CN104250438B - A kind of plasticizing enhancement nylon composite and preparation method - Google Patents
A kind of plasticizing enhancement nylon composite and preparation method Download PDFInfo
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- CN104250438B CN104250438B CN201310264255.4A CN201310264255A CN104250438B CN 104250438 B CN104250438 B CN 104250438B CN 201310264255 A CN201310264255 A CN 201310264255A CN 104250438 B CN104250438 B CN 104250438B
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- nylon composite
- toughener
- antioxidant
- plasticizing
- plasticizing enhancement
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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
Abstract
The invention discloses a kind of plasticizing enhancement nylon composite and preparation method.Described nylon composite materials includes the following components being blended: nylon 6 resin 100 weight portion；Glass fibre 10～70 weight portion；Toughener 0.1～1 weight portion；Auxiliary agent 0.3 1.4 weight portion；The amides compound that described toughener is is load with nano silicon；Described auxiliary agent includes lubricant and antioxidant.Preparation method includes: described component is by preparing described plasticizing enhancement nylon composite after described consumption melt blending.The present invention is not only greatly improved the impact property of nylon composite materials, and its hot strength, bending strength and bending modulus are strengthened the most simultaneously.
Description
Technical field
The present invention relates to nylon field, say further, relate to a kind of plasticizing enhancement nylon composite and preparation side
Method.
Background technology
Nylon 6 is a kind of purposes engineering plastics widely, caprolactam polymerization prepare, and its fusing point is 215～225
DEG C, use temperature range at-40 DEG C～150 DEG C, owing to common nylon 6 is affected by temperature and environment, performance there will be significantly
Degree change, so its application receives greatly restriction.There is the shortcomings such as impact strength is relatively low without modified nylon, limit
Its application.Therefore, it can by it is filled with enhancing modified so that it is combination property is obviously improved.
The nylon used on automobile mostly is activeness and quietness nylon, and its Enhancement Method mainly fills inorganic filler, such as glass
Fiber (GF) and carbon fiber (CF)；Method to toughening nylon is addition rubber elastomer in nylon matrix.Rubber elastomer
At nylon matrix dispersibility, with matrix poor compatibility.On the other hand, due to the easy oxidation stain of rubber, cause outside nylon product
Sight color and luster is poor, affects attractive in appearance.
Introducing other reinforcements in addition to glass fibre is to improve the most scattered effective ways of glass fibre, its
Principle is to utilize the feature of the autohemagglutination power that the active force between them is weaker than reinforcement of the same race relatively, overcomes its autohemagglutination to be inclined to,
Make reinforcement form fine dispersion in blending procedure, thus give full play to the respective advantage of different reinforcement, embody good
Sintering action, the common macro property improving composite.The common composite strengthening system based on glass fibre has: glass
Fiber/carbon fiber, glass fibre/nanometer particle, glass fibre/inorganic mineral etc..
Chinese patent CN102719092A discloses a kind of composite enhancement nylon compositions, compositions by nylon, carbon fiber,
Glass fibre, nano imvite, toughener form；Patent CN102212205A discloses a kind of fiberglass composite reinforced material
And preparation method thereof, it is that resin spinning is formed polymer fiber, glass and polymer fiber regular volume under electric field action
It is woven in together, defines glass composite reinforcing material.Chinese patent CN101851417A discloses a kind of low-cost and high-performance glass
Glass fiber reinforced nylon 6 composite and preparation method thereof, this composite includes nylon, compatibilization and toughening agent, whisker, nucleation
Agent, glass fibre, antioxidant etc..The tensile property of glass fibre reinforced nylon or bending modulus can obtain the biggest enhancing, but
Bring the decline of toughness, be reflected as the decline of impact strength.
Summary of the invention
For solving problems of the prior art, the invention provides a kind of plasticizing enhancement nylon composite and preparation
Method.The toughener of the present invention be nano silicon be load amides compound.Hydrophilic gas phase nano silicon dioxide
Particle, is processed by sense dough, interacts with the amides compound with amide group, and amides compound absorption exists
Nano-silica surface.Become hydrophobicity by the nano silicon so processed by hydrophilic, greatly reduce particle
Between interaction, decrease particle aggregation, thus be better dispersed in matrix playing the effect of toughener.Glass fibre and
Toughener acts on jointly so that the every mechanical property of modified nylon resin increases substantially more than 100%.
