CN101759931B - High-lustrousness material filled with modified polypropylene and preparation method thereof - Google Patents

High-lustrousness material filled with modified polypropylene and preparation method thereof Download PDF

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Publication number
CN101759931B
CN101759931B CN2008102075806A CN200810207580A CN101759931B CN 101759931 B CN101759931 B CN 101759931B CN 2008102075806 A CN2008102075806 A CN 2008102075806A CN 200810207580 A CN200810207580 A CN 200810207580A CN 101759931 B CN101759931 B CN 101759931B
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polypropylene
districts
antioxidant
irgasfos
barium sulfate
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CN101759931A (en
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张新亚
张鹰
张祥福
周文
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Shanghai Pret Composites Co Ltd
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Shanghai Pret Composites Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/36Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
    • B29C48/40Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/04Particle-shaped

Abstract

The invention discloses a high-lustrousness material filled with modified polypropylene, which comprises the following ingredients in percentage by weight: 70 to 90 of polypropylene, 4 to 15 of inorganic mineral fillers, 4 to 15 of calcium carbonate crystal whiskers, 0.1 to 1 of antioxidizers and 0 to 2 of other accessory agents. The invention has the advantages that 1, the invention adopts the high-lustrousness homopolymerized polypropylene as basic resin, and simultaneously adopts the calcium carbonate crystal whiskers which is helpful for the improvement of the surface laser to improve therigidity of the material, so the material can obtain high lustrousness and high rigidity at the same time; and 2, both the lustrousness and the rigidity of the material are improved to a certain degree through the compounding of the inorganic minerals and the calcium carbonate crystal whiskers, and the integral performance of the material is more balanced.

