CN1272373C - Preparation of polypropylene / organic montmorillonite nanometer composite material - Google Patents
Preparation of polypropylene / organic montmorillonite nanometer composite material Download PDFInfo
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- CN1272373C CN1272373C CN 200410066433 CN200410066433A CN1272373C CN 1272373 C CN1272373 C CN 1272373C CN 200410066433 CN200410066433 CN 200410066433 CN 200410066433 A CN200410066433 A CN 200410066433A CN 1272373 C CN1272373 C CN 1272373C
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- polypropylene
- organic montmorillonite
- composite material
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- montmorillonite
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- -1 polypropylene Polymers 0.000 title claims abstract description 83
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 57
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 55
- 229910017059 organic montmorillonite Inorganic materials 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000002131 composite material Substances 0.000 title abstract description 5
- 239000000463 material Substances 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 239000003822 epoxy resin Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 9
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 6
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 30
- 239000004593 Epoxy Substances 0.000 claims description 23
- 229920005989 resin Polymers 0.000 claims description 22
- 239000011347 resin Substances 0.000 claims description 22
- 239000002114 nanocomposite Substances 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 9
- 150000002460 imidazoles Chemical class 0.000 claims description 8
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 8
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 5
- LCFVJGUPQDGYKZ-UHFFFAOYSA-N Bisphenol A diglycidyl ether Chemical group C=1C=C(OCC2OC2)C=CC=1C(C)(C)C(C=C1)=CC=C1OCC1CO1 LCFVJGUPQDGYKZ-UHFFFAOYSA-N 0.000 claims description 4
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 claims description 4
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 4
- 239000003760 tallow Substances 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- ULKLGIFJWFIQFF-UHFFFAOYSA-N 5K8XI641G3 Chemical compound CCC1=NC=C(C)N1 ULKLGIFJWFIQFF-UHFFFAOYSA-N 0.000 claims description 2
- 238000005469 granulation Methods 0.000 claims description 2
- 230000003179 granulation Effects 0.000 claims description 2
- 239000004848 polyfunctional curative Substances 0.000 claims description 2
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- 229920001519 homopolymer Polymers 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000010276 construction Methods 0.000 abstract description 2
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000007711 solidification Methods 0.000 abstract 4
- 230000008023 solidification Effects 0.000 abstract 4
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 abstract 1
- 238000011065 in-situ storage Methods 0.000 abstract 1
- 239000011976 maleic acid Substances 0.000 abstract 1
- 238000010008 shearing Methods 0.000 abstract 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 4
- 241000446313 Lamella Species 0.000 description 3
- 239000004927 clay Substances 0.000 description 3
- 230000002687 intercalation Effects 0.000 description 3
- 238000009830 intercalation Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- 229920005992 thermoplastic resin Polymers 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 238000005453 pelletization Methods 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000945 filler Substances 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
- 239000010410 layer Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000012764 mineral filler Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229920006113 non-polar polymer Polymers 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 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 preparation method of a polypropylene / organic montmorillonite nanometer composite material. A dynamic solidification technology is used in a polypropylene / organic montmorillonite / epoxy resin system, i.e. a solidification reaction occurs during melt blending; polypropylene, grafting maleic acid anhydridized polypropylene, organic montmorillonite, epoxy resin and a solidification agent are orderly added to a double-screw extruder and are mixed with each other at certain mixing temperature; then, the epoxy resin has an 'in-situ solidification reaction' and is intercalated between slice layers of the organic montmorillonite under the action of high shearing force so as strip the organic montmorillonite. The rigidity and the toughness of the polypropylene are greatly improved, and the obtained blending objects can meet requirements of engineering materials. The method has the advantages of simple production process, good processing performance, strong applicability, etc. The obtained polypropylene / organic montmorillonite nanometer composite materials can be used as materials for civil construction, vehicle fittings, household appliances, etc.
Description
Technical field
The present invention relates to a kind of preparation method of polypropylene/organic montmorillonite nano composite material, particularly the dynamical cure method is applied to prepare polypropylene composite material in polypropylene/organic montmorillonite/epoxy-resin systems.
