CN102286167B - Toughened polypropylene resin composition and preparation method thereof - Google Patents
Toughened polypropylene resin composition and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a toughened polypropylene resin composition comprising the following components: 100% of polypropylene (1), 7-35% of powdered styrene-butadiene rubber modified by carboxylic styrene butadiene latex (2) and 2-7% of grafted polypropylene (3). The notch impact strength of the polypropylene resin composition is 10 times more than that of polypropylene base resin; and through optimizing the components, the toughness of the polypropylene is greatly enhanced, and meanwhile, the strength and the rigidity of the resin are remained to the maximum extent, and the obtained polypropylene material has excellent combination property. The invention further discloses a preparation method of the toughened polypropylene resin composition.
Description
Technical field
The present invention relates to a kind of tenacity-increased profax resin composition and preparation method thereof, be specifically related to polypropylene resin composite of powdered rubber toughening modifying and preparation method thereof.
The background art
Polypropylene (PP) is kind with fastest developing speed in current general synthetic resin, and it is one of important developing direction of PP material for the manufacture of automobile, household electrical appliances, furniture parts that PP replaces engineering plastics.But because PP is semicrystalline polymer, structural characteristics cause the notched Izod impact strength of resin low, and fragile under low temperature disconnected, shrinking percentage is large, and creep resistance is poor, has greatly limited the further application of resin.Thus, the high performance study on the modification of PP has obtained people's generally attention, is particularly carrying out a large amount of research work aspect toughening modifying research.The PP toughening modifying also adopts various thermoplastic elastic bodies and PP blend to realize usually, as the rubber clone of toughening modifying comprise ethylene-propylene rubber(EPR) (as: US4983647, US4130535A, clear and 730145, ZL98121713.3, ZL91106759.0, ZL200410011367.X etc.), styrene-butadiene rubber(SBR) (ZL200310103222.8, US6150442, US5073447, US4734450), etc.
Powdered rubber refers to that particle diameter is less than the rubber of 1.0mm.Powdered rubber has good dispersiveness, can with resin grafting, blend, thereby give resin special performance, have widely in the resin modified field and use.ZL200510002252.9 discloses the resin combination that is comprised of homopolymer polypropylene, terpolymer EP rubber, Powdered Rubber of Ultrafine Styrene Butadiene, nucleator and rheology conditioner etc., composition has high impelling strength, the basic resin-phase of tensile strength and rigidity and polypropylene is worked as, and is applicable to prepare the higher large thin-wall goods of appearance requirement.Proposed to comprise that as CN101270212 (application number 200710064645.1) polypropylene, butylbenzene powdered rubber are or/and the blend composition of Carboxy powdered rubber, carbon black composition.ZL01110737.5 discloses a kind of tenacity-increased profax and preparation method thereof, comprise PP and mixed rubber component, wherein the mixed rubber component is comprised of the powdered rubber with crosslinking structure and at least a unvulcanized rubber and thermoplastic elastomer, powder PP+ sulfide powder butylbenzene+SIS is disclosed in enforcement, the composition system of powder PP+ sulfide powder butylbenzene+terpolymer EP rubber.It is raw material that Zhang Xiaohong etc. utilize fully cured ultrafine powdered styrene-butadiene rubber (PSBR) and polypropylene (PP), adopt the twin screw extruder blend method to prepare PP/PSBR fully sulfurized thermoplastic elastomer (China Synthetic Rubber Industry, 29 2 phases of volume in 2006, the 91-95 page).
Summary of the invention
The object of the invention is to provide a kind of tenacity-increased profax resin composition, and this polypropylene resin composite has good shock resistance.The present invention further proposes the preparation method of said composition.
The contriver finds by research, and under existing blending equipment condition, powdered rubber is prone to skewness, the unsettled problem of size and affects toughening effect in the polypropylene matrix resin as properties-correcting agent.At this point, the present invention proposes a kind of tenacity-increased profax resin composition, and take polyacrylic weight as a hundred per cent, composition comprises:
(1) polypropylene 100%
(2) modified powder styrene-butadiene rubber(SBR) 7%～35%
(3) graft polypropylene 2%～7%
Wherein, modified powder styrene-butadiene rubber(SBR) is the powder styrene butadiene rubber of carboxylic styrene butadiene latex modification.The contriver finds by research, and the powder styrene butadiene rubber particle diameter has certain influence to toughening effect; On the other hand, powdered rubber can have a negative impact to intensity, the rigidity of base resin in toughness reinforcing.Be to obtain the better resin combination of over-all properties, preferred rubber particle diameter of the present invention 0.2～0.7mm, 100 ℃ of mooney viscosity ML (1+4) are 41～123, and further 100 ℃ of preferred rubber mooney viscosity ML (1+4) are 80～120.