An object of the present invention is to provide a kind of plasticizing enhancement nylon composite.
Following components including being blended:
Nylon 6 resin 100 weight portion；
Glass fibre 10～70 weight portion；Preferably: 20～50 weight portions；
Toughener 0.1～1 weight portion；Preferably: 0.1～0.5 weight portion；
Auxiliary agent 0.3-1.4 weight portion；Preferably: 0.3-1.0 weight portion.
Described nylon 6 resin is the range of viscosities polyamide at 2.4-2.9；
Described glass fibre is a kind of surface alkali-free glass fibre through coupling agent modified process, and a diameter of 8-15 is micro-
Rice.
The amides compound that described toughener is is load with nano silicon；It is by hydrophilic gas phase nano dioxy
SiClx and amides compound are prepared from, and the weight ratio of hydrophilic gas phase nano silicon dioxide and amides compound is 90:
10～10:90 are preferably 80:20～50:50.
Amides compound 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 toughener includes: by hydrophilic gas phase nano silicon dioxide with amides compound by described
Consumption mixes, and is dissolved in ethanol or glycerol, stands, solidifies, prepares described toughener granule after drying after stirring.
Wherein said hydrophilic gas phase nano silicon dioxide refers to the nano silicon prepared with hydrophilic vapor phase method.
Described auxiliary agent is the common auxiliary agent of nylon manufacture field, generally comprises lubricant and antioxidant, lubricant and antioxygen
Agent can be selected for the lubricant generally used and the antioxidant of nylon manufacture field, in the present invention lubricant can use erucyl amide,
One in stearic amide, oleamide, antioxidant can use antioxidant 1098 to compound by weight 1:1 with irgasfos 168
Form.Lubricant and antioxidant ratio are preferably 1:3.Also can add other auxiliary agents, such as: antistatic additive, resistance according to practical situation
Combustion agent, releasing agent, dyestuff, montmorillonite, Muscovitum, nucleator etc..
The two of the purpose of the present invention are to provide the preparation method of a kind of plasticizing enhancement nylon composite.
Including: described component is by preparing described plasticizing enhancement nylon composite after described consumption melt blending.
The preparation method of the present invention can use the common preparation method of nylon processing in this area, specifically can be by following step
Suddenly carry out:
Nylon 6 resin, toughener, other auxiliary agents are mixed in high speed agitator discharging in 0.5～5 minute mixed
Thing, then controls processing temperature 200-240 DEG C of double screw extruder, screw speed 200～400 revs/min, is placed in by mixture
Double screw extruder, glass fibre and from glass fibre mouth enter, extruding pelletization, obtain product.
It is an advantage of the current invention that use amides compound is nylon toughener, it is to avoid the rubber toughened variable color brought
With problems such as the compatibilitys.There is siloxanes and silanol in hydrophilic gas phase nano silica particles, with amide-type
Compound is together after the reason of official's energy dough surface, and amides compound is supported on silica surface, silica surface
Becoming hydrophobicity, the interphase interaction of granule reduces, and reduce further the reunion of nano-particle, so that amides compound
Can more preferably with less size dispersion between matrix.Silicon dioxide also plays nucleation simultaneously and promotes the effect of crystallization.
And strengthening action is played in the addition of glass fibre.The impact property of nylon composite materials is not only greatly improved,
Its hot strength, bending strength and bending modulus are strengthened the most simultaneously so that the every mechanical property of modified nylon resin
More than 100% can be increased substantially.
Detailed description of the invention
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.
Hydrophilic gas phase nano silicon dioxide, particle diameter 4-50nm, AEROSIL company produces.
Amides compound: N, N '-dicyclohexyl-2,6-aphthalimide, N, N, N ', N '-tetraalkyl paraphenylene terephthalamide
Amine, Isosorbide-5-Nitrae-penylene dicyclohexyl Methanamide, commercially available prod.
Antioxidant 1098, irgasfos 168, BASF Ciba produces.
Lubricant: erucyl amide, oleamide, stearic amide, commercially available.
The preparation of toughener:
Embodiment 1
First 9g aerosil sample is put in 250ml beaker, adds 75ml ethanol wet, be subsequently adding 1g N,
N '-dicyclohexyl-2,6-aphthalimide, stand after stirring at normal temperature, be dried after material solidification, it is thus achieved that with nano silicon be
The hydrophobicity toughener granule 1 of load.
