CN104250438A - Toughening and enhancing nylon composite material and preparation method thereof - Google Patents
Toughening and enhancing nylon composite material and preparation method thereof Download PDFInfo
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- CN104250438A CN104250438A CN201310264255.4A CN201310264255A CN104250438A CN 104250438 A CN104250438 A CN 104250438A CN 201310264255 A CN201310264255 A CN 201310264255A CN 104250438 A CN104250438 A CN 104250438A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a toughening and enhancing nylon composite material and a preparation method thereof. The nylon composite material comprises the following components: 100 parts of nylon 6 resin, 10-70 parts of glass fibre, 0.1-1 part of flexibilizer, and 0.3-1.4 parts of auxiliary agent. The flexibilizer is amide compound by taking nano silica as a support, and the auxiliary agent comprises a lubricant and an anti-oxidant. The preparation method is characterized in that the components are performed with melt blending according to the amount to prepare the toughening and enhancing nylon composite material. The method greatly increases the impact performance of the nylon composite material, and the tensile strength, bending strength and flexural modulus of the composite material can be simultaneously enhanced.
Description
Technical field
The present invention relates to nylon field, say further, relate to a kind of plasticizing enhancement nylon matrix material and preparation method.
Background technology
Nylon 6 is a kind of purposes engineering plastics widely, is obtained by caprolactam polymerization, and its fusing point is 215 ~ 225 DEG C, use temperature scope is at-40 DEG C ~ 150 DEG C, because common nylon 6 is by the impact of temperature and environment, performance there will be and significantly changes, so its application receives very big restriction.There is the shortcomings such as shock strength is lower in the nylon without modification, limits its application.Therefore, can, by carrying out filling enhancing modified to it, its over-all properties obviously be promoted.
The nylon that automobile uses mostly is activeness and quietness nylon, and its Enhancement Method mainly fills mineral filler, as glass fibre (GF) and carbon fiber (CF); Add rubber elastomer in nylon matrix to the method for toughening nylon.Rubber elastomer is dispersed at nylon matrix, with matrix poor compatibility.On the other hand, due to the easy oxidation stain of rubber, cause nylon product appearance luster poor, affect attractive in appearance.
Other reinforcements introduced except glass fibre are effective ways that raising glass fibre disperses in the base, its principle is to utilize the reactive force between them to be relatively weaker than the feature of the autohemagglutination power of reinforcement of the same race, overcome its autohemagglutination tendency, reinforcement is made to form good distribution in blending procedure, thus give full play to the respective advantage of different reinforcement, embody good sintering action, the common macro property improving matrix material.The common composite strengthening system based on glass fibre has: glass fibre/carbon fiber, glass fibre/nanometer particle, glass fibre/inorganic mineral etc.
Chinese patent CN102719092A discloses a kind of composite enhancement nylon composition, and composition is made up of nylon, carbon fiber, glass fibre, nano imvite, toughner; Patent CN102212205A discloses a kind of fiberglass composite reinforced material and preparation method thereof, is resin spinning is formed polymer fiber, glass and polymer fiber is regular under electric field action is woven together, and defines glass composite reinforcing material.Chinese patent CN101851417A discloses a kind of low-cost and high-performance glass fiber reinforced nylon 6 composite material and preparation method thereof, and this matrix material comprises nylon, compatibilization and toughening agent, whisker, nucleator, glass fibre, oxidation inhibitor etc.The tensile property of glass fibre reinforced nylon or modulus in flexure can obtain very large enhancing, but bring the decline of toughness, are reflected as the decline of shock strength.
Summary of the invention
For solving problems of the prior art, the invention provides a kind of plasticizing enhancement nylon matrix material and preparation method.The amides of toughner of the present invention to be nano silicon be load.Wetting ability gas phase nano silicon dioxide granule, by functionalization process, interact with the amides with amide group, amides is adsorbed on nano-silica surface.Become hydrophobicity by the nano silicon processed like this by wetting ability, greatly reduce interparticle interaction, decrease particle aggregation, thus disperse the effect playing toughner in the base better.Glass fibre and toughner acting in conjunction, make the every mechanical property of modified nylon resin increase substantially more than 100%.
An object of the present invention is to provide a kind of plasticizing enhancement nylon matrix material.
Comprise blended following component:
Nylon 6 100 weight part;
Glass fibre 10 ~ 70 weight part; Preferred: 20 ~ 50 weight parts;
Toughner 0.1 ~ 1 weight part; Preferred: 0.1 ~ 0.5 weight part;
Auxiliary agent 0.3-1.4 weight part; Preferred: 0.3-1.0 weight part.
Described Nylon 6 is the polyamide resin of range of viscosities at 2.4-2.9;
Described glass fibre is the alkali free glass fibre of a kind of surface through coupling agent modified process, and diameter is 8-15 micron.
