CN107955270A - A kind of novel polypropylene nanocomposite and preparation method thereof - Google Patents
A kind of novel polypropylene nanocomposite and preparation method thereof Download PDFInfo
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- CN107955270A CN107955270A CN201711132227.1A CN201711132227A CN107955270A CN 107955270 A CN107955270 A CN 107955270A CN 201711132227 A CN201711132227 A CN 201711132227A CN 107955270 A CN107955270 A CN 107955270A
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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
- C08L23/14—Copolymers of propene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/14—Copolymers of propene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/10—Homopolymers or copolymers of propene
- C08J2423/12—Polypropene
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- C—CHEMISTRY; METALLURGY
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
- C08L2205/03—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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Abstract
The present invention discloses a kind of novel polypropylene nanocomposite and preparation method thereof.The composite material is mainly prepared by following constituent mass parts：40 80 parts of polypropylene, 5 15 parts of toughener, 0.2 0.5 parts of antioxidant, 0.3 0.8 parts of lubricant, nanometer 20 65 parts of master batch of enhancing.PP composite material obtained by the present invention has preferable comprehensive performance and higher cost performance, wherein melt flow rate (MFR) ＞ 25g/10min (230 DEG C of 2.16kg), 23 DEG C of simply supported beam notch impact strength ＞ 25KJ/m2, bending modulus ＞ 1500MPa.The injection that the composite material is particularly suitable for the large-scale inner and outer decorative parts such as automobile (including new-energy automobile) instrument board, door skin, bumper is manufactured.
Description
Technical field
The present invention relates to a kind of novel polypropylene nanocomposite and preparation method thereof, belong to polymeric material field.
Background technology
Polypropylene has many excellent performances as a kind of general-purpose plastics, but because mechanical strength is low, poor heat resistance, contraction
The defects of deformation is big, creep resistance is poor.It is upper in application, especially as structural material, much limited, be not belonging to high-performance
Engineering plastics.Therefore, polypropylene is modified, being allowed to engineering just becomes an important research topic.
Polypropylene is strengthened now and is modified, its method is using addition regular grade talcum powder and calcium carbonate mostly.This filling changes
Although the extensive use on automobile component of the polypropylene material of property, in order to compensate for caused by addition talcum powder, calcium carbonate
Shock resistance significantly decline, it is necessary to add substantial amounts of toughener to improve shock resistance.So as to cost increase.
The content of the invention
The main object of the present invention, is to provide a kind of novel polypropylene nanocomposite.It is especially suitable for automobile component.
Technical scheme is as follows：Nanometer composite polypropylene material, in terms of mass parts, component includes 40-80 parts of polypropylene,
5-15 parts of toughener, 0.2-0.5 parts of antioxidant, 0.3-0.8 parts of lubricant, nanometer 20-65 parts of master batch of enhancing；
The polypropylene, preferably homopolypropylene are 1 with being copolymerized polyacrylic mixture, both mixed proportions:4-6, product are
Powdery is granular, and melt flow rate (MFR) is measured as 10-60g/10min at 230 DEG C under the conditions of 2.16KG.
The toughener is polyolefin elastomer ethylene-propylene-octene copolymer, styrene-butadiene copolymer, the benzene of hydrogenation
Mixture more than one or both of ethylene-butadiene-styrene block copolymer, mixed proportion are any；It is preferred that polyene
Olefin elastomer ethylene-propylene-octene copolymer (POE), trade mark DF610.
The mixture of the preferred phenolic antioxidant 1010 of the antioxidant and phosphoric acid ester irgasfos 168, its ratio is preferably 1:2.
The lubricant is more than one or both of calcium stearate, fatty acid ester blends, ethylene bis stearamide mixed
Compound.Preferred fat acid ester mixtures, preferred product trade mark TR044.
Wherein, the nanometer enhancing master batch prepares formula is included by mass parts：
In above-mentioned formula, homopolypropylene is powder, and melt flow rate (MFR) is measured at 230 DEG C, under the conditions of 2.16kg to be more than
30g/10 minutes；
Nanometer is washed one's hair to be washed one's hair by Anhui Province Xiusong County with powder and produced with mining industry Co., Ltd, is silico-calcium complex, contained chemical element is
Silicon (Si), calcium (Ca), magnesium (Mg), oxygen (O), oxygen element 64-65%, the summation of tri- kinds of elements of other Si, Ca, Mg are 35-
36%, particle diameter is less than 100 nanometers.Wash one's hair and contain a certain proportion of sheet-like particle in powder, and traditional talcum particles be with
The bar-like structural bodies of certain draw ratio, sheet-like particle quantity are seldom.Using washing one's hair with the effect of powder modified polypropene with traditional cunning
Mountain flour modified effect is suitable, but with the elongation at break higher washed one's hair with powder modified polypropene.Washed one's hair using nanoscale and changed with powder
Property, polyacrylic shock resistance not only can be preferably kept, and the additive amount of toughener is significantly declined, so as to drop
Low material cost.
