CN102070833A - Filler masterbatch used for increasing polarity of polypropylene and preparation method thereof - Google Patents
Filler masterbatch used for increasing polarity of polypropylene and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a filler masterbatch used for increasing the polarity of polypropylene and a preparation method thereof. The filler masterbatch is characterized by comprising the following components by weight percent: 50%-79% of inorganic filler, 15%-30% of carrier, 5%-17% of polar additive and 1%-3% of processing additive; and the polar additive is one or more of thermoplastic polyurethane resin (TPU), maleic anhydride grafted polypropylene, epoxy resin, ethylene acrylate, ethylene vinyl acetate, polyether amine and polybutylene polyol. In the preparation method of the invention, the added carrier can not improve the polarity of polypropylene, the inorganic filler is used to increase the rigidity of the material; the key is to introduce the polar additive with high unipolarity, thus the filler masterbatch used for increasing the polarity of polypropylene can be prepared; when the filler masterbatch is combined with the polypropylene material for production, the surface polarity of the filled and modified polypropylene material can be increased, the surface energy of the filled and modified polypropylene can be reduced, the dimension stability can be increased, the modified polypropylene material can have good paint adhesion and the material can be used to form exterior trimming parts such as bumpers and interior trimming parts such instrument panels.
Description
Technical field
The invention belongs to material modified technical field, be specifically related to a kind of filler parent granule that polypropylene polarity is used that improves.
Background technology
Usually, in the plastic working process, mineral filler such as talcum powder, lime carbonate etc. are mixed and made into filler parent granule with vector resin, has lot of advantages, good as the plastics stability, metered charge in being easy to produce and blend operation purify Working environment etc.At the preparation filler parent granule simultaneously, we can also prepare the filler parent granule that can improve some functional usefulness of polypropylene material by adding functional auxiliary agent.
Current, modified polypropylene material is because its wide material sources, density are little, harmonious good, the resistance to chemical attack of mechanics, easily processing and outstanding advantage such as cheap, thereby be widely used, especially exploitation on automobile and application is the focus that automotive industry and plastics industry are paid close attention to always.
Because polypropylene material is a non-polar material, surface energy is low, make that the consistency of itself and most polymers is poor, be difficult for infiltration, bonding and printing, coating property is poor, when picture uses in the collision bumper of paint spraying, will be low because of its cohesive strength with paint, and must adopt certain methods to improve its polarity.In addition,, need sometimes to carry out bondingly, also need polypropylene material that good adhesiveproperties is arranged with other materials for some automotive upholsteries such as door-plate or dashboard.Usually plastic part is in order to improve material surface tension force, promptly improve PASS, before application, at first need to carry out surface treatment, eliminate antistatic and dust adsorbed greasy dirt by solvent, carry out surface modification with flame, corona discharge, tensio-active agent, gas plasma etc., improve the polar group on surface, strengthen coating adhesion.These class technological difficulties be should form uniform surface, again can not excessive handling, otherwise can cause the polymer chain fracture on surface, thus the performance of influence, the polarity that therefore improves polypropylene substrate becomes an extremely attractive problem.
Raising PP polar method commonly used has surface grafting method, surface-crosslinked method, surface coating modified method, adds polar material blending method etc.Patent CN1182097 discloses a kind of method for preparing high-polarity modified polypropylene material, this preparation method is parent stock with the polypropylene, add a certain proportion of polarity unisexuality, cografting polar monomer and initiator, reacted 1-3 minute down at 170 ℃-220 ℃, the high-polarity polypropylene material that makes, can improve the polarity of goods, improve the surface daub on a wall of goods; Patent CN1230554 adds a certain proportion of maleic anhydride, cografting monomer and initiator, melt pelletization, and the high-polarity polypropylene material of preparation can improve the polarity of goods, improves the surface daub on a wall of goods; Patent CN1238786 discloses the method for preparing polar modified polypropylene waxes, and by nonpolar homopolymer polypropylene or copolymer waxes and α, β-undersaturated carboxylic acid or derivatives thereof reacts in the presence of free radical, the polarity PP wax polarity height that makes; CN1858104 discloses a kind of polypropylene, polyethylene treating agent, it is made of following component: Chlorinated Polypropylene III, chlorinated rubber, toluene, butyl acrylate, vinylbenzene, maleic anhydride, benzoyl peroxide, antioxidant BHT, react with polypropylene, has good stability, advantage such as avidity is strong.
