CN109679216A - A kind of high rigid-tough balance, resistance to stress whiten, halogen-free flame retardant polypropylene composite material and preparation method thereof - Google Patents
A kind of high rigid-tough balance, resistance to stress whiten, halogen-free flame retardant polypropylene composite material and preparation method thereof Download PDFInfo
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- CN109679216A CN109679216A CN201811623435.6A CN201811623435A CN109679216A CN 109679216 A CN109679216 A CN 109679216A CN 201811623435 A CN201811623435 A CN 201811623435A CN 109679216 A CN109679216 A CN 109679216A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention discloses a kind of high rigid-tough balance, resistance to stress to whiten, halogen-free flame retardant polypropylene composite material and preparation method thereof, it comprises the following raw materials by weight percent: polypropylene 32~96, talcum powder 0~30, cage type polysilsesquioxane 1~20, elastomer 1~15, antioxidant 0.1~1, other auxiliary agents 0~2.The present invention in conventional talc powder reinforced polypropylene basic components by introducing cage type polysilsesquioxane nanoparticle, pass through the compounding of two kinds of different scale systems, the rigidity and shock resistance of PP composite material can be significantly improved, nanoscale cage type polysilsesquioxane particle can play the role of nucleating agent simultaneously, improve the crystallinity of PP composite material；In addition, cage type polysilsesquioxane preferably can be improved the oxygen index (OI) of PP composite material at carbon effect, improve its incendive problem, PP composite material resistance to stress while with high rigidity-toughness balanced performance is whitened, and good flame resistance.
Description
Technical field
The present invention relates to a kind of high rigid-tough balance, resistance to stress to whiten, halogen-free flame retardant polypropylene composite material and its preparation
Method is a kind of simple process, PP composite material at low cost, good combination property, is mainly used in household electrical appliance, automobile
Interior exterior trim etc., belongs to polymer modification and processing technique field.
Background technique
Polypropylene is while light inexpensive because having preferable processing performance and excellent mechanics, physics, chemical property, extensively
It is general to be applied to the industries such as automobile interior exterior decorations, household electrical appliance and electronics, it is the most fast universal thermoplastic of current growth rate.
In recent years, with the rapid development of the automotive industry, major automobile main frame maker proposes the performance of automobile interior decoration part higher
Requirement, such as the instrument board as automobile interior decoration, door-plate, column part not only need higher rigidity as structural support,
It also needs to have both preferable toughness simultaneously, when by foreign impacts or shock, apparent rupture or sharp fragments will not be generated,
The personal safety of protection driver and passenger to greatest extent.In addition, polypropylene articles in injection moulding process, be easy ejection position by
Power is concentrated and generates crazing, leads to stress whitening phenomenon, influences products appearance.Meanwhile polypropylene it is inflammable and burn when along with
Molten drop phenomenon, easily causes fire, it is made to be very limited in practical applications.Therefore how PP composite material is improved
Rigidity-toughness balanced performance, improve its stress whitening phenomenon, and have both high anti-flammability and become and develop one urgent needs of this kind of material and solve
Certainly the problem of.
Currently, the rigidity-toughness balanced performance for improving PP composite material mainly passes through a large amount of inorganic filler of addition and elasticity
Body, but excessive filling will cause the weight increase and the decline of heat resistance of composite material, while will cause material and answering
Blushing is generated under power.Current existing patent is improved in a certain respect or in terms of part only for above-mentioned, but can not
Have both the comprehensive study of rigid-tough balance, stress-whitening resistance and anti-flammability of material etc..As patent CN106273350A is logical
It crosses and alkali magnesium sulfate crystal whisker and high mesh number talcum powder is added to improve the rigidity and toughness of composite material, but be not directed to resistance to stress hair
White property and anti-flammability.Patent CN103113661A realizes the high rigidity of composite material by the way that long glass fibres and fire retardant is added
High tenacity and anti-flammability, but composite material preparation process is complicated, but cannot achieve halogen-free flameproof, while being not directed to resistance to stress and whitening
Performance.Patent CN106700232A by addition low density polyethylene (LDPE) and glass fibre come improve material stress whitening performance and
Rigidity, but its processing performance and products appearance will receive influence, and not consider flame retardant property.Patent CN106810762A is by adding
Add different types of fire retardant to realize the flame retardant effect of material, but can not be applied in the components that high rigidity high tenacity requires.