The coupling agent is silane coupling agent, and the preferred product trade mark is KH560.
The preferred Tissuemat E of dispersant.
Toughener is ethylene methyl methacrylate copolymer (EMMA), the preferred product trade mark WH303, MMA content of monomer >=
18%.；
Polyolefin surfaces inorganic agent is polyolefin plastics regenerative agent, and profit is produced up to scientific and technological (Fujian) Co., Ltd, trade mark LD-301.
The preparation method of the nanometer composite polypropylene material, includes the following steps：
1) prepared by nanometer enhancing master batch：
(1) silane coupling agent is diluted with diluent (preferably technical grade absolute ethyl alcohol) spare, extension rate is equal
For 9-11 times, i.e., it is 1 with the ratio between absolute ethyl alcohol:9-11.
(2) load weighted nanometer is washed one's hair to pour into kneader with powder and stirred 5-10 minutes, then spray the silane coupling agent diluted,
Continue closing stirring 30-45 minutes.It is disposed spare.
(3) powdery homopolypropylene is weighed and poured into homogenizer, be subsequently added into the polyolefin surfaces inorganic agent, so
Stir 5-8 minutes afterwards, material is released spare.
(4) strengthen formula of master batch design requirement according to nanometer, weigh the nanometer that step (2) is handled well respectively and wash one's hair and powder, step (3)
Polypropylene, toughener, the dispersant handled well, are poured into homogenizer successively, are then stirred 3-5 minutes.
(5) the good material of above-mentioned high-speed stirred is sent into special twin screw extruder to be granulated, strengthens master batch up to nanometer.
2) prepared by nanometer composite polypropylene material：
(1) each component is weighed according to the formula rate, poured into successively in homogenizer, stirred 3-5 minutes.
(2) the above-mentioned material being stirred is sent into double screw extruder extruding pelletization, 120-225 DEG C of temperature control, cooling, mix
Close, detect, packaging, up to nanometer composite polypropylene material finished product.
Compared with prior art, the present invention its advantage is：
1) outstanding feature of technical solution of the present invention：First, being washed one's hair to nanometer and powder is surface-treated；Second, moulded using polyolefin
Material regenerative agent is surface-treated polypropylene, it is using chemical reaction and polymerization principle, mainly in plastic interface and body
Generation concerted reaction, chain extending reaction occurs at the same time for the functional group of grafted polar in polypropylene molecular chain, is improving molecular weight
While increase the interface polarity and cohesive energy of polypropylene plastics, wash one's hair compatibility with powder with nanometer so as to improve, have synchronous
Realize enhancing and the effect of toughness reinforcing.Make first nanometer enhancing master batch, so use it is more convenient, filling enhancing effect more
It is good.
2) ethylene methyl methacrylate copolymer (EMMA) is a kind of copolymer of newer type, safety and sanitation.The present invention uses
EMMA improves the processing heat stability and processing fluidity of nanometer enhancing master batch product, washes one's hair nanometer and more effectively disperses with powder
Among acrylic resin.
3) using iso standard detection, performance can reach nanometer composite polypropylene material made from formula of the present invention and technique
To the requirement of following standard：
Nanometer composite polypropylene material produced by the present invention has prominent impact strength, bending
Modulus and processing fluidity, are particularly suitable for automobile (including new-energy automobile) instrument board, car
The injection of the large-scale inside gadget such as door face board is manufactured, and sexual valence is higher.
Embodiment
Technical solution of the present invention is described in detail below, but protection scope of the present invention is not limited to the implementation
Example.
In following embodiment and comparative example,
Copolymer polypropylene produces for Beijing Yanshan Petrochemical, product grade K7726H
Toughener is SUMITOMO CHEMICAL chemical production, product grade WH303
Antioxidant is the refined precious production in the U.S., and product grade is 1010 and 168
Lubricant produces for american exxon, product grade TR044
Homopolypropylene produces for Ningxia Petrochemical company, product grade NX40S
Nanometer is washed one's hair to wash one's hair for Anhui Province Xiusong County with powder and produced with mining industry Co., Ltd, is silico-calcium complex
Coupling agent produces for Nanjing dawn, product grade KH560
The Tissuemat E that dispersant produces for U.S. Honeywell, product grade AC6
Toughener produces for Mitsui, product grade DF610
Polyolefin surfaces inorganic agent produces for profit up to scientific and technological (Fujian) Co., Ltd, trade mark LD-301.
Wherein, the nanometer enhancing master batch prepares formula is included by mass parts：
In the present embodiment, prepare formula is included by mass parts：
In the present embodiment, the nanometer enhancing agglomerate preparation method is as follows：
The silane coupling agent is diluted spare with absolute ethyl alcohol, and extension rate is 10 times, i.e., with the ratio between absolute ethyl alcohol
For 1:10.
