CN106832582A - A kind of preparation method of high-ductility polypropylene based composites - Google Patents
A kind of preparation method of high-ductility polypropylene based composites Download PDFInfo
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
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- C08K2201/004—Additives being defined by their length
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2201/011—Nanostructured additives
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- 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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- 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
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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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
- C08L2205/24—Crystallisation aids
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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
- C08L2205/24—Crystallisation aids
- C08L2205/242—Beta spherulite nucleating agents
Abstract
The invention discloses a kind of preparation method of high-ductility polypropylene based composites, have main steps that polypropylene and nucleator by 90 99:1 10 mass ratio, is obtained polypropylene/nucleator composite, as masterbatch 1 after drying by double screw extruder；Ethylene propylene diene rubber and CNT are pressed 80 95:5 20 mass ratio, is obtained ethylene propylene diene rubber/carbon nano tube compound material, as masterbatch 2 after drying by double screw extruder；Masterbatch 1, masterbatch 2 and polypropylene, ethylene propylene diene rubber are pressed 0.2 10:1‑20:70‑90:0 19 mass ratio, composite is obtained by double screw extruder.In the behavior of polypropylene composites for obtaining, the content of ethylene propylene diene rubber is 10 20%, and content of carbon nanotubes is 0.1 3%, and the content of polypropylene nucleater is 0.01 0.5%.Polypropylene Nanocomposites impact strength obtained in the method is high and tensile strength is preferable, and its process is simple, is conducive to large-scale production.
Description
Technical field
The invention belongs to field of high polymer material processing, more particular to a kind of preparation of high-ductility polypropylene composite material
Method.
Background technology
Polypropylene is one of five big general-purpose plastics, because its raw material sources is abundant, simple production process, it is easy to be processed into
Type, product excellent combination property, does not absorb water and resistant to chemical etching, density is small, heat-resist, electrical insulating property is excellent, cheap,
Its product is nontoxic, tasteless, can be widely applied to the fields such as household supplies, packaging for foodstuff and medicine equipment.Although having numerous excellent
Different performance, but polypropylene there is also some shortcomings part, wherein most prominent shortcoming is exactly very sensitive to breach, breach punching
Hit intensity is low, especially the fragility under low temperature or high strain rate substantially, this greatly limits application.Therefore, polypropylene
Toughening modifying be always research a focus.
Current polypropylene toughening mainly uses two methods of chemical modification and physical modification.The former passes through copolymerization, connects
The method such as branch or crosslinking can reach modified purpose, but generally process is complicated, relatively costly.The latter is included with polypropylene as base
Body, adds plasticizer, elastomer, toughness high polymer, inorganic filler, nucleator etc., and because method is simple and easy to apply, cost is relatively low,
So using relatively broad.
For plasticizer, elastomer and toughness high polymer, toughening effect is played to polypropylene, the amount being usually added into
It is big, typically in more than 20wt%, while after adding these material modified in large quantities, polyacrylic intensity can be substantially reduced.And
For the inorganic fillers such as such as montmorillonite, carbon black, CNT, although their addition can improve the machine of composite
Tool performance, hot property and electric property etc., but filler dispersity, and between matrix compatibility influence it is larger,
Simultaneously to the raising limitation of toughness.
Isotactic polypropylene is a kind of crystalline polymer, and crystal structure and pattern have large effect to its performance.It is poly-
Propylene crystal has various crystal formations, and of greatest concern is α and beta crystal, and the former is higher so more universal due to stability, but due to
Crystal structure is dense and causes polypropylene impact flexibility relatively low；The latter is needed using addition β types nucleator, shearing force, temperature
Any special measures such as degree gradient can just be obtained, but the loose structure of β crystal can improve polyacrylic toughness, so using nucleator
Carrying out toughening modifying can typically use β type nucleators.