Summary of the invention
The object of the present invention is to provide a kind of high rigid-tough balance, resistance to stress to whiten, halogen-free flame retardant polypropylene composite material
And preparation method thereof, to solve the above problem of the prior art.
In order to improve the rigid-tough balance of PP composite material, the stress-whitening resistance of composite material is improved, and solve
The problem of Flame Retardancy difference, the technical scheme is that adding in the basic components of composite talcum powder filled material of polypropylene
Enter cage type polysilsesquioxane, in squeezing out Blending Processes, by the compounding of two kinds of different scale systems, can significantly improve poly-
The rigidity and shock resistance of propylene material, while nanoscale cage type polysilsesquioxane particle can play the work of nucleating agent
With improving the crystallinity of PP composite material；In addition, cage type polysilsesquioxane preferably can be improved poly- third at carbon effect
The oxygen index (OI) of alkene composite material reaches the characteristics of inhibiting material combustion.
A kind of high rigid-tough balance, resistance to stress whiten, halogen-free flame retardant polypropylene composite material, by following weight percent
Raw material is configured to:
In the PP composite material system that the present invention is applicable in,
For the polypropylene under 230 DEG C, 2.16kg loading condiction, melt flow rate (MFR) is 5~60g/10min.
The polypropylene is homo-polypropylene or block copolymerization propylene；The crystallinity of the homo-polypropylene 70% or more, etc.
Normality is greater than 99%；The comonomer of the block copolymerization polypropylene is ethylene, and vinyl monomer repetitive unit molar content is 4
~10%.
The talcum powder is micron order talcum powder, and whiteness is 80%~90%, and particle size range is 5~25 μm, close
Degree is 2.7~2.8g/cm3。
The cage type polysilsesquioxane, is a kind of novel nanostructure hybrid systems, particle size range is 1~
30nm。
The elastomer is the combination of ethylene-octene linear copolymer or Ethylene/Butylene linear copolymer or both,
Density is 0.88~0.90g/cm3, melt flow rate (MFR) is 0.5~10g/10min.
The antioxidant includes primary antioxidant and auxiliary anti-oxidant, and primary antioxidant is hindered phenol or sulphur ester antioxidant；It is auxiliary
Antioxidant is phosphorite kind antioxidant.
The primary antioxidant is one or more of 3114,1010 and DSTP mixing；Auxiliary anti-oxidant is 618 and 168
One or both of.
Other described additives are various colors additive, light stabilizer, various esters or fatty acid lubricant etc..
Above-mentioned high rigid-tough balance, resistance to stress whiten, the preparation method of halogen-free flame retardant polypropylene composite material, specific to walk
It is rapid as follows:
(1) raw material is weighed by above-mentioned weight proportion；
(2) each raw material is placed in super mixer and is mixed 3~5 minutes；
(3) mixed raw material is placed in dual-screw-stem machine, through melting extrusion, is granulated, technique an are as follows: area 190~200
DEG C, two 200~210 DEG C of areas, three 210~220 DEG C of areas, four 205~215 DEG C of areas；The residence time of entire extrusion process is 1~2
Minute, pressure is 12~18MPa, and purging vacuum degree reaches 5~20kPa.
The invention has the advantages that
1, the present invention is using micron-sized talcum powder and nanoscale cage type polysilsesquioxane in composite system
Compounding, so that obtained PP composite material rigidity with higher and shock resistance.
2, the cage type polysilsesquioxane that the present invention uses, can play the role of nucleating agent in composite system,
The crystallinity of composite material is improved, stress-whitening resistance energy is improved.
3, the present invention greatly improves the oxygen index (OI) of composite material using cage type polysilsesquioxane preferably at carbon effect,
Promote the flame retardant property of composite material.
4, high tenacity proposed by the present invention, resistance to stress are whitened, the preparation process of halogen-free flame retardant polypropylene composite material is simple,
Production cost is low.
Specific embodiment
Below by the mode of embodiment and comparative example, the present invention is described in further detail, does not therefore send out this
It is bright to be limited among the embodiment described range.
Embodiment 1
PP composite material main component of the present invention includes 90.6% polypropylene, 5% cage type polysilsesquioxane, 2%
Elastomer, 0.1% antioxidant 3114 and 0.2% irgasfos 168,0.1% auxiliary anti-oxidant DSTP and 2% other auxiliary agents.