More than these methods can improve PP polarity, but these production technique more complicated, and because the modified polypropylene material that automobile is used mostly is filling product, the blanking homogeneity can be influential when actual production.The present invention is directed to these problems, the employing mineral filler is a main body, thermoplastic elastomer, thermoplastic resin etc. are carrier, add TPU, maleic anhydride inoculated polypropylene, Resins, epoxy, ethylene-acrylate (EEA), ethylene vinyl acetate (EVA), polyetheramine isopolarity material simultaneously and prepare easy dispersion, high polar filler parent granule, during the compound production of itself and polypropylene material, be easy to metered charge and blend operation, simultaneously can purify Working environment, improve the polarity of polypropylene material simultaneously, thereby reach the purpose of improving polypropylene paint sticking power.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of filler parent granule is provided, this filler parent granule can improve the dispersiveness of polar additive, the easier product surface of moving to when adding in the polypropylene, thereby the surface polarity of raising polypropylene product.
A kind of raising polypropylene polarity filler parent granule, form by following components in weight percentage:
Mineral filler 50% ~ 79%
Carrier 15% ~ 30%
Polar additive 5% ~ 17%
Processing aid 1%-3%;
Described polar additive is one or more mixing in TPU, maleic anhydride inoculated polypropylene, Resins, epoxy, ethylene-acrylate, ethylene vinyl acetate, polyetheramine, the polybutene polyvalent alcohol.
With in the filler parent granule, described mineral filler is preferably one or more mixing in talcum powder, lime carbonate, kaolin, barium sulfate, aluminium hydroxide, the titanium dioxide in above-mentioned raising polypropylene polarity.
Use in the filler parent granule in above-mentioned raising polypropylene polarity, described carrier is preferably one or more mixing in polypropylene, new LDPE (film grade), high density polyethylene(HDPE), hydroxy-terminated polybutadienes, ethene-hexene copolymer, ethylene-butene copolymer, ethylene-octene copolymer, ethylene-propylene-octene terpolymer, the hydrogenation of ethylene-butadiene-styrene copolymer, and it melts to refer to be 0.5 ~ 60g/10min.
With in the filler parent granule, described processing aid is preferably one or more mixing in suffocated amine antioxidant, Hinered phenols antioxidant, phosphite, stearic acid, calcium stearate, Zinic stearas, whiteruss, the naphthenic oil in above-mentioned raising polypropylene polarity.
Above-mentioned raising polypropylene polarity comprises the steps: each component is mixed in proportion granulation again with the preparation method of filler parent granule.
Above-mentioned raising polypropylene polarity comprises the steps: that with the using method of filler parent granule above-mentioned filler parent granule mixes with polypropylene, puts into forcing machine then and carries out the melt blending extruding pelletization and get final product.
Compared with prior art, the present invention has following beneficial effect:
1, the carrier that the present invention added is nonpolar, and itself can not improve polyacrylic polarity; The adding of mineral filler is in order to improve the rigidity of material; The component of most critical is by introducing the high polar additive (materials such as TPU, Resins, epoxy, ethylene-acrylate, ethylene vinyl acetate, polyetheramine) of polarity unipolarity, the filler parent granule that the polypropylene polarity that is improved is used, during the compound production of itself and polypropylene material, can improve the surface polarity of filling modified polypropylene material, reduce the surface energy of filled modified polypropylene, improve dimensional stability, make modified polypropylene material have good PASS, can use this material to come inside gadgets such as exterior trimming parts such as moulding collision bumper and dashboard.
2, polar additive adding proportion in prescription is very little usually, in the modified polypropene system, be difficult to be uniformly dispersed, the present invention is by being made into master batch earlier, add in the polypropylene with the master batch form again, help improving the dispersiveness of polar additive like this, and the easier product surface of moving to, thereby improve the product surface polarity.