It is limited using the toughening effect for adding single filler or Nucleating Agent on Pp, and be individually added into plasticizer,
Although elastomer or toughness high polymer have preferable toughening effect, but the strength of materials can be caused to decline to a great extent simultaneously, so mesh
Preceding most of method for toughening can using multicomponent material with it is polypropene blended, adding, a small amount of plasticizer, elastomer or toughness are high
After polymers, filler or nucleator are added, to reach preferable coordination plasticizing effect, while will not also lose excessive strong
Degree.Having result of study to show to be added in polypropylene/elastomer blend a small amount of β types nucleator and nano silicon can be with
Improve intensity, modulus and the toughness of co-mixing system simultaneously, reach the purpose of activeness and quietness simultaneously, refer to, Wu Lili, β nucleation
Agent and the composite modified PP/POE composites research of nanosized SiO_2, plastic additive, the 3rd phase：34-39,2010.
Despite the use of the method that multiple material is blended carries out toughening modifying to polypropylene, but major part is both needed to use
More elastomer or toughness high polymer, causes matrix material intensity in itself to decline, while using β the nucleator for adding more
Type nucleator, induction polypropylene matrix generates more loose beta crystal, can be only achieved toughness reinforcing purpose.And in low content bullet
Under gonosome or toughness high polymer, the research on the influence of α type Nucleating Agent on Pp toughening effect is less.
The content of the invention
The purpose of the present invention is to put forward a kind of preparation method of high-ductility polypropylene based composites, and the method adds low consumption
Rubber, obtained Polypropylene Nanocomposites impact strength is high and tensile strength is preferable, and its process is simple, is conducive to big
Large-scale production.
A kind of preparation method of high-ductility polypropylene based composites of the invention, key step is as follows：
1) polypropylene and nucleator are pressed into 90-99:The mass ratio of 1-10, by double screw extruder be obtained polypropylene/into
Core agent composite, as masterbatch 1 after drying；Extrusion temperature is 180-230 DEG C, and rotating speed is 100-250rpm；
2) ethylene propylene diene rubber and CNT are pressed into 80-95:The mass ratio of 5-20, three are obtained by double screw extruder
First EP rubbers/carbon nano tube compound material, as masterbatch 2 after drying；Extrusion temperature is 180-230 DEG C, and rotating speed is 100-
250rpm；
3) masterbatch 1, masterbatch 2 and polypropylene, ethylene propylene diene rubber are pressed into 0.2-10:1-20:70-90:The mass ratio of 0-19,
Composite is obtained by double screw extruder；Temperature during extrusion is 180-230 DEG C, and rotating speed is 100-250rpm.
In a kind of preparation method of high-ductility polypropylene based composites of the invention, described polypropylene is isotactic poly- third
Alkene.
In a kind of preparation method of high-ductility polypropylene based composites of the invention, described CNT is a diameter of 5-
200nm, length is the SWCN or multi-walled carbon nano-tubes of 100nm-50m.
In a kind of preparation method of high-ductility polypropylene based composites of the invention, described nucleator is polypropylene α types
Nucleator：Adipic acid, Sodium Benzoate, talcum powder, meat sodium metasilicate, p-tert-butyl benzoic acid hydroxy Al, dibenzal sorbitol, (1,
3:2,4)-two (to the benzal of methyl two) sorbierites, two (benzal of 3,4- dimethyl two) sorbierite, phosphoric acid 2 or 2- methenes-(4,6-
And tert-butyl-phenyl) sodium.
In a kind of preparation method of high-ductility polypropylene based composites of the invention, described nucleator is β type nucleators,
Such as：Aryl amide compound, aromatic amine compound, dicyclohexyl are to this diformamide, pimelic acid aluminium or calcium pimelate.
Compared with prior art, the beneficial effects of the invention are as follows：
Very well, polypropylene toughening generally needed to be added larger amount of rubber just obvious toughening effect to the toughness of rubber,
But rubber intensity in itself and modulus are relatively low, and the intensity of whole behavior of polypropylene composites and modulus urgency can be caused when addition is more
Play declines.The present invention uses a small amount of rubber, with CNT, nucleator coordination plasticizing polypropylene, is reaching preferable toughness reinforcing
While effect, the intensity and modulus of composite can also be avoided from being greatly reduced；
CNT is distributed on the interface of rubber phase region the inside or rubber and polypropylene matrix, substantially through whole
Individual rubber phase region, increases by two alternate interaction forces, and when composite is acted on by external force, CNT can promote should
Power enables stress field to be superimposed in the transmission of material internal, improves the mechanical property of material；
The addition of nucleator can refine polyacrylic crystalline size, and less crystal grain is conducive to improving polyacrylic impact
Toughness, can together with rubber, CNT coordination plasticizing polypropylene.