Described toughner is take nano silicon as the amides of load; Be be prepared from by wetting ability gas phase nano silicon-dioxide and amides, the weight ratio of wetting ability gas phase nano silicon-dioxide and amides is that 90:10 ~ 10:90 is preferably 80:20 ~ 50:50.
Amides is aromatic amine compounds, and structural formula is R1-NHCO-Y-CONH-R2 or R1-NHCO-Y-NHCO-R2, or R1-CONH-Y-NHCO-R2, R1, R2 can be saturated alkyl or cycloalkyl, and Y can be phenyl ring or naphthalene nucleus.
The preparation method of described toughner comprises: wetting ability gas phase nano silicon-dioxide is mixed by described consumption with amides, is dissolved in ethanol or glycerol, leaves standstill after stirring, solidifies, dry after obtained described toughner particle.
Wherein said wetting ability gas phase nano silicon-dioxide refers to the nano silicon prepared with wetting ability vapor phase process.
Described auxiliary agent is the common auxiliary agent of nylon manufacture field, generally comprise lubricant and oxidation inhibitor, lubricant and oxidation inhibitor can select lubricant and the oxidation inhibitor of the usual employing of nylon manufacture field, in the present invention, lubricant can adopt the one in erucicamide, stearic amide, amine hydroxybenzene, and oxidation inhibitor can adopt oxidation inhibitor 1098 to form by weight 1:1 is composite with irgasfos 168.Lubricant and oxidation inhibitor ratio are preferably 1:3.Also can add other auxiliary agents according to practical situation, as: static inhibitor, fire retardant, releasing agent, dyestuff, polynite, mica, nucleator etc.
Two of object of the present invention is to provide a kind of preparation method of plasticizing enhancement nylon matrix material.
Comprise: described component is by described plasticizing enhancement nylon matrix material obtained after described consumption melt blending.
Preparation method of the present invention can adopt the common preparation method of nylon processing in this area, specifically can carry out according to the following steps:
Nylon 6, toughner, other auxiliary agents are mixed discharging in 0.5 ~ 5 minute in high speed agitator and obtains mixture, then the processing temperature 200-240 DEG C of twin screw extruder is controlled, screw speed 200 ~ 400 revs/min, mixture is placed in twin screw extruder, glass fibre and entering from glass fibre mouth, extruding pelletization, obtains product.
The invention has the advantages that, use amides is nylon toughener, avoids the rubber toughened problem such as variable color and consistency brought.There is siloxanes and silanol in wetting ability gas phase nano silica particles, with amides together after functionalization surface treatment, amides load is at silica sphere, silica sphere becomes hydrophobicity, the interphase interaction of particle reduces, reduce further the reunion of nano particle, thus make amides can better with less size dispersion between matrix.Silicon-dioxide also serves the effect that nucleation promotes crystallization simultaneously.
And strengthening action is played in adding of glass fibre.Not only increased substantially the impact property of nylon composite materials, its tensile strength, flexural strength and modulus in flexure are also enhanced simultaneously, make the every mechanical property of modified nylon resin increase substantially more than 100%.
Embodiment
Below in conjunction with embodiment, further illustrate the present invention.
Embodiment is raw materials used
Nylon 6, trade mark M2800, Mei Da company limited of Xinhui of Guangdong Province produces.
Glass fibre, diameter 8-15 micron, commercially available.
Wetting ability gas phase nano silicon-dioxide, particle diameter 4-50nm, AEROSIL company produces.
Amides: N, N '-dicyclohexyl-2,6-aphthalimide, N, N, N ', N '-tetraalkyl terephthalamide, Isosorbide-5-Nitrae-penylene dicyclohexyl methane amide, commercially available prod.
Oxidation inhibitor 1098, irgasfos 168, BASF vapour Bagong department produces.
Lubricant: erucicamide, amine hydroxybenzene, stearic amide, commercially available.
The preparation of toughner:
Embodiment 1
First 9g aerosil sample is put into 250ml beaker, add 75ml ethanol wet, then add 1g N, N '-dicyclohexyl-2,6-aphthalimide, leaves standstill after stirring at normal temperature, material solidifies rear drying, and obtaining with nano silicon is the hydrophobicity toughner particle 1 of load.
Embodiment 2
First 8g aerosil sample is put into 250ml beaker, add 75ml ethanol wet, then add 2g N, N '-dicyclohexyl-2,6-aphthalimide, leaves standstill after stirring at normal temperature, material solidifies rear drying, and obtaining with nano silicon is the hydrophobicity toughner particle 2 of load.