3, the filler parent granule used of raising polypropylene polarity provided by the present invention adds corresponding additive (oxidation inhibitor, photostabilizer, lubricant etc.), through twin screw and polypropylene fusion blend, filler parent granule is evenly spread in the resin matrix, excellent performance.
Embodiment
Provide embodiment below so that the present invention is carried out concrete description; be necessary to be pointed out that at this following examples only are used for the present invention is further specified; can not be interpreted as limiting the scope of the invention, content still belongs to protection scope of the present invention to some nonessential improvement and the adjustment that the present invention makes to the person skilled in the art in this field according to the present invention.
Comparative example 1: prescription is as table 1.
Table 1
| Component | Weight percentage |
| Talcum powder | 70% |
| Polypropylene (the molten finger is 30g/10min) | 29% |
| Suffocated amine antioxidant | 0.25% |
| Hinered phenols antioxidant | 0.25% |
| Stearic acid | 0.5% |
To go up the table starting material and at room temperature drop in the Banbury mixer, and take out the back and uses single screw extrusion machine granulation, temperature to be controlled at 150 ℃ 80 ℃ of banburyings.
This talcum powder master batch, POE, polypropylene are put into super mixer mixing 3min earlier by the weight ratio of 20:10:70, and then put into twin screw extruder, temperature is controlled at 200 ℃, and extruding pelletization makes the composite property test result and sees Table 3 under 450 rev/mins of conditions of screw speed.
Embodiment 1: prescription is as table 2.
Table 2
| Component | Weight percentage |
| Talcum powder | 70% |
| Polypropylene (the molten finger is 30g/10min) | 14% |
| Ethylene vinyl acetate (EVA) | 15% |
| Suffocated amine antioxidant | 0.25% |
| Hinered phenols antioxidant | 0.25% |
| Stearic acid | 0.5% |
To go up the table starting material and at room temperature drop in the Banbury mixer, and take out the back and uses single screw extrusion machine granulation, temperature to be controlled at 150 ℃ 80 ℃ of banburyings.
This talcum powder master batch, POE, polypropylene are put into super mixer mixing 3min earlier by the weight ratio of 20:10:70, and then put into twin screw extruder, temperature is controlled at 200 ℃, under 450 rev/mins of conditions of screw speed extruding pelletization promptly, its composite property test result sees Table 3.
Table 3 performance table
| Performance | Testing standard | International unit | Comparative example 1 | Embodiment 1 |
| Melt mass flow rate | ISO1133-91 | g/10min | 10 | 11 |
| Tensile strength | ISO527/2-93 | MPa | 16 | 17 |
| Elongation at break | ISO527/2-93 | % | >100 | >100 |
| Flexural strength | ISO178-93 | MPa | 21 | 20 |
| Modulus in flexure | ISO178-93 | MPa | 1106 | 1051 |
| The socle girder notched Izod impact strength | ISO180-93 | KJ/m2 | 45 | 47 |
| Surface tension | Ford?Test Method | Dynes/cm | 29 | 42 |
Embodiment 2: prescription is as table 4.
Table 4 formulation content
| Component | Weight percentage |
| Talcum powder | 70% |
| New LDPE (film grade) (the molten finger is 20g/10min) | 10% |
| High density polyethylene(HDPE) (the molten finger is 5g/10min) | 9% |
| TPU | 10% |
| Phosphite | 0.5% |
| Zinic stearas | 0.5% |
To go up the table starting material and at room temperature drop in the Banbury mixer, and take out the back and uses single screw extrusion machine granulation, temperature to be controlled at 200 ℃ 80 ℃ of banburyings.
This talcum powder master batch, POE, polypropylene are put into super mixer mixing 3min earlier by the weight ratio of 20:10:70, and then put into twin screw extruder, temperature is controlled at 215 ℃, under 450 rev/mins of conditions of screw speed extruding pelletization promptly, its composite property test result sees Table 5.