It is demonstrated experimentally that the obtained behavior of polypropylene composites of the present invention, when ethylene propylene diene rubber content is 15%, carbon nanometer
When pipe content is 1%, nucleation agent content is 0.2%, the notch impact strength of composite is 51.2kJ/m2, is virgin pp
More than 13 times, be Pp/epdm (85/15) blend more than 3 times, be a kind of high-ductility polypropylene base composite wood
Material.
Specific embodiment
The present invention is described in further details with reference to specific embodiment.
Embodiment 1
1) isotactic polypropylene and nucleator are pressed 95:5 mass ratio, polypropylene/nucleation is obtained by double screw extruder
Agent composite, as masterbatch 1 after drying；Extrusion temperature is 200 DEG C, and rotating speed is 150rpm；
2) ethylene propylene diene rubber and CNT are pressed 90:10 mass ratio, ternary second is obtained by double screw extruder
Third rubber/carbon nano tube compound material, as masterbatch 2 after drying；Extrusion temperature is 190 DEG C, and rotating speed is 150rpm；
Masterbatch 1, masterbatch 2 and polypropylene, ethylene propylene diene rubber are pressed 4:10:81:6 mass ratio, by twin-screw extrusion
Mechanism obtains composite；Temperature during extrusion is 200 DEG C, and rotating speed is 150rpm.The CNT for wherein using is a diameter of
50nm, length is 10-20 μm of acidifying multi-walled carbon nano-tubes, and nucleator is (3, the 4- dimethyl dibenzyls of polypropylene α types nucleator two
Fork) sorbierite (commercially available DMDBS).
Comparative example 1：
Isotactic polypropylene, ethylene propylene diene rubber are pressed 85:15 mass ratio, composite wood is obtained by double screw extruder
Material, extrusion temperature is 200 DEG C, and rotating speed is 150rpm.The polypropylene for wherein using is isotactic polypropylene.
Comparative example 2：
Polypropylene and nucleator are pressed 95:5 mass ratio, is obtained polypropylene/nucleator and is combined by double screw extruder
Material, as masterbatch after drying；Extrusion temperature is 200 DEG C, and rotating speed is 150rpm；
Masterbatch and polypropylene, ethylene propylene diene rubber are pressed 4:81:10 mass ratio, is obtained compound by double screw extruder
Material；Temperature during extrusion is 200 DEG C, and rotating speed is 150rpm.The nucleator for wherein using is polypropylene α type nucleators DMDBS.
Comparative example 3：
Ethylene propylene diene rubber and CNT are pressed 90:10 mass ratio, EPDM is obtained by double screw extruder
Rubber/carbon nano tube compound material, as masterbatch after drying；Extrusion temperature is 190 DEG C, and rotating speed is 150rpm；
Masterbatch and isotactic polypropylene, ethylene propylene diene rubber are pressed 10:85:6 mass ratio, is obtained by double screw extruder
Composite；Temperature during extrusion is 200 DEG C, and rotating speed is 150rpm.The CNT for wherein using is a diameter of 50nm, length
It is 10-20 μm of acidifying multi-walled carbon nano-tubes.
The notch impact strength of made sample is as shown in table 1 above.
As it can be seen from table 1 CNT and polypropylene α types nucleator can coordination plasticizing behavior of polypropylene composites,
Notch impact strength can reach 51.2MPa, belong to high-ductility polypropylene based composites.
The tensile strength of made sample is as shown in table 1 above.As can be seen from the table, the tensile strength of comparative example one is
26.4MPa, the tensile strength than virgin pp is somewhat reduced, but reduction amplitude is simultaneously little, and the tensile strength of embodiment 1 is
27.3MPa, on the basis of tensile strength is kept, more also increases, and illustrates that CNT and nucleator are poly- in coordination plasticizing
While propylene based composites, polyacrylic intensity can be preferably kept.By polypropylene-base nanometer obtained in this method
Composite impact intensity is high and tensile strength is preferable.