Carboxylic styrene butadiene latex is take divinyl, vinylbenzene as main monomer, and unsaturated carboxylic acid is that function monomer obtains through letex polymerization, and unsaturated carboxylic acid wherein is vinylformic acid, methacrylic acid or 2-ethylacrylic acid, preferred vinylformic acid.The solids content 41～55% of carboxylic styrene butadiene latex, latex particle size 100～175nm.
Polypropylene can be homopolymer or the multipolymer of propylene, can be powdery or granular resin, melt flow rate (MFR) (MFR) 0.5～40g/10min, density 0.900～0.921g/cm3.Preferred powdery acrylic resin.
Graft polypropylene is polar monomer and polyacrylic grafts, and polar monomer is selected from maleic anhydride, acrylic or methacrylic acid, preferred maleic anhydride inoculated polypropylene (PP-g-MAH), percentage of grafting 0.5～11%, MFR 〉=40g/10min.
The present invention also need add the auxiliary agents such as separant, dispersion agent, oxidation inhibitor, thermo-stabilizer in the preparation process of modified powder styrene-butadiene rubber(SBR) and polypropene composition, to satisfy processing and preparation technology's requirement.The preparation of polypropylene resin composite can be carried out in Banbury mixer, kneader, twin screw extruder, 185～220 ℃ of temperature of reaction, reaction times 3～5min, preferred twin screw extruder.When selecting twin screw extruder to prepare, the preparation technology that can adopt raw material to be pre-mixed, to extrude again.
Particularly, toughened polypropylene composition preparation method provided by the invention comprises:
(1) preparation of modified powder styrene-butadiene rubber(SBR)
Be water and 7～11% carboxylic styrene butadiene latexs (pressing the weight percent meter of the powder styrene butadiene rubber) mixing of 1: 2～1: 5 with weight percent; Mixed serum is warming up to 50～60 ℃ under whipped state; Add 2～5% separants (pressing the weight percent meter of carboxylic styrene butadiene latex) to mix 1～10min; Add again powder styrene butadiene rubber to mix 30～60min; Through discharging, dehydration, drying, obtain modified powder styrene-butadiene rubber(SBR);
(2) preparation of polypropene composition
With polyacrylic weight percent meter, with the dispersion agent high-speed mixing 1～10min of polypropylene, graft polypropylene and 0.3～0.9%; Add again modified powder styrene-butadiene rubber(SBR), 0.14%～0.26% stablizer and 0.1%～0.2% oxidation inhibitor, high-speed mixing 5～15min; Mixed material is added twin screw extruder, 185～220 ℃ of temperature of reaction, reaction times 3～5min extrudes, cooling, granulation, obtains toughened polypropylene composition.
Wherein, separant is the compound that fatty acid soaps compounds, stearate compounds and silicon compound form according to a certain ratio.Dispersion agent is selected from Poly Propylene Wax, polyethylene wax or white oil, optimization polypropylene wax.Oxidation inhibitor is selected from one or several compounds in phenols, hindered amines, phosphite ester kind antioxidant.Stablizer is selected from stearate, as Zinic stearas or calcium stearate a kind of or its compound wherein.
The present invention is by carrying out respectively modification to powder styrene butadiene rubber, polypropylene, both consistencies have obviously been improved, Uniform Dispersion and particle diameter are stable as far as possible in polypropylene matrix to make the powdered rubber particle, thereby improved significantly polyacrylic toughness, the notched Izod impact strength of composition improves more than 10 times than the basic resin of polypropylene.
Embodiment
(1) raw material
Powder butylbenzene 1500a particle diameter: 0.25～0.55mm; Petroleum Chemical Engineering Institute of PetroChina Company Limited.
100 ℃ of mooney viscosity ML (1+4) are 50
Powder butylbenzene 1500b particle diameter: 0.25～0.55mm; Petroleum Chemical Engineering Institute of PetroChina Company Limited.
100 ℃ of mooney viscosity ML (1+4) are 43
Powder butylbenzene 1712a particle diameter: 0.35～0.65mm, Petroleum Chemical Engineering Institute of PetroChina Company Limited.