Embodiment 2
First 8g aerosil sample is put in 250ml beaker, adds 75ml ethanol wet, be subsequently adding 2g N,
N '-dicyclohexyl-2,6-aphthalimide, stand after stirring at normal temperature, be dried after material solidification, it is thus achieved that with nano silicon be
The hydrophobicity toughener granule 2 of load.
Embodiment 3
First 5g aerosil sample is put in 250ml beaker, adds 75ml ethanol wet, be subsequently adding 5g N,
N '-dicyclohexyl-2,6-aphthalimide, stand after stirring at normal temperature, be dried after material solidification, it is thus achieved that with nano silicon be
The hydrophobicity toughener granule 3 of load.
Embodiment 4
First 1g aerosil sample is put in 250ml beaker, adds 75ml ethanol wet, be subsequently adding 9g N,
N '-dicyclohexyl-2,6-aphthalimide, stand after stirring at normal temperature, be dried after material solidification, it is thus achieved that with nano silicon be
The hydrophobicity toughener granule 4 of load.
Embodiment 5
First 8g aerosil sample is put in 250ml beaker, adds 75ml ethanol wet, be subsequently adding 2g N,
N, N ', N '-tetraalkyl terephthalamide, stand after stirring at normal temperature, be dried after material solidification, it is thus achieved that with nano silicon be
The hydrophobicity toughener granule 5 of load.
Embodiment 6
First 5g aerosil sample is put in 250ml beaker, adds 75ml ethanol wet, be subsequently adding 5g N,
N, N ', N '-tetraalkyl terephthalamide, stand after stirring at normal temperature, be dried after material solidification, it is thus achieved that with nano silicon be
The hydrophobicity toughener granule 6 of load.
Embodiment 7
First 1g aerosil sample is put in 250ml beaker, adds 75ml ethanol wet, be subsequently adding 9g N,
N, N ', N '-tetraalkyl terephthalamide, stand after stirring at normal temperature, be dried after material solidification, it is thus achieved that with nano silicon be
The hydrophobicity toughener granule 7 of load.
Embodiment 8
First 8g aerosil sample is put in 250ml beaker, adds 80ml glycerol moistening, be subsequently adding 2g1,
4-penylene dicyclohexyl Methanamide, stands after stirring at normal temperature, is dried, it is thus achieved that with nano silicon for load after material solidification
Hydrophobicity toughener granule 8.
Embodiment 9
First 5g aerosil sample is put in 250ml beaker, adds 80ml glycerol moistening, be subsequently adding 5g1,
4-penylene dicyclohexyl Methanamide, stands after stirring at normal temperature, is dried, it is thus achieved that with nano silicon for load after material solidification
Hydrophobicity toughener granule 9.
The preparation of plasticizing enhancement nylon composite:
Respectively nylon 6, toughener, antioxidant and lubricant are together added in high speed agitator, motor speed 1300 turns/
Point, at room temperature mixing was taken out after 2 minutes, the material mixed was added in the hopper of Ф 25 double screw extruder, glass fibre
Be simultaneously introduced from side feeding mouth, through melting, extrude, cooling down, pelletize can be prepared by fiberglass reinforced tenacity increased nylon composite material.Double
Screw extruder controls at 200-210 DEG C, 210-220 DEG C, 210-230 DEG C, 200-respectively from the temperature of first paragraph to the 5th section
240 DEG C, head temperature is at 200-240 DEG C, and screw speed is at 200～400 revs/min.Cooling water temperature is 20-40 DEG C.It is molded into
Each section of temperature 190-240 DEG C of type machine, it is thus achieved that embodiment 10-45.
Embodiment 10-45 and each composition proportion of comparative example 1-12 are described in table 1.Unit is parts by weight.Embodiment 10-25
And comparative example 1-6 is with lubricator erucyl amide, antioxidant is antioxidant 1098, compounding of irgasfos 168, and ratio is 1:
1.Lubricant and antioxidant ratio are 1:3.
Being with lubricator oleamide in embodiment 28-37 and comparative example 7-9, antioxidant is antioxidant 1098, antioxygen
Compounding of agent 168, ratio is 1:1.Lubricant and antioxidant ratio are 1:2.
It embodiment 38-45 and comparative example 10-12 is with lubricator stearic amide.Antioxidant is antioxidant 1098,
Compounding of irgasfos 168, ratio is 2:1.Lubricant and antioxidant ratio are 1:3.
