CN1184258C - Reinforced toughened polypropylene material preparing method - Google Patents
Reinforced toughened polypropylene material preparing method Download PDFInfo
- Publication number
- CN1184258C CN1184258C CNB031293786A CN03129378A CN1184258C CN 1184258 C CN1184258 C CN 1184258C CN B031293786 A CNB031293786 A CN B031293786A CN 03129378 A CN03129378 A CN 03129378A CN 1184258 C CN1184258 C CN 1184258C
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- Prior art keywords
- polypropylene
- epoxy resin
- polypropylene material
- maleic anhydride
- epoxy
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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- 239000004743 Polypropylene Substances 0.000 title claims abstract description 49
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 49
- -1 polypropylene Polymers 0.000 title claims abstract description 45
- 239000000463 material Substances 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 14
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000003822 epoxy resin Substances 0.000 claims abstract description 10
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims description 10
- 230000002708 enhancing effect Effects 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 9
- 229920001577 copolymer Polymers 0.000 claims description 8
- LCFVJGUPQDGYKZ-UHFFFAOYSA-N Bisphenol A diglycidyl ether Chemical compound C=1C=C(OCC2OC2)C=CC=1C(C)(C)C(C=C1)=CC=C1OCC1CO1 LCFVJGUPQDGYKZ-UHFFFAOYSA-N 0.000 claims description 6
- 229920001971 elastomer Polymers 0.000 claims description 6
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical group O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 claims description 4
- 229920001897 terpolymer Polymers 0.000 claims description 4
- ULKLGIFJWFIQFF-UHFFFAOYSA-N 5K8XI641G3 Chemical compound CCC1=NC=C(C)N1 ULKLGIFJWFIQFF-UHFFFAOYSA-N 0.000 claims description 3
- 238000001125 extrusion Methods 0.000 claims description 2
- 229940015043 glyoxal Drugs 0.000 claims description 2
- 239000004848 polyfunctional curative Substances 0.000 claims description 2
- 239000011347 resin Substances 0.000 abstract description 22
- 229920005989 resin Polymers 0.000 abstract description 22
- 238000001723 curing Methods 0.000 abstract description 9
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000010276 construction Methods 0.000 abstract description 2
- 238000011065 in-situ storage Methods 0.000 abstract 1
- 238000003754 machining Methods 0.000 abstract 1
- 238000003801 milling Methods 0.000 abstract 1
- 239000004593 Epoxy Substances 0.000 description 21
- 229920002943 EPDM rubber Polymers 0.000 description 7
- 238000012360 testing method Methods 0.000 description 6
- 229920000181 Ethylene propylene rubber Polymers 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 230000035939 shock Effects 0.000 description 4
- 229920001935 styrene-ethylene-butadiene-styrene Polymers 0.000 description 3
- 229920002725 thermoplastic elastomer Polymers 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 2
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 2
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 235000012204 lemonade/lime carbonate Nutrition 0.000 description 2
- 239000012764 mineral filler Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 229960001866 silicon dioxide Drugs 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- IBVAQQYNSHJXBV-UHFFFAOYSA-N adipic acid dihydrazide Chemical compound NNC(=O)CCCCC(=O)NN IBVAQQYNSHJXBV-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 150000002118 epoxides Chemical group 0.000 description 1
- 229920001038 ethylene copolymer Polymers 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 229940042795 hydrazides for tuberculosis treatment Drugs 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229920003031 santoprene Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Epoxy Resins (AREA)
Abstract
The present invention provides a preparing method of a reinforced and toughened polypropylene material. A dynamic curing method is used for a polypropylene/epoxy resin system, namely that when epoxy resin and polypropylene is melted and blended, curing reaction occurs. Under a certain blending temperature, polypropylene resin, an elastic body grafted by maleic anhydride, epoxy resin and a curing agent are orderly added in a Banbury mixer, a blender mill or a screw extruder for milling, the epoxy resin generates 'in situ curing ' and is dispersed into micron order particles under the function of high shear force, and the micron order particles are evenly distributed in the polypropylene so as to enhance the rigidity and the modulus of the polypropylene; on one hand, the elastic body in the system performs the function of compatibilization; on the other hand, the elastic body performs the function of toughening the polypropylene. Both the rigidity and the toughness of the polypropylene material prepared by the dynamic curing method are increased in larger degree, which can satisfy the requirements of engineering materials. The process has the advantages of simple production technology, good machining performance, strong applicability, etc.; the prepared polypropylene material can be used as materials of civil constructions, automobile fittings, household appliances, etc.