100 ℃ of mooney viscosity ML (1+4) are 96
Carboxylic styrene butadiene latex contains 52% Petroleum Chemical Engineering Institute of PetroChina Company Limited. admittedly
Latex particle size 145nm
Separant (fatty acid calcium and Magnesium Stearate and silicone oil are by the mixture of 8: 5: 3 compositions) self-control
4.3% Shanghai day of graft polypropylene (PP-g-MAH) percentage of grafting rise chemical company
Poly Propylene Wax (WPP type) Jiangyin profit of a specified duration is moulded industry company limited
Antioxidant 1010 Switzerland vapour Bagong department
Zinic stearas Yangtse River in Chongqing chemical plant
(2) performance test standard
Socle girder notched Izod impact strength (23 ℃) GB1843
Melt flow rate (MFR) MFR (g/10min) GB/T3682-2000
Tensile strength GB/T1040-1992
Modulus in flexure GB/T9341
Rockwell hardness (R scale) GB9342
(3) equipment and instrument
Φ 34 Screw Extrusion captain/footpaths=34/1 German Lestreiz company
10L high-speed mixer Fuxin plastics machinery factory
15L cohesion still (whipped form: two layer of three oblique oar of leaf) sky, Lanzhou China scientific ﹠ technical corporation
Embodiment 1
(1) preparation of modified powder styrene-butadiene rubber(SBR): 0.05kg water and 0.2kg carboxylic styrene butadiene latex are joined in the cohesion still of 15L, pass into low-pressure steam, slurries are warming up to 55 ℃, mix 3min; Add 8g separant mixing 3min; Add again 2kg powder styrene butadiene rubber 1500a mixing 40min; Stop stirring discharging, centrifuge dehydration, under 50 ℃ dry 24hr, namely make modified powder styrene-butadiene rubber(SBR).
(2) preparation of polypropene composition: first with polypropylene F4012kg; Graft polypropylene 0.1kg; Poly Propylene Wax 10g mixes 3min in high-speed mixer; Add again modified powder styrene-butadiene rubber(SBR) 1500a 0.4kg, antioxidant 1010 3g, Zinic stearas 5g, high-speed mixing 5min after stopping mixing; The material that mixes is joined extruding pelletization in Φ 34 screw extrusion presss, and the extruding and pelletizing process condition sees Table 1, and the composition pellet of preparation is made standard test specimen with injecting method, and performance sees Table 2 after tested.
Embodiment 2
(1) preparation of modified powder styrene-butadiene rubber(SBR): 0.05kg water and 0.2kg carboxylic styrene butadiene latex are joined in the cohesion still of 15L, pass into low-pressure steam, slurries are warming up to 55 ℃, mix 3min; Add 8g separant mixing 3min; Add again 2kg powder styrene butadiene rubber 1500b mixing 30min; Stop stirring discharging, centrifuge dehydration, under 50 ℃ dry 24hr, namely make modified powder styrene-butadiene rubber(SBR).
(2) preparation of polypropene composition: first with polypropylene F4012kg; Graft polypropylene 0.12kg; Poly Propylene Wax 10g mixes 3min in high-speed mixer; Add again modified powder styrene-butadiene rubber(SBR) 1500b 0.5kg, antioxidant 1010 3g, Zinic stearas 5g, high-speed mixing 5min after stopping mixing; The material that mixes is joined extruding pelletization in Φ 34 twin screw extruders, and the extruding and pelletizing process condition sees Table 1, and the composition pellet of preparation is made standard test specimen with injecting method, and performance sees Table 2 after tested.
Embodiment 3
(1) preparation of modified powder styrene-butadiene rubber(SBR): 0.05kg water and 0.2kg carboxylic styrene butadiene latex are joined in the cohesion still of 15L, pass into low-pressure steam, slurries are warming up to 55 ℃, mix 3min; Add 8g separant mixing 3min; Add again 2kg powder styrene butadiene rubber 1712a mixing 30min; Stop stirring discharging, centrifuge dehydration, under 50 ℃ dry 24hr, namely make modified powder styrene-butadiene rubber(SBR).
(2) preparation of polypropene composition: first with polypropylene F4012kg; Graft polypropylene 0.08kg; Poly Propylene Wax 10g mixes 3min in high-speed mixer; Add again modified powder styrene-butadiene rubber(SBR) 1712a 0.16kg, antioxidant 1010 3g, Zinic stearas 5g, high-speed mixing 5min after stopping mixing; The material that mixes is joined extruding pelletization in Φ 34 twin screw extruders, and the extruding and pelletizing process condition sees Table 1, and the composition pellet of preparation is made standard test specimen with injecting method, and performance sees Table 2 after tested.
Embodiment 4
(1) preparation of modified powder styrene-butadiene rubber(SBR) is fully identical with embodiment 1.