Table 1. activeness and quietness nylon composite materials formula
Other auxiliary agents in * table 1 are antioxidant and lubricant
Mechanics Performance Testing
Sample quantitative measurement is carried out by national standard respectively: hot strength carries out stretching by ASTM D638-03 and surveys
Examination, rate of extension is 50mm/min；Bending strength is tested by ASTM D790-07, and loading velocity is 1.3mm/min；Impact
Intensity is tested by ASTM D256-06a, uses V-notch, maximum impact energy 2.75J；
Test result is listed in table 2.
Table 2. is toughness reinforcing strengthens dragon composite materials property
From the mechanical performance data of table 2 it can be seen that after adding toughener, the hot strength of nylon 6, bending are by force
Degree, impact strength and bending modulus have raising in various degree, in embodiment 44-45, add the stretching of the nylon 6 of toughener
Strength ratio improves 12% without toughener, and impact strength improves 12%, and bending modulus increases by 10%, improves Buddhist nun the most simultaneously
Tensile property, toughness and the rigidity of dragon.
Claims (8)
1. a plasticizing enhancement nylon composite, it is characterised in that include the following components being blended:
The amides compound that described toughener is is load with nano silicon, described amides compound is aromatic amine
Compound, structural formula is R1-NHCO-Y-CONH-R2 or R1-NHCO-Y-NHCO-R2, or R1-CONH-Y-NHCO-R2, R1, R2
Being saturated alkyl or cycloalkyl, Y is phenyl ring or naphthalene nucleus；
Described auxiliary agent includes lubricant and antioxidant.
2. plasticizing enhancement nylon composite as claimed in claim 1, it is characterised in that:
Described toughener is to be prepared from by hydrophilic gas phase nano silicon dioxide and amides compound, hydrophilic gas phase nano
The weight ratio of silicon dioxide and amides compound is 90:10～10:90.
3. plasticizing enhancement nylon composite as claimed in claim 2, it is characterised in that:
Described hydrophilic gas phase nano silicon dioxide and weight ratio 80:20 of amides compound～50:50.
4. plasticizing enhancement nylon composite as claimed in claim 2, it is characterised in that:
The preparation method of described toughener includes: by hydrophilic gas phase nano silicon dioxide with amides compound by described consumption
Mixing, is dissolved in ethanol or glycerol, stands, solidifies, prepares toughener granule after drying after stirring.
5. plasticizing enhancement nylon composite as claimed in claim 1, it is characterised in that include the following components being blended:
6. plasticizing enhancement nylon composite as claimed in claim 1, it is characterised in that:
Described lubricant is the one in erucyl amide, stearic amide, oleamide, and antioxidant is antioxidant 1098 and antioxygen
Agent 168 forms by weight 1:1 is compounding.
7. plasticizing enhancement nylon composite as claimed in claim 6, it is characterised in that:
Described lubricant and antioxidant ratio are 1:3.
8. the preparation method of the plasticizing enhancement nylon composite as described in one of claim 1～7 includes:
Described component is by preparing described plasticizing enhancement nylon composite after described consumption melt blending.
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Families Citing this family (6)
| 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 |
| CN107501695B (en) * | 2017-10-10 | 2020-08-25 | 宏岳塑胶集团股份有限公司 | Antibacterial polyethylene pipe 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 |
| 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 |
| 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 |
| 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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| CN101724258A (en) * | 2008-10-31 | 2010-06-09 | 比亚迪股份有限公司 | Nylon composition, method for preparing same and application thereof |
| CN102558852A (en) * | 2011-12-16 | 2012-07-11 | 深圳市富恒塑胶新材料有限公司 | Low-cost flame-retardant glass fiber reinforced polyamide 6 (PA6) engineering plastic and preparation method thereof |
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| CN101412845A (en) * | 2007-10-16 | 2009-04-22 | 佛山市顺德区高怡新塑料有限公司 | High performance fiber reinforced nylon composite material and preparation thereof |
| CN101249964A (en) * | 2008-03-07 | 2008-08-27 | 南京工业大学 | Method for preparing super-hydrophobic silica |
| CN101724258A (en) * | 2008-10-31 | 2010-06-09 | 比亚迪股份有限公司 | Nylon composition, method for preparing same and application thereof |
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