Description
Technical field: the present invention relates to a kind of enhancing flexibilized polypropylene material preparation method, particularly with in dynamical cure method using polypropylene/epoxy-resin systems, curing reaction takes place when being Resins, epoxy and polypropylene fusion blend, Resins, epoxy after the curing can increase polyacrylic intensity and modulus, and the elastomerics of maleic anhydride graft can increase polypropylene toughness.
Background technology: polypropylene (PP) is the general-purpose plastics that a class is of wide application, and has good processing properties and mechanical property, but low, the poor toughness of its notched Izod impact strength is difficult to satisfy the requirement of engineering materials.Usually improve polypropylene flexible method and be to wherein adding a certain amount of rubber-like elastomerics (US Patent, 5,292,811, US Patent, 5,763,532), as terpolymer EP rubber (EPDM), ethylene-propylene rubber(EPR) (EPR), ethylene-octene copolymer (POE), styrene-ethylene-butylene-styrene segmented copolymer (SEBS) etc., but elastomeric adding unavoidably can reduce polypropylene rigidity and modulus.In order to make polyacrylic over-all properties be able to balance, when adding the rubber-like elastomerics, also adding mineral filler simultaneously increases its rigidity and modulus.This class mineral filler mainly contains talcum powder, lime carbonate, silicon-dioxide etc.Properties of Polypropylene after modification can reach the requirement of engineering materials, has obtained widespread use on bumper.The super polyolefine (SOP) of Toyota Motor, mitsui petrochemical industry, the exploitation of Sumitomo Chemical affiliated company, the quaternary co-mixing system that SOP is made up of 60% PP, 30% EPR and ethylene copolymer and 10% talcum powder, wherein amorphous component surpasses 50% (volume fraction) and constitutes external phase, be that a kind of higher order structure that carries out on nanometer level designs formed novel polymer material, can replace the use of some engineering plastics.In recent years, begin the research of inorganic nano-filler enhancing Toughened PP both at home and abroad, comprised the research of Nano fillings filling PP such as polynite, lime carbonate, silicon-dioxide.But inorganic nano-particle is bigger with the PP polarity difference, and the two consistency is poor, and nanoparticle surface can be high and very easily reunite, so be difficult to obtain the matrix material of excellent performance.People such as Xiao Qihai propose the polyethylene tenacity-increased profax with ultra-high molecular weight, and polyacrylic toughness and rigidity are able to good balance (CN1127272).
1972, the K.Fisher of U.S. Uniroyal company developed dynamic part sulfuration EPT rubber/thermoplastic elastomer (US Patent 3,758,643).At the beginning of the eighties, the A.Y.Coran of U.S. Monsanto company develops the dynamic full vulcanization EPT rubber/thermoplastic elastomer, and has formally realized suitability for industrialized production with trade(brand)name Santoprene in nineteen eighty-two.The intensity of this thermoplastic elastomer and modulus are higher than the intensity and the modulus of the prepared EPDM/PP blend of simple blend, but are difficult to reach the desired intensity of engineering materials.
Summary of the invention: the objective of the invention is to the dynamical cure method is applied in Resins, epoxy/polypropylene system, propose a kind of novel method that strengthens tenacity-increased profax.It is simple that this method has production technique, good processability, advantage such as suitability is strong.Elastomerics with maleic anhydride graft of active group can react with hydroxyl in the Resins, epoxy and epoxide group, Resins, epoxy and polyacrylic consistency have been promoted, after adding solidifying agent, because under the effect of high shear force, Resins, epoxy " solidifies on the spot " and is dispersed into micron particles, be evenly distributed in the polypropylene, greatly improved polyacrylic rigidity and modulus.Elastomerics as the maleic anhydride graft of expanding material can improve polyacrylic toughness, and the adding of Resins, epoxy can make toughening effect more remarkable.