(1) load weighted nanometer is washed one's hair to pour into kneader with powder and stirred 5 minutes, then spray the silane coupling agent diluted, after
Continuous closing stirring 30 minutes.It is disposed spare.
(2) the powdery homopolypropylene is weighed and poured into homogenizer, is subsequently added at the polyolefin surfaces
Agent is managed, is then stirred 5 minutes, material is released spare.
(3) strengthen formula of master batch design requirement according to nanometer, weigh the nanometer that step (1) is handled well respectively and wash one's hair and powder, step (2)
Polypropylene, toughener, the dispersant handled well, are poured into homogenizer successively, are then stirred 4 minutes.
(4) the good material of above-mentioned high-speed stirred is sent into special twin screw extruder to be granulated, strengthens master batch up to nanometer.
Embodiment 1：
Implement formula
Implementing process：
1) each component is weighed according to the formula rate, poured into successively in homogenizer, stirred 4 minutes.
2) the above-mentioned material being stirred is sent into double screw extruder extruding pelletization, cooling, mixing, detection, packaging, up to poly- third
Alkene nanocomposite produces product.Wherein, double screw extruder draw ratio is 40：1, twin-screw temperature setting for 120 DEG C, 170
DEG C, 170 DEG C, 180 DEG C, 180 DEG C, 200 DEG C, 200 DEG C, 210 DEG C, 210 DEG C, 225 DEG C of extruder rotating speeds are 200rpm, sink temperature
40 DEG C, pelleter rotating speed is 600rpm.
Embodiment 2：
| Formula materials | Percentage by weight (%) |
| Copolymer polypropylene | 51.2 |
| Toughener | 8 |
| Antioxidant | 0.3 |
| Lubricant | 0.5 |
| Nanometer enhancing master batch | 40 |
| It is total | 100 |
Implementing process：
1) each component is weighed according to the formula rate, poured into successively in homogenizer, stirred 4 minutes.
2) the above-mentioned material being stirred is sent into double screw extruder extruding pelletization, cooling, mixing, detection, packaging, up to poly- third
Alkene nanocomposite produces product.Wherein, double screw extruder draw ratio is 40：1, twin-screw temperature setting for 120 DEG C, 170
DEG C, 170 DEG C, 180 DEG C, 180 DEG C, 200 DEG C, 200 DEG C, 210 DEG C, 210 DEG C, 225 DEG C of extruder rotating speeds are 200rpm, sink temperature
40 DEG C, pelleter rotating speed is 600rpm.
Embodiment 2：
Implementing process：
1) each component is weighed according to the formula rate, poured into successively in homogenizer, stirred 4 minutes.
2) the above-mentioned material being stirred is sent into double screw extruder extruding pelletization, cooling, mixing, detection, packaging, up to poly- third
Alkene nanocomposite produces product.Wherein, double screw extruder draw ratio is 40：1, twin-screw temperature setting for 120 DEG C, 170
DEG C, 170 DEG C, 180 DEG C, 180 DEG C, 200 DEG C, 200 DEG C, 210 DEG C, 210 DEG C, 225 DEG C of extruder rotating speeds are 200rpm, sink temperature
40 DEG C, pelleter rotating speed is 600rpm.
Comparative example 1
The dosage of nanometer enhancing master batch is 0 part in this comparative example, other feed intake and processing step is the same as embodiment 1-3.
Embodiment 1-3 and 1 gained sample of comparative example are tested for the property, it is as a result as follows：
As can be seen from the above table, embodiment 1-3 is compared with comparative example 1, and tensile yield strength and bending modulus are with nanometer
Strengthen the increase of master batch additive amount and significantly increase, this explanation nanometer is washed one's hair has good humidification with powder.
As can be seen from the above table, embodiment 1-3 is compared with comparative example 1, and simply supported beam notch impact strength is increased slightly, this says
Bright nanometer is washed one's hair not only has good humidification, and also certain toughening effect with powder.
As can be seen from the above table, embodiment 1-3 is compared with comparative example 1, with nanometer enhancing master batch additive amount increase, melt
Flow rate is reducing successively, but melt flow rate (MFR) reduces amplitude very little, the processing of this explanation nanometer composite polypropylene material
Mobility is fine.
As described above, although the present invention has been represented and described with reference to specific preferred embodiment, but it must not be explained
For to the limitation of itself of the invention.Within the scope of the appended claims, can various changes can be made in the form and details to it.