Description

A kind of high-lustrousness material filled with modified polypropylene and preparation method thereof
Technical field
The present invention relates to a kind of high-lustrousness material filled with modified polypropylene, and provide the preparation method of this polypropylene material, this material to have high gloss, high rigidity, high heat-resisting characteristics.
Background technology
Polypropylene is widely used in the industries such as automobile, household electrical appliances as a kind of general-purpose plastics.But the rigidity of plain polypropylene resin, thermotolerance are not high, usually are difficult to satisfy the various practical applications of every profession and trade.Utilizing the Inorganic Fillers Filled polypropylene to obtain the modified polypropylene material of low-cost and high-performance, is one of effective, the most most economical approach that obtains in the high performance polymer matrix material.People adopt mineral-filled method to improve rigidity, thermotolerance and the dimensional stability of polypropylene material usually.But when using mineral filled polypropylene, the surface gloss of polypropylene material also can significantly reduce along with the increase of mineral-filled amount.Therefore will be to sacrifice polypropylene material surface luster as cost with the inorganic materials filled modified polypropylene.And the application such as household appliances shell have higher requirements to the surface gloss of material.For this problem, people attempt adopting the whole bag of tricks to solve.Application number 00117199 discloses a kind of household electrical appliances with the ageing-resistant polypropylene material of high gloss, and the method promotes crystalling propylene by nucleator, yet along with the progress of polypropylene synthesis technique, high-crystallinity polypropylene is better than the use nucleator at crystal property; The Chinese patent of application number 200610027888.3 has also been announced the shock-resistant filled modified polypropylene of a kind of high gloss and method for making and application, it mainly is the toughness that improves material by polyolefin elastomer, but so also so that the glossiness of material and rigidity all have been subject to certain impact.
Whisker is the fiber that a kind of monocrystalline form growth forms, and diameter is minimum, has the atomic arrangement of high-sequential, does not have large lattice defect, has had high strength and modulus, can give matrix material high intensity.Easy and the resin compounded of whisker, visual appearance is good, is fit to very much make the product complex-shaped, that dimensional precision is high, surface smoothness is high.
Summary of the invention
The objective of the invention is for a kind of high-lustrousness material filled with modified polypropylene is provided, and the method for preparing this high-lustrousness material filled with modified polypropylene, when the glossiness of material was significantly improved, rigidity and the thermotolerance of material also improved.
Purpose of the present invention can be achieved through the following technical solutions.
A kind of high-lustrousness material filled with modified polypropylene, it comprises the raw material of following weight percent meter:
Polypropylene 70-90%
Inorganic mineral filler 4-15%
Calcium carbonate crystal whisker 4-15%
Oxidation inhibitor 0.1-1%
Other auxiliary agents 0-2%
Under the test condition of 230 ℃ * 2.16kg, described polypropylene be degree of crystallinity more than 70%, degree of isotacticity is greater than 99% homo-polypropylene, its melt flow rate (MFR) is 2~60g/10min.
Described inorganic mineral filler is one or more the mixture in barium sulfate, calcium carbonate and the titanium dioxide, and its particle diameter is 0.5 μ m~20 μ m.
The length-to-diameter ratio of described calcium carbonate crystal whisker is L/D>40, particle diameter<10 μ m.
Described oxidation inhibitor is primary antioxidant and auxiliary anti-oxidant, wherein primary antioxidant be selected from hindered phenol or sulphur ester antioxidant as 3114,1010 and DSTP in one or more; Auxiliary anti-oxidant is selected the phosphorite kind antioxidant.Such as in 618,168 one or both.
Described other auxiliary agent can be silane coupling agent, titanate coupling agent, lubricant, anti UV agent and pigment.
Preparation method of the present invention is as follows:
(1) weighs raw material by proportioning;
(2) polypropylene, inorganic mineral filler, oxidation inhibitor and other auxiliary agent are placed high mixer, high-speed stirring was mixed 5-10 minute;
(3) raw material that mixes is placed the dual-screw-stem machine extruding pelletization, way by the side direction feeding, calcium carbonate crystal whisker is joined in the forcing machine, the rotating speed of twin screw extruder is 180~600 rev/mins,, temperature is 190~200 ℃ in a district, 200~210 ℃ in two districts, 210~220 ℃ in three districts, 205~215 ℃ in four districts; The residence time of whole extrusion is 1~2 minute, and pressure is 12~18Mpa.
Advantage of the present invention is:
1, the present invention adopted glossiness preferably homo-polypropylene adopt simultaneously the rigidity that increases material to improving the helpful calcium carbonate crystal whisker of material surface gloss, so that material can obtain preferably glossiness and rigidity simultaneously as base resin.