(2) preparation of polypropene composition: first with polypropylene 77262kg; Graft polypropylene 0.1kg; Poly Propylene Wax 10g mixes 3min in high-speed mixer; Add again modified powder styrene-butadiene rubber(SBR) 1500a 0.4kg, antioxidant 1010 3g, Zinic stearas 5g, high-speed mixing 5min after stopping mixing; The material that mixes is joined extruding pelletization in Φ 34 twin screw extruders, and the extruding and pelletizing process condition sees Table 1, and the composition pellet of preparation is made standard test specimen with injecting method, and performance sees Table 2 after tested.
Embodiment 5
(1) preparation of modified powder styrene-butadiene rubber(SBR) is fully identical with embodiment 2.
(2) preparation of polypropene composition: first with polypropylene 77262kg; Graft polypropylene 0.12kg; Poly Propylene Wax 10g mixes 3min in high-speed mixer; Add again modified powder styrene-butadiene rubber(SBR) 1500b 0.5kg, antioxidant 1010 3g, Zinic stearas 5g, high-speed mixing 5min after stopping mixing; The material that mixes is joined extruding pelletization in Φ 34 twin screw extruders, and the extruding and pelletizing process condition sees Table 1, and the composition pellet of preparation is made standard test specimen with injecting method, and performance sees Table 2 after tested.
Embodiment 6
(1) preparation of modified powder styrene-butadiene rubber(SBR) is fully identical with embodiment 3.
(2) preparation of polypropene composition: first with polypropylene 77262kg; Graft polypropylene 0.08kg; Poly Propylene Wax 10g mixes 3min in high-speed mixer; Add again modified powder styrene-butadiene rubber(SBR) 1712a 0.16kg, antioxidant 1010 3g, Zinic stearas 5g, high-speed mixing 5min after stopping mixing; The material that mixes is joined extruding pelletization in Φ 34 twin screw extruders, and the extruding and pelletizing process condition sees Table 1, and the composition pellet of preparation is made standard test specimen with injecting method, and performance sees Table 2 after tested.
Comparative Examples 1
Cancel the powdered rubber modification procedure, direct choice of powder styrene-butadiene rubber(SBR) 1500a, the preparation process of polypropene composition and test process are with embodiment 1.
Comparative Examples 2
Cancel the powdered rubber modification procedure, direct choice of powder styrene-butadiene rubber(SBR) 1500b, the preparation process of polypropene composition and test process are with embodiment 4.
Comparative Examples 3
Cancel the powdered rubber modification procedure, direct choice of powder styrene-butadiene rubber(SBR) 1712a, the preparation process of polypropene composition and test process are with embodiment 6.
Comparative Examples 4
(1) preparation of modified powder styrene-butadiene rubber(SBR) is fully identical with embodiment 1.
(2) do not add in the preparation process of polypropene composition graft polypropylene, other are identical with embodiment 1.
Comparative Examples 5
(1) preparation of modified powder styrene-butadiene rubber(SBR) is fully identical with embodiment 3.
(2) do not add in the preparation process of polypropene composition graft polypropylene, other are identical with embodiment 3.
Comparative Examples 6
(1) preparation of modified powder styrene-butadiene rubber(SBR) is fully identical with embodiment 4.
(2) do not add in the preparation process of polypropene composition graft polypropylene, other are identical with embodiment 4.
The twin-screw extrusion preparation condition of table 1 polypropene composition
The physical and mechanical properties of table 2 polypropene composition
| Numbering | Socle girder notched Izod impact strength (23 ℃), J/m | MFR，g/10min | Tensile strength, Mpa | Modulus in flexure, Mpa | Rockwell hardness, the R scale |
| Embodiment 1 | 312.4 | 1.7 | 23.3 | 1550 | 87 |
| Embodiment 2 | 298.2 | 2.1 | 21.1 | 1272 | 83 |
| Embodiment 3 | 306.1 | 1.5 | 30.4 | 1602 | 92 |
| Embodiment 4 | 674.5 | 25.4 | 16.3 | 1163 | 67 |
| Embodiment 5 | 663.1 | 27.2 | 15.8 | 1074 | 63 |
| Embodiment 6 | 672.3 | 26.7 | 22.3 | 1236 | 77 |
| Comparative Examples 1 | 47.2 | 1.3 | 22.4 | 1402 | 81 |
| Comparative Examples 2 | 123.4 | 18.2 | 16.7 | 1168 | 69 |
| Comparative Examples 3 | 215.3 | 25.3 | 21.7 | 1248 | 81 |
| Comparative Examples 4 | 117.2 | 1.8 | 23.4 | 1346 | 71 |
| Comparative Examples 5 | 217.2 | 1.4 | 26.3 | 1544 | 81 |
| Comparative Examples 6 | 317.2 | 23.8 | 13.4 | 1045 | 72 |
| Reference sample 1 * | 29.1 | 2.4 | 35.4 | 1712 | 100 |
| Reference sample 2 * | 65.2 | 29 | 25.1 | 1430 | 84 |
Reference sample 1
*: commercially available Petrochina Lanzhou Petrochemical Company produce polypropylene F401 powder from measured value.