Embodiment 3
First 5g aerosil sample is put into 250ml beaker, add 75ml ethanol wet, then add 5g N, N '-dicyclohexyl-2,6-aphthalimide, leaves standstill after stirring at normal temperature, material solidifies rear drying, and obtaining with nano silicon is the hydrophobicity toughner particle 3 of load.
Embodiment 4
First 1g aerosil sample is put into 250ml beaker, add 75ml ethanol wet, then add 9g N, N '-dicyclohexyl-2,6-aphthalimide, leaves standstill after stirring at normal temperature, material solidifies rear drying, and obtaining with nano silicon is the hydrophobicity toughner particle 4 of load.
Embodiment 5
First 8g aerosil sample is put into 250ml beaker, add 75ml ethanol wet, then add 2g N, N, N ', N '-tetraalkyl terephthalamide, leave standstill after stirring at normal temperature, material solidifies rear drying, and obtaining with nano silicon is the hydrophobicity toughner particle 5 of load.
Embodiment 6
First 5g aerosil sample is put into 250ml beaker, add 75ml ethanol wet, then add 5g N, N, N ', N '-tetraalkyl terephthalamide, leave standstill after stirring at normal temperature, material solidifies rear drying, and obtaining with nano silicon is the hydrophobicity toughner particle 6 of load.
Embodiment 7
First 1g aerosil sample is put into 250ml beaker, add 75ml ethanol wet, then add 9g N, N, N ', N '-tetraalkyl terephthalamide, leave standstill after stirring at normal temperature, material solidifies rear drying, and obtaining with nano silicon is the hydrophobicity toughner particle 7 of load.
Embodiment 8
First 8g aerosil sample is put into 250ml beaker, add 80ml glycerol and soak, then add 2g1,4-penylene dicyclohexyl methane amide, leave standstill after stirring at normal temperature, material solidifies rear drying, and obtaining with nano silicon is the hydrophobicity toughner particle 8 of load.
Embodiment 9
First 5g aerosil sample is put into 250ml beaker, add 80ml glycerol and soak, then add 5g1,4-penylene dicyclohexyl methane amide, leave standstill after stirring at normal temperature, material solidifies rear drying, and obtaining with nano silicon is the hydrophobicity toughner particle 9 of load.
The preparation of plasticizing enhancement nylon matrix material:
Respectively nylon 6, toughner, oxidation inhibitor and lubricant are together added in high speed agitator, motor speed 1300 revs/min, take out after at room temperature mixing 2 minutes, the material mixed is added in the hopper of Ф 25 twin screw extruder, glass fibre adds from side feeding mouth simultaneously, through melting, extrude, cool, granulation can obtain fiberglass reinforced tenacity increased nylon composite material.Twin screw extruder from first paragraph to the temperature of the 5th section control respectively 200-210 DEG C, 210-220 DEG C, 210-230 DEG C, 200-240 DEG C, head temperature is at 200-240 DEG C, and screw speed is at 200 ~ 400 revs/min.Temperature of cooling water is 20-40 DEG C.Injection moulding machine each section of temperature 190-240 DEG C, obtains embodiment 10-45.
The each composition proportion of embodiment 10-45 and comparative example 1-12 is for described in table 1.Unit is parts by weight.Be with lubricator erucicamide in embodiment 10-25 and comparative example 1-6, oxidation inhibitor is oxidation inhibitor 1098, irgasfos 168 composite, and ratio is 1:1.Lubricant and oxidation inhibitor ratio are 1:3.
Be with lubricator amine hydroxybenzene in embodiment 28-37 and comparative example 7-9, oxidation inhibitor is oxidation inhibitor 1098, irgasfos 168 composite, and ratio is 1:1.Lubricant and oxidation inhibitor ratio are 1:2.
It is with lubricator stearic amide in embodiment 38-45 and comparative example 10-12.Oxidation inhibitor is oxidation inhibitor 1098, irgasfos 168 composite, and ratio is 2:1.Lubricant and oxidation inhibitor ratio are 1:3.
Table 1. activeness and quietness nylon composite materials is filled a prescription
Other auxiliary agents in * table 1 are oxidation inhibitor and lubricant
Mechanics Performance Testing
Sample quantitative measurement is undertaken by national standard respectively: tensile strength carries out Elongation test by ASTM D638-03, and rate of extension is 50mm/min; Flexural strength is tested by ASTM D790-07, and loading velocity is 1.3mm/min; Shock strength is tested by ASTM D256-06a, adopts V-notch, maximum impact energy 2.75J;
Test result lists in table 2.
Table 2. toughen and intensify dragon composite materials property
As can be seen from the mechanical performance data of table 2, after interpolation toughner, the tensile strength of nylon 6, flexural strength, shock strength and modulus in flexure have raising in various degree, in embodiment 44-45, the tensile strength of adding the nylon 6 of toughner improves 12% than what do not add toughner, shock strength improves 12%, and modulus in flexure increases by 10%, namely improves the tensile property of nylon, toughness and rigidity simultaneously.