2, composite by inorganic mineral and calcium carbonate crystal whisker of the present invention, to a certain degree lifting is arranged on the rigidity of material and the toughness glossiness, the over-all properties of material is balance more.
Specific embodiments
Below in conjunction with embodiment, the present invention is described in further detail:
In embodiment and Comparative Examples composite-material formula, polypropylene is the homo-polypropylene that oil of SPC is produced, and commodity are called S700.Described inorganic mineral is that particle diameter is the barium sulfate of 10 μ m.Described calcium salt whisker is that length-to-diameter ratio L/D is 50, particle diameter is the calcium carbonate crystal whisker of 8 μ m.Used primary antioxidant is the DSTP that Britain ICE company produces, and trade names are NegonoxDSTP, and chemical name is the thio-2 acid octadecyl ester, and Ciba company produce 3114, trade names are Irganox 3114, and chemical name is 3,5-di-tert-butyl-4-hydroxyl benzyl diethyl phosphoric acid.Auxiliary anti-oxidant is 168 of Ciba company product, and trade names are Irgafos 168, and chemical name is three (2,4-di-tert-butyl-phenyl) phosphorous acid ester.The color additives black toner is also used in this experiment in addition.
Take by weighing raw material by proportioning, polypropylene, inorganic mineral, oxidation inhibitor and other auxiliary agent were placed high-speed mixer and mixing 5-10 minute together, afterwards the raw material that mixes is placed the twin screw extruder granulation, and by the way of side direction feeding the calcium salt whisker is joined in the forcing machine, the rotating speed of twin screw extruder is 180~600 rev/mins, and temperature is 190~200 ℃ in a district, 200~210 ℃ in two districts, 210~220 ℃ in three districts, 205~215 ℃ in four districts; The residence time of whole extrusion is 1~2 minute, and pressure is 12~18Mpa.
Performance evaluation mode and implementation standard:
With the particulate material of finishing as stated above granulation in 90~100 ℃ convection oven dry 2~3 hours in advance, and then the particulate material that drying is good carried out the injection molding sample preparation at injection moulding machine.
Tensile property carries out according to ISO 527; The bending property test is undertaken by ISO 178; The simply supported beam notched Izod impact strength is undertaken by ISO179,23 ℃ of probe temperatures; Heat-drawn wire is undertaken by ISO 75, and specimen size is 120*10*3.0mm, and load is 0.45MPa; The glossiness test tries by 60 ° of angular measurements by standard GB8807 with vancometer.
The numerical value of melt flow rate (MFR), the tensile strength of the comprehensive mechanical property of material by the test gained, modulus in flexure, notched Izod impact strength shrinking percentage is passed judgment on.Embodiment 1-5 and Comparative Examples 1-3 prescription and properties test result see the following form 1 and table 2:
Table 1 embodiment 1-5 and Comparative Examples 1-3 prescription:
Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 Comparative Examples 1 Comparative Examples 2 Comparative Examples 3
S700 (% by weight) 89.15 84.15 79.15 74.15 74.15 89.15 79.15 74.15
Barium sulfate (% by weight) 5 5 10 15 10 10 20 25
Calcium carbonate crystal whisker (% by weight) 5 10 10 10 15 - - -
3114, % by weight 0.15 0.15 0.15 0.15 0.15 0.15 0.15 0.15
DSTP, % by weight 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3
168, % by weight 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2
Black toner, % by weight 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2
The test result of embodiment and Comparative Examples is as follows:
The test result of table 2 embodiment 1-5 and Comparative Examples 1-3
Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 Comparative Examples 1 Comparative Examples 2 Comparative Examples 3
Tensile strength (g/10min) 34.5 33.6 32.2 31.8 32 33 30.5 29
Modulus in flexure (MPa) 1980 2220 2850 3150 3320 1720 2600 2830
Notched Izod impact strength (kJ/m 2) 3.5 3.3 3.1 3.2 2.9 3.7 3.4 3.0
Heat-drawn wire (℃) 105 108 115 126.5 128 103 112 120
Glossiness 73 69 68 63 65 47 39 36
Can find out from the contrast of embodiment 1-5 and Comparative Examples 1-3, along with mineral-filled gradually increase, the glossiness of polypropylene composite material is reducing gradually, but in the situation of same loading level, the independent barium sulfate of the composite certain ratio of the filling of calcium carbonate crystal whisker and barium sulfate is filled the glossiness that can obviously improve the polypropylene composite materials system, and the heat-drawn wire (being the resistance toheat of material) of the tensile strength of material and modulus in flexure (being the rigidity of material) and material also can be improved simultaneously.In sum, the glossiness of material is significantly improved calcium carbonate crystal whisker and composite being filled into of barium sulfate, simultaneously the rigidity of material and thermotolerance are improved, can satisfy household electric appliances and other industry to the requirement of polypropylene material high gloss.