Reference sample 2
*: commercially available Sinopec Yanshan Petrochemical company produce polypropylene 7726 pellets from measured value.
Claims (8)
1. tenacity-increased profax resin composition is characterized in that composition comprises take polyacrylic weight as absolutely:
(1) polypropylene 100%
(2) modified powder styrene-butadiene rubber(SBR) 7%～35%
(3) graft polypropylene 2%～7%
Wherein, modified powder styrene-butadiene rubber(SBR) is the powder styrene butadiene rubber of carboxylic styrene butadiene latex modification, powdered rubber particle diameter 0.2～0.7mm, and 100 ℃ of mooney viscosity ML (1+4) are 41～123; The solids content 41～55% of carboxylic styrene butadiene latex, latex particle size 100～175nm; Graft polypropylene is polar monomer and polyacrylic grafts, percentage of grafting 0.5～11%, melt flow rate (MFR) 〉=40g/10min.
2. resin combination according to claim 1, is characterized in that graft polypropylene is maleic anhydride inoculated polypropylene.
3. resin combination according to claim 1 is characterized in that 100 ℃ of powdered rubber mooney viscosity ML (1+4) in modified powder styrene-butadiene rubber(SBR) are 80～120; Carboxylic styrene butadiene latex is take divinyl, vinylbenzene as main monomer, and vinylformic acid is that function monomer obtains through letex polymerization.
4. resin combination according to claim 1, is characterized in that polypropylene is homopolymer or the multipolymer of propylene, melt flow rate (MFR) 0.5～40g/10min, density 0.900～0.921g/cm
3
5. resin combination according to claim 4, is characterized in that polypropylene is the powdered polypropylene resin.
6. method for preparing one of the described resin combination of claim 1-5 is characterized in that the preparation method comprises:
(1) preparation of modified powder styrene-butadiene rubber(SBR)
Weight by powder styrene butadiene rubber is a hundred per cent, and the water and 7～11% carboxylic styrene butadiene latexs that are 1:2～1:5 with weight ratio mix; Mixed serum is warming up to 50～60 ℃ under whipped state; Weight by carboxylic styrene butadiene latex is a hundred per cent, adds 2～5% separants to mix 1～10min; Add again powder styrene butadiene rubber to mix 30～60min; Through discharging, dehydration, drying, obtain modified powder styrene-butadiene rubber(SBR);
(2) preparation of polypropene composition
With polyacrylic weight percent meter, with the dispersion agent high-speed mixing 1～10min of polypropylene, graft polypropylene and 0.3～0.9%; Add again modified powder styrene-butadiene rubber(SBR), 0.14%～0.26% stablizer and 0.1%～0.2% oxidation inhibitor, high-speed mixing 5～15min; Mixed material is added twin screw extruder, 185～220 ℃ of temperature of reaction, reaction times 3～5min extrudes, cooling, granulation, obtains toughened polypropylene composition.
7. the preparation method of resin combination according to claim 6, is characterized in that separant is the compound that fatty acid soaps compounds, stearate compounds and silicon compound form according to a certain ratio; Dispersion agent is Poly Propylene Wax, polyethylene wax or white oil; Oxidation inhibitor is one or several compounds in phenols, hindered amines, phosphite ester kind antioxidant; Stablizer is stearate.
8. the preparation method of resin combination according to claim 7, is characterized in that dispersion agent is Poly Propylene Wax; Stablizer is Zinic stearas or calcium stearate a kind of or its compound wherein.
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| WO2020112546A1 (en) | 2018-11-28 | 2020-06-04 | Braskem America, Inc. | Blends of polyolefins with functionalized polybutadienes |
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| CN1908052A (en) * | 2005-08-02 | 2007-02-07 | 中国石油天然气股份有限公司 | Reinforced polypropylene composition and method of preparing the same |
| CN101270212A (en) * | 2007-03-22 | 2008-09-24 | 中国石油化工股份有限公司 | Polypropelene composition capable of making with laser and preparation method thereof |
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| CN1908052A (en) * | 2005-08-02 | 2007-02-07 | 中国石油天然气股份有限公司 | Reinforced polypropylene composition and method of preparing the same |
| CN101270212A (en) * | 2007-03-22 | 2008-09-24 | 中国石油化工股份有限公司 | Polypropelene composition capable of making with laser and preparation method thereof |
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