Embodiment 2
PP composite material main component of the present invention includes 82.6% polypropylene, 5% talcum powder, the poly- sesquialter of 5% cage type
Siloxanes, 5% elastomer, 0.1% antioxidant 3114 and 0.2% irgasfos 168,0.1% auxiliary anti-oxidant DSTP and 2% are other
Auxiliary agent.
Embodiment 3
PP composite material main component of the present invention includes 74.6% polypropylene, 10% talcum powder, the poly- sesquialter of 5% cage type
Siloxanes, 8% elastomer, 0.1% antioxidant 3114 and 0.2% irgasfos 168,0.1% auxiliary anti-oxidant DSTP and 2% are other
Auxiliary agent.
Embodiment 4
PP composite material main component of the present invention includes 67.6% polypropylene, 15% talcum powder, the poly- sesquialter of 5% cage type
Siloxanes, 10% elastomer, 0.1% antioxidant 3114 and 0.2% irgasfos 168,0.1% auxiliary anti-oxidant DSTP and 2% its
Its auxiliary agent.
Embodiment 5
PP composite material main component of the present invention includes 60.6% polypropylene, 20% talcum powder, the poly- sesquialter of 5% cage type
Siloxanes, 12% elastomer, 0.1% antioxidant 3114 and 0.2% irgasfos 168,0.1% auxiliary anti-oxidant DSTP and 2% its
Its auxiliary agent.
Embodiment 6
PP composite material main component of the present invention includes 74.6% polypropylene, 5% talcum powder, the poly- sesquialter of 10% cage type
Siloxanes, 8% elastomer, 0.1% antioxidant 3114 and 0.2% irgasfos 168,0.1% auxiliary anti-oxidant DSTP and 2% are other
Auxiliary agent.
Embodiment 7
PP composite material main component of the present invention includes 67.6% polypropylene, 10% talcum powder, poly- times of 10% cage type
Half siloxanes, 10% elastomer, 0.1% antioxidant 3114 and 0.2% irgasfos 168,0.1% auxiliary anti-oxidant DSTP and 2%
Other auxiliary agents.
Embodiment 8
PP composite material main component of the present invention includes 60.6% polypropylene, 15% talcum powder, poly- times of 10% cage type
Half siloxanes, 12% elastomer, 0.1% antioxidant 3114 and 0.2% irgasfos 168,0.1% auxiliary anti-oxidant DSTP and 2%
Other auxiliary agents.
Comparative example 1
PP composite material main component of the present invention include 90.6% polypropylene, 5% talcum powder, 2% elastomer,
0.1% antioxidant 3114 and 0.2% irgasfos 168,0.1% auxiliary anti-oxidant DSTP and 2% other auxiliary agents.
Comparative example 2
PP composite material main component of the present invention include 82.6% polypropylene, 10% talcum powder, 5% elastomer,
0.1% antioxidant 3114 and 0.2% irgasfos 168,0.1% auxiliary anti-oxidant DSTP and 2% other auxiliary agents.
Comparative example 3
PP composite material main component of the present invention include 74.6% polypropylene, 15% talcum powder, 8% elastomer,
0.1% antioxidant 3114 and 0.2% irgasfos 168,0.1% auxiliary anti-oxidant DSTP and 2% other auxiliary agents.
Comparative example 4
PP composite material main component of the present invention include 67.6% polypropylene, 20% talcum powder, 10% elastomer,
0.1% antioxidant 3114 and 0.2% irgasfos 168,0.1% auxiliary anti-oxidant DSTP and 2% other auxiliary agents.
Comparative example 5
PP composite material main component of the present invention include 60.6% polypropylene, 25% talcum powder, 12% elastomer,
0.1% antioxidant 3114 and 0.2% irgasfos 168,0.1% auxiliary anti-oxidant DSTP and 2% other auxiliary agents.
Embodiment and comparative example main component mass percentage are shown in Table 1.