Embodiment 2：
Polypropylene and nucleator are pressed 99:1 mass ratio, is obtained polypropylene/nucleator and is combined by double screw extruder
Material, as masterbatch 1 after drying；Extrusion temperature is 180 DEG C, and rotating speed is 100rpm；
Ethylene propylene diene rubber and CNT are pressed 95:5 mass ratio, ethylene-propylene-diene monomer is obtained by double screw extruder
Glue/carbon nano tube compound material, as masterbatch 2 after drying；Extrusion temperature is 180 DEG C, and rotating speed is 100rpm；
Masterbatch 1, masterbatch 2 and polypropylene, ethylene propylene diene rubber are pressed 10:1:70:19 mass ratio, by twin-screw extrusion
Mechanism obtains composite；Temperature during extrusion is 180 DEG C, and rotating speed is 100rpm.
Wherein polypropylene is isotactic polypropylene, and CNT is a diameter of 5nm, and length is the SWCN of 10nm,
Nucleator is polypropylene beta type nucleator (TMB-5) aromatic amine compound.
Embodiment 3：
Polypropylene and nucleator are pressed 90:10 mass ratio, is obtained polypropylene/nucleator and is combined by double screw extruder
Material, as masterbatch 1 after drying；Extrusion temperature is 230 DEG C, and rotating speed is 250rpm；
Ethylene propylene diene rubber and CNT are pressed 80:20 mass ratio, EPDM is obtained by double screw extruder
Rubber/carbon nano tube compound material, as masterbatch 2 after drying；Extrusion temperature is 230 DEG C, and rotating speed is 250rpm；
Masterbatch 1, masterbatch 2 and polypropylene are pressed 0.2:20:80 mass ratio, composite wood is obtained by double screw extruder
Material；Temperature during extrusion is 230 DEG C, and rotating speed is 250rpm.
Wherein polypropylene is isotactic polypropylene, and CNT is a diameter of 200nm, and length is 50 μm of multi-wall carbon nano-tube
Pipe, nucleator is polypropylene α type nucleator Sodium Benzoates.
Embodiment 4：
Polypropylene and nucleator are pressed 93:7 mass ratio, is obtained polypropylene/nucleator and is combined by double screw extruder
Material, as masterbatch 1 after drying；Extrusion temperature is 210 DEG C, and rotating speed is 200rpm；
Ethylene propylene diene rubber and CNT are pressed 85:15 mass ratio, EPDM is obtained by double screw extruder
Rubber/carbon nano tube compound material, as masterbatch 2 after drying；Extrusion temperature is 200 DEG C, and rotating speed is 220rpm；
Masterbatch 1, masterbatch 2 and polypropylene, ethylene propylene diene rubber are pressed 0.2:1:90:9 mass ratio, by twin-screw extrusion
Mechanism obtains composite；Temperature during extrusion is 210 DEG C, and rotating speed is 220rpm.
Wherein polypropylene is isotactic polypropylene, and CNT is a diameter of 50nm, and length is 1 μm of SWCN,
Nucleator is polypropylene beta type nucleator CHB-5 aryl amide compounds.
Embodiment 5：
Polypropylene and nucleator are pressed 97:3 mass ratio, is obtained polypropylene/nucleator and is combined by double screw extruder
Material, as masterbatch 1 after drying；Extrusion temperature is 220 DEG C, and rotating speed is 160rpm；
Ethylene propylene diene rubber and CNT are pressed 85:15 mass ratio, EPDM is obtained by double screw extruder
Rubber/carbon nano tube compound material, as masterbatch 2 after drying；Extrusion temperature is 210 DEG C, and rotating speed is 180rpm；
Masterbatch 1, masterbatch 2 and polypropylene, ethylene propylene diene rubber are pressed 3:20:74:3 mass ratio, by twin-screw extrusion
Mechanism obtains composite；Temperature during extrusion is 220 DEG C, and rotating speed is 190rpm.
