pretreated nano-diamond powder, 0~20 part deionized water, 0~0.5 part catalyzer, 0.2~0.5 part oxidation inhibitor and 0~1 part molecular weight regulator, sealed reactor; Substitute vacuum towards nitrogen 3 times, start whipping appts, temperature transfers to 180-230 ℃, reaction 1-3 hour;
(2) temperature of reaction is risen to 240-285 ℃, pressure remains on 1.5-2.5MPa, reacts 2-4 hour, opens the venting valve; Slowly venting behind the recovery normal pressure, was reacted 1-2 hour; The open vacuum pump vacuumizes, and gauge pressure is-0.1MPA; Stop after 1-2 hour to stir, close vacuum pump, discharging obtains the nano-diamond powder filling nylon composite material.
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CN113061334A (en) * | 2020-01-02 | 2021-07-02 | 合肥杰事杰新材料股份有限公司 | Nylon 66 alloy and preparation method thereof |
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