Claims (5)

1. high-lustrousness material filled with modified polypropylene is comprised of the raw material of following weight percent meter:
Polypropylene S700 89.15%, barium sulfate 5%, calcium carbonate crystal whisker 5%, antioxidant 3114 0.15%, oxidation inhibitor DSTP0.3%, irgasfos 168 0.2%, black toner 0.2%; Described polypropylene S700 is the homo-polypropylene that oil of SPC is produced; The barium sulfate particle diameter is 10 μ m; Calcium carbonate crystal whisker is that length-to-diameter ratio L/D is 50, particle diameter is 8 μ m; Described oxidation inhibitor is the DSTP that Britain ICE company produces, trade names are Negonox DSTP, chemical name is the thio-2 acid octadecyl ester, described antioxidant 3114 is 3114 of Ciba company product, trade names are Irganox3114, chemical name is 3,5-di-tert-butyl-4-hydroxyl benzyl diethyl phosphoric acid; Described irgasfos 168 is 168 of Ciba company product, and trade names are Irgafos168, and chemical name is three (2,4-di-tert-butyl-phenyl) phosphorous acid ester;
The preparation method is: take by weighing raw material by proportioning, with polypropylene S700, barium sulfate, antioxidant 3114 0.15%, oxidation inhibitor DSTP, irgasfos 168 and black toner placed high-speed mixer and mixing 5-10 minute together, afterwards the raw material that mixes is placed the twin screw extruder granulation, and by the way of side direction feeding the calcium salt whisker is joined in the forcing machine, the rotating speed of twin screw extruder is 180~600 rev/mins, and temperature is 190~200 ℃ in a district, 200~210 ℃ in two districts, 210~220 ℃ in three districts, 205~215 ℃ in four districts; The residence time of whole extrusion is 1~2 minute, and pressure is 12~18Mpa.
2. high-lustrousness material filled with modified polypropylene is comprised of the raw material of following weight percent meter:
Polypropylene S700 84.15%, barium sulfate 5%, calcium carbonate crystal whisker 10%, antioxidant 3114 0.15%, oxidation inhibitor DSTP0.3%, irgasfos 168 0.2%, black toner 0.2%; Described polypropylene S700 is the homo-polypropylene that oil of SPC is produced; The barium sulfate particle diameter is 10 μ m; Calcium carbonate crystal whisker is that length-to-diameter ratio L/D is 50, particle diameter is 8 μ m; Described oxidation inhibitor is the DSTP that Britain ICE company produces, trade names are Negonox DSTP, chemical name is the thio-2 acid octadecyl ester, described antioxidant 3114 is 3114 of Ciba company product, trade names are Irganox3114, chemical name is 3,5-di-tert-butyl-4-hydroxyl benzyl diethyl phosphoric acid; Described irgasfos 168 is 168 of Ciba company product, and trade names are Irgafos168, and chemical name is three (2,4-di-tert-butyl-phenyl) phosphorous acid ester;
The preparation method is: take by weighing raw material by proportioning, with polypropylene S700, barium sulfate, antioxidant 3114 0.15%, oxidation inhibitor DSTP, irgasfos 168 and black toner placed high-speed mixer and mixing 5-10 minute together, afterwards the raw material that mixes is placed the twin screw extruder granulation, and by the way of side direction feeding the calcium salt whisker is joined in the forcing machine, the rotating speed of twin screw extruder is 180~600 rev/mins, and temperature is 190~200 ℃ in a district, 200~210 ℃ in two districts, 210~220 ℃ in three districts, 205~215 ℃ in four districts; The residence time of whole extrusion is 1~2 minute, and pressure is 12~18Mpa.
3. high-lustrousness material filled with modified polypropylene is comprised of the raw material of following weight percent meter:
Polypropylene S700 79.15%, barium sulfate 10%, calcium carbonate crystal whisker 10%, antioxidant 3114 0.15%, oxidation inhibitor DSTP0.3%, irgasfos 168 0.2%, black toner 0.2%; Described polypropylene S700 is the homo-polypropylene that oil of SPC is produced; The barium sulfate particle diameter is 10 μ m; Calcium carbonate crystal whisker is that length-to-diameter ratio L/D is 50, particle diameter is 8 μ m; Described oxidation inhibitor is the DSTP that Britain ICE company produces, trade names are Negonox DSTP, chemical name is the thio-2 acid octadecyl ester, described antioxidant 3114 is 3114 of Ciba company product, trade names are Irganox3114, chemical name is 3,5-di-tert-butyl-4-hydroxyl benzyl diethyl phosphoric acid; Described irgasfos 168 is 168 of Ciba company product, and trade names are Irgafos168, and chemical name is three (2,4-di-tert-butyl-phenyl) phosphorous acid ester;
The preparation method is: take by weighing raw material by proportioning, with polypropylene S700, barium sulfate, antioxidant 3114 0.15%, oxidation inhibitor DSTP, irgasfos 168 and black toner placed high-speed mixer and mixing 5-10 minute together, afterwards the raw material that mixes is placed the twin screw extruder granulation, and by the way of side direction feeding the calcium salt whisker is joined in the forcing machine, the rotating speed of twin screw extruder is 180~600 rev/mins, and temperature is 190~200 ℃ in a district, 200~210 ℃ in two districts, 210~220 ℃ in three districts, 205~215 ℃ in four districts; The residence time of whole extrusion is 1~2 minute, and pressure is 12~18Mpa.
4. high-lustrousness material filled with modified polypropylene is comprised of the raw material of following weight percent meter:
Polypropylene S700 74.15%, barium sulfate 15%, calcium carbonate crystal whisker 10%, antioxidant 3114 0.15%, oxidation inhibitor DSTP0.3%, irgasfos 168 0.2%, black toner 0.2%; Described polypropylene S700 is the homo-polypropylene that oil of SPC is produced; The barium sulfate particle diameter is 10 μ m; Calcium carbonate crystal whisker is that length-to-diameter ratio L/D is 50, particle diameter is 8 μ m; Described oxidation inhibitor is the DSTP that Britain ICE company produces, trade names are Negonox DSTP, chemical name is the thio-2 acid octadecyl ester, described antioxidant 3114 is 3114 of Ciba company product, trade names are Irganox3114, chemical name is 3,5-di-tert-butyl-4-hydroxyl benzyl diethyl phosphoric acid; Described irgasfos 168 is 168 of Ciba company product, and trade names are Irgafos168, and chemical name is three (2,4-di-tert-butyl-phenyl) phosphorous acid ester;
The preparation method is: take by weighing raw material by proportioning, with polypropylene S700, barium sulfate, antioxidant 3114 0.15%, oxidation inhibitor DSTP, irgasfos 168 and black toner placed high-speed mixer and mixing 5-10 minute together, afterwards the raw material that mixes is placed the twin screw extruder granulation, and by the way of side direction feeding the calcium salt whisker is joined in the forcing machine, the rotating speed of twin screw extruder is 180~600 rev/mins, and temperature is 190~200 ℃ in a district, 200~210 ℃ in two districts, 210~220 ℃ in three districts, 205~215 ℃ in four districts; The residence time of whole extrusion is 1~2 minute, and pressure is 12~18Mpa.
5. high-lustrousness material filled with modified polypropylene is comprised of the raw material of following weight percent meter:
Polypropylene S700 74.15%, barium sulfate 10%, calcium carbonate crystal whisker 15%, antioxidant 3114 0.15%, oxidation inhibitor DSTP0.3%, irgasfos 168 0.2%, black toner 0.2%; Described polypropylene S700 is the homo-polypropylene that oil of SPC is produced; The barium sulfate particle diameter is 10 μ m; Calcium carbonate crystal whisker is that length-to-diameter ratio L/D is 50, particle diameter is 8 μ m; Described oxidation inhibitor is the DSTP that Britain ICE company produces, trade names are Negonox DSTP, chemical name is the thio-2 acid octadecyl ester, described antioxidant 3114 is 3114 of Ciba company product, trade names are Irganox3114, chemical name is 3,5-di-tert-butyl-4-hydroxyl benzyl diethyl phosphoric acid; Described irgasfos 168 is 168 of Ciba company product, and trade names are Irgafos168, and chemical name is three (2,4-di-tert-butyl-phenyl) phosphorous acid ester;
The preparation method is: take by weighing raw material by proportioning, with polypropylene S700, barium sulfate, antioxidant 3114 0.15%, oxidation inhibitor DSTP, irgasfos 168 and black toner placed high-speed mixer and mixing 5-10 minute together, afterwards the raw material that mixes is placed the twin screw extruder granulation, and by the way of side direction feeding the calcium salt whisker is joined in the forcing machine, the rotating speed of twin screw extruder is 180~600 rev/mins, and temperature is 190~200 ℃ in a district, 200~210 ℃ in two districts, 210~220 ℃ in three districts, 205~215 ℃ in four districts; The residence time of whole extrusion is 1~2 minute, and pressure is 12~18Mpa.
CN2008102075806A 2008-12-23 2008-12-23 High-lustrousness material filled with modified polypropylene and preparation method thereof Active CN101759931B (en)