Wherein polypropylene is isotactic polypropylene, and CNT is a diameter of 100nm, and length is 20 μm of multi-wall carbon nano-tube
Pipe, nucleator is organic phosphate (NA-11).
Embodiment 6：
Polypropylene and nucleator are pressed 95:5 mass ratio, is obtained polypropylene/nucleator and is combined by double screw extruder
Material, as masterbatch 1 after drying；Extrusion temperature is 200 DEG C, and rotating speed is 120rpm；
Ethylene propylene diene rubber and CNT are pressed 90:10 mass ratio, EPDM is obtained by double screw extruder
Rubber/carbon nano tube compound material, as masterbatch 2 after drying；Extrusion temperature is 180 DEG C, and rotating speed is 140rpm；
Masterbatch 1, masterbatch 2 and polypropylene, ethylene propylene diene rubber are pressed 7:10:72:11 mass ratio, by twin-screw extrusion
Mechanism obtains composite；Temperature during extrusion is 230 DEG C, and rotating speed is 250rpm.
Wherein polypropylene is isotactic polypropylene, and CNT is a diameter of 150nm, and length is 40 μm of single
Pipe, nucleator is polypropylene beta type nucleator calcium pimelate.
Table 1
Table 2
Claims (5)
1. a kind of preparation method of high-ductility polypropylene based composites, key step is as follows：
1) polypropylene and nucleator are pressed into 90-99:The mass ratio of 1-10, polypropylene/nucleator is obtained by double screw extruder
Composite, as masterbatch 1 after drying；Extrusion temperature is 180-230 DEG C, and rotating speed is 100-250rpm；
2) ethylene propylene diene rubber and CNT are pressed into 80-95:The mass ratio of 5-20, ternary second is obtained by double screw extruder
Third rubber/carbon nano tube compound material, as masterbatch 2 after drying；Extrusion temperature is 180-230 DEG C, and rotating speed is 100-250rpm；
3) masterbatch 1, masterbatch 2 and polypropylene, ethylene propylene diene rubber are pressed into 0.2-10:1-20:70-90:The mass ratio of 0-19, passes through
Double screw extruder is obtained composite；Temperature during extrusion is 180-230 DEG C, and rotating speed is 100-250rpm.
2. according to a kind of preparation method of the high-ductility polypropylene based composites described in claim 1, it is characterised in that described
Polypropylene is isotactic polypropylene.
3. according to a kind of preparation method of the high-ductility polypropylene based composites described in claim 1, it is characterised in that：Described
CNT is a diameter of 5-200nm, and length is 100nm-50 μm of SWCN or multi-walled carbon nano-tubes.
4. according to a kind of preparation method of high-ductility polypropylene based composites described in claim 1, it is characterised in that it is described into
Core agent is polypropylene α type nucleators：Adipic acid, Sodium Benzoate, talcum powder, meat sodium metasilicate, p-tert-butyl benzoic acid hydroxy Al, two
Benzylidene sorbitol, (1,3:2,4)-two (to the benzal of methyl two) sorbierites, two (benzal of 3,4- dimethyl two) sorbierites, phosphoric acid 2
Or 2- methenes-(4,6- and tert-butyl-phenyl) sodium.
5. according to a kind of preparation method of high-ductility polypropylene based composites described in claim 1, it is characterised in that it is described into
Core agent is β type nucleators, such as：Aryl amide compound, aromatic amine compound, dicyclohexyl are to this diformamide, pimelic acid aluminium
Or calcium pimelate.
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| CN110343332A (en) * | 2019-07-11 | 2019-10-18 | 西北工业大学 | A kind of high-toughness polypropylene/elastic composite and preparation method |
| CN111763372A (en) * | 2020-06-10 | 2020-10-13 | 杭州联通管业有限公司 | Reinforced modified polypropylene power tube and preparation method thereof |
| CN115851150A (en) * | 2021-09-26 | 2023-03-28 | 大正新型材料(肇庆)有限公司 | High-toughness polypropylene decorative film and preparation method and application thereof |
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