A kind of enhancing flexibilized polypropylene material preparation method of the present invention is applied in the dynamical cure method in the polypropylene/epoxy resin system, i.e. curing reaction takes place during Resins, epoxy and polypropylene fusion blend.Under 180～230 ℃ blending temperature, in Banbury mixer, mill or screw extrusion press, the elastomerics, Resins, epoxy, the solidifying agent that add acrylic resin, maleic anhydride graft successively carry out mixing.Wherein used polypropylene consumption is 30～75 weight parts, and the elastomeric consumption of maleic anhydride graft is 20～40 weight parts, and content of epoxy resin is 5～30 weight parts, and hardener dose is 0.2～5 weight part, and the blend time is 7～15min.
The Resins, epoxy that uses among the present invention is bisphenol-A diglycidyl ether type, Bisphenol F diglycidyl ether-type and line style phenolic aldehyde polyglycidyl ether type Resins, epoxy.
The elastomerics of the maleic anhydride graft that uses among the present invention is terpolymer EP rubber (MAH-g-EPDM), ethylene-octene copolymer (MAH-g-POE) and styrene-ethylene-butylene-styrene segmented copolymer (MAH-g-SEBS).
The solidifying agent that the present invention uses is dicyanamide, glyoxal ethyline, 2-ethyl-4-methylimidazole, adipic acid dihydrazide, m-phthalic acid two hydrazides, certain herbaceous plants with big flowers hydrazine etc.
Polypropylene material modulus and toughness that the present invention makes are all significantly improved, stable performance, and suitability is strong, can satisfy the requirement of engineering materials, can be used as materials such as civil construction, auto parts machinery, household electrical appliance.Preparation method provided by the present invention is easy to operate, and technology is simple, and excellent industrial application foreground is arranged.Compare with glass fibre and rubber-like elastomerics enhancing tenacity-increased profax with conventional inorganic fillers, the material that the present invention makes improving tensile strength and shock strength simultaneously, has kept high rigidity and modulus.
Description of drawings: figure the-1st, the electromicroscopic photograph figure of enhancing flexibilized polypropylene material.
Embodiment: the following examples are to further specify of the present invention, rather than limit the scope of the invention.
Embodiment 1-4; By the prescription in the table-1, under 190 ℃ temperature, in Banbury mixer or mill, at first add polypropylene, the terpolymer EP rubber (MAH-g-EPDM), the Resins, epoxy (bisphenol-A diglycidyl ether type that add maleic anhydride graft then successively, the trade mark: E-06), 2-ethyl-4-methylimidazole (EMI-2,4), Resins, epoxy generation curing reaction in the blend process, and under high shear, disperse to be micron particles and be distributed in the polypropylene and (see figure-1).The blend that makes is in blocks with the vulcanizing press mold pressing.Tailor batten by standard size, sample is pressed ASTM D638 respectively, ASTM D790, performance index such as ASTM D256 standard testing stretching, bending, impact.
Test result is shown in table-1.After adding MAH-g-EPDM, though the toughness of PP improves a lot, rigidity obviously reduces.In the PP/MAH-g-EPDM co-mixing system, add Resins, epoxy and dynamical cure, rigidity and the toughness of PP are all significantly improved.
Table-1
Example reference examples reference examples 1234
Prescription (parts by weight)
Polypropylene 75 100 70 65 55 45
Resins, epoxy 5 10 20 30
EMI-2，4 0.2 0.4 0.8 1.2
MAH-g-EPDM 25 25 25 25 25
Physical and mechanical properties
Shock strength, J/m 115 30 216 310 360 230
Tensile strength, MPa 27.5 30.6 29.5 33.3 34.8 35.2
Elongation at break, % 412 300 210 134 54 46
Modulus in flexure, MPa 854 1,142 1,065 1,234 1,513 1678
Embodiment 5-7; By the prescription in the table-2, under 190 ℃ temperature, in Banbury mixer or mill, at first add polypropylene, the ethylene-octene copolymer (MAH-g-POE), the Resins, epoxy (bisphenol-A diglycidyl ether type that add maleic anhydride graft then successively, the trade mark: E-06), solidifying agent (EMI-2,4), Resins, epoxy dynamical cure in the blend process.Specimen preparation and testing standard are operated by example 1-4.Test result is shown in table-2.