1 embodiment 1-8 of table and comparative example 1-5 material prescription table (weight %)
In above-described embodiment and comparative example composite-material formula, the copolymerization poly- third of the polypropylene oil of SPC production
Alkene, trade names M2600R, melt flow rate (MFR) are 30g/10min (test condition: 230 DEG C × 2.16kg).The cunning
Mountain flour is 1250 mesh, and average grain diameter is 10 μm, commercially available.The cage type polysilsesquioxane self-control, average grain diameter 10nm,
Molecular weight is between 30000~80000.Elastomer used is the ethylene-octene copolymer of DOW company, trade name
Engage8150, density 0.868g/cm3, melt index are 0.5g/10min (test condition: 190 DEG C × 2.16kg).Institute
The primary antioxidant stated is 3114 that BASF AG produces, trade names Irganox3114, chemical name 3,5- di-t-butyl-
The DSTP that 4- hydroxybenzyl phosphate diethylester and ICE company, Britain produce, trade names are Negonox DSTP, chemical name
For thio-2 acid octadecyl ester.Auxiliary anti-oxidant is 168 that BASF AG produces, and trade names are Irgafos 168, and chemical name is
Three (2,4- di-tert-butyl-phenyl) phosphite esters.Other auxiliary agents include various colors additive, light stabilizer, various esters
Class or fatty acid lubricant etc..
Each resin and various additives are dry-mixed 3~5 minutes in super mixer in above-described embodiment and comparative example, then
Through melting extrusion in double screw extruder, it is granulated, technique are as follows: 190~200 DEG C of an area, two 200~210 DEG C of areas, three areas 210
~220 DEG C, four 205~215 DEG C of areas；The residence time of entire extrusion process is 1~2 minute, and pressure is 12~18MPa, exhaust
Vacuum degree reaches 5~20kPa.
The particulate material that will be prepared according to the above method, it is 2~3 hours dry in 90~100 DEG C of convection oven, then again
Dried particulate material is subjected to injection moulding sample preparation on injection (mo(u)lding) machine, and is tested for the property.
Density measurement: being carried out by ISO 1183-1 standard, and specimen size is 10 × 10 × 4mm；
Tensile property test: being carried out by ISO 527-2 standard, and specimen size is 170 × 10 × 4mm, and tensile speed is
50mm/min；
Bending property test: being carried out by 178 standard of ISO, and specimen size is 80 × 10 × 4mm, rate of bending 2mm/
Min, span 64mm；
Notch impact strength test: being carried out by ISO 179-1 standard, and specimen size is 80 × 10 × 4mm, and notch depth is
The one third of sample thickness；
Stress-whitening resistance can test: it is carried out by germany volkswagen PV3966 standard, specimen size is 70 × 70 × 3.2mm,
Under standard sources compare falling sphere before and after sample stress whitening situation, be divided into three grades: A, unstressed to whiten；B, it slightly answers
Power is whitened；C, obvious stress whitening；
Flame retardant property test: according to the oxygen index (OI) of GB/T2406 Standards for Testing Materials.
Material stiffness and toughness are judged by the bending modulus and notch impact strength of test material, stress-whitening resistance
It can be judged by the stress whitening situation before and after comparison falling sphere, flame retardant property is judged by the oxygen index (OI) of test material.
The performance test results of 1~5 PP composite material of the embodiment of the present invention 1~8 and comparative example are shown in Table 2 respectively.
2 embodiment 1-8 of table and comparative example 1-5 material property table
The comparison of comparison and embodiment 6-8 and comparative example 3-5 from embodiment 1-5 and comparative example 1-5 can be seen that cage
The addition of shape polysilsesquioxane can significantly improve the rigidity and toughness of PP composite material, and with poly- times of cage type
The promotion of the increase of half content of siloxane, composite material rigidity-toughness balanced performance is more obvious.From embodiment 3-5, embodiment 6-8 with it is right
The comparison of ratio 3-5, which can be seen that cage type polysilsesquioxane, can improve the stress-whitening resistance energy of composite system, and
With the increase of its content, the stress-whitening resistance of composite material can be improved significantly.From embodiment 1-8 and comparative example 1-5
Comparison it can be found that cage type polysilsesquioxane can greatly promote the oxygen index (OI) of composite material, and its additive amount is more, multiple
The oxygen index (OI) of condensation material system is bigger, shows that the anti-flammability of composite material is better.In addition, talc is compared, poly- times of cage type
The addition of half siloxanes can reduce the density of composite material, can realize the lightweight of product to a certain extent.
Claims (10)
1. a kind of high rigid-tough balance, resistance to stress are whitened, halogen-free flame retardant polypropylene composite material, it is characterised in that: by following heavy
The raw material of amount percentage is configured to:
2. a kind of high rigid-tough balance according to claim 1, resistance to stress are whitened, halogen-free flame retardant polypropylene composite material,
It is characterized by: the polypropylene, under 230 DEG C, 2.16kg loading condiction, melt flow rate (MFR) is 5~60g/10min.