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Publication number Priority date Publication date Assignee Title
CN102485785A (en) * 2010-12-02 2012-06-06 合肥杰事杰新材料股份有限公司 Heat-resisting scratch-resisting highlight polypropylene material and preparation method thereof
CN103571059B (en) * 2012-08-02 2017-12-22 辽宁辽杰科技有限公司 A kind of PP composite material and its production and use
CN103360680B (en) * 2013-05-23 2015-09-16 建德市新裕塑胶材料有限公司 Polypropylene and polyethylene Calcium carbonate filler master batch and preparation technology thereof
CN104231515A (en) * 2014-09-11 2014-12-24 常州大学 Anti-friction polypropylene material and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1532221A (en) * 2003-03-21 2004-09-29 上海日之升新技术发展有限公司 Mineral/ whisker reinforced polypropylene composition
CN101250303A (en) * 2008-03-20 2008-08-27 江南模塑科技股份有限公司 Mineral/whisker reinforced polypropylene composite material having good spraying property

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1532221A (en) * 2003-03-21 2004-09-29 上海日之升新技术发展有限公司 Mineral/ whisker reinforced polypropylene composition
CN101250303A (en) * 2008-03-20 2008-08-27 江南模塑科技股份有限公司 Mineral/whisker reinforced polypropylene composite material having good spraying property

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