Table 5 performance table
| Performance | Testing standard | International unit | Embodiment 2 |
| Melt mass flow rate | ISO1133-91 | g/10min | 12 |
| Tensile strength | ISO527/2-93 | MPa | 18 |
| Elongation at break | ISO527/2-93 | % | >100 |
| Flexural strength | ISO178-93 | MPa | 21 |
| Modulus in flexure | ISO178-93 | MPa | 1050 |
| The socle girder notched Izod impact strength | ISO180-93 | KJ/m2 | 46 |
| Surface tension | Ford?Test Method | Dynes/cm | 42 |
Embodiment 3: prescription is as table 6.
Table 6
| Component | Weight percentage |
| Lime carbonate | 70% |
| Ethene-hexene copolymer (the molten finger is 0.5 g/10min) | 9% |
| Resins, epoxy | 10% |
| Polyetheramine | 10% |
| Suffocated amine antioxidant | 0.25% |
| Hinered phenols antioxidant | 0.25% |
| Whiteruss | 0.5% |
To go up the table starting material and at room temperature drop in the Banbury mixer, and take out the back and uses single screw extrusion machine granulation, temperature to be controlled at 200 ℃ 100 ℃ of banburyings.
This talcum powder master batch, POE, polypropylene are put into super mixer mixing 3min earlier by the weight ratio of 20:10:70, and then put into twin screw extruder, temperature is controlled at 210 ℃, under 450 rev/mins of conditions of screw speed extruding pelletization promptly, its composite property test result sees Table 7.
Table 7 performance table
| Performance | Testing standard | International unit | Embodiment 3 |
| Melt mass flow rate | ISO1133-91 | g/10min | 14 |
| Tensile strength | ISO527/2-93 | MPa | 16 |
| Elongation at break | ISO527/2-93 | % | >100 |
| Flexural strength | ISO178-93 | MPa | 20 |
| Modulus in flexure | ISO178-93 | MPa | 850 |
| The socle girder notched Izod impact strength | ISO180-93 | KJ/m2 | 40 |
| Surface tension | Ford?Test Method | Dynes/cm | 42 |
Embodiment 5: prescription is as table 8.
Table 8
| Component | Weight percentage |
| Kaolin | 20% |
| Aluminium hydroxide | 50% |
| Ethylene-butene copolymer (the molten finger is 1.0 g/10min) | 11% |
| Ethylene-acrylate (EEA) | 18% |
| Suffocated amine antioxidant | 0.25% |
| Hinered phenols antioxidant | 0.25% |
| Calcium stearate | 0.5% |
To go up the table starting material and at room temperature drop in the Banbury mixer, and take out the back and uses single screw extrusion machine granulation, temperature to be controlled at 180 ℃ 60 ℃ of banburyings.
This talcum powder master batch, POE, polypropylene are put into super mixer mixing 3min earlier by the weight ratio of 20:10:70, and then put into twin screw extruder, temperature is controlled at 215 ℃, under 450 rev/mins of conditions of screw speed extruding pelletization promptly, its composite property test result sees Table 9.
Table 9 performance table
| Performance | Testing standard | International unit | Embodiment 5 |
| Melt mass flow rate | ISO1133-91 | g/10min | 11 |
| Tensile strength | ISO527/2-93 | MPa | 19 |
| Elongation at break | ISO527/2-93 | % | >100 |
| Flexural strength | ISO178-93 | MPa | 23 |
| Modulus in flexure | ISO178-93 | MPa | 1150 |
| The socle girder notched Izod impact strength | ISO180-93 | KJ/m2 | 42 |
| Surface tension | Ford?Test Method | Dynes/cm | 41 |
Embodiment 6: prescription is as table 10.
Table 10
| Component | Weight percentage |
| Titanium dioxide | 10% |
| Talcum powder | 60% |
| Ethylene-propylene-octene terpolymer (the molten finger is 0.5 g/10min) | 13% |
| The polybutene polyvalent alcohol | 16% |
| Suffocated amine antioxidant | 0.25% |
| Hinered phenols antioxidant | 0.25% |
| Calcium stearate | 0.5% |
To go up the table starting material and at room temperature drop in the Banbury mixer, and take out the back and uses single screw extrusion machine granulation, temperature to be controlled at 180 ℃ 60 ℃ of banburyings.