Background technology
Polypropylene is a kind of polyolefin resin of present large usage quantity, has the good mechanical performance, but its rigidity and modulus are not high, is difficult to satisfy the requirement of engineering materials.In order to improve polyacrylic rigidity and modulus, add mineral filler and glass fibre usually therein, strengthen that with filler toughness of material is descended, adopt nanoparticle then can realize enhancing and toughness reinforcing simultaneously.In recent years, the research of relevant polypropylene (PP)/organo montmorillonite (OMMT) nano composite material is active day by day.But these polypropylene/organic montmorillonite nano composite materials of having reported belong to intercalation type nano composite material mostly, can not give full play to the nanoscale effect of nano-dispersed phase, so its highly malleablized effect does not reach expected value (seeing Chinese patent CN1247206A, CN1267682A, U.S. Pat 5910523).Peel off even reach, mechanical property is also undesirable.The such non-polar polymer macromolecular chain of PP is difficult to enter into organo montmorillonite sheet interlayer by the melt intercalation, and the dispersion of clay lamella in the PP matrix is also very difficult simultaneously.
Resins, epoxy (EP) is a kind of important thermosetting resin, solidify back cross-linking density height, be tridimensional network, can strengthen the bonding interface between some thermoplastic resin (as polyvinyl chloride etc.) and thermoplastic resin and the fiber, and the consistency of improving the incompatible thermoplastic resin co-mixing system.The river is learned good general's dynamic vulcanization technology and is applied in the polypropylene/epoxy resin co-mixing system, select maleic anhydride graft PP as expanding material, the tensile strength and the modulus in flexure of prepared dynamical cure polypropylene/epoxy resin blend are higher, and over-all properties is (seeing Chinese patent CN 1425709A) better.
Resins, epoxy and organo montmorillonite have good consistency, Resins, epoxy can insert organic montmorillonite layer and solidify back formation Resins, epoxy/organic montmorillonite nano composite material, organo montmorillonite reaches peels off attitude, improves the mechanical property (seeing Chinese patent CN 1354198A) of material greatly.
Summary of the invention
The objective of the invention is the dynamical cure technology is applied to polypropylene/organic montmorillonite/Resins, epoxy compound system, propose a kind of novel method that strengthens tenacity-increased profax.Dynamical cure is meant that Resins, epoxy in the process of polypropylene and organo montmorillonite blend curing reaction takes place, and it is simple that this method has production technique, good processability, advantage such as suitability is strong.The liquor-saturated grafted polypropylene of toxilic acid with active group can react with hydroxyl in two (2-hydroxyethyl) methyl tallow based quaternary ammonium salt montmorillonite modified, promote organo montmorillonite and polyacrylic consistency, organo montmorillonite and Resins, epoxy also have good consistency.Resins, epoxy can be inserted into organo montmorillonite sheet interlayer in the blend process, add solidifying agent curing back formation reticulated structure organo montmorillonite is peeled off, and greatly improves polyacrylic rigidity and toughness.
The preparation method of a kind of polypropylene/organic montmorillonite nano composite material of the present invention is as follows: add polypropylene in twin screw extruder, maleic anhydride inoculated polypropylene, organo montmorillonite, Resins, epoxy and solidifying agent, under 190～200 ℃ blending temperature, carry out mixing, wherein used polypropylene consumption is 70～85 weight parts, the consumption of maleic anhydride inoculated polypropylene is 10 weight parts, content of epoxy resin is 2～10 weight parts, hardener dose is 0.08～0.4 weight part, the organo montmorillonite consumption is 1～5 weight part, the blend time is 2～10min, blend under the screw speed of 100～200rpm obtains polypropylene/organic montmorillonite nano composite material through granulation.
The used Resins, epoxy of the present invention is bisphenol-A diglycidyl ether type or Bisphenol F diglycidyl ether-type.
The used organo montmorillonite of the present invention is two (2-hydroxyethyl) methyl tallow based quaternary ammonium salt montmorillonite modified or octadecyl tribromide ammonium montmorillonite modified.
The used solidifying agent of the present invention is a Dyhard RU 100, imidazoles (EMI) or 2-ethyl-4-methylimidazole.