Claims (5)
- A kind of 1. novel polypropylene nanocomposite, it is characterised in that：The composite material is mainly by following constituent mass part systems It is standby to form：5-15 parts of toughener of 40-80 parts of polypropylene0.3-0.8 parts of lubricant of 0.2-0.5 parts of antioxidantNanometer 20-65 parts of master batch of enhancing；The polypropylene is homopolypropylene with being copolymerized polyacrylic mixture, mixed proportion 1：4-6, product are powdery or grain Shape；Melt flow rate (MFR) is measured as 10-60g/10 minutes at 230 DEG C under the conditions of 2.16KG；The toughener is polyolefin elastic Body ethylene-propylene-octene copolymer, styrene-butadiene copolymer, the s-B-S block copolymerization of hydrogenation Mixture more than one or both of thing；The nanometer enhancing master batch is mainly prepared by following constituent mass parts：In above-mentioned formula, homopolypropylene is powder, and melt flow rate (MFR) is measured at 230 DEG C, under the conditions of 2.16kg to be more than 30g/10 minutes；It is silico-calcium complex that nanometer, which is washed one's hair with powder, and particle diameter is less than 100 nanometers；Coupling agent is silane coupling agent；Dispersant is Tissuemat E；Toughener is ethylene methyl methacrylate copolymer；Polyolefin surfaces inorganic agent regenerates for polyolefin plastics Agent, profit are produced up to scientific and technological (Fujian) Co., Ltd, trade mark LD-301；The nanometer enhancing agglomerate preparation method includes the following steps：(1) silane coupling agent is diluted with absolute ethyl alcohol it is spare, extension rate be 9-11 times, i.e., same to absolute ethyl alcohol The ratio between be 1:9-11；(2) load weighted nanometer is washed one's hair to pour into kneader with powder and stirred 5-10 minutes, then spray the silane coupling agent diluted, Continue closing stirring 30-45 minutes；It is disposed spare；(3) homopolypropylene is poured into homogenizer, is subsequently added into the polyolefin surfaces inorganic agent, then Stirring 5-8 minutes, material is spare；(4) formula of master batch is strengthened according to nanometer, the nanometer that weighing step (2) is handled well respectively is washed one's hair to be handled well with powder, step (3) Polypropylene, toughener, dispersant, are poured into homogenizer successively, are then stirred 3-5 minutes；(5) the good material of above-mentioned high-speed stirred is sent into special twin screw extruder to be granulated, strengthens master batch up to nanometer.
- 2. novel polypropylene nanocomposite according to claim 1, it is characterised in that：The antioxidant resists for phenols Oxygen agent 1010 and the mixture of phosphoric acid ester irgasfos 168, its ratio be 1:2.
- 3. novel polypropylene nanocomposite according to claim 1, it is characterised in that：Lubricant for calcium stearate, Mixture more than one or both of fatty acid ester blends, ethylene bis stearamide.
- 4. the application of novel polypropylene nanocomposite according to any one of claims 1 to 3, it is large-scale that it is used for automobile Inner and outer decorative parts.
- 5. the preparation method of novel polypropylene nanocomposite according to any one of claims 1 to 3, including following step Suddenly：1) prepared by nanometer enhancing master batch：(1) silane coupling agent described in claim 1 is diluted with absolute ethyl alcohol it is spare, extension rate be 9-11 times, i.e., It is 1 with the ratio between absolute ethyl alcohol:9-11；(2) load weighted nanometer is washed one's hair to pour into kneader with powder and stirred 5-10 minutes,The silane coupling agent diluted is sprayed again, continues closing stirring 30-45 minutes；It is disposed spare；(3) the powdery homopolypropylene described in claim 1 is poured into homogenizer, be subsequently added into described in claim 1 Polyolefin surfaces inorganic agent, then stir 5-8 minutes, material is spare；(4) formula of master batch is strengthened according to nanometer, the nanometer that weighing step (2) is handled well respectively is washed one's hair to be handled well with powder, step (3) Polypropylene, toughener, dispersant, are poured into homogenizer successively, are then stirred 3-5 minutes；(5) the good material of above-mentioned high-speed stirred is sent into special twin screw extruder to be granulated, strengthens master batch up to nanometer；2) prepared by nanometer composite polypropylene material：(1) formula rate described in accordance with the claim 1 weighs each component, pours into successively in homogenizer, 3-5 points of stirring Clock；(2) the above-mentioned material being stirred is sent into double screw extruder extruding pelletization, 120-225 DEG C of temperature control, cooling, mix Close, detect, packaging, up to nanometer composite polypropylene material finished product.
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| CN111471240A (en) * | 2019-01-23 | 2020-07-31 | 赵勤宽 | Polypropylene and graphene composite conductive functional material and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111471240A (en) * | 2019-01-23 | 2020-07-31 | 赵勤宽 | Polypropylene and graphene composite conductive functional material and preparation method thereof |
| CN110894319A (en) * | 2019-10-28 | 2020-03-20 | 中广核俊尔（上海）新材料有限公司 | Polypropylene material for battery cover plate and preparation method thereof |
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