This talcum powder master batch, POE, polypropylene are put into super mixer mixing 3min earlier by the weight ratio of 20:10:70, and then put into twin screw extruder, temperature is controlled at 200 ℃, under 450 rev/mins of conditions of screw speed extruding pelletization promptly, its composite property test result sees Table 11.
Table 11 performance table
| Performance | Testing standard | International unit | Embodiment 6 |
| Melt mass flow rate | ISO1133-91 | g/10min | 10 |
| Tensile strength | ISO527/2-93 | MPa | 18 |
| Elongation at break | ISO527/2-93 | % | >100 |
| Flexural strength | ISO178-93 | MPa | 23 |
| Modulus in flexure | ISO178-93 | MPa | 1030 |
| The socle girder notched Izod impact strength | ISO180-93 | KJ/m2 | 43 |
| Surface tension | Ford?Test Method | Dynes/cm | 41 |
Embodiment 7: prescription is as table 12.
Table 12
| Component | Weight percentage |
| Barium sulfate | 70% |
| Ethylene-octene copolymer (the molten finger is 1.0 g/10min) | 9% |
| Maleic anhydride inoculated polypropylene | 20% |
| Suffocated amine antioxidant | 0.25% |
| Hinered phenols antioxidant | 0.25% |
| Calcium stearate | 0.5% |
To go up the table starting material and at room temperature drop in the Banbury mixer, and take out the back and uses single screw extrusion machine granulation, temperature to be controlled at 180 ℃ 70 ℃ of banburyings.
This talcum powder master batch, POE, polypropylene are put into super mixer mixing 3min earlier by the weight ratio of 20:10:70, and then put into twin screw extruder, temperature is controlled at 215 ℃, under 450 rev/mins of conditions of screw speed extruding pelletization promptly, its composite property test result sees Table 13.
Table 13 performance table
| Performance | Testing standard | International unit | Embodiment 7 |
| Melt mass flow rate | ISO1133-91 | g/10min | 15 |
| Tensile strength | ISO527/2-93 | MPa | 17 |
| Elongation at break | ISO527/2-93 | % | >100 |
| Flexural strength | ISO178-93 | MPa | 22 |
| Modulus in flexure | ISO178-93 | MPa | 1130 |
| The socle girder notched Izod impact strength | ISO180-93 | KJ/m2 | 41 |
| Surface tension | Ford?Test Method | Dynes/cm | 41 |
Claims (6)
1. one kind is improved polypropylene polarity filler parent granule, it is characterized in that being made up of following components in weight percentage:
Mineral filler 50% ~ 79%
Carrier 15% ~ 30%
Polar additive 5% ~ 17%
Processing aid 1%-3%;
Described polar additive is one or more mixing in TPU, maleic anhydride inoculated polypropylene, Resins, epoxy, ethylene-acrylate, ethylene vinyl acetate, polyetheramine, the polybutene polyvalent alcohol.
2. raising polypropylene polarity filler parent granule according to claim 1 is characterized in that: described mineral filler is one or more mixing in talcum powder, lime carbonate, kaolin, barium sulfate, aluminium hydroxide, the titanium dioxide.
3. raising polypropylene polarity filler parent granule according to claim 1, it is characterized in that: described carrier is one or more mixing in polypropylene, new LDPE (film grade), high density polyethylene(HDPE), hydroxy-terminated polybutadienes, ethene-hexene copolymer, ethylene-butene copolymer, ethylene-octene copolymer, ethylene-propylene-octene terpolymer, the hydrogenation of ethylene-butadiene-styrene copolymer, and it melts to refer to be 0.5 ~ 60g/10min.
4. raising polypropylene polarity filler parent granule according to claim 1 is characterized in that: described processing aid is one or more mixing in suffocated amine antioxidant, Hinered phenols antioxidant, phosphite, stearic acid, calcium stearate, Zinic stearas, whiteruss, the naphthenic oil.
5. the described raising polypropylene of claim 1 polarity is characterized in that comprising the steps: each component is mixed in proportion granulation again with the preparation method of filler parent granule.
6. the described raising polypropylene of claim 1 polarity is characterized in that with the using method of filler parent granule: the described filler parent granule of claim 1 is mixed with polypropylene, put into forcing machine then and carry out the melt blending extruding pelletization and get final product.
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