Table-2
Example reference examples 567
Prescription (parts by weight)
Polypropylene 75 70 65 55
Resins, epoxy 5 10 20
EMI-2，4 0.2 0.4 0.8
MAH-g-POE 25 25 25 25
Physical and mechanical properties
Shock strength, J/m 124 175 268 301
Tensile strength, MPa 24.5 29.2 31.2 33.8
Elongation at break, % 530 248 126 79
Modulus in flexure, MPa 824 968 1,156 1356
Embodiment 8-10; By the prescription in the table-3, under 190 ℃ temperature, in Banbury mixer or mill, at first add polypropylene, the styrene-ethylene-butylene-styrene segmented copolymer (MAH-g-SEBS), the Resins, epoxy (bisphenol-A diglycidyl ether type that add maleic anhydride graft then successively, the trade mark: E-06), solidifying agent (EMI-2,4), Resins, epoxy dynamical cure in the blend process.Specimen preparation and testing standard are operated by example 1-4.Test result is shown in table-3.
Table-3
Example reference examples 89 10
Prescription (parts by weight)
Polypropylene 80 70 60 50
Resins, epoxy 10 20 30
EMI-2，4 0.4 0.8 1.2
MAH-g-SEBS 20 20 20 20
Physical and mechanical properties
Shock strength, J/m 285 360 312 295
Tensile strength, MPa 30.2 33.4 34.4 33.2
Elongation at break, % 456 320 285 223
Modulus in flexure, MPa 830 1,275 1,396 1454
Claims (3)
1, a kind of enhancing flexibilized polypropylene material preparation method, it is characterized in that, the dynamical cure method is applied in the polypropylene/epoxy resin system, under 180～230 ℃ blending temperature, to Banbury mixer, add polypropylene in mill or the screw extrusion press successively, the elastomerics of maleic anhydride graft, bisphenol-A diglycidyl ether type epoxy resin, solidifying agent carries out mixing, wherein used polypropylene consumption is 30～75 weight parts, the elastomeric consumption of maleic anhydride graft is 20～40 weight parts, the bisphenol-A diglycidyl ether type epoxy resin consumption is 5～30 weight parts, hardener dose is 0.2～5 weight part, and the blend time is 7～15min.
2, enhancing flexibilized polypropylene material preparation method according to claim 1 is characterized in that, the elastomerics of used maleic anhydride graft is terpolymer EP rubber, ethylene-octene copolymer or styrene-ethylene-butylene-styrene segmented copolymer.
3, enhancing flexibilized polypropylene material preparation method according to claim 1 is characterized in that, used solidifying agent is glyoxal ethyline or 2-ethyl-4-methylimidazole.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031293786A CN1184258C (en) | 2003-06-19 | 2003-06-19 | Reinforced toughened polypropylene material preparing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031293786A CN1184258C (en) | 2003-06-19 | 2003-06-19 | Reinforced toughened polypropylene material preparing method |
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| Publication Number | Publication Date |
|---|---|
| CN1472246A CN1472246A (en) | 2004-02-04 |
| CN1184258C true CN1184258C (en) | 2005-01-12 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB031293786A Expired - Lifetime CN1184258C (en) | 2003-06-19 | 2003-06-19 | Reinforced toughened polypropylene material preparing method |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100349937C (en) * | 2005-06-28 | 2007-11-21 | 茂名众和化塑有限公司 | Cellulosine plastic composite compatiblizing agent and method for making same |
| CN102873875A (en) * | 2012-09-12 | 2013-01-16 | 中原工学院 | Method for toughening and enhancing polypropylene |
| CN103044796B (en) * | 2012-12-27 | 2015-12-09 | 安徽科聚新材料有限公司 | A kind of epoxy resin strengthens polystyrene bittern-free flame-proof material and preparation method thereof |
| CN114410016B (en) * | 2021-12-17 | 2023-10-13 | 国家能源集团宁夏煤业有限责任公司 | Polypropylene composition, method for preparing toughened impact-resistant copolymer polypropylene resin, toughened impact-resistant copolymer polypropylene resin and application thereof |
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2003
- 2003-06-19 CN CNB031293786A patent/CN1184258C/en not_active Expired - Lifetime
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| Publication number | Publication date |
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| CN1472246A (en) | 2004-02-04 |
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