3. a kind of high rigid-tough balance according to claim 1, resistance to stress are whitened, halogen-free flame retardant polypropylene composite material,
It is characterized by: the polypropylene is homo-polypropylene or block copolymerization propylene；The crystallinity of the homo-polypropylene 70% or more,
Isotacticity is greater than 99%；The comonomer of the block copolymerization polypropylene is ethylene, vinyl monomer repetitive unit molar content
It is 4~10%.
4. a kind of high rigid-tough balance according to claim 1, resistance to stress are whitened, halogen-free flame retardant polypropylene composite material,
It is characterized by: the talcum powder is micron order talcum powder, whiteness is 80%~90%, and particle size range is 5~25 μm,
Density is 2.7~2.8g/cm3。
5. a kind of high rigid-tough balance according to claim 1, resistance to stress are whitened, halogen-free flame retardant polypropylene composite material,
It is characterized by: the cage type polysilsesquioxane, is a kind of novel nanostructure hybrid systems, particle size range 1
~30nm.
6. a kind of high rigid-tough balance according to claim 1, resistance to stress are whitened, halogen-free flame retardant polypropylene composite material,
It is characterized by: the elastomer is the group of ethylene-octene linear copolymer or Ethylene/Butylene linear copolymer or both
It closes, density is 0.88~0.90g/cm3, melt flow rate (MFR) is 0.5~10g/10min.
7. a kind of high rigid-tough balance according to claim 1, resistance to stress are whitened, halogen-free flame retardant polypropylene composite material,
It is characterized by: the antioxidant includes primary antioxidant and auxiliary anti-oxidant, primary antioxidant is hindered phenol or sulphur ester antioxidant；
Auxiliary anti-oxidant is phosphorite kind antioxidant.
8. a kind of high rigid-tough balance according to claim 7, resistance to stress are whitened, halogen-free flame retardant polypropylene composite material,
It is characterized by: the primary antioxidant is one or more of 3114,1010 and DSTP mixing；Auxiliary anti-oxidant is 618 Hes
One or both of 168.
9. a kind of high rigid-tough balance according to claim 1, resistance to stress are whitened, halogen-free flame retardant polypropylene composite material,
It is characterized by: other described additives are various colors additive, light stabilizer, various esters or fatty acid lubricant
One of or it is a variety of.
10. high rigid-tough balance described in claim 1-9 is one of any, resistance to stress are whitened, halogen-free flame retardant polypropylene composite material
And preparation method thereof, it is characterised in that: the specific steps of which are as follows:
(1) raw material is weighed by above-mentioned weight proportion；
(2) each raw material is placed in super mixer and is mixed 3~5 minutes；
(3) mixed raw material is placed in dual-screw-stem machine, through melting extrusion, is granulated, technique are as follows: 190~200 DEG C of an area, two
200~210 DEG C of area, three 210~220 DEG C of areas, four 205~215 DEG C of areas；The residence time of entire extrusion process is 1~2 minute,
Pressure is 12~18MPa, and purging vacuum degree reaches 5~20kPa.
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Cited By (6)
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| CN111087690A (en) * | 2019-12-23 | 2020-05-01 | 上海普利特复合材料股份有限公司 | Flame-retardant polypropylene composite material with electromagnetic shielding effect and scratch resistance and preparation method thereof |
| CN112143103A (en) * | 2020-09-25 | 2020-12-29 | 华东理工大学 | Cage-type silsesquioxane modified polypropylene composite material and preparation method thereof |
| CN112159594A (en) * | 2020-09-25 | 2021-01-01 | 华东理工大学 | Cage type silsesquioxane nucleating agent and preparation method and application thereof |
| CN112662112A (en) * | 2020-12-15 | 2021-04-16 | 浙江普利特新材料有限公司 | Polypropylene composite material with long-acting thermal-oxidative-aging resistance, low odor and stickiness resistance and preparation method thereof |
| BE1027908B1 (en) * | 2019-12-24 | 2021-07-26 | Verhelst Bouwmaterialen Nv | SPACER, PROCEDURE FOR THEIR MANUFACTURE AND USE IN REINFORCED CONCRETE PRODUCTS |
| CN115637005A (en) * | 2022-11-04 | 2023-01-24 | 常州瑞杰新材料科技有限公司 | Polypropylene composite material with rigidity, toughness, heat resistance and high flame retardance |
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