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 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
Fig. 1 is the X-ray diffractogram of the nano composite material of different organo montmorillonite content
Prescription: (polypropylene+organo montmorillonite) 80, Resins, epoxy 10, imidazoles 0.4
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 200 ℃ temperature; in twin screw extruder, add polypropylene (F401; melting index 2.3g/10min; raise sub-petrochemical corporation (complex)); the polypropylene of maleic anhydride graft (MAH-g-PP, percentage of grafting 1%, Shanghai day rise plastics company limited); Resins, epoxy (bisphenol-A diglycidyl ether type; the trade mark: E-12 epoxy equivalent (weight) 810g/eq; Shanghai resin T company limited); imidazoles (EMI, analytical pure, Shanghai chemical reagent factory); organo montmorillonite (two (2-hydroxyethyl) methyl tallow based quaternary ammonium salt modification; the DK2 type, Zhejiang Feng Hong clay company limited) extruding pelletization, screw speed 110 commentaries on classics/min.Resins, epoxy generation curing reaction in extrusion, and under high shear, be inserted in the organo montmorillonite lamella.The composite material granular that makes is made the standard batten with injection moulding machine, and sample is pressed performance index such as ASTM D638, ASTM D790, ASTM D256 standard testing stretching, bending, impact respectively.
The result in the polypropylene/organic montmorillonite co-mixing system, adds Resins, epoxy and dynamical cure shown in table-1, rigidity and the toughness of PP are all significantly improved.Compare with pure PP, toughness improves 160%, and rigidity improves 65%.The prescription of table 1 carries out X-ray diffraction test, the result as shown in Figure 1, organo montmorillonite was less than 2% o'clock as shown in Figure 1, organo montmorillonite reaches peels off attitude, other the time be in the intercalation attitude.
Table-1
| Example | Reference examples | Reference examples | 1 | 2 | 3 | 4 |
| Prescription (weight fraction) polypropylene maleic anhydride inoculated polypropylene organo montmorillonite Resins, epoxy imidazoles physical and mechanical properties shock strength, the J/m tensile strength, the MPa elongation at break, % | 100 30 31 300 | 88 10 2 46 44.6 120 | 80 10 10 0.4 36 35 20 | 78 10 2 10 0.4 78 54.4 100 | 77 10 3 10 0.4 60 53.8 98 | 75 10 5 10 0.4 44 52.9 95 |
| Modulus in flexure, MPa | 1150 | 1550 | 1749 | 1902 | 1930 | 1998 |
Embodiment 5～8: by the prescription in the table-2; under 200 ℃ temperature; in twin screw extruder, add polypropylene (F401; melting index 2.3g/10min; raise sub-petrochemical corporation (complex)); polypropylene (the MAH-g-PP of maleic anhydride graft; percentage of grafting 1%; Shanghai day rise plastics company limited); Resins, epoxy (bisphenol-A diglycidyl ether type, the trade mark: E-12 epoxy equivalent (weight) 810g/eq, Shanghai Resin Factory Co., Ltd.); imidazoles (EMI; analytical pure; Shanghai chemical reagent factory), organo montmorillonite (modification of octadecyl tribromide ammonium, DK1 type; Zhejiang Feng Hong clay company limited) extruding pelletization; Resins, epoxy generation curing reaction in the blend process, and under high shear, be inserted in the organo montmorillonite lamella.The blend that makes is made the standard batten with injection moulding machine, and specimen preparation and testing standard are operated by example 1-1.
Test result is as shown in table 2, and the polynite of adding usefulness octadecyl tribromide ammonium modification is dynamical cure again, compares with pure PP, and toughness improves 66%, and rigidity improves 55%.
Table-2
| Example | Reference examples | Reference examples | 5 | 6 | 7 | 8 |
| Prescription (weight fraction) polypropylene maleic anhydride inoculated polypropylene organo montmorillonite Resins, epoxy imidazoles physical and mechanical properties shock strength, the J/m tensile strength, the MPa elongation at break, the % modulus in flexure, MPa | 100 30 31 300 1150 | 88 10 2 38 40.6 85 1350 | 80 10 10 0.4 36 35 20 1749 | 78 10 2 10 0.4 50 42.4 75 1785 | 77 10 3 10 0.4 41 41.6 98 1789 | 75 10 5 10 0.4 38 40.5 95 1820 |
Claims (6)
1. the preparation method of a polypropylene/organic montmorillonite nano composite material, it is characterized in that the dynamical cure method is applied to polypropylene/organic montmorillonite/epoxy-resin systems, in twin screw extruder, add polypropylene, maleic anhydride inoculated polypropylene, organo montmorillonite, Resins, epoxy and solidifying agent, under 190～200 ℃ blending temperature, carry out mixing, wherein used polypropylene consumption is 70～85 weight parts, the consumption of maleic anhydride inoculated polypropylene is 10 weight parts, content of epoxy resin is 2～10 weight parts, hardener dose is 0.08～0.4 weight part, the organo montmorillonite consumption is 1～5 weight part, the blend time is 2～10min, blend under the screw speed of 100～200rpm obtains polypropylene/organic montmorillonite nano composite material through granulation.