Claims (8)
1. a plasticizing enhancement nylon matrix material, is characterized in that comprising blended following component:
Nylon 6 100 weight part;
Glass fibre 10 ~ 70 weight part;
Toughner 0.1 ~ 1 weight part;
Auxiliary agent 0.3-1.4 weight part;
Described toughner is take nano silicon as the amides of load;
Described auxiliary agent comprises lubricant and oxidation inhibitor.
2. plasticizing enhancement nylon matrix material as claimed in claim 1, is characterized in that:
Described toughner is prepared from by wetting ability gas phase nano silicon-dioxide and amides, and the weight ratio of wetting ability gas phase nano silicon-dioxide and amides is 90:10 ~ 10:90.
3. plasticizing enhancement nylon matrix material as claimed in claim 2, is characterized in that:
Weight ratio 80:20 ~ the 50:50 of described wetting ability gas phase nano silicon-dioxide and amides.
4. plasticizing enhancement nylon matrix material as claimed in claim 2, is characterized in that:
The preparation method of described toughner comprises: wetting ability gas phase nano silicon-dioxide is mixed by described consumption with amides, is dissolved in ethanol or glycerol, leaves standstill after stirring, solidifies, dry after obtained toughner particle.
5. plasticizing enhancement nylon matrix material as claimed in claim 1, is characterized in that comprising blended following component:
Nylon 6 100 weight part;
Glass fibre 20 ~ 50 weight part;
Toughner 0.1 ~ 0.5 weight part;
Auxiliary agent 0.3-1.0 weight part.
6. plasticizing enhancement nylon matrix material as claimed in claim 1, is characterized in that:
Described lubricant is the one in erucicamide, stearic amide, amine hydroxybenzene, and oxidation inhibitor is that oxidation inhibitor 1098 forms by weight 1:1 is composite with irgasfos 168.
7. plasticizing enhancement nylon matrix material as claimed in claim 6, is characterized in that:
Described lubricant and oxidation inhibitor ratio are 1:3.
8. the preparation method of the plasticizing enhancement nylon matrix material as described in one of claim 1 ~ 7 comprises:
Described component is by described plasticizing enhancement nylon matrix material obtained after described consumption melt blending.
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| CN104817727A (en) * | 2015-04-17 | 2015-08-05 | 广州合成材料研究院有限公司 | Carried antioxygen and preparation method thereof |
| CN107501695A (en) * | 2017-10-10 | 2017-12-22 | 宏岳塑胶集团股份有限公司 | A kind of antimicrobial form polyvinyl piping materials and preparation method thereof |
| CN110452530A (en) * | 2019-08-16 | 2019-11-15 | 东莞市众一新材料科技有限公司 | A kind of natural fiber reinforcement biology base nylon material and preparation method thereof |
| CN114437538A (en) * | 2020-10-30 | 2022-05-06 | 中国石油化工股份有限公司 | Long glass fiber reinforced nylon composite material and preparation method and application thereof |
| CN114437539A (en) * | 2020-10-30 | 2022-05-06 | 中国石油化工股份有限公司 | Reinforced nylon material and preparation method and application thereof |
| CN117582042A (en) * | 2023-11-21 | 2024-02-23 | 广东奔立尔实业集团有限公司 | School uniform with positioning function |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104817727A (en) * | 2015-04-17 | 2015-08-05 | 广州合成材料研究院有限公司 | Carried antioxygen and preparation method thereof |
| CN107501695A (en) * | 2017-10-10 | 2017-12-22 | 宏岳塑胶集团股份有限公司 | A kind of antimicrobial form polyvinyl piping materials and preparation method thereof |
| CN110452530A (en) * | 2019-08-16 | 2019-11-15 | 东莞市众一新材料科技有限公司 | A kind of natural fiber reinforcement biology base nylon material and preparation method thereof |
| CN114437538A (en) * | 2020-10-30 | 2022-05-06 | 中国石油化工股份有限公司 | Long glass fiber reinforced nylon composite material and preparation method and application thereof |
| CN114437539A (en) * | 2020-10-30 | 2022-05-06 | 中国石油化工股份有限公司 | Reinforced nylon material and preparation method and application thereof |
| CN114437539B (en) * | 2020-10-30 | 2024-02-13 | 中国石油化工股份有限公司 | Reinforced nylon material and preparation method and application thereof |
| CN117582042A (en) * | 2023-11-21 | 2024-02-23 | 广东奔立尔实业集团有限公司 | School uniform with positioning function |
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| CN104250438B (en) | 2016-08-17 |
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