2. according to the preparation method of the described a kind of polypropylene/organic montmorillonite nano composite material of claim 1, it is characterized in that polypropylene is a homopolymer, melting index 2～3g/10min.
3. according to the preparation method of the described a kind of polypropylene/organic montmorillonite nano composite material of claim 1, it is characterized in that the maleic anhydride inoculated polypropylene percentage of grafting is 0.8～1%.
4. according to the preparation method of the described a kind of polypropylene/organic montmorillonite nano composite material of claim 1, it is characterized in that Resins, epoxy is bisphenol-A diglycidyl ether type or Bisphenol F diglycidyl ether-type.
5. according to the preparation method of the described a kind of polypropylene/organic montmorillonite nano composite material of claim 1, it is characterized in that organo montmorillonite is two (2-hydroxyethyl) methyl tallow based quaternary ammonium salt montmorillonite modified or octadecyl tribromide ammonium montmorillonite modified.
6. according to the preparation method of the described a kind of polypropylene/organic montmorillonite nano composite material of claim 1, it is characterized in that solidifying agent is Dyhard RU 100, imidazoles or 2-ethyl-4-methylimidazole.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410066433 CN1272373C (en) | 2004-09-16 | 2004-09-16 | Preparation of polypropylene / organic montmorillonite nanometer composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410066433 CN1272373C (en) | 2004-09-16 | 2004-09-16 | Preparation of polypropylene / organic montmorillonite nanometer composite material |
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| Publication Number | Publication Date |
|---|---|
| CN1613905A CN1613905A (en) | 2005-05-11 |
| CN1272373C true CN1272373C (en) | 2006-08-30 |
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100347233C (en) * | 2005-11-02 | 2007-11-07 | 苏州大学 | Irradiant polymer/nanometer sulfide composite material and its preparation |
| CN101880421B (en) * | 2010-06-13 | 2013-02-13 | 中国石油化工股份有限公司 | Polypropylene/ organic montmorillonite nano composite material and preparation method thereof |
| CN102618007A (en) * | 2012-03-23 | 2012-08-01 | 中国科学院化学研究所 | Polycarbonate/organic clay composite material and preparation method thereof |
| CN105219006B (en) * | 2015-10-22 | 2017-07-11 | 同济大学 | The automotive line heat-resisting weather-proof polypropylene nano-composite insulating material of halogen-free flameproof and its preparation technology |
| CN105800579B (en) * | 2016-03-07 | 2019-01-18 | 南方科技大学 | Layered nano-particles, stripping method and application |
| JP6486409B2 (en) * | 2017-05-26 | 2019-03-20 | コンティニューム株式会社 | Operation method of air conditioner and reticulated resin molding |
| CN108794884A (en) * | 2018-05-25 | 2018-11-13 | 宁波星陆汽车部件有限公司 | Nano modification Anti-aging, high-strength degree wheel cover preparation process |
| CN113348336B (en) * | 2018-11-22 | 2022-11-15 | 肯梯钮穆株式会社 | Net-shaped resin molded article and method for operating air conditioner using same |
| CN111499980A (en) * | 2020-03-27 | 2020-08-07 | 杭州联通管业有限公司 | High-strength and high-toughness MPP (modified Polypropylene) power tube and preparation method thereof |
| CN111621114B (en) * | 2020-06-09 | 2022-09-20 | 浙江利帆家具有限公司 | Modified polypropylene furniture composite material and preparation method and application thereof |
| CN114409999B (en) * | 2021-12-31 | 2024-12-06 | 金发科技股份有限公司 | A polypropylene composition and preparation method thereof |
| CN114775169B (en) * | 2022-04-28 | 2023-12-01 | 杭州朝盛塑业有限公司 | Flame-retardant antibacterial non-woven fabric and